# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2266 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H21 O6 P W' _chemical_formula_sum 'C27 H21 O6 P W' _chemical_formula_weight 656.26 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.1595(2) _cell_length_b 10.5241(3) _cell_length_c 19.7949(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.6003(14) _cell_angle_gamma 90.00 _cell_volume 2510.86(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6943 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 4.704 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5388 _exptl_absorpt_correction_T_max 0.7342 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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' _diffrn_measurement_method 'ccd, thin slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42848 _diffrn_reflns_av_R_equivalents 0.1325 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.99 _reflns_number_total 6035 _reflns_number_gt 4237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0352P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6035 _refine_ls_number_parameters 319 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 C1 C 0.2032(3) 0.4229(5) 0.9316(2) 0.0212(9) Uani 1 1 d . . . C2 C 0.2585(4) 0.4547(4) 1.0049(2) 0.0243(10) Uani 1 1 d . . . C3 C 0.2096(4) 0.5473(5) 1.0417(2) 0.0314(12) Uani 1 1 d . . . H3A H 0.1460 0.5917 1.0209 0.038 Uiso 1 1 calc R . . C4 C 0.2536(4) 0.5752(5) 1.1091(2) 0.0321(11) Uani 1 1 d . . . H4A H 0.2191 0.6373 1.1341 0.038 Uiso 1 1 calc R . . C5 C 0.3469(4) 0.5124(5) 1.1392(2) 0.0325(12) Uani 1 1 d . . . H5A H 0.3777 0.5327 1.1845 0.039 Uiso 1 1 calc R . . C6 C 0.3956(4) 0.4200(5) 1.1035(2) 0.0321(11) Uani 1 1 d . . . H6A H 0.4591 0.3755 1.1244 0.039 Uiso 1 1 calc R . . C7 C 0.3509(4) 0.3922(4) 1.0363(2) 0.0269(11) Uani 1 1 d . . . H7A H 0.3849 0.3288 1.0119 0.032 Uiso 1 1 calc R . . C8 C 0.1581(4) 0.5460(4) 0.8958(2) 0.0241(10) Uani 1 1 d . . . C9 C 0.0506(4) 0.5582(5) 0.8623(2) 0.0277(11) Uani 1 1 d . . . H9A H 0.0008 0.4885 0.8617 0.033 Uiso 1 1 calc R . . C10 C 0.0149(4) 0.6709(5) 0.8295(3) 0.0346(13) Uani 1 1 d . . . H10A H -0.0586 0.6774 0.8066 0.042 Uiso 1 1 calc R . . C11 C 0.0867(4) 0.7736(5) 0.8303(3) 0.0352(12) Uani 1 1 d . . . H11A H 0.0628 0.8502 0.8074 0.042 Uiso 1 1 calc R . . C12 C 0.1936(4) 0.7640(5) 0.8646(3) 0.0329(12) Uani 1 1 d . . . H12A H 0.2429 0.8342 0.8658 0.040 Uiso 1 1 calc R . . C13 C 0.2280(4) 0.6522(4) 0.8971(2) 0.0268(11) Uani 1 1 d . . . H13A H 0.3010 0.6470 0.9209 0.032 Uiso 1 1 calc R . . C14 C 0.1147(4) 0.3193(5) 0.9325(2) 0.0243(10) Uani 1 1 d . . . C15 C 0.0760(4) 0.2817(5) 0.9922(2) 0.0288(11) Uani 1 1 d . . . H15A H 0.1040 0.3217 1.0340 0.035 Uiso 1 1 calc R . . C16 C -0.0034(4) 0.1860(5) 0.9919(3) 0.0326(12) Uani 1 1 d . . . H16A H -0.0285 0.1611 1.0334 0.039 Uiso 1 1 calc R . . C17 C -0.0457(4) 0.1275(5) 0.9319(3) 0.0321(12) Uani 1 1 d . . . H17A H -0.0996 0.0622 0.9319 0.039 Uiso 1 1 calc R . . C18 C -0.0092(4) 0.1642(5) 0.8721(3) 0.0309(12) Uani 1 1 d . . . H18A H -0.0385 0.1242 0.8306 0.037 Uiso 1 1 calc R . . C19 C 0.0693(4) 0.2586(4) 0.8717(2) 0.0264(11) Uani 1 1 d . . . H19A H 0.0932 0.2831 0.8298 0.032 Uiso 1 1 calc R . . C20 C 0.2786(5) 0.4993(5) 0.7621(3) 0.0395(13) Uani 1 1 d . . . H20A H 0.3524 0.5359 0.7784 0.047 Uiso 1 1 calc R . . H20B H 0.2215 0.5634 0.7687 0.047 Uiso 1 1 calc R . . C21 C 0.2721(4) 0.4674(5) 0.6892(3) 0.0361(13) Uani 1 1 d . . . H21A H 0.2812 0.5350 0.6586 0.043 Uiso 1 1 calc R . . C22 C 0.2547(5) 0.3533(6) 0.6628(3) 0.0439(14) Uani 1 1 d . . . H22B H 0.2451 0.2830 0.6915 0.053 Uiso 1 1 calc R . . H22A H 0.2517 0.3412 0.6150 0.053 Uiso 1 1 calc R . . C23 C 0.4555(4) -0.0358(5) 0.8819(2) 0.0311(12) Uani 1 1 d . . . C24 C 0.5266(4) 0.1918(5) 0.9497(2) 0.0295(11) Uani 1 1 d . . . C25 C 0.3055(4) 0.0796(5) 0.9594(2) 0.0275(10) Uani 1 1 d . . . C26 C 0.2625(4) 0.0826(5) 0.8123(2) 0.0273(10) Uani 1 1 d U . . C27 C 0.4752(4) 0.1959(5) 0.8059(2) 0.0290(11) Uani 1 1 d . . . O1 O 0.2614(3) 0.3866(3) 0.80038(16) 0.0282(8) Uani 1 1 d . . . O2 O 0.4905(3) -0.1367(4) 0.8830(2) 0.0430(9) Uani 1 1 d . . . O3 O 0.6053(3) 0.2169(4) 0.98476(19) 0.0452(10) Uani 1 1 d . . . O4 O 0.2599(3) 0.0402(3) 1.00189(19) 0.0408(9) Uani 1 1 d . . . O5 O 0.1940(3) 0.0460(3) 0.77220(17) 0.0379(9) Uani 1 1 d . . . O6 O 0.5237(3) 0.2254(4) 0.76256(18) 0.0416(9) Uani 1 1 d . . . P P 0.31266(10) 0.35990(12) 0.87897(6) 0.0226(3) Uani 1 1 d . . . H23 H 0.390(3) 0.456(4) 0.890(2) 0.027 Uiso 1 1 d . . . W W 0.390690(14) 0.139924(18) 0.882959(9) 0.02294(8) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(2) 0.021(2) 0.020(2) -0.001(2) 0.0015(18) -0.0010(19) C2 0.023(2) 0.024(3) 0.026(2) 0.001(2) 0.0029(19) -0.0047(19) C3 0.032(3) 0.033(3) 0.029(3) 0.001(2) 0.002(2) 0.004(2) C4 0.038(3) 0.029(3) 0.029(3) -0.005(2) 0.003(2) 0.001(2) C5 0.041(3) 0.029(3) 0.025(3) -0.004(2) -0.001(2) -0.006(2) C6 0.035(3) 0.029(3) 0.030(3) 0.002(2) -0.005(2) 0.000(2) C7 0.027(3) 0.025(3) 0.028(3) -0.003(2) 0.001(2) 0.0015(19) C8 0.026(2) 0.022(3) 0.025(2) 0.001(2) 0.0006(19) 0.0009(19) C9 0.025(2) 0.024(3) 0.033(3) -0.003(2) 0.001(2) -0.004(2) C10 0.031(3) 0.030(3) 0.040(3) -0.003(2) -0.006(2) 0.002(2) C11 0.047(3) 0.022(3) 0.034(3) 0.002(2) -0.003(2) 0.005(2) C12 0.033(3) 0.027(3) 0.037(3) 0.002(2) 0.001(2) -0.005(2) C13 0.022(2) 0.024(3) 0.032(3) -0.003(2) -0.004(2) 0.000(2) C14 0.021(2) 0.023(3) 0.028(3) 0.001(2) 0.0009(19) 0.0018(19) C15 0.027(3) 0.030(3) 0.030(3) -0.002(2) 0.002(2) 0.001(2) C16 0.032(3) 0.030(3) 0.038(3) 0.007(2) 0.013(2) 0.000(2) C17 0.023(3) 0.028(3) 0.046(3) 0.002(2) 0.006(2) -0.004(2) C18 0.028(3) 0.027(3) 0.036(3) -0.005(2) 0.001(2) -0.007(2) C19 0.026(2) 0.025(3) 0.029(3) 0.001(2) 0.006(2) 0.001(2) C20 0.056(4) 0.031(3) 0.033(3) 0.006(3) 0.010(3) -0.005(3) C21 0.038(3) 0.042(4) 0.029(3) 0.009(3) 0.007(2) 0.002(2) C22 0.054(4) 0.049(4) 0.030(3) 0.006(3) 0.007(3) -0.006(3) C23 0.028(3) 0.035(3) 0.031(3) 0.001(2) 0.006(2) 0.000(2) C24 0.028(3) 0.031(3) 0.029(3) 0.001(2) 0.002(2) 0.002(2) C25 0.029(3) 0.022(3) 0.030(3) -0.003(2) -0.001(2) 0.005(2) C26 0.028(2) 0.025(3) 0.028(2) 0.006(2) 0.0017(16) 0.000(2) C27 0.032(3) 0.027(3) 0.026(3) -0.002(2) 0.000(2) 0.004(2) O1 0.0330(19) 0.027(2) 0.0246(17) 0.0038(14) 0.0036(14) -0.0025(14) O2 0.043(2) 0.031(2) 0.056(3) 0.0028(19) 0.0148(19) 0.0090(18) O3 0.039(2) 0.051(3) 0.042(2) -0.0013(19) -0.0082(18) -0.0073(19) O4 0.048(2) 0.038(2) 0.040(2) 0.0072(18) 0.0203(18) 0.0025(17) O5 0.037(2) 0.036(2) 0.037(2) 0.0008(17) -0.0094(16) -0.0003(16) O6 0.044(2) 0.048(3) 0.036(2) 0.0029(18) 0.0174(18) -0.0031(18) P 0.0224(6) 0.0230(6) 0.0225(6) 0.0019(5) 0.0031(5) -0.0012(5) W 0.02233(11) 0.02302(12) 0.02334(11) 0.00046(9) 0.00251(7) 0.00072(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 C1 C14 1.534(6) . ? C1 C8 1.542(6) . ? C1 C2 1.552(6) . ? C1 P 1.915(4) . ? C2 C7 1.378(6) . ? C2 C3 1.396(6) . ? C3 C4 1.401(7) . ? C3 H3A 0.9500 . ? C4 C5 1.378(7) . ? C4 H4A 0.9500 . ? C5 C6 1.380(7) . ? C5 H5A 0.9500 . ? C6 C7 1.399(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.391(6) . ? C8 C13 1.403(6) . ? C9 C10 1.394(7) . ? C9 H9A 0.9500 . ? C10 C11 1.389(7) . ? C10 H10A 0.9500 . ? C11 C12 1.389(7) . ? C11 H11A 0.9500 . ? C12 C13 1.378(7) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.386(6) . ? C14 C19 1.409(6) . ? C15 C16 1.394(7) . ? C15 H15A 0.9500 . ? C16 C17 1.375(7) . ? C16 H16A 0.9500 . ? C17 C18 1.374(7) . ? C17 H17A 0.9500 . ? C18 C19 1.378(6) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 O1 1.438(6) . ? C20 C21 1.474(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.314(7) . ? C21 H21A 0.9500 . ? C22 H22B 0.9500 . ? C22 H22A 0.9500 . ? C23 O2 1.143(6) . ? C23 W 2.011(6) . ? C24 O3 1.137(6) . ? C24 W 2.048(5) . ? C25 O4 1.144(5) . ? C25 W 2.045(5) . ? C26 O5 1.139(6) . ? C26 W 2.043(5) . ? C27 O6 1.147(5) . ? C27 W 2.035(5) . ? O1 P 1.622(3) . ? P W 2.4993(13) . ? P H23 1.38(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 C14 C1 C8 113.3(4) . . ? C14 C1 C2 111.1(4) . . ? C8 C1 C2 109.4(4) . . ? C14 C1 P 107.4(3) . . ? C8 C1 P 105.7(3) . . ? C2 C1 P 109.7(3) . . ? C7 C2 C3 118.4(4) . . ? C7 C2 C1 123.1(4) . . ? C3 C2 C1 118.5(4) . . ? C2 C3 C4 120.6(5) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C2 C7 C6 121.4(5) . . ? C2 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C9 C8 C13 117.7(4) . . ? C9 C8 C1 123.4(4) . . ? C13 C8 C1 118.9(4) . . ? C8 C9 C10 121.0(4) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 119.6(5) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C8 121.7(4) . . ? C12 C13 H13A 119.2 . . ? C8 C13 H13A 119.2 . . ? C15 C14 C19 117.4(4) . . ? C15 C14 C1 122.0(4) . . ? C19 C14 C1 120.6(4) . . ? C14 C15 C16 121.0(5) . . ? C14 C15 H15A 119.5 . . ? C16 C15 H15A 119.5 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 119.4(5) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 120.7(5) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C18 C19 C14 121.0(4) . . ? C18 C19 H19A 119.5 . . ? C14 C19 H19A 119.5 . . ? O1 C20 C21 109.6(4) . . ? O1 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? O1 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C22 C21 C20 125.6(5) . . ? C22 C21 H21A 117.2 . . ? C20 C21 H21A 117.2 . . ? C21 C22 H22B 120.0 . . ? C21 C22 H22A 120.0 . . ? H22B C22 H22A 120.0 . . ? O2 C23 W 177.8(4) . . ? O3 C24 W 176.4(4) . . ? O4 C25 W 176.7(4) . . ? O5 C26 W 176.8(4) . . ? O6 C27 W 178.8(4) . . ? C20 O1 P 125.8(3) . . ? O1 P C1 104.83(18) . . ? O1 P W 106.66(13) . . ? C1 P W 126.30(15) . . ? O1 P H23 101.2(17) . . ? C1 P H23 99.6(17) . . ? W P H23 115.2(18) . . ? C23 W C27 91.20(19) . . ? C23 W C26 89.2(2) . . ? C27 W C26 89.30(19) . . ? C23 W C25 87.71(19) . . ? C27 W C25 178.70(19) . . ? C26 W C25 89.99(18) . . ? C23 W C24 88.2(2) . . ? C27 W C24 87.80(19) . . ? C26 W C24 176.03(18) . . ? C25 W C24 92.87(18) . . ? C23 W P 177.38(14) . . ? C27 W P 86.31(14) . . ? C26 W P 89.99(14) . . ? C25 W P 94.78(14) . . ? C24 W P 92.51(15) . . ? 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 C14 C1 C2 C7 89.3(5) . . . . ? C8 C1 C2 C7 -144.9(4) . . . . ? P C1 C2 C7 -29.4(5) . . . . ? C14 C1 C2 C3 -88.0(5) . . . . ? C8 C1 C2 C3 37.9(5) . . . . ? P C1 C2 C3 153.4(4) . . . . ? C7 C2 C3 C4 -0.2(7) . . . . ? C1 C2 C3 C4 177.1(4) . . . . ? C2 C3 C4 C5 1.0(8) . . . . ? C3 C4 C5 C6 -1.5(8) . . . . ? C4 C5 C6 C7 1.2(8) . . . . ? C3 C2 C7 C6 -0.1(7) . . . . ? C1 C2 C7 C6 -177.3(4) . . . . ? C5 C6 C7 C2 -0.4(7) . . . . ? C14 C1 C8 C9 -5.5(6) . . . . ? C2 C1 C8 C9 -130.1(4) . . . . ? P C1 C8 C9 111.9(4) . . . . ? C14 C1 C8 C13 174.2(4) . . . . ? C2 C1 C8 C13 49.6(5) . . . . ? P C1 C8 C13 -68.5(5) . . . . ? C13 C8 C9 C10 1.7(7) . . . . ? C1 C8 C9 C10 -178.6(4) . . . . ? C8 C9 C10 C11 -0.4(7) . . . . ? C9 C10 C11 C12 -0.8(8) . . . . ? C10 C11 C12 C13 0.6(8) . . . . ? C11 C12 C13 C8 0.8(7) . . . . ? C9 C8 C13 C12 -1.9(7) . . . . ? C1 C8 C13 C12 178.4(4) . . . . ? C8 C1 C14 C15 -111.2(5) . . . . ? C2 C1 C14 C15 12.4(6) . . . . ? P C1 C14 C15 132.4(4) . . . . ? C8 C1 C14 C19 68.6(5) . . . . ? C2 C1 C14 C19 -167.7(4) . . . . ? P C1 C14 C19 -47.8(5) . . . . ? C19 C14 C15 C16 1.0(7) . . . . ? C1 C14 C15 C16 -179.1(4) . . . . ? C14 C15 C16 C17 -0.5(8) . . . . ? C15 C16 C17 C18 -0.2(8) . . . . ? C16 C17 C18 C19 0.2(7) . . . . ? C17 C18 C19 C14 0.4(7) . . . . ? C15 C14 C19 C18 -1.0(7) . . . . ? C1 C14 C19 C18 179.2(4) . . . . ? O1 C20 C21 C22 -0.9(8) . . . . ? C21 C20 O1 P 150.9(4) . . . . ? C20 O1 P C1 90.9(4) . . . . ? C20 O1 P W -133.2(4) . . . . ? C14 C1 P O1 82.3(3) . . . . ? C8 C1 P O1 -38.9(3) . . . . ? C2 C1 P O1 -156.8(3) . . . . ? C14 C1 P W -41.9(3) . . . . ? C8 C1 P W -163.2(2) . . . . ? C2 C1 P W 79.0(3) . . . . ? O2 C23 W C27 178(100) . . . . ? O2 C23 W C26 -93(13) . . . . ? O2 C23 W C25 -3(13) . . . . ? O2 C23 W C24 90(13) . . . . ? O2 C23 W P -165(10) . . . . ? O6 C27 W C23 -3(22) . . . . ? O6 C27 W C26 -92(22) . . . . ? O6 C27 W C25 -35(26) . . . . ? O6 C27 W C24 85(22) . . . . ? O6 C27 W P 178(100) . . . . ? O5 C26 W C23 -18(8) . . . . ? O5 C26 W C27 73(8) . . . . ? O5 C26 W C25 -106(8) . . . . ? O5 C26 W C24 30(9) . . . . ? O5 C26 W P 159(8) . . . . ? O4 C25 W C23 -2(7) . . . . ? O4 C25 W C27 30(13) . . . . ? O4 C25 W C26 87(7) . . . . ? O4 C25 W C24 -91(7) . . . . ? O4 C25 W P 177(100) . . . . ? O3 C24 W C23 40(7) . . . . ? O3 C24 W C27 -51(7) . . . . ? O3 C24 W C26 -9(9) . . . . ? O3 C24 W C25 127(7) . . . . ? O3 C24 W P -138(7) . . . . ? O1 P W C23 35(3) . . . . ? C1 P W C23 158(3) . . . . ? O1 P W C27 52.49(19) . . . . ? C1 P W C27 175.9(2) . . . . ? O1 P W C26 -36.81(18) . . . . ? C1 P W C26 86.6(2) . . . . ? O1 P W C25 -126.79(18) . . . . ? C1 P W C25 -3.3(2) . . . . ? O1 P W C24 140.12(18) . . . . ? C1 P W C24 -96.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.728 _refine_diff_density_min -2.054 _refine_diff_density_rms 0.202 _database_code_depnum_ccdc_archive 'CCDC 953770' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_s:\2224\xshape\2224 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 O6 P W' _chemical_formula_sum 'C25 H19 O6 P W' _chemical_formula_weight 630.22 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.6274(5) _cell_length_b 11.7450(5) _cell_length_c 17.5953(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.748(4) _cell_angle_gamma 90.00 _cell_volume 2343.65(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5235 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 29.33 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 5.036 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.5833 _exptl_absorpt_correction_T_max 0.8636 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 223 frames, detector distance = 100 mm ; _diffrn_reflns_number 12379 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5614 _reflns_number_gt 3532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5614 _refine_ls_number_parameters 302 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0341 _refine_ls_wR_factor_gt 0.0311 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 C1 C 0.1452(4) 0.0244(3) 0.9451(3) 0.0324(10) Uani 1 1 d . . . H1A H 0.2203 -0.0168 0.9548 0.039 Uiso 1 1 calc R . . H1B H 0.0879 -0.0144 0.9041 0.039 Uiso 1 1 calc R . . H1C H 0.1153 0.0263 0.9930 0.039 Uiso 1 1 calc R . . C2 C 0.1172(3) 0.3014(3) 0.8065(2) 0.0127(7) Uani 1 1 d . . . C3 C 0.0055(3) 0.3168(3) 0.8391(2) 0.0134(8) Uani 1 1 d . . . C4 C -0.0716(2) 0.2280(3) 0.8435(2) 0.0156(8) Uani 1 1 d . . . H4A H -0.0545 0.1541 0.8270 0.019 Uiso 1 1 calc R . . C5 C -0.1733(3) 0.2447(3) 0.8715(2) 0.0239(9) Uani 1 1 d . . . H5A H -0.2244 0.1823 0.8742 0.029 Uiso 1 1 calc R . . C6 C -0.2002(3) 0.3510(4) 0.8955(2) 0.0275(10) Uani 1 1 d . . . H6A H -0.2697 0.3625 0.9146 0.033 Uiso 1 1 calc R . . C7 C -0.1247(3) 0.4409(4) 0.8914(3) 0.0286(11) Uani 1 1 d . . . H7A H -0.1425 0.5148 0.9076 0.034 Uiso 1 1 calc R . . C8 C -0.0235(3) 0.4235(3) 0.8637(2) 0.0203(9) Uani 1 1 d . . . H8A H 0.0276 0.4860 0.8615 0.024 Uiso 1 1 calc R . . C9 C 0.2058(2) 0.3968(3) 0.83842(18) 0.0140(7) Uani 1 1 d . . . C10 C 0.2646(2) 0.3943(4) 0.91628(18) 0.0155(7) Uani 1 1 d . . . H10A H 0.2531 0.3317 0.9480 0.019 Uiso 1 1 calc R . . C11 C 0.3400(3) 0.4819(3) 0.9484(2) 0.0213(9) Uani 1 1 d . . . H11A H 0.3803 0.4786 1.0015 0.026 Uiso 1 1 calc R . . C12 C 0.3563(3) 0.5740(3) 0.9029(2) 0.0207(9) Uani 1 1 d . . . H12A H 0.4083 0.6338 0.9247 0.025 Uiso 1 1 calc R . . C13 C 0.2965(3) 0.5787(3) 0.8255(2) 0.0210(9) Uani 1 1 d . . . H13A H 0.3065 0.6424 0.7943 0.025 Uiso 1 1 calc R . . C14 C 0.2218(3) 0.4902(3) 0.7936(2) 0.0166(8) Uani 1 1 d . . . H14A H 0.1813 0.4937 0.7405 0.020 Uiso 1 1 calc R . . C15 C 0.0882(3) 0.2900(3) 0.7174(2) 0.0133(8) Uani 1 1 d . . . C16 C 0.1776(3) 0.2949(3) 0.6759(2) 0.0141(8) Uani 1 1 d . . . H16A H 0.2557 0.3123 0.7029 0.017 Uiso 1 1 calc R . . C17 C 0.1558(3) 0.2751(3) 0.5972(2) 0.0190(9) Uani 1 1 d . . . H17A H 0.2183 0.2800 0.5706 0.023 Uiso 1 1 calc R . . C18 C 0.0433(3) 0.2481(3) 0.5563(2) 0.0221(9) Uani 1 1 d . . . H18A H 0.0281 0.2341 0.5018 0.027 Uiso 1 1 calc R . . C19 C -0.0468(3) 0.2419(3) 0.5961(2) 0.0212(9) Uani 1 1 d . . . H19A H -0.1243 0.2229 0.5687 0.025 Uiso 1 1 calc R . . C20 C -0.0252(3) 0.2629(3) 0.6751(2) 0.0180(8) Uani 1 1 d . . . H20A H -0.0883 0.2589 0.7012 0.022 Uiso 1 1 calc R . . C21 C 0.5610(3) 0.0441(3) 0.8483(2) 0.0189(8) Uani 1 1 d U . . C22 C 0.3778(3) 0.0979(4) 0.7153(2) 0.0200(8) Uani 1 1 d . . . C23 C 0.4603(3) 0.2719(3) 0.8233(2) 0.0204(9) Uani 1 1 d . . . C24 C 0.4314(3) 0.1340(3) 0.9513(3) 0.0191(9) Uani 1 1 d U . . C25 C 0.3447(3) -0.0543(3) 0.8368(3) 0.0241(10) Uani 1 1 d . . . O1 O 0.16260(18) 0.13848(19) 0.92097(15) 0.0204(6) Uani 1 1 d . . . O2 O 0.6526(2) 0.0017(2) 0.85990(17) 0.0306(7) Uani 1 1 d U . . O3 O 0.3740(2) 0.0951(3) 0.64992(16) 0.0309(7) Uani 1 1 d . . . O4 O 0.4968(2) 0.3590(2) 0.81446(18) 0.0338(8) Uani 1 1 d . . . O5 O 0.4523(2) 0.1498(2) 1.01758(17) 0.0371(8) Uani 1 1 d . . . O6 O 0.3157(2) -0.1468(2) 0.8370(2) 0.0403(9) Uani 1 1 d . . . P P 0.19105(7) 0.15905(8) 0.83604(6) 0.0142(2) Uani 1 1 d U . . H26 H 0.106(2) 0.095(3) 0.7968(18) 0.017 Uiso 1 1 d . . . W W 0.399356(12) 0.109924(13) 0.834293(10) 0.01485(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(3) 0.022(2) 0.031(3) 0.003(2) 0.022(2) -0.0033(19) C2 0.0118(14) 0.0094(16) 0.016(2) 0.0016(15) 0.0023(14) 0.0002(12) C3 0.0123(15) 0.0189(18) 0.0073(18) 0.0004(15) -0.0016(13) -0.0033(13) C4 0.0173(18) 0.0160(17) 0.012(2) -0.0023(16) 0.0006(15) -0.0035(13) C5 0.0151(16) 0.031(2) 0.025(2) -0.0001(19) 0.0026(16) -0.0071(15) C6 0.0148(17) 0.043(3) 0.027(2) 0.000(2) 0.0080(16) 0.0047(16) C7 0.0196(19) 0.032(2) 0.035(3) -0.006(2) 0.0077(18) 0.0054(17) C8 0.0157(16) 0.017(2) 0.027(2) -0.0034(16) 0.0022(16) 0.0002(13) C9 0.0109(12) 0.0120(15) 0.0182(17) -0.0034(19) 0.0013(12) 0.0017(16) C10 0.0179(13) 0.0113(15) 0.0177(17) 0.001(2) 0.0053(12) 0.0026(17) C11 0.0181(17) 0.023(2) 0.022(2) -0.0051(18) 0.0006(16) 0.0016(15) C12 0.0191(16) 0.0154(19) 0.027(2) -0.0089(16) 0.0028(16) -0.0062(13) C13 0.0241(17) 0.013(2) 0.027(2) -0.0008(15) 0.0092(16) -0.0004(13) C14 0.0165(16) 0.0121(17) 0.020(2) -0.0026(15) 0.0019(15) -0.0005(13) C15 0.0173(16) 0.0094(17) 0.0131(19) 0.0038(15) 0.0030(14) 0.0017(13) C16 0.0163(16) 0.0082(17) 0.017(2) 0.0026(15) 0.0027(15) 0.0039(13) C17 0.0240(19) 0.019(2) 0.016(2) 0.0039(17) 0.0084(17) 0.0027(16) C18 0.0254(18) 0.023(2) 0.015(2) 0.0003(17) -0.0016(16) -0.0015(15) C19 0.0214(17) 0.024(2) 0.015(2) 0.0001(17) -0.0039(16) -0.0019(15) C20 0.0155(16) 0.0196(19) 0.020(2) -0.0015(17) 0.0062(15) -0.0009(14) C21 0.0199(14) 0.0148(18) 0.024(2) 0.0018(16) 0.0088(16) 0.0003(12) C22 0.0156(15) 0.017(2) 0.028(2) -0.001(2) 0.0049(15) 0.0017(16) C23 0.0183(17) 0.0167(19) 0.025(2) 0.0003(18) 0.0028(16) 0.0028(15) C24 0.0190(17) 0.013(2) 0.0243(16) 0.0037(16) 0.0032(16) 0.0032(14) C25 0.0202(18) 0.018(2) 0.034(3) -0.004(2) 0.0045(17) 0.0032(15) O1 0.0267(12) 0.0158(15) 0.0205(14) 0.0000(11) 0.0090(10) -0.0015(10) O2 0.0186(11) 0.0303(16) 0.0434(19) 0.0042(14) 0.0081(12) 0.0076(11) O3 0.0309(13) 0.0361(19) 0.0260(16) -0.0058(16) 0.0071(12) 0.0043(14) O4 0.0274(13) 0.0199(17) 0.055(2) 0.0068(14) 0.0101(13) -0.0033(11) O5 0.0403(15) 0.048(2) 0.0212(17) -0.0003(15) 0.0025(13) -0.0011(13) O6 0.0380(16) 0.0135(15) 0.070(2) 0.0000(15) 0.0124(16) -0.0048(12) P 0.0154(4) 0.0124(4) 0.0148(5) 0.0013(4) 0.0035(4) -0.0010(3) W 0.01394(5) 0.01092(5) 0.01967(7) 0.00055(10) 0.00366(4) 0.00070(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.434(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C15 1.535(5) . ? C2 C3 1.541(5) . ? C2 C9 1.542(4) . ? C2 P 1.899(3) . ? C3 C4 1.389(4) . ? C3 C8 1.392(5) . ? C4 C5 1.392(5) . ? C4 H4A 0.9500 . ? C5 C6 1.376(5) . ? C5 H5A 0.9500 . ? C6 C7 1.386(5) . ? C6 H6A 0.9500 . ? C7 C8 1.385(5) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C14 1.388(5) . ? C9 C10 1.390(4) . ? C10 C11 1.388(5) . ? C10 H10A 0.9500 . ? C11 C12 1.382(5) . ? C11 H11A 0.9500 . ? C12 C13 1.387(5) . ? C12 H12A 0.9500 . ? C13 C14 1.391(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.398(5) . ? C15 C20 1.400(4) . ? C16 C17 1.370(5) . ? C16 H16A 0.9500 . ? C17 C18 1.384(5) . ? C17 H17A 0.9500 . ? C18 C19 1.384(6) . ? C18 H18A 0.9500 . ? C19 C20 1.379(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 O2 1.152(4) . ? C21 W 1.997(3) . ? C22 O3 1.142(4) . ? C22 W 2.058(4) . ? C23 O4 1.131(4) . ? C23 W 2.055(4) . ? C24 O5 1.153(5) . ? C24 W 2.030(4) . ? C25 O6 1.138(4) . ? C25 W 2.035(4) . ? O1 P 1.618(3) . ? P W 2.4966(9) . ? P H26 1.31(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C15 C2 C3 112.1(2) . . ? C15 C2 C9 114.4(3) . . ? C3 C2 C9 109.3(3) . . ? C15 C2 P 100.8(2) . . ? C3 C2 P 111.7(2) . . ? C9 C2 P 108.3(2) . . ? C4 C3 C8 117.1(3) . . ? C4 C3 C2 122.7(3) . . ? C8 C3 C2 120.2(3) . . ? C3 C4 C5 121.5(3) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 119.1(4) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C8 C7 C6 120.2(4) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C7 C8 C3 121.7(3) . . ? C7 C8 H8A 119.2 . . ? C3 C8 H8A 119.2 . . ? C14 C9 C10 118.6(3) . . ? C14 C9 C2 122.0(3) . . ? C10 C9 C2 119.2(3) . . ? C11 C10 C9 121.0(4) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C9 C14 C13 120.7(3) . . ? C9 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C16 C15 C20 116.9(3) . . ? C16 C15 C2 120.6(3) . . ? C20 C15 C2 122.2(3) . . ? C17 C16 C15 121.9(3) . . ? C17 C16 H16A 119.1 . . ? C15 C16 H16A 119.1 . . ? C16 C17 C18 120.5(4) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C19 118.9(4) . . ? C17 C18 H18A 120.6 . . ? C19 C18 H18A 120.6 . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C15 121.2(4) . . ? C19 C20 H20A 119.4 . . ? C15 C20 H20A 119.4 . . ? O2 C21 W 175.7(3) . . ? O3 C22 W 174.8(3) . . ? O4 C23 W 176.5(4) . . ? O5 C24 W 178.0(3) . . ? O6 C25 W 178.4(5) . . ? C1 O1 P 119.0(2) . . ? O1 P C2 102.20(15) . . ? O1 P W 111.92(8) . . ? C2 P W 125.58(11) . . ? O1 P H26 96.8(14) . . ? C2 P H26 96.9(14) . . ? W P H26 118.7(14) . . ? C21 W C24 88.39(15) . . ? C21 W C25 85.41(14) . . ? C24 W C25 95.63(17) . . ? C21 W C23 92.02(14) . . ? C24 W C23 88.68(15) . . ? C25 W C23 174.91(19) . . ? C21 W C22 89.94(15) . . ? C24 W C22 174.60(16) . . ? C25 W C22 89.35(18) . . ? C23 W C22 86.25(16) . . ? C21 W P 167.77(11) . . ? C24 W P 85.22(10) . . ? C25 W P 84.86(11) . . ? C23 W P 98.23(10) . . ? C22 W P 97.33(9) . . ? 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 C15 C2 C3 C4 74.4(4) . . . . ? C9 C2 C3 C4 -157.7(3) . . . . ? P C2 C3 C4 -37.9(4) . . . . ? C15 C2 C3 C8 -104.0(4) . . . . ? C9 C2 C3 C8 23.9(4) . . . . ? P C2 C3 C8 143.8(3) . . . . ? C8 C3 C4 C5 -0.2(5) . . . . ? C2 C3 C4 C5 -178.6(3) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? C4 C5 C6 C7 -0.1(6) . . . . ? C5 C6 C7 C8 -0.2(6) . . . . ? C6 C7 C8 C3 0.3(6) . . . . ? C4 C3 C8 C7 -0.1(5) . . . . ? C2 C3 C8 C7 178.3(3) . . . . ? C15 C2 C9 C14 24.2(4) . . . . ? C3 C2 C9 C14 -102.4(4) . . . . ? P C2 C9 C14 135.7(3) . . . . ? C15 C2 C9 C10 -161.3(3) . . . . ? C3 C2 C9 C10 72.1(4) . . . . ? P C2 C9 C10 -49.8(4) . . . . ? C14 C9 C10 C11 -1.5(5) . . . . ? C2 C9 C10 C11 -176.2(3) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C10 C11 C12 C13 0.5(5) . . . . ? C11 C12 C13 C14 -1.0(5) . . . . ? C10 C9 C14 C13 1.0(5) . . . . ? C2 C9 C14 C13 175.6(3) . . . . ? C12 C13 C14 C9 0.2(5) . . . . ? C3 C2 C15 C16 169.1(3) . . . . ? C9 C2 C15 C16 43.9(4) . . . . ? P C2 C15 C16 -72.0(3) . . . . ? C3 C2 C15 C20 -17.7(4) . . . . ? C9 C2 C15 C20 -142.9(3) . . . . ? P C2 C15 C20 101.2(3) . . . . ? C20 C15 C16 C17 0.6(5) . . . . ? C2 C15 C16 C17 174.2(3) . . . . ? C15 C16 C17 C18 -0.8(5) . . . . ? C16 C17 C18 C19 0.3(5) . . . . ? C17 C18 C19 C20 0.4(5) . . . . ? C18 C19 C20 C15 -0.6(5) . . . . ? C16 C15 C20 C19 0.1(5) . . . . ? C2 C15 C20 C19 -173.4(3) . . . . ? C1 O1 P C2 146.9(3) . . . . ? C1 O1 P W -76.3(3) . . . . ? C15 C2 P O1 -151.9(2) . . . . ? C3 C2 P O1 -32.7(2) . . . . ? C9 C2 P O1 87.7(2) . . . . ? C15 C2 P W 79.5(2) . . . . ? C3 C2 P W -161.36(17) . . . . ? C9 C2 P W -40.9(3) . . . . ? O2 C21 W C24 51(4) . . . . ? O2 C21 W C25 -45(4) . . . . ? O2 C21 W C23 140(4) . . . . ? O2 C21 W C22 -134(4) . . . . ? O2 C21 W P -7(5) . . . . ? O5 C24 W C21 62(10) . . . . ? O5 C24 W C25 148(10) . . . . ? O5 C24 W C23 -30(10) . . . . ? O5 C24 W C22 -10(11) . . . . ? O5 C24 W P -128(10) . . . . ? O6 C25 W C21 -49(15) . . . . ? O6 C25 W C24 -137(15) . . . . ? O6 C25 W C23 11(16) . . . . ? O6 C25 W C22 41(15) . . . . ? O6 C25 W P 138(15) . . . . ? O4 C23 W C21 50(5) . . . . ? O4 C23 W C24 139(5) . . . . ? O4 C23 W C25 -9(6) . . . . ? O4 C23 W C22 -39(5) . . . . ? O4 C23 W P -136(5) . . . . ? O3 C22 W C21 -49(4) . . . . ? O3 C22 W C24 23(5) . . . . ? O3 C22 W C25 -134(4) . . . . ? O3 C22 W C23 43(4) . . . . ? O3 C22 W P 141(4) . . . . ? O1 P W C21 36.5(5) . . . . ? C2 P W C21 161.1(5) . . . . ? O1 P W C24 -22.24(14) . . . . ? C2 P W C24 102.38(17) . . . . ? O1 P W C25 73.87(16) . . . . ? C2 P W C25 -161.51(19) . . . . ? O1 P W C23 -110.20(15) . . . . ? C2 P W C23 14.41(18) . . . . ? O1 P W C22 162.55(15) . . . . ? C2 P W C22 -72.84(18) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.604 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.116 _database_code_depnum_ccdc_archive 'CCDC 953769' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H19 O6 P W' _chemical_formula_sum 'C16 H19 O6 P W' _chemical_formula_weight 522.13 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5181(5) _cell_length_b 8.6529(5) _cell_length_c 13.6246(8) _cell_angle_alpha 93.925(5) _cell_angle_beta 99.505(5) _cell_angle_gamma 108.288(4) _cell_volume 932.62(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 18569 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 29.53 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 6.305 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.2535 _exptl_absorpt_correction_T_max 0.5713 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 242 frames, detector distance = 100 mm ; _diffrn_reflns_number 9446 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4463 _reflns_number_gt 4405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0301P)^2^+0.8541P] 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 4463 _refine_ls_number_parameters 226 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 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 C1 C 0.7070(6) 1.1353(4) 0.6675(3) 0.0432(9) Uani 1 1 d . . . H1C H 0.7247 1.2472 0.6973 0.052 Uiso 1 1 calc R . . H1B H 0.6087 1.1007 0.6123 0.052 Uiso 1 1 calc R . . H1A H 0.8070 1.1325 0.6417 0.052 Uiso 1 1 calc R . . C2 C 0.5379(3) 0.7509(3) 0.81577(19) 0.0163(4) Uani 1 1 d . . . C3 C 0.6751(3) 0.7888(3) 0.90891(19) 0.0176(5) Uani 1 1 d . . . C4 C 0.6945(3) 0.6460(3) 0.9337(2) 0.0201(5) Uani 1 1 d . . . C5 C 0.5750(3) 0.5087(3) 0.8614(2) 0.0202(5) Uani 1 1 d . . . C6 C 0.4814(3) 0.5662(3) 0.7930(2) 0.0187(5) Uani 1 1 d . . . C7 C 0.3956(4) 0.8188(4) 0.8278(2) 0.0238(5) Uani 1 1 d . . . H7A H 0.4420 0.9384 0.8444 0.029 Uiso 1 1 calc R . . H7B H 0.3414 0.7709 0.8819 0.029 Uiso 1 1 calc R . . H7C H 0.3121 0.7905 0.7649 0.029 Uiso 1 1 calc R . . C8 C 0.7610(4) 0.9579(4) 0.9636(2) 0.0283(6) Uani 1 1 d . . . H8A H 0.6762 1.0048 0.9800 0.034 Uiso 1 1 calc R . . H8B H 0.8280 1.0269 0.9210 0.034 Uiso 1 1 calc R . . H8C H 0.8353 0.9531 1.0256 0.034 Uiso 1 1 calc R . . C9 C 0.8112(4) 0.6219(4) 1.0215(2) 0.0286(6) Uani 1 1 d . . . H9A H 0.7453 0.5590 1.0667 0.034 Uiso 1 1 calc R . . H9B H 0.8840 0.7290 1.0574 0.034 Uiso 1 1 calc R . . H9C H 0.8810 0.5618 0.9979 0.034 Uiso 1 1 calc R . . C10 C 0.5619(4) 0.3330(4) 0.8698(3) 0.0298(6) Uani 1 1 d . . . H10A H 0.5180 0.2999 0.9300 0.036 Uiso 1 1 calc R . . H10B H 0.6739 0.3218 0.8746 0.036 Uiso 1 1 calc R . . H10C H 0.4856 0.2627 0.8103 0.036 Uiso 1 1 calc R . . C11 C 0.3365(4) 0.4715(4) 0.7106(2) 0.0265(6) Uani 1 1 d . . . H11C H 0.3329 0.3571 0.7010 0.032 Uiso 1 1 calc R . . H11B H 0.3508 0.5197 0.6483 0.032 Uiso 1 1 calc R . . H11A H 0.2310 0.4758 0.7285 0.032 Uiso 1 1 calc R . . C12 C 1.0349(4) 0.7034(3) 0.5782(2) 0.0226(5) Uani 1 1 d . . . C13 C 0.6851(3) 0.5253(3) 0.5861(2) 0.0188(5) Uani 1 1 d U . . C14 C 0.9268(3) 0.6331(4) 0.7649(2) 0.0223(5) Uani 1 1 d . . . C15 C 0.7940(4) 0.8516(3) 0.5225(2) 0.0206(5) Uani 1 1 d . . . C16 C 1.0300(4) 0.9641(4) 0.7202(2) 0.0250(5) Uani 1 1 d U . . O1 O 0.6787(3) 1.0266(3) 0.74198(17) 0.0297(5) Uani 1 1 d . . . O2 O 1.1339(3) 0.6831(3) 0.5372(2) 0.0353(5) Uani 1 1 d . . . O3 O 0.7603(4) 0.9076(3) 0.45187(18) 0.0350(5) Uani 1 1 d . . . O4 O 0.5924(3) 0.3988(2) 0.55508(17) 0.0252(4) Uani 1 1 d . . . O5 O 0.9729(3) 0.5641(4) 0.8251(2) 0.0366(6) Uani 1 1 d . . . O6 O 1.1261(4) 1.0811(3) 0.7638(2) 0.0410(6) Uani 1 1 d . . . P P 0.63580(9) 0.83081(8) 0.71006(5) 0.01666(12) Uani 1 1 d U . . H19 H 0.513(4) 0.813(4) 0.644(3) 0.020 Uiso 1 1 d . . . W W 0.857922(11) 0.748491(10) 0.646500(7) 0.01499(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.077(3) 0.0249(15) 0.0371(18) 0.0143(14) 0.0220(19) 0.0215(17) C2 0.0150(11) 0.0185(11) 0.0173(11) 0.0025(9) 0.0075(9) 0.0059(9) C3 0.0167(11) 0.0207(11) 0.0159(11) 0.0030(9) 0.0069(9) 0.0050(9) C4 0.0207(12) 0.0256(12) 0.0183(12) 0.0080(10) 0.0094(10) 0.0098(10) C5 0.0221(12) 0.0186(11) 0.0234(12) 0.0053(10) 0.0130(10) 0.0066(10) C6 0.0183(11) 0.0172(11) 0.0216(12) 0.0029(9) 0.0110(10) 0.0037(9) C7 0.0233(13) 0.0285(13) 0.0259(13) 0.0048(11) 0.0112(11) 0.0140(11) C8 0.0316(15) 0.0240(13) 0.0240(14) -0.0032(11) 0.0009(11) 0.0057(12) C9 0.0299(15) 0.0399(16) 0.0212(13) 0.0100(12) 0.0060(11) 0.0170(13) C10 0.0360(16) 0.0194(12) 0.0400(17) 0.0102(12) 0.0192(14) 0.0103(12) C11 0.0208(13) 0.0249(13) 0.0284(14) -0.0008(11) 0.0074(11) -0.0006(11) C12 0.0190(12) 0.0232(12) 0.0262(13) 0.0012(11) 0.0097(10) 0.0056(10) C13 0.0173(11) 0.0172(10) 0.0218(12) 0.0033(9) 0.0031(9) 0.0059(9) C14 0.0136(11) 0.0294(14) 0.0252(13) 0.0063(11) 0.0071(10) 0.0068(10) C15 0.0229(13) 0.0164(11) 0.0200(12) 0.0011(10) 0.0060(10) 0.0021(10) C16 0.0235(13) 0.0250(12) 0.0206(13) -0.0001(10) 0.0065(10) -0.0005(10) O1 0.0445(13) 0.0205(9) 0.0303(11) 0.0063(8) 0.0163(10) 0.0145(9) O2 0.0268(11) 0.0405(13) 0.0421(14) 0.0015(11) 0.0177(10) 0.0112(10) O3 0.0507(15) 0.0286(11) 0.0236(11) 0.0091(9) 0.0083(10) 0.0082(11) O4 0.0229(10) 0.0186(9) 0.0308(11) 0.0013(8) 0.0021(8) 0.0040(8) O5 0.0309(12) 0.0550(15) 0.0363(13) 0.0222(12) 0.0136(10) 0.0244(12) O6 0.0410(14) 0.0305(12) 0.0337(13) -0.0063(10) 0.0055(11) -0.0099(11) P 0.0192(3) 0.0163(3) 0.0170(3) 0.0048(2) 0.0067(2) 0.0072(2) W 0.01370(6) 0.01496(6) 0.01569(6) 0.00174(4) 0.00582(4) 0.00244(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.429(4) . ? C1 H1C 0.9800 . ? C1 H1B 0.9800 . ? C1 H1A 0.9800 . ? C2 C6 1.511(3) . ? C2 C3 1.516(4) . ? C2 C7 1.529(3) . ? C2 P 1.849(3) . ? C3 C4 1.355(4) . ? C3 C8 1.494(4) . ? C4 C5 1.472(4) . ? C4 C9 1.495(4) . ? C5 C6 1.349(4) . ? C5 C10 1.503(4) . ? C6 C11 1.496(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11C 0.9800 . ? C11 H11B 0.9800 . ? C11 H11A 0.9800 . ? C12 O2 1.135(4) . ? C12 W 2.019(3) . ? C13 O4 1.133(4) . ? C13 W 2.043(3) . ? C14 O5 1.137(4) . ? C14 W 2.053(3) . ? C15 O3 1.142(4) . ? C15 W 2.038(3) . ? C16 O6 1.134(4) . ? C16 W 2.044(3) . ? O1 P 1.628(2) . ? P W 2.4779(7) . ? P H19 1.22(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 O1 C1 H1C 109.5 . . ? O1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? O1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? C6 C2 C3 103.6(2) . . ? C6 C2 C7 114.1(2) . . ? C3 C2 C7 113.9(2) . . ? C6 C2 P 105.58(16) . . ? C3 C2 P 108.51(17) . . ? C7 C2 P 110.57(18) . . ? C4 C3 C8 128.5(3) . . ? C4 C3 C2 108.5(2) . . ? C8 C3 C2 122.8(2) . . ? C3 C4 C5 109.4(2) . . ? C3 C4 C9 127.8(3) . . ? C5 C4 C9 122.8(2) . . ? C6 C5 C4 109.8(2) . . ? C6 C5 C10 127.7(3) . . ? C4 C5 C10 122.5(3) . . ? C5 C6 C11 128.6(2) . . ? C5 C6 C2 108.7(2) . . ? C11 C6 C2 122.6(2) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11C 109.5 . . ? C6 C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? C6 C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? O2 C12 W 177.1(3) . . ? O4 C13 W 177.4(2) . . ? O5 C14 W 173.8(3) . . ? O3 C15 W 178.4(3) . . ? O6 C16 W 177.8(3) . . ? C1 O1 P 119.3(2) . . ? O1 P C2 99.56(11) . . ? O1 P W 116.16(9) . . ? C2 P W 125.33(8) . . ? O1 P H19 96.5(16) . . ? C2 P H19 102.7(17) . . ? W P H19 112.1(16) . . ? C12 W C15 86.35(12) . . ? C12 W C13 91.86(11) . . ? C15 W C13 91.47(11) . . ? C12 W C16 90.47(12) . . ? C15 W C16 93.70(12) . . ? C13 W C16 174.45(10) . . ? C12 W C14 90.21(11) . . ? C15 W C14 175.91(10) . . ? C13 W C14 86.43(11) . . ? C16 W C14 88.52(12) . . ? C12 W P 171.23(9) . . ? C15 W P 85.06(8) . . ? C13 W P 90.13(8) . . ? C16 W P 88.31(9) . . ? C14 W P 98.44(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C2 C3 C4 0.9(3) . . . . ? C7 C2 C3 C4 125.4(2) . . . . ? P C2 C3 C4 -111.0(2) . . . . ? C6 C2 C3 C8 -175.7(2) . . . . ? C7 C2 C3 C8 -51.2(3) . . . . ? P C2 C3 C8 72.4(3) . . . . ? C8 C3 C4 C5 176.0(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C8 C3 C4 C9 -1.7(5) . . . . ? C2 C3 C4 C9 -178.0(2) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C9 C4 C5 C6 177.4(2) . . . . ? C3 C4 C5 C10 -178.4(2) . . . . ? C9 C4 C5 C10 -0.5(4) . . . . ? C4 C5 C6 C11 -175.0(3) . . . . ? C10 C5 C6 C11 2.8(4) . . . . ? C4 C5 C6 C2 1.1(3) . . . . ? C10 C5 C6 C2 178.8(2) . . . . ? C3 C2 C6 C5 -1.2(3) . . . . ? C7 C2 C6 C5 -125.5(2) . . . . ? P C2 C6 C5 112.8(2) . . . . ? C3 C2 C6 C11 175.2(2) . . . . ? C7 C2 C6 C11 50.8(3) . . . . ? P C2 C6 C11 -70.9(3) . . . . ? C1 O1 P C2 -160.1(3) . . . . ? C1 O1 P W 62.5(3) . . . . ? C6 C2 P O1 176.83(18) . . . . ? C3 C2 P O1 -72.66(19) . . . . ? C7 C2 P O1 52.9(2) . . . . ? C6 C2 P W -51.3(2) . . . . ? C3 C2 P W 59.21(19) . . . . ? C7 C2 P W -175.22(15) . . . . ? O2 C12 W C15 19(5) . . . . ? O2 C12 W C13 111(5) . . . . ? O2 C12 W C16 -74(5) . . . . ? O2 C12 W C14 -163(5) . . . . ? O2 C12 W P 8(6) . . . . ? O3 C15 W C12 14(9) . . . . ? O3 C15 W C13 -77(9) . . . . ? O3 C15 W C16 105(9) . . . . ? O3 C15 W C14 -18(10) . . . . ? O3 C15 W P -167(9) . . . . ? O4 C13 W C12 74(6) . . . . ? O4 C13 W C15 160(6) . . . . ? O4 C13 W C16 -41(6) . . . . ? O4 C13 W C14 -16(6) . . . . ? O4 C13 W P -115(6) . . . . ? O6 C16 W C12 -100(8) . . . . ? O6 C16 W C15 174(8) . . . . ? O6 C16 W C13 15(8) . . . . ? O6 C16 W C14 -10(8) . . . . ? O6 C16 W P 89(8) . . . . ? O5 C14 W C12 -12(3) . . . . ? O5 C14 W C15 20(3) . . . . ? O5 C14 W C13 79(3) . . . . ? O5 C14 W C16 -103(3) . . . . ? O5 C14 W P 169(3) . . . . ? O1 P W C12 -59.6(6) . . . . ? C2 P W C12 175.3(6) . . . . ? O1 P W C15 -71.34(13) . . . . ? C2 P W C15 163.57(13) . . . . ? O1 P W C13 -162.80(12) . . . . ? C2 P W C13 72.10(13) . . . . ? O1 P W C16 22.53(13) . . . . ? C2 P W C16 -102.57(14) . . . . ? O1 P W C14 110.78(13) . . . . ? C2 P W C14 -14.31(14) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.061 _refine_diff_density_min -1.433 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 953768' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2127 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H25 O6 P Si2 W' _chemical_formula_sum 'C15 H25 O6 P Si2 W' _chemical_formula_weight 572.35 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' 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' W W -0.8490 6.8722 '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/a' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 14.8631(7) _cell_length_b 9.4639(3) _cell_length_c 16.6281(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.845(4) _cell_angle_gamma 90.00 _cell_volume 2238.60(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8550 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 29.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 5.363 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.3254 _exptl_absorpt_correction_T_max 0.6161 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 270 frames, detector distance = 100 mm ; _diffrn_reflns_number 11102 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5275 _reflns_number_gt 4326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0265P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5275 _refine_ls_number_parameters 235 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0499 _refine_ls_wR_factor_gt 0.0485 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 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 C1 C 0.2160(2) 0.4245(3) 0.6047(2) 0.0256(7) Uani 1 1 d . . . H1B H 0.2247 0.5163 0.5794 0.031 Uiso 1 1 calc R . . H1A H 0.1654 0.3721 0.5636 0.031 Uiso 1 1 calc R . . C2 C 0.3048(2) 0.3420(4) 0.6245(2) 0.0303(7) Uani 1 1 d . . . H2A H 0.3053 0.2503 0.6479 0.036 Uiso 1 1 calc R . . C3 C 0.3824(3) 0.3882(5) 0.6114(3) 0.0437(10) Uani 1 1 d . . . H3B H 0.3841 0.4795 0.5881 0.052 Uiso 1 1 calc R . . H3A H 0.4371 0.3306 0.6253 0.052 Uiso 1 1 calc R . . C4 C 0.20287(19) 0.5482(3) 0.83232(18) 0.0175(5) Uani 1 1 d . . . H4A H 0.1896 0.6405 0.8559 0.021 Uiso 1 1 calc R . . C5 C 0.0528(2) 0.4854(4) 0.9150(2) 0.0302(7) Uani 1 1 d . . . H5A H 0.0428 0.5877 0.9156 0.036 Uiso 1 1 calc R . . H5B H 0.1009 0.4572 0.9665 0.036 Uiso 1 1 calc R . . H5C H -0.0062 0.4363 0.9117 0.036 Uiso 1 1 calc R . . C6 C 0.1182(2) 0.2447(3) 0.8197(2) 0.0293(7) Uani 1 1 d . . . H6A H 0.1678 0.2188 0.8708 0.035 Uiso 1 1 calc R . . H6B H 0.1393 0.2235 0.7703 0.035 Uiso 1 1 calc R . . H6C H 0.0612 0.1905 0.8168 0.035 Uiso 1 1 calc R . . C7 C -0.0055(2) 0.4802(4) 0.7258(2) 0.0322(8) Uani 1 1 d . . . H7A H 0.0136 0.4571 0.6757 0.039 Uiso 1 1 calc R . . H7B H -0.0205 0.5811 0.7255 0.039 Uiso 1 1 calc R . . H7C H -0.0612 0.4246 0.7258 0.039 Uiso 1 1 calc R . . C8 C 0.3680(2) 0.3355(3) 0.8637(2) 0.0310(7) Uani 1 1 d . . . H8A H 0.3815 0.3678 0.8124 0.037 Uiso 1 1 calc R . . H8B H 0.3233 0.2568 0.8502 0.037 Uiso 1 1 calc R . . H8C H 0.4264 0.3040 0.9045 0.037 Uiso 1 1 calc R . . C9 C 0.2987(3) 0.4235(4) 1.0109(2) 0.0362(8) Uani 1 1 d . . . H9A H 0.2589 0.3390 1.0009 0.043 Uiso 1 1 calc R . . H9B H 0.2682 0.4987 1.0340 0.043 Uiso 1 1 calc R . . H9C H 0.3598 0.4012 1.0508 0.043 Uiso 1 1 calc R . . C10 C 0.3991(2) 0.6364(4) 0.9330(2) 0.0301(7) Uani 1 1 d . . . H10C H 0.4549 0.6112 0.9790 0.036 Uiso 1 1 calc R . . H10B H 0.3681 0.7181 0.9496 0.036 Uiso 1 1 calc R . . H10A H 0.4179 0.6600 0.8828 0.036 Uiso 1 1 calc R . . C11 C 0.1272(2) 1.0077(3) 0.6059(2) 0.0312(7) Uani 1 1 d . . . C12 C 0.2729(2) 0.8051(3) 0.6100(2) 0.0247(6) Uani 1 1 d . . . C13 C 0.0743(2) 0.7156(3) 0.5689(2) 0.0242(6) Uani 1 1 d U . . C14 C 0.0677(2) 0.8433(3) 0.7267(2) 0.0274(7) Uani 1 1 d . . . C15 C 0.2577(2) 0.9197(3) 0.7656(2) 0.0262(7) Uani 1 1 d U . . O1 O 0.18919(15) 0.4485(2) 0.68140(14) 0.0232(5) Uani 1 1 d . . . O2 O 0.1055(2) 1.1118(3) 0.5712(2) 0.0482(8) Uani 1 1 d . . . O3 O 0.33342(18) 0.7940(3) 0.58229(17) 0.0381(6) Uani 1 1 d . . . O4 O 0.02436(17) 0.6536(3) 0.51598(18) 0.0381(6) Uani 1 1 d . . . O5 O 0.0138(2) 0.8576(3) 0.7623(2) 0.0433(7) Uani 1 1 d . . . O6 O 0.30729(18) 0.9720(3) 0.82352(17) 0.0382(6) Uani 1 1 d . . . P P 0.22281(5) 0.59388(8) 0.73352(5) 0.01784(15) Uani 1 1 d U . . H11 H 0.315(2) 0.583(3) 0.746(2) 0.021 Uiso 1 1 d . . . Si1 Si 0.09247(6) 0.43771(8) 0.82196(6) 0.02038(17) Uani 1 1 d . . . Si2 Si 0.31620(5) 0.48395(9) 0.90961(5) 0.02041(16) Uani 1 1 d . . . W W 0.167206(8) 0.822984(11) 0.665370(8) 0.01924(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0287(16) 0.0278(15) 0.0223(15) -0.0047(12) 0.0107(13) 0.0018(12) C2 0.0316(17) 0.0328(17) 0.0279(16) -0.0037(14) 0.0110(14) 0.0055(14) C3 0.0327(19) 0.060(3) 0.040(2) -0.007(2) 0.0131(17) 0.0048(18) C4 0.0152(13) 0.0184(12) 0.0207(14) -0.0002(11) 0.0081(11) 0.0004(10) C5 0.0272(16) 0.0315(17) 0.0364(18) 0.0033(15) 0.0165(14) -0.0021(13) C6 0.0283(16) 0.0202(15) 0.042(2) 0.0011(14) 0.0135(15) -0.0044(12) C7 0.0184(14) 0.0385(18) 0.0361(18) 0.0023(16) 0.0022(14) -0.0038(13) C8 0.0250(15) 0.0284(16) 0.0365(18) -0.0002(15) 0.0040(14) 0.0098(13) C9 0.0352(19) 0.046(2) 0.0240(17) 0.0071(15) 0.0031(15) -0.0006(16) C10 0.0228(15) 0.0318(16) 0.0328(17) -0.0040(14) 0.0033(14) -0.0032(13) C11 0.0348(17) 0.0225(15) 0.0385(19) 0.0070(15) 0.0138(15) 0.0027(14) C12 0.0237(15) 0.0278(16) 0.0230(14) 0.0000(13) 0.0074(13) -0.0050(12) C13 0.0231(15) 0.0203(13) 0.0279(15) 0.0027(11) 0.0055(11) -0.0005(10) C14 0.0275(16) 0.0247(15) 0.0329(17) 0.0016(13) 0.0131(14) 0.0040(12) C15 0.0284(16) 0.0211(14) 0.0294(15) -0.0032(11) 0.0089(11) 0.0006(11) O1 0.0280(11) 0.0201(10) 0.0233(11) -0.0038(8) 0.0101(9) -0.0016(8) O2 0.0521(17) 0.0284(13) 0.065(2) 0.0197(14) 0.0188(16) 0.0075(12) O3 0.0313(13) 0.0552(16) 0.0320(13) 0.0003(12) 0.0157(11) -0.0059(12) O4 0.0325(13) 0.0321(13) 0.0405(15) -0.0001(11) -0.0041(12) -0.0023(10) O5 0.0411(15) 0.0430(15) 0.0557(18) 0.0020(13) 0.0295(14) 0.0049(12) O6 0.0364(13) 0.0341(13) 0.0422(15) -0.0111(12) 0.0086(12) -0.0082(11) P 0.0168(3) 0.0177(3) 0.0205(4) 0.0006(3) 0.0078(3) 0.0010(3) Si1 0.0172(4) 0.0191(4) 0.0262(4) 0.0018(3) 0.0084(3) -0.0003(3) Si2 0.0175(4) 0.0209(4) 0.0216(4) 0.0002(3) 0.0036(3) 0.0012(3) W 0.01980(6) 0.01615(6) 0.02274(6) 0.00306(5) 0.00769(4) 0.00008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.459(4) . ? C1 C2 1.487(4) . ? C1 H1B 0.9900 . ? C1 H1A 0.9900 . ? C2 C3 1.309(6) . ? C2 H2A 0.9500 . ? C3 H3B 0.9500 . ? C3 H3A 0.9500 . ? C4 P 1.804(3) . ? C4 Si2 1.899(3) . ? C4 Si1 1.911(3) . ? C4 H4A 1.0000 . ? C5 Si1 1.863(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si1 1.869(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si1 1.868(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si2 1.868(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si2 1.866(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si2 1.864(3) . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C11 O2 1.140(4) . ? C11 W 2.012(3) . ? C12 O3 1.128(4) . ? C12 W 2.045(3) . ? C13 O4 1.136(4) . ? C13 W 2.057(3) . ? C14 O5 1.133(4) . ? C14 W 2.035(4) . ? C15 O6 1.142(4) . ? C15 W 2.031(3) . ? O1 P 1.626(2) . ? P W 2.4750(7) . ? P H11 1.34(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 109.8(3) . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? H1B C1 H1A 108.2 . . ? C3 C2 C1 123.8(4) . . ? C3 C2 H2A 118.1 . . ? C1 C2 H2A 118.1 . . ? C2 C3 H3B 120.0 . . ? C2 C3 H3A 120.0 . . ? H3B C3 H3A 120.0 . . ? P C4 Si2 110.21(15) . . ? P C4 Si1 114.34(15) . . ? Si2 C4 Si1 117.12(15) . . ? P C4 H4A 104.6 . . ? Si2 C4 H4A 104.6 . . ? Si1 C4 H4A 104.6 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10C 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? Si2 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O2 C11 W 178.7(4) . . ? O3 C12 W 177.5(3) . . ? O4 C13 W 178.4(3) . . ? O5 C14 W 178.0(3) . . ? O6 C15 W 177.9(3) . . ? C1 O1 P 118.6(2) . . ? O1 P C4 100.17(13) . . ? O1 P W 119.15(8) . . ? C4 P W 120.36(10) . . ? O1 P H11 99.0(14) . . ? C4 P H11 106.1(16) . . ? W P H11 109.4(15) . . ? C5 Si1 C7 107.60(16) . . ? C5 Si1 C6 111.68(17) . . ? C7 Si1 C6 107.85(17) . . ? C5 Si1 C4 105.23(14) . . ? C7 Si1 C4 113.30(14) . . ? C6 Si1 C4 111.17(14) . . ? C10 Si2 C9 107.78(18) . . ? C10 Si2 C8 109.98(17) . . ? C9 Si2 C8 108.64(18) . . ? C10 Si2 C4 107.25(14) . . ? C9 Si2 C4 112.37(15) . . ? C8 Si2 C4 110.75(14) . . ? C11 W C15 92.44(14) . . ? C11 W C14 90.56(14) . . ? C15 W C14 87.20(14) . . ? C11 W C12 90.40(14) . . ? C15 W C12 89.63(13) . . ? C14 W C12 176.73(13) . . ? C11 W C13 90.60(13) . . ? C15 W C13 176.44(13) . . ? C14 W C13 90.91(14) . . ? C12 W C13 92.21(13) . . ? C11 W P 176.66(11) . . ? C15 W P 88.02(9) . . ? C14 W P 92.77(9) . . ? C12 W P 86.29(9) . . ? C13 W P 89.06(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -119.1(4) . . . . ? C2 C1 O1 P 93.4(3) . . . . ? C1 O1 P C4 -164.3(2) . . . . ? C1 O1 P W 62.3(2) . . . . ? Si2 C4 P O1 96.46(15) . . . . ? Si1 C4 P O1 -37.94(17) . . . . ? Si2 C4 P W -130.80(11) . . . . ? Si1 C4 P W 94.80(14) . . . . ? P C4 Si1 C5 -150.41(16) . . . . ? Si2 C4 Si1 C5 78.46(19) . . . . ? P C4 Si1 C7 -33.1(2) . . . . ? Si2 C4 Si1 C7 -164.25(18) . . . . ? P C4 Si1 C6 88.52(19) . . . . ? Si2 C4 Si1 C6 -42.6(2) . . . . ? P C4 Si2 C10 65.6(2) . . . . ? Si1 C4 Si2 C10 -161.43(18) . . . . ? P C4 Si2 C9 -176.17(17) . . . . ? Si1 C4 Si2 C9 -43.2(2) . . . . ? P C4 Si2 C8 -54.5(2) . . . . ? Si1 C4 Si2 C8 78.5(2) . . . . ? O2 C11 W C15 107(16) . . . . ? O2 C11 W C14 -166(16) . . . . ? O2 C11 W C12 17(16) . . . . ? O2 C11 W C13 -75(16) . . . . ? O2 C11 W P 9(18) . . . . ? O6 C15 W C11 127(8) . . . . ? O6 C15 W C14 36(8) . . . . ? O6 C15 W C12 -143(8) . . . . ? O6 C15 W C13 -22(9) . . . . ? O6 C15 W P -56(8) . . . . ? O5 C14 W C11 -75(9) . . . . ? O5 C14 W C15 18(9) . . . . ? O5 C14 W C12 32(10) . . . . ? O5 C14 W C13 -165(9) . . . . ? O5 C14 W P 106(9) . . . . ? O3 C12 W C11 133(7) . . . . ? O3 C12 W C15 41(7) . . . . ? O3 C12 W C14 26(8) . . . . ? O3 C12 W C13 -136(7) . . . . ? O3 C12 W P -47(7) . . . . ? O4 C13 W C11 147(11) . . . . ? O4 C13 W C15 -64(12) . . . . ? O4 C13 W C14 -122(11) . . . . ? O4 C13 W C12 57(11) . . . . ? O4 C13 W P -29(11) . . . . ? O1 P W C11 -73.9(18) . . . . ? C4 P W C11 162.0(18) . . . . ? O1 P W C15 -171.80(14) . . . . ? C4 P W C15 64.07(15) . . . . ? O1 P W C14 101.10(14) . . . . ? C4 P W C14 -23.03(14) . . . . ? O1 P W C12 -82.04(13) . . . . ? C4 P W C12 153.83(14) . . . . ? O1 P W C13 10.23(14) . . . . ? C4 P W C13 -113.89(14) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.789 _refine_diff_density_min -1.282 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 953767' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_GSTR289 _vrf_RINTA01_GSTR289 ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: The sample consisted of small and weak diffracting crystals which needed very long exposure times, but still showed very weak intensities at higher diffraction angles. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H23 O6 P Si2 W' _chemical_formula_sum 'C13 H23 O6 P Si2 W' _chemical_formula_weight 546.31 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' 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' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.6986(5) _cell_length_b 9.4668(6) _cell_length_c 22.8326(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.053(4) _cell_angle_gamma 90.00 _cell_volume 2075.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5395 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 29.29 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 5.779 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.4777 _exptl_absorpt_correction_T_max 0.8018 _exptl_absorpt_process_details 'STOE XRed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 187 frames, detector distance = 100 mm ; _diffrn_reflns_number 11962 _diffrn_reflns_av_R_equivalents 0.2624 _diffrn_reflns_av_sigmaI/netI 0.2094 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3853 _reflns_number_gt 2400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3853 _refine_ls_number_parameters 218 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1748 _refine_ls_R_factor_gt 0.1187 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.005 _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 C1 C 0.0372(10) 0.4339(11) 0.9113(6) 0.050(4) Uani 1 1 d U . . H1C H 0.0320 0.5324 0.9240 0.060 Uiso 1 1 calc R . . H1B H 0.0190 0.3711 0.9435 0.060 Uiso 1 1 calc R . . H1A H -0.0325 0.4172 0.8766 0.060 Uiso 1 1 calc R . . C2 C 0.3447(9) 0.3062(9) 0.8272(4) 0.023(2) Uani 1 1 d U . . H2A H 0.3888 0.2142 0.8189 0.028 Uiso 1 1 calc R . . C3 C 0.1642(9) 0.5379(13) 0.7590(4) 0.035(2) Uani 1 1 d . . . H3A H 0.2096 0.6055 0.7880 0.041 Uiso 1 1 calc R . . H3B H 0.0792 0.5021 0.7724 0.041 Uiso 1 1 calc R . . H3C H 0.1405 0.5850 0.7207 0.041 Uiso 1 1 calc R . . C4 C 0.1993(11) 0.2490(10) 0.7033(5) 0.035(3) Uani 1 1 d U . . H4A H 0.1181 0.2139 0.7200 0.042 Uiso 1 1 calc R . . H4B H 0.2646 0.1712 0.7004 0.042 Uiso 1 1 calc R . . H4C H 0.1691 0.2879 0.6638 0.042 Uiso 1 1 calc R . . C5 C 0.4360(10) 0.4546(14) 0.7165(4) 0.045(3) Uani 1 1 d U . . H5A H 0.5047 0.3789 0.7157 0.054 Uiso 1 1 calc R . . H5B H 0.4790 0.5343 0.7396 0.054 Uiso 1 1 calc R . . H5C H 0.4033 0.4857 0.6760 0.054 Uiso 1 1 calc R . . C6 C 0.4502(12) 0.5984(10) 0.8751(6) 0.039(3) Uani 1 1 d U . . H6A H 0.3577 0.6160 0.8862 0.047 Uiso 1 1 calc R . . H6B H 0.4534 0.6341 0.8350 0.047 Uiso 1 1 calc R . . H6C H 0.5206 0.6470 0.9029 0.047 Uiso 1 1 calc R . . C7 C 0.6552(11) 0.3710(12) 0.8507(6) 0.050(3) Uani 1 1 d . . . H7A H 0.6490 0.3974 0.8089 0.059 Uiso 1 1 calc R . . H7B H 0.6772 0.2702 0.8552 0.059 Uiso 1 1 calc R . . H7C H 0.7287 0.4265 0.8740 0.059 Uiso 1 1 calc R . . C8 C 0.5036(11) 0.3421(11) 0.9553(5) 0.041(3) Uani 1 1 d . . . H8A H 0.5218 0.2403 0.9560 0.049 Uiso 1 1 calc R . . H8B H 0.4174 0.3610 0.9717 0.049 Uiso 1 1 calc R . . H8C H 0.5812 0.3910 0.9790 0.049 Uiso 1 1 calc R . . C9 C 0.1593(11) -0.1494(12) 0.9584(5) 0.032(3) Uani 1 1 d . . . C10 C 0.1698(10) -0.0615(10) 0.8362(5) 0.028(3) Uani 1 1 d . . . C11 C 0.3907(11) -0.0040(10) 0.9263(4) 0.027(3) Uani 1 1 d U . . C12 C 0.2034(9) 0.1452(10) 0.9937(5) 0.023(3) Uani 1 1 d . . . C13 C -0.0276(10) 0.0578(10) 0.9058(4) 0.025(2) Uani 1 1 d U . . O1 O 0.1744(7) 0.4057(6) 0.8964(3) 0.0301(18) Uani 1 1 d . . . O2 O 0.1454(8) -0.2547(8) 0.9824(3) 0.041(2) Uani 1 1 d . . . O3 O 0.1675(8) -0.1111(8) 0.7900(4) 0.040(2) Uani 1 1 d . . . O4 O 0.5080(6) -0.0295(9) 0.9317(3) 0.0373(18) Uani 1 1 d . . . O5 O 0.2120(7) 0.2144(7) 1.0359(3) 0.0369(19) Uani 1 1 d . . . O6 O -0.1482(7) 0.0685(7) 0.8996(3) 0.0352(19) Uani 1 1 d . . . P P 0.1960(3) 0.2592(3) 0.86285(12) 0.0234(6) Uani 1 1 d . . . H9 H 0.100(8) 0.293(9) 0.829(4) 0.028 Uiso 1 1 d . . . Si1 Si 0.2853(3) 0.3875(3) 0.75117(12) 0.0259(7) Uani 1 1 d . . . Si2 Si 0.4855(3) 0.4071(3) 0.87726(14) 0.0293(7) Uani 1 1 d . . . W W 0.18195(5) 0.03337(5) 0.91641(2) 0.02242(10) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(6) 0.034(8) 0.077(9) -0.006(6) 0.032(6) 0.004(5) C2 0.020(5) 0.012(5) 0.038(6) 0.003(4) 0.007(4) 0.000(4) C3 0.039(6) 0.036(6) 0.027(6) 0.006(6) -0.003(4) 0.003(6) C4 0.050(6) 0.022(6) 0.032(6) 0.007(5) 0.004(5) 0.003(5) C5 0.066(7) 0.049(7) 0.022(5) 0.012(6) 0.015(5) -0.007(7) C6 0.041(7) 0.022(7) 0.055(8) -0.002(6) 0.013(6) -0.014(5) C7 0.034(7) 0.039(7) 0.076(10) 0.015(6) 0.009(6) -0.001(5) C8 0.042(7) 0.035(7) 0.041(7) 0.006(5) -0.012(5) -0.002(5) C9 0.033(6) 0.041(8) 0.023(6) 0.001(5) 0.007(5) 0.006(5) C10 0.029(5) 0.013(7) 0.042(7) 0.003(5) 0.002(5) 0.007(4) C11 0.046(5) 0.014(7) 0.023(5) -0.005(4) 0.007(4) 0.001(4) C12 0.012(5) 0.017(6) 0.041(7) 0.012(5) 0.007(5) 0.002(4) C13 0.031(2) 0.018(6) 0.024(5) -0.003(4) -0.003(4) 0.000(5) O1 0.033(4) 0.023(4) 0.037(5) -0.003(3) 0.014(4) 0.000(3) O2 0.051(5) 0.029(5) 0.046(5) 0.013(4) 0.012(4) 0.001(4) O3 0.049(5) 0.040(5) 0.030(5) -0.014(4) -0.003(4) 0.002(4) O4 0.031(4) 0.047(4) 0.035(4) -0.007(5) 0.007(3) 0.003(4) O5 0.047(5) 0.034(5) 0.030(5) -0.008(4) 0.009(4) 0.000(4) O6 0.029(4) 0.032(5) 0.045(5) 0.005(3) 0.005(4) -0.002(3) P 0.0272(15) 0.0180(16) 0.0263(16) 0.0013(11) 0.0087(12) 0.0008(12) Si1 0.0343(16) 0.0203(16) 0.0245(16) -0.0001(12) 0.0094(13) 0.0002(13) Si2 0.0291(16) 0.0239(19) 0.0336(19) 0.0067(13) 0.0003(14) -0.0049(12) W 0.02735(18) 0.01785(18) 0.02307(18) 0.0014(3) 0.00710(13) -0.0013(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 C1 O1 1.444(10) . ? C1 H1C 0.9800 . ? C1 H1B 0.9800 . ? C1 H1A 0.9800 . ? C2 P 1.808(8) . ? C2 Si2 1.909(10) . ? C2 Si1 1.913(10) . ? C2 H2A 1.0000 . ? C3 Si1 1.870(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si1 1.832(11) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si1 1.869(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si2 1.842(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si2 1.864(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si2 1.869(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O2 1.155(11) . ? C9 W 2.005(11) . ? C10 O3 1.152(12) . ? C10 W 2.029(11) . ? C11 O4 1.152(10) . ? C11 W 2.037(10) . ? C12 O5 1.158(12) . ? C12 W 2.044(12) . ? C13 O6 1.162(10) . ? C13 W 2.026(10) . ? O1 P 1.612(6) . ? P W 2.476(3) . ? P H9 1.17(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1C 109.5 . . ? O1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? O1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? P C2 Si2 113.7(5) . . ? P C2 Si1 110.5(5) . . ? Si2 C2 Si1 116.2(4) . . ? P C2 H2A 105.1 . . ? Si2 C2 H2A 105.1 . . ? Si1 C2 H2A 105.1 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 W 179.5(11) . . ? O3 C10 W 176.8(9) . . ? O4 C11 W 178.0(9) . . ? O5 C12 W 176.4(9) . . ? O6 C13 W 178.5(9) . . ? C1 O1 P 117.2(6) . . ? O1 P C2 99.6(4) . . ? O1 P W 119.2(2) . . ? C2 P W 122.5(3) . . ? O1 P H9 86(4) . . ? C2 P H9 104(4) . . ? W P H9 118(4) . . ? C4 Si1 C5 107.9(5) . . ? C4 Si1 C3 111.3(5) . . ? C5 Si1 C3 108.7(5) . . ? C4 Si1 C2 108.0(4) . . ? C5 Si1 C2 111.6(4) . . ? C3 Si1 C2 109.4(4) . . ? C6 Si2 C7 109.9(5) . . ? C6 Si2 C8 110.0(6) . . ? C7 Si2 C8 106.3(6) . . ? C6 Si2 C2 111.2(5) . . ? C7 Si2 C2 107.7(5) . . ? C8 Si2 C2 111.7(5) . . ? C9 W C13 88.9(4) . . ? C9 W C10 93.1(4) . . ? C13 W C10 90.7(4) . . ? C9 W C11 88.3(4) . . ? C13 W C11 176.5(4) . . ? C10 W C11 87.4(4) . . ? C9 W C12 92.2(4) . . ? C13 W C12 91.3(4) . . ? C10 W C12 174.4(4) . . ? C11 W C12 90.8(4) . . ? C9 W P 176.9(3) . . ? C13 W P 88.1(3) . . ? C10 W P 86.4(3) . . ? C11 W P 94.7(3) . . ? C12 W P 88.5(3) . . ? 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 C1 O1 P C2 156.4(8) . . . . ? C1 O1 P W -67.6(8) . . . . ? Si2 C2 P O1 43.7(5) . . . . ? Si1 C2 P O1 -89.0(5) . . . . ? Si2 C2 P W -90.3(5) . . . . ? Si1 C2 P W 136.9(3) . . . . ? P C2 Si1 C4 -67.5(6) . . . . ? Si2 C2 Si1 C4 161.0(5) . . . . ? P C2 Si1 C5 174.0(5) . . . . ? Si2 C2 Si1 C5 42.6(7) . . . . ? P C2 Si1 C3 53.7(6) . . . . ? Si2 C2 Si1 C3 -77.8(6) . . . . ? P C2 Si2 C6 -86.7(6) . . . . ? Si1 C2 Si2 C6 43.2(6) . . . . ? P C2 Si2 C7 152.8(5) . . . . ? Si1 C2 Si2 C7 -77.3(6) . . . . ? P C2 Si2 C8 36.5(6) . . . . ? Si1 C2 Si2 C8 166.4(5) . . . . ? O2 C9 W C13 27(100) . . . . ? O2 C9 W C10 -63(100) . . . . ? O2 C9 W C11 -151(100) . . . . ? O2 C9 W C12 119(100) . . . . ? O2 C9 W P 16(100) . . . . ? O6 C13 W C9 -33(30) . . . . ? O6 C13 W C10 60(30) . . . . ? O6 C13 W C11 4(35) . . . . ? O6 C13 W C12 -125(30) . . . . ? O6 C13 W P 146(30) . . . . ? O3 C10 W C9 -142(17) . . . . ? O3 C10 W C13 129(17) . . . . ? O3 C10 W C11 -54(17) . . . . ? O3 C10 W C12 18(20) . . . . ? O3 C10 W P 41(17) . . . . ? O4 C11 W C9 34(23) . . . . ? O4 C11 W C13 -2(28) . . . . ? O4 C11 W C10 -59(23) . . . . ? O4 C11 W C12 127(23) . . . . ? O4 C11 W P -145(23) . . . . ? O5 C12 W C9 -146(12) . . . . ? O5 C12 W C13 -57(12) . . . . ? O5 C12 W C10 54(14) . . . . ? O5 C12 W C11 126(12) . . . . ? O5 C12 W P 31(12) . . . . ? O1 P W C9 87(6) . . . . ? C2 P W C9 -148(6) . . . . ? O1 P W C13 75.4(4) . . . . ? C2 P W C13 -158.9(5) . . . . ? O1 P W C10 166.2(4) . . . . ? C2 P W C10 -68.1(5) . . . . ? O1 P W C11 -106.7(4) . . . . ? C2 P W C11 19.0(5) . . . . ? O1 P W C12 -16.0(4) . . . . ? C2 P W C12 109.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.246 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.187 _database_code_depnum_ccdc_archive 'CCDC 953773' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2100 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H27 O6 P Si2 W' _chemical_formula_sum 'C15 H27 O6 P Si2 W' _chemical_formula_weight 574.37 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' 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' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3698(2) _cell_length_b 10.3785(2) _cell_length_c 12.2990(2) _cell_angle_alpha 76.1508(14) _cell_angle_beta 85.9396(14) _cell_angle_gamma 88.6518(12) _cell_volume 1158.30(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5849 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 5.182 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.5752 _exptl_absorpt_correction_T_max 0.8195 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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' _diffrn_measurement_method 'ccd, thin slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29506 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5556 _reflns_number_gt 4832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0236P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5556 _refine_ls_number_parameters 237 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 C1 C 0.8954(4) 0.9915(4) 0.2230(3) 0.0323(8) Uani 1 1 d . . . H1A H 0.8870 1.0013 0.3021 0.039 Uiso 1 1 calc R . . C2 C 1.0493(4) 0.9670(5) 0.1902(4) 0.0524(12) Uani 1 1 d . . . H2A H 1.1071 1.0424 0.1955 0.063 Uiso 1 1 calc R . . H2B H 1.0578 0.9565 0.1129 0.063 Uiso 1 1 calc R . . H2C H 1.0834 0.8860 0.2408 0.063 Uiso 1 1 calc R . . C3 C 0.8336(5) 1.1129(4) 0.1476(4) 0.0475(11) Uani 1 1 d . . . H3C H 0.7343 1.1256 0.1739 0.057 Uiso 1 1 calc R . . H3B H 0.8365 1.1013 0.0707 0.057 Uiso 1 1 calc R . . H3A H 0.8899 1.1907 0.1491 0.057 Uiso 1 1 calc R . . C4 C 0.6783(3) 0.6514(3) 0.2505(3) 0.0201(7) Uani 1 1 d . . . H4A H 0.6318 0.5853 0.3154 0.024 Uiso 1 1 calc R . . C5 C 0.3724(4) 0.6353(4) 0.1896(3) 0.0408(10) Uani 1 1 d . . . H5A H 0.3491 0.5919 0.2686 0.049 Uiso 1 1 calc R . . H5B H 0.4003 0.5680 0.1480 0.049 Uiso 1 1 calc R . . H5C H 0.2886 0.6844 0.1577 0.049 Uiso 1 1 calc R . . C6 C 0.4583(4) 0.8861(4) 0.2488(3) 0.0338(9) Uani 1 1 d . . . H6A H 0.5371 0.9464 0.2491 0.041 Uiso 1 1 calc R . . H6B H 0.4231 0.8462 0.3263 0.041 Uiso 1 1 calc R . . H6C H 0.3806 0.9357 0.2078 0.041 Uiso 1 1 calc R . . C7 C 0.5745(4) 0.8288(4) 0.0274(3) 0.0348(9) Uani 1 1 d . . . H7A H 0.6056 0.7590 -0.0105 0.042 Uiso 1 1 calc R . . H7B H 0.6528 0.8915 0.0219 0.042 Uiso 1 1 calc R . . H7C H 0.4917 0.8759 -0.0083 0.042 Uiso 1 1 calc R . . C8 C 0.8903(4) 0.4206(4) 0.2651(3) 0.0394(10) Uani 1 1 d . . . H8A H 0.8244 0.3543 0.3113 0.047 Uiso 1 1 calc R . . H8B H 0.9408 0.4639 0.3136 0.047 Uiso 1 1 calc R . . H8C H 0.9598 0.3770 0.2221 0.047 Uiso 1 1 calc R . . C9 C 0.6695(4) 0.4576(4) 0.0936(3) 0.0374(9) Uani 1 1 d . . . H9A H 0.6190 0.5218 0.0371 0.045 Uiso 1 1 calc R . . H9B H 0.5997 0.4049 0.1485 0.045 Uiso 1 1 calc R . . H9C H 0.7280 0.3987 0.0568 0.045 Uiso 1 1 calc R . . C10 C 0.9137(4) 0.6550(4) 0.0603(3) 0.0387(10) Uani 1 1 d . . . H10C H 0.9716 0.5998 0.0194 0.046 Uiso 1 1 calc R . . H10B H 0.9766 0.7014 0.0985 0.046 Uiso 1 1 calc R . . H10A H 0.8593 0.7202 0.0074 0.046 Uiso 1 1 calc R . . C11 C 0.7280(4) 0.7449(4) 0.6788(3) 0.0360(9) Uani 1 1 d U . . C12 C 0.5474(4) 0.6832(3) 0.5196(3) 0.0264(8) Uani 1 1 d . . . C13 C 0.8201(3) 0.5585(4) 0.5452(3) 0.0242(7) Uani 1 1 d U . . C14 C 0.9568(4) 0.8161(4) 0.5082(3) 0.0295(8) Uani 1 1 d . . . C15 C 0.6805(4) 0.9438(4) 0.4717(3) 0.0278(8) Uani 1 1 d . . . O1 O 0.8075(2) 0.8813(2) 0.21451(19) 0.0262(5) Uani 1 1 d . . . O2 O 0.7186(4) 0.7386(3) 0.7732(2) 0.0600(9) Uani 1 1 d . . . O3 O 0.4345(3) 0.6430(3) 0.5258(2) 0.0401(7) Uani 1 1 d . . . O4 O 0.8570(3) 0.4503(3) 0.5615(2) 0.0328(6) Uani 1 1 d . . . O5 O 1.0710(3) 0.8526(3) 0.5052(3) 0.0490(8) Uani 1 1 d . . . O6 O 0.6425(3) 1.0514(3) 0.4452(3) 0.0404(7) Uani 1 1 d . . . P P 0.79519(9) 0.74538(9) 0.31317(7) 0.02037(18) Uani 1 1 d D . . H11 H 0.9325(15) 0.687(3) 0.297(3) 0.024 Uiso 1 1 d D . . Si1 Si 0.52345(10) 0.75236(10) 0.17894(8) 0.0250(2) Uani 1 1 d . . . Si2 Si 0.78699(10) 0.54759(10) 0.16634(8) 0.0250(2) Uani 1 1 d . . . W W 0.751584(14) 0.750886(13) 0.513396(11) 0.02235(6) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(2) 0.027(2) 0.036(2) -0.0136(16) 0.0059(16) -0.0114(17) C2 0.038(3) 0.048(3) 0.072(3) -0.019(2) 0.012(2) -0.019(2) C3 0.061(3) 0.024(2) 0.054(3) -0.0024(19) 0.001(2) -0.009(2) C4 0.0235(17) 0.0173(17) 0.0198(16) -0.0044(13) -0.0023(13) -0.0018(14) C5 0.029(2) 0.056(3) 0.040(2) -0.015(2) -0.0054(17) -0.0037(19) C6 0.029(2) 0.040(2) 0.033(2) -0.0099(17) -0.0069(16) 0.0121(18) C7 0.040(2) 0.034(2) 0.0286(19) -0.0030(17) -0.0068(16) 0.0096(18) C8 0.047(2) 0.034(2) 0.045(2) -0.0190(19) -0.0219(19) 0.0159(19) C9 0.045(2) 0.032(2) 0.041(2) -0.0193(18) -0.0178(19) 0.0065(18) C10 0.039(2) 0.041(2) 0.040(2) -0.0183(19) 0.0054(18) 0.0032(19) C11 0.048(2) 0.033(2) 0.0308(16) -0.0146(17) -0.0026(17) -0.0048(19) C12 0.030(2) 0.0218(19) 0.0274(18) -0.0048(15) -0.0023(15) 0.0009(16) C13 0.0193(17) 0.0273(16) 0.0251(17) -0.0039(15) -0.0031(13) -0.0033(14) C14 0.031(2) 0.025(2) 0.035(2) -0.0072(16) -0.0119(16) -0.0015(16) C15 0.0178(17) 0.027(2) 0.041(2) -0.0142(17) 0.0032(15) -0.0039(15) O1 0.0300(13) 0.0196(13) 0.0290(13) -0.0050(10) -0.0024(10) -0.0047(10) O2 0.086(2) 0.069(2) 0.0299(16) -0.0219(16) 0.0013(16) -0.0080(19) O3 0.0270(15) 0.0369(17) 0.0535(18) -0.0047(13) -0.0018(12) -0.0078(13) O4 0.0298(14) 0.0259(15) 0.0409(15) -0.0045(12) -0.0029(11) 0.0022(12) O5 0.0323(16) 0.0351(17) 0.079(2) -0.0049(15) -0.0236(15) -0.0068(13) O6 0.0270(14) 0.0265(16) 0.069(2) -0.0144(14) 0.0016(13) 0.0011(12) P 0.0210(4) 0.0192(5) 0.0218(4) -0.0062(3) -0.0026(3) -0.0006(4) Si1 0.0234(5) 0.0290(6) 0.0227(5) -0.0060(4) -0.0054(4) 0.0036(4) Si2 0.0294(5) 0.0231(5) 0.0253(5) -0.0100(4) -0.0088(4) 0.0045(4) W 0.02278(8) 0.02293(9) 0.02313(8) -0.00825(6) -0.00377(5) -0.00113(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.452(4) . ? C1 C2 1.502(5) . ? C1 C3 1.505(5) . ? C1 H1A 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3C 0.9800 . ? C3 H3B 0.9800 . ? C3 H3A 0.9800 . ? C4 P 1.810(3) . ? C4 Si2 1.898(3) . ? C4 Si1 1.910(3) . ? C4 H4A 1.0000 . ? C5 Si1 1.864(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si1 1.869(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si1 1.874(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si2 1.868(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si2 1.863(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si2 1.871(4) . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C11 O2 1.145(4) . ? C11 W 2.016(4) . ? C12 O3 1.137(4) . ? C12 W 2.044(4) . ? C13 O4 1.142(4) . ? C13 W 2.038(4) . ? C14 O5 1.138(4) . ? C14 W 2.045(4) . ? C15 O6 1.142(4) . ? C15 W 2.052(4) . ? O1 P 1.626(2) . ? P W 2.4816(8) . ? P H11 1.43(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 O1 C1 C2 110.3(3) . . ? O1 C1 C3 105.8(3) . . ? C2 C1 C3 112.8(3) . . ? O1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? C3 C1 H1A 109.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3C 109.5 . . ? C1 C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? C1 C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? P C4 Si2 110.50(16) . . ? P C4 Si1 114.09(17) . . ? Si2 C4 Si1 116.61(16) . . ? P C4 H4A 104.8 . . ? Si2 C4 H4A 104.8 . . ? Si1 C4 H4A 104.8 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10C 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? Si2 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O2 C11 W 177.6(4) . . ? O3 C12 W 178.0(3) . . ? O4 C13 W 178.7(3) . . ? O5 C14 W 179.8(4) . . ? O6 C15 W 177.9(3) . . ? C1 O1 P 121.8(2) . . ? O1 P C4 99.70(13) . . ? O1 P W 121.33(9) . . ? C4 P W 120.11(11) . . ? O1 P H11 100.7(13) . . ? C4 P H11 102.9(13) . . ? W P H11 109.1(12) . . ? C5 Si1 C6 107.32(18) . . ? C5 Si1 C7 109.49(18) . . ? C6 Si1 C7 108.89(18) . . ? C5 Si1 C4 106.90(17) . . ? C6 Si1 C4 112.98(15) . . ? C7 Si1 C4 111.12(16) . . ? C9 Si2 C8 107.61(18) . . ? C9 Si2 C10 109.38(19) . . ? C8 Si2 C10 109.52(19) . . ? C9 Si2 C4 111.48(16) . . ? C8 Si2 C4 108.45(16) . . ? C10 Si2 C4 110.34(16) . . ? C11 W C13 91.44(15) . . ? C11 W C12 89.88(15) . . ? C13 W C12 88.19(13) . . ? C11 W C14 89.93(15) . . ? C13 W C14 91.05(13) . . ? C12 W C14 179.22(13) . . ? C11 W C15 91.89(15) . . ? C13 W C15 176.53(13) . . ? C12 W C15 90.85(13) . . ? C14 W C15 89.92(14) . . ? C11 W P 175.65(11) . . ? C13 W P 84.74(9) . . ? C12 W P 92.07(10) . . ? C14 W P 88.06(10) . . ? C15 W P 91.96(10) . . ? 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 C2 C1 O1 P 81.4(4) . . . . ? C3 C1 O1 P -156.3(3) . . . . ? C1 O1 P C4 -178.5(2) . . . . ? C1 O1 P W 47.1(3) . . . . ? Si2 C4 P O1 91.31(17) . . . . ? Si1 C4 P O1 -42.41(19) . . . . ? Si2 C4 P W -133.55(12) . . . . ? Si1 C4 P W 92.73(17) . . . . ? P C4 Si1 C5 -150.27(19) . . . . ? Si2 C4 Si1 C5 78.9(2) . . . . ? P C4 Si1 C6 -32.4(2) . . . . ? Si2 C4 Si1 C6 -163.22(19) . . . . ? P C4 Si1 C7 90.3(2) . . . . ? Si2 C4 Si1 C7 -40.5(2) . . . . ? P C4 Si2 C9 -176.51(18) . . . . ? Si1 C4 Si2 C9 -44.1(2) . . . . ? P C4 Si2 C8 65.2(2) . . . . ? Si1 C4 Si2 C8 -162.4(2) . . . . ? P C4 Si2 C10 -54.8(2) . . . . ? Si1 C4 Si2 C10 77.7(2) . . . . ? O2 C11 W C13 35(9) . . . . ? O2 C11 W C12 123(9) . . . . ? O2 C11 W C14 -56(9) . . . . ? O2 C11 W C15 -146(9) . . . . ? O2 C11 W P 6(10) . . . . ? O4 C13 W C11 139(14) . . . . ? O4 C13 W C12 49(14) . . . . ? O4 C13 W C14 -131(14) . . . . ? O4 C13 W C15 -25(15) . . . . ? O4 C13 W P -43(14) . . . . ? O3 C12 W C11 -42(10) . . . . ? O3 C12 W C13 49(10) . . . . ? O3 C12 W C14 34(17) . . . . ? O3 C12 W C15 -134(10) . . . . ? O3 C12 W P 134(10) . . . . ? O5 C14 W C11 -111(100) . . . . ? O5 C14 W C13 157(100) . . . . ? O5 C14 W C12 172(100) . . . . ? O5 C14 W C15 -19(100) . . . . ? O5 C14 W P 73(100) . . . . ? O6 C15 W C11 165(9) . . . . ? O6 C15 W C13 -31(10) . . . . ? O6 C15 W C12 -105(9) . . . . ? O6 C15 W C14 76(9) . . . . ? O6 C15 W P -12(9) . . . . ? O1 P W C11 -134.6(15) . . . . ? C4 P W C11 99.9(15) . . . . ? O1 P W C13 -163.24(14) . . . . ? C4 P W C13 71.24(15) . . . . ? O1 P W C12 108.76(14) . . . . ? C4 P W C12 -16.76(15) . . . . ? O1 P W C14 -72.01(14) . . . . ? C4 P W C14 162.47(16) . . . . ? O1 P W C15 17.85(14) . . . . ? C4 P W C15 -107.67(15) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.567 _refine_diff_density_min -1.779 _refine_diff_density_rms 0.173 _database_code_depnum_ccdc_archive 'CCDC 953766' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2493f _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H25 Mo O6 P Si2' _chemical_formula_sum 'C15 H25 Mo O6 P Si2' _chemical_formula_weight 484.44 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' Mo Mo -1.6832 0.6857 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.6435(7) _cell_length_b 9.4805(4) _cell_length_c 14.8822(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.9120(10) _cell_angle_gamma 90.00 _cell_volume 2246.69(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5130 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 29.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 0.9618 _exptl_absorpt_process_details 'SADABS (2009/2), Bruker AXS 2009' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8-KappaApexII' _diffrn_measurement_method '\f and \w CCD rotation images, thin slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13098 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5414 _reflns_number_gt 4625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5414 _refine_ls_number_parameters 235 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 C1 C 0.39435(13) 1.0769(2) 0.28363(16) 0.0230(5) Uani 1 1 d . . . H1A H 0.4198 0.9853 0.2754 0.028 Uiso 1 1 calc R . . H1B H 0.4353 1.1295 0.3342 0.028 Uiso 1 1 calc R . . C2 C 0.37539(15) 1.1588(3) 0.19465(18) 0.0280(5) Uani 1 1 d . . . H2A H 0.3525 1.2506 0.1942 0.034 Uiso 1 1 calc R . . C3 C 0.38815(16) 1.1128(3) 0.11673(18) 0.0382(6) Uani 1 1 d . . . H3A H 0.4110 1.0214 0.1147 0.046 Uiso 1 1 calc R . . H3B H 0.3745 1.1709 0.0624 0.046 Uiso 1 1 calc R . . C4 C 0.16752(12) 0.9526(2) 0.29746(14) 0.0159(4) Uani 1 1 d . . . H4A H 0.1440 0.8605 0.3108 0.019 Uiso 1 1 calc R . . C5 C 0.08516(15) 1.0148(2) 0.44786(16) 0.0269(5) Uani 1 1 d . . . H5A H 0.0859 0.9133 0.4604 0.032 Uiso 1 1 calc R . . H5B H 0.0334 1.0392 0.3990 0.032 Uiso 1 1 calc R . . H5C H 0.0875 1.0669 0.5055 0.032 Uiso 1 1 calc R . . C6 C 0.17993(15) 1.2560(2) 0.38186(17) 0.0268(5) Uani 1 1 d . . . H6A H 0.1285 1.2821 0.3331 0.032 Uiso 1 1 calc R . . H6B H 0.2288 1.2771 0.3600 0.032 Uiso 1 1 calc R . . H6C H 0.1837 1.3099 0.4391 0.032 Uiso 1 1 calc R . . C7 C 0.27396(14) 1.0209(3) 0.50557(15) 0.0270(5) Uani 1 1 d . . . H7A H 0.3240 1.0435 0.4864 0.032 Uiso 1 1 calc R . . H7B H 0.2743 0.9203 0.5209 0.032 Uiso 1 1 calc R . . H7C H 0.2740 1.0769 0.5609 0.032 Uiso 1 1 calc R . . C8 C 0.06681(15) 0.8636(2) 0.10031(16) 0.0272(5) Uani 1 1 d . . . H8A H 0.0431 0.7860 0.1279 0.033 Uiso 1 1 calc R . . H8B H 0.1188 0.8321 0.0882 0.033 Uiso 1 1 calc R . . H8C H 0.0263 0.8928 0.0412 0.033 Uiso 1 1 calc R . . C9 C 0.13636(15) 1.1642(2) 0.13209(17) 0.0259(5) Uani 1 1 d . . . H9A H 0.1867 1.1309 0.1171 0.031 Uiso 1 1 calc R . . H9B H 0.1515 1.2417 0.1775 0.031 Uiso 1 1 calc R . . H9C H 0.0951 1.1975 0.0747 0.031 Uiso 1 1 calc R . . C10 C -0.01099(14) 1.0775(3) 0.20142(18) 0.0306(5) Uani 1 1 d . . . H10C H -0.0513 1.0984 0.1403 0.037 Uiso 1 1 calc R . . H10B H -0.0010 1.1628 0.2403 0.037 Uiso 1 1 calc R . . H10A H -0.0338 1.0033 0.2329 0.037 Uiso 1 1 calc R . . C11 C 0.39408(15) 0.4920(2) 0.37227(17) 0.0274(5) Uani 1 1 d U . . C12 C 0.23409(14) 0.5805(2) 0.24226(16) 0.0225(4) Uani 1 1 d U . . C13 C 0.27340(15) 0.6570(2) 0.43317(17) 0.0251(5) Uani 1 1 d U . . C14 C 0.43226(14) 0.7851(2) 0.42545(16) 0.0225(4) Uani 1 1 d U . . C15 C 0.39020(14) 0.6957(2) 0.22634(16) 0.0228(4) Uani 1 1 d U . . O1 O 0.31783(9) 1.05286(15) 0.31021(11) 0.0205(3) Uani 1 1 d . . . O2 O 0.42876(13) 0.38797(19) 0.39436(14) 0.0434(5) Uani 1 1 d . . . O3 O 0.17685(11) 0.52806(19) 0.19236(13) 0.0351(4) Uani 1 1 d . . . O4 O 0.23762(12) 0.6421(2) 0.48666(13) 0.0379(4) Uani 1 1 d . . . O5 O 0.48539(11) 0.84626(18) 0.47539(13) 0.0332(4) Uani 1 1 d . . . O6 O 0.41792(11) 0.7074(2) 0.16570(13) 0.0340(4) Uani 1 1 d . . . Si1 Si 0.17781(4) 1.06264(6) 0.40745(4) 0.01828(13) Uani 1 1 d . . . Si2 Si 0.09020(4) 1.01618(6) 0.18379(4) 0.01840(13) Uani 1 1 d . . . P P 0.26650(3) 0.90676(5) 0.27721(4) 0.01608(12) Uani 1 1 d . . . H18 H 0.2516(13) 0.920(2) 0.1867(16) 0.019 Uiso 1 1 d . . . Mo Mo 0.334907(11) 0.677738(18) 0.332618(12) 0.01767(7) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0194(10) 0.0222(11) 0.0298(12) 0.0012(9) 0.0107(9) -0.0040(9) C2 0.0259(12) 0.0274(12) 0.0333(13) 0.0039(10) 0.0124(10) -0.0033(10) C3 0.0357(14) 0.0492(17) 0.0324(14) 0.0048(12) 0.0143(11) -0.0057(12) C4 0.0176(9) 0.0129(9) 0.0189(10) 0.0011(8) 0.0077(8) 0.0000(8) C5 0.0320(12) 0.0260(12) 0.0279(12) -0.0005(10) 0.0170(10) 0.0023(10) C6 0.0367(13) 0.0169(11) 0.0298(12) -0.0023(9) 0.0145(10) 0.0006(10) C7 0.0322(12) 0.0275(12) 0.0205(11) -0.0016(9) 0.0062(9) 0.0021(10) C8 0.0317(12) 0.0248(12) 0.0240(11) -0.0025(10) 0.0063(10) -0.0054(10) C9 0.0323(12) 0.0205(12) 0.0226(11) 0.0055(9) 0.0043(10) -0.0025(9) C10 0.0226(11) 0.0354(14) 0.0333(13) 0.0011(11) 0.0072(10) 0.0046(10) C11 0.0344(12) 0.0203(11) 0.0297(12) -0.0016(9) 0.0125(10) 0.0047(9) C12 0.0289(11) 0.0154(10) 0.0267(11) -0.0013(9) 0.0136(9) -0.0017(8) C13 0.0312(12) 0.0187(11) 0.0280(12) 0.0026(9) 0.0126(10) 0.0031(9) C14 0.0283(11) 0.0157(10) 0.0237(11) 0.0030(9) 0.0079(9) 0.0058(8) C15 0.0205(10) 0.0222(11) 0.0264(11) -0.0035(9) 0.0082(9) 0.0016(9) O1 0.0238(7) 0.0149(7) 0.0264(8) -0.0007(6) 0.0131(6) -0.0035(6) O2 0.0603(13) 0.0224(9) 0.0501(12) 0.0067(9) 0.0202(10) 0.0172(9) O3 0.0383(10) 0.0304(10) 0.0375(10) -0.0079(8) 0.0127(8) -0.0109(8) O4 0.0486(11) 0.0374(10) 0.0373(10) 0.0043(8) 0.0275(9) 0.0004(9) O5 0.0385(10) 0.0248(9) 0.0303(9) -0.0017(7) 0.0006(8) 0.0008(7) O6 0.0297(9) 0.0452(11) 0.0327(10) -0.0055(8) 0.0177(8) 0.0011(8) Si1 0.0240(3) 0.0145(3) 0.0187(3) -0.0007(2) 0.0100(2) 0.0013(2) Si2 0.0202(3) 0.0156(3) 0.0191(3) 0.0012(2) 0.0054(2) -0.0001(2) P 0.0196(3) 0.0130(2) 0.0179(3) 0.0006(2) 0.0090(2) 0.0005(2) Mo 0.02185(11) 0.01202(11) 0.02118(11) -0.00018(6) 0.00948(8) 0.00233(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.457(2) . ? C1 C2 1.487(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.313(4) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C3 H3B 0.9500 . ? C4 P 1.812(2) . ? C4 Si2 1.901(2) . ? C4 Si1 1.906(2) . ? C4 H4A 1.0000 . ? C5 Si1 1.867(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si1 1.875(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si1 1.868(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si2 1.873(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si2 1.869(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si2 1.871(2) . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C11 O2 1.142(3) . ? C11 Mo 2.020(2) . ? C12 O3 1.138(3) . ? C12 Mo 2.040(2) . ? C13 O4 1.133(3) . ? C13 Mo 2.053(2) . ? C14 O5 1.135(3) . ? C14 Mo 2.066(2) . ? C15 O6 1.132(3) . ? C15 Mo 2.055(2) . ? O1 P 1.6264(15) . ? P Mo 2.4788(6) . ? P H18 1.30(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 O1 C1 C2 110.35(18) . . ? O1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? O1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C3 C2 C1 124.5(2) . . ? C3 C2 H2A 117.8 . . ? C1 C2 H2A 117.8 . . ? C2 C3 H3A 120.0 . . ? C2 C3 H3B 120.0 . . ? H3A C3 H3B 120.0 . . ? P C4 Si2 109.93(10) . . ? P C4 Si1 114.53(10) . . ? Si2 C4 Si1 117.32(10) . . ? P C4 H4A 104.5 . . ? Si2 C4 H4A 104.5 . . ? Si1 C4 H4A 104.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10C 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? Si2 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O2 C11 Mo 178.8(2) . . ? O3 C12 Mo 178.6(2) . . ? O4 C13 Mo 177.5(2) . . ? O5 C14 Mo 178.7(2) . . ? O6 C15 Mo 177.5(2) . . ? C1 O1 P 118.37(13) . . ? C5 Si1 C7 107.26(11) . . ? C5 Si1 C6 111.65(10) . . ? C7 Si1 C6 107.67(11) . . ? C5 Si1 C4 105.52(10) . . ? C7 Si1 C4 113.43(10) . . ? C6 Si1 C4 111.29(10) . . ? C9 Si2 C10 108.60(11) . . ? C9 Si2 C8 109.75(11) . . ? C10 Si2 C8 108.13(11) . . ? C9 Si2 C4 110.57(10) . . ? C10 Si2 C4 112.19(10) . . ? C8 Si2 C4 107.55(10) . . ? O1 P C4 99.71(8) . . ? O1 P Mo 119.70(6) . . ? C4 P Mo 120.43(7) . . ? O1 P H18 99.0(10) . . ? C4 P H18 103.9(9) . . ? Mo P H18 111.0(10) . . ? C11 Mo C12 92.07(9) . . ? C11 Mo C13 90.45(9) . . ? C12 Mo C13 87.04(9) . . ? C11 Mo C15 90.44(9) . . ? C12 Mo C15 89.81(9) . . ? C13 Mo C15 176.76(9) . . ? C11 Mo C14 90.76(9) . . ? C12 Mo C14 176.66(8) . . ? C13 Mo C14 91.15(9) . . ? C15 Mo C14 91.96(9) . . ? C11 Mo P 176.80(7) . . ? C12 Mo P 88.09(6) . . ? C13 Mo P 92.75(6) . . ? C15 Mo P 86.36(6) . . ? C14 Mo P 89.19(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -118.6(3) . . . . ? C2 C1 O1 P 93.71(19) . . . . ? P C4 Si1 C5 -150.20(11) . . . . ? Si2 C4 Si1 C5 78.69(13) . . . . ? P C4 Si1 C7 -33.08(15) . . . . ? Si2 C4 Si1 C7 -164.18(11) . . . . ? P C4 Si1 C6 88.52(13) . . . . ? Si2 C4 Si1 C6 -42.58(14) . . . . ? P C4 Si2 C9 -54.54(14) . . . . ? Si1 C4 Si2 C9 78.65(14) . . . . ? P C4 Si2 C10 -175.94(11) . . . . ? Si1 C4 Si2 C10 -42.75(15) . . . . ? P C4 Si2 C8 65.28(13) . . . . ? Si1 C4 Si2 C8 -161.53(11) . . . . ? C1 O1 P C4 -164.60(15) . . . . ? C1 O1 P Mo 61.83(16) . . . . ? Si2 C4 P O1 96.27(11) . . . . ? Si1 C4 P O1 -38.32(12) . . . . ? Si2 C4 P Mo -130.61(7) . . . . ? Si1 C4 P Mo 94.80(10) . . . . ? O2 C11 Mo C12 129(11) . . . . ? O2 C11 Mo C13 -144(11) . . . . ? O2 C11 Mo C15 39(11) . . . . ? O2 C11 Mo C14 -53(11) . . . . ? O2 C11 Mo P 36(12) . . . . ? O3 C12 Mo C11 142(9) . . . . ? O3 C12 Mo C13 51(9) . . . . ? O3 C12 Mo C15 -128(9) . . . . ? O3 C12 Mo C14 -6(10) . . . . ? O3 C12 Mo P -42(9) . . . . ? O4 C13 Mo C11 -75(5) . . . . ? O4 C13 Mo C12 17(5) . . . . ? O4 C13 Mo C15 31(6) . . . . ? O4 C13 Mo C14 -166(5) . . . . ? O4 C13 Mo P 105(5) . . . . ? O6 C15 Mo C11 139(5) . . . . ? O6 C15 Mo C12 47(5) . . . . ? O6 C15 Mo C13 33(5) . . . . ? O6 C15 Mo C14 -130(5) . . . . ? O6 C15 Mo P -41(5) . . . . ? O5 C14 Mo C11 153(9) . . . . ? O5 C14 Mo C12 -60(10) . . . . ? O5 C14 Mo C13 -117(9) . . . . ? O5 C14 Mo C15 62(9) . . . . ? O5 C14 Mo P -24(9) . . . . ? O1 P Mo C11 -79.2(13) . . . . ? C4 P Mo C11 156.7(13) . . . . ? O1 P Mo C12 -171.97(9) . . . . ? C4 P Mo C12 63.95(10) . . . . ? O1 P Mo C13 101.09(9) . . . . ? C4 P Mo C13 -22.99(10) . . . . ? O1 P Mo C15 -82.03(9) . . . . ? C4 P Mo C15 153.89(10) . . . . ? O1 P Mo C14 9.98(9) . . . . ? C4 P Mo C14 -114.10(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.812 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 953771' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2494f _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H25 Cr O6 P Si2' _chemical_formula_sum 'C15 H25 Cr O6 P Si2' _chemical_formula_weight 440.50 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' Cr Cr 0.3209 0.6236 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.500(2) _cell_length_b 9.2871(12) _cell_length_c 14.7982(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.024(3) _cell_angle_gamma 90.00 _cell_volume 2168.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5450 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 29.47 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8667 _exptl_absorpt_correction_T_max 0.9854 _exptl_absorpt_process_details 'SADABS (2009/2), Bruker AXS 2009' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8-KappaApexII' _diffrn_measurement_method '\f and \w CCD rotation images, thin slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23154 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5218 _reflns_number_gt 3949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.5579P] 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 5218 _refine_ls_number_parameters 235 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 C1 C 0.60096(12) 1.0725(2) 0.21349(14) 0.0190(4) Uani 1 1 d . . . H1A H 0.5746 0.9795 0.2216 0.023 Uiso 1 1 calc R . . H1B H 0.5599 1.1270 0.1628 0.023 Uiso 1 1 calc R . . C2 C 0.62103(13) 1.1554(2) 0.30313(14) 0.0236(5) Uani 1 1 d . . . H2A H 0.6448 1.2488 0.3040 0.028 Uiso 1 1 calc R . . C3 C 0.60793(15) 1.1078(3) 0.38148(16) 0.0341(6) Uani 1 1 d . . . H3A H 0.5842 1.0149 0.3829 0.041 Uiso 1 1 calc R . . H3B H 0.6222 1.1663 0.4366 0.041 Uiso 1 1 calc R . . C4 C 0.82987(12) 0.9463(2) 0.20086(13) 0.0135(4) Uani 1 1 d . . . H4A H 0.8544 0.8529 0.1878 0.016 Uiso 1 1 calc R . . C5 C 0.91292(14) 1.0110(2) 0.05020(14) 0.0229(5) Uani 1 1 d . . . H5A H 0.9133 0.9068 0.0399 0.027 Uiso 1 1 calc R . . H5B H 0.9651 1.0393 0.0985 0.027 Uiso 1 1 calc R . . H5C H 0.9095 1.0613 -0.0090 0.027 Uiso 1 1 calc R . . C6 C 0.72258(14) 1.0190(2) -0.00897(14) 0.0240(5) Uani 1 1 d . . . H6A H 0.6720 1.0400 0.0106 0.029 Uiso 1 1 calc R . . H6B H 0.7226 0.9171 -0.0260 0.029 Uiso 1 1 calc R . . H6C H 0.7223 1.0786 -0.0637 0.029 Uiso 1 1 calc R . . C7 C 0.81769(14) 1.2556(2) 0.11706(15) 0.0237(5) Uani 1 1 d . . . H7A H 0.8709 1.2826 0.1641 0.028 Uiso 1 1 calc R . . H7B H 0.7701 1.2760 0.1421 0.028 Uiso 1 1 calc R . . H7C H 0.8111 1.3111 0.0590 0.028 Uiso 1 1 calc R . . C8 C 0.93105(14) 0.8591(2) 0.40009(14) 0.0223(5) Uani 1 1 d . . . H8A H 0.9537 0.7786 0.3721 0.027 Uiso 1 1 calc R . . H8B H 0.8791 0.8287 0.4140 0.027 Uiso 1 1 calc R . . H8C H 0.9731 0.8893 0.4587 0.027 Uiso 1 1 calc R . . C9 C 1.00875(13) 1.0757(3) 0.29806(15) 0.0266(5) Uani 1 1 d . . . H9A H 0.9985 1.1620 0.2582 0.032 Uiso 1 1 calc R . . H9B H 1.0323 0.9996 0.2674 0.032 Uiso 1 1 calc R . . H9C H 1.0490 1.0985 0.3596 0.032 Uiso 1 1 calc R . . C10 C 0.85962(14) 1.1630(2) 0.36650(14) 0.0238(5) Uani 1 1 d . . . H10C H 0.9002 1.1949 0.4257 0.029 Uiso 1 1 calc R . . H10B H 0.8076 1.1295 0.3790 0.029 Uiso 1 1 calc R . . H10A H 0.8462 1.2434 0.3217 0.029 Uiso 1 1 calc R . . C11 C 0.61203(14) 0.5014(2) 0.12987(15) 0.0232(5) Uani 1 1 d U . . C12 C 0.72494(13) 0.6594(2) 0.07416(14) 0.0207(4) Uani 1 1 d U . . C13 C 0.57620(13) 0.7780(2) 0.07783(14) 0.0195(4) Uani 1 1 d U . . C14 C 0.61308(13) 0.6941(2) 0.26348(14) 0.0192(4) Uani 1 1 d U . . C15 C 0.76016(14) 0.5884(2) 0.25226(14) 0.0201(4) Uani 1 1 d U . . O1 O 0.67755(8) 1.04599(15) 0.18647(9) 0.0174(3) Uani 1 1 d . . . O2 O 0.57850(11) 0.39344(18) 0.10813(12) 0.0362(4) Uani 1 1 d U . . O3 O 0.76146(10) 0.64320(18) 0.02052(11) 0.0327(4) Uani 1 1 d U . . O4 O 0.52322(10) 0.83969(16) 0.02533(10) 0.0298(4) Uani 1 1 d U . . O5 O 0.58388(9) 0.70489(18) 0.32415(10) 0.0283(4) Uani 1 1 d U . . O6 O 0.81813(10) 0.53487(17) 0.30313(11) 0.0287(4) Uani 1 1 d U . . Si1 Si 0.81951(4) 1.05974(6) 0.09050(4) 0.01569(13) Uani 1 1 d . . . Si2 Si 0.90684(3) 1.01306(6) 0.31526(4) 0.01581(13) Uani 1 1 d . . . P P 0.72998(3) 0.89784(5) 0.21991(3) 0.01335(12) Uani 1 1 d . . . H11 H 0.7463(12) 0.905(2) 0.3118(13) 0.016 Uiso 1 1 d . . . Cr Cr 0.66616(2) 0.67794(3) 0.16629(2) 0.01560(9) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0152(10) 0.0193(11) 0.0236(10) -0.0006(9) 0.0071(8) 0.0031(8) C2 0.0185(11) 0.0251(12) 0.0271(11) -0.0045(9) 0.0063(9) 0.0033(9) C3 0.0296(13) 0.0475(16) 0.0260(12) -0.0034(11) 0.0095(10) 0.0060(12) C4 0.0126(9) 0.0120(10) 0.0163(9) -0.0014(8) 0.0048(8) 0.0006(8) C5 0.0285(12) 0.0222(12) 0.0220(10) -0.0004(9) 0.0138(9) -0.0021(10) C6 0.0286(12) 0.0254(12) 0.0170(10) 0.0038(9) 0.0047(9) -0.0007(10) C7 0.0308(12) 0.0178(11) 0.0243(10) 0.0027(9) 0.0111(9) 0.0008(10) C8 0.0243(12) 0.0212(12) 0.0188(10) 0.0017(9) 0.0021(9) 0.0030(9) C9 0.0191(11) 0.0317(13) 0.0274(11) 0.0000(10) 0.0044(9) -0.0054(10) C10 0.0268(12) 0.0210(12) 0.0208(10) -0.0050(9) 0.0023(9) 0.0011(10) C11 0.0269(12) 0.0187(10) 0.0250(11) 0.0012(9) 0.0090(9) -0.0027(9) C12 0.0246(12) 0.0145(11) 0.0221(10) -0.0029(9) 0.0051(8) -0.0035(9) C13 0.0215(11) 0.0158(11) 0.0209(10) -0.0036(8) 0.0057(8) -0.0064(8) C14 0.0150(10) 0.0180(11) 0.0234(10) 0.0043(8) 0.0037(8) -0.0025(8) C15 0.0263(11) 0.0140(11) 0.0223(10) 0.0003(8) 0.0107(8) -0.0007(8) O1 0.0179(7) 0.0149(7) 0.0212(7) 0.0014(6) 0.0086(6) 0.0031(6) O2 0.0467(11) 0.0199(9) 0.0429(10) -0.0041(7) 0.0144(8) -0.0134(8) O3 0.0417(10) 0.0312(10) 0.0319(9) -0.0036(7) 0.0213(8) -0.0003(8) O4 0.0311(9) 0.0242(9) 0.0277(8) 0.0017(7) -0.0013(7) -0.0006(7) O5 0.0241(8) 0.0375(10) 0.0259(8) 0.0051(7) 0.0115(7) -0.0007(7) O6 0.0300(9) 0.0250(9) 0.0301(8) 0.0062(7) 0.0073(7) 0.0075(7) Si1 0.0203(3) 0.0133(3) 0.0147(2) 0.0005(2) 0.0069(2) -0.0011(2) Si2 0.0157(3) 0.0146(3) 0.0158(3) -0.0011(2) 0.0027(2) -0.0002(2) P 0.0153(3) 0.0123(3) 0.0130(2) 0.00008(19) 0.00498(19) -0.0002(2) Cr 0.01804(18) 0.01170(17) 0.01743(16) 0.00045(13) 0.00575(13) -0.00221(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.454(2) . ? C1 C2 1.485(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.317(3) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C3 H3B 0.9500 . ? C4 P 1.8084(19) . ? C4 Si2 1.8985(19) . ? C4 Si1 1.9087(19) . ? C4 H4A 1.0000 . ? C5 Si1 1.864(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si1 1.868(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si1 1.863(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 Si2 1.867(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 Si2 1.866(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 Si2 1.862(2) . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C11 O2 1.145(3) . ? C11 Cr 1.869(2) . ? C12 O3 1.138(2) . ? C12 Cr 1.898(2) . ? C13 O4 1.139(2) . ? C13 Cr 1.909(2) . ? C14 O5 1.141(2) . ? C14 Cr 1.896(2) . ? C15 O6 1.143(2) . ? C15 Cr 1.887(2) . ? O1 P 1.6234(14) . ? P Cr 2.3281(6) . ? P H11 1.308(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 110.42(16) . . ? O1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? O1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C3 C2 C1 124.1(2) . . ? C3 C2 H2A 117.9 . . ? C1 C2 H2A 117.9 . . ? C2 C3 H3A 120.0 . . ? C2 C3 H3B 120.0 . . ? H3A C3 H3B 120.0 . . ? P C4 Si2 110.15(10) . . ? P C4 Si1 114.42(10) . . ? Si2 C4 Si1 116.85(10) . . ? P C4 H4A 104.7 . . ? Si2 C4 H4A 104.7 . . ? Si1 C4 H4A 104.7 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10C 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? Si2 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O2 C11 Cr 179.4(2) . . ? O3 C12 Cr 177.30(19) . . ? O4 C13 Cr 178.95(19) . . ? O5 C14 Cr 177.57(18) . . ? O6 C15 Cr 178.57(19) . . ? C1 O1 P 119.21(12) . . ? C7 Si1 C5 111.75(10) . . ? C7 Si1 C6 107.52(10) . . ? C5 Si1 C6 107.23(10) . . ? C7 Si1 C4 111.18(9) . . ? C5 Si1 C4 105.33(9) . . ? C6 Si1 C4 113.83(9) . . ? C10 Si2 C9 108.89(11) . . ? C10 Si2 C8 109.35(10) . . ? C9 Si2 C8 107.85(10) . . ? C10 Si2 C4 110.91(9) . . ? C9 Si2 C4 111.99(9) . . ? C8 Si2 C4 107.77(9) . . ? O1 P C4 99.80(8) . . ? O1 P Cr 119.48(5) . . ? C4 P Cr 120.47(7) . . ? O1 P H11 101.8(9) . . ? C4 P H11 103.3(9) . . ? Cr P H11 109.4(9) . . ? C11 Cr C15 92.13(9) . . ? C11 Cr C14 90.01(9) . . ? C15 Cr C14 89.68(9) . . ? C11 Cr C12 90.84(9) . . ? C15 Cr C12 87.26(9) . . ? C14 Cr C12 176.86(9) . . ? C11 Cr C13 91.11(9) . . ? C15 Cr C13 176.13(9) . . ? C14 Cr C13 92.43(9) . . ? C12 Cr C13 90.57(9) . . ? C11 Cr P 176.29(7) . . ? C15 Cr P 87.49(6) . . ? C14 Cr P 86.30(6) . . ? C12 Cr P 92.83(6) . . ? C13 Cr P 89.42(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -118.5(2) . . . . ? C2 C1 O1 P 92.64(18) . . . . ? P C4 Si1 C7 89.26(12) . . . . ? Si2 C4 Si1 C7 -41.58(14) . . . . ? P C4 Si1 C5 -149.53(11) . . . . ? Si2 C4 Si1 C5 79.64(12) . . . . ? P C4 Si1 C6 -32.35(14) . . . . ? Si2 C4 Si1 C6 -163.18(11) . . . . ? P C4 Si2 C10 -54.48(13) . . . . ? Si1 C4 Si2 C10 78.31(13) . . . . ? P C4 Si2 C9 -176.35(10) . . . . ? Si1 C4 Si2 C9 -43.56(14) . . . . ? P C4 Si2 C8 65.19(12) . . . . ? Si1 C4 Si2 C8 -162.02(11) . . . . ? C1 O1 P C4 -163.13(13) . . . . ? C1 O1 P Cr 63.34(14) . . . . ? Si2 C4 P O1 95.83(10) . . . . ? Si1 C4 P O1 -38.19(11) . . . . ? Si2 C4 P Cr -131.24(7) . . . . ? Si1 C4 P Cr 94.73(10) . . . . ? O2 C11 Cr C15 93(27) . . . . ? O2 C11 Cr C14 4(27) . . . . ? O2 C11 Cr C12 -179(100) . . . . ? O2 C11 Cr C13 -89(27) . . . . ? O2 C11 Cr P 9(28) . . . . ? O6 C15 Cr C11 109(8) . . . . ? O6 C15 Cr C14 -161(8) . . . . ? O6 C15 Cr C12 18(8) . . . . ? O6 C15 Cr C13 -38(8) . . . . ? O6 C15 Cr P -75(8) . . . . ? O5 C14 Cr C11 131(4) . . . . ? O5 C14 Cr C15 38(4) . . . . ? O5 C14 Cr C12 25(6) . . . . ? O5 C14 Cr C13 -138(4) . . . . ? O5 C14 Cr P -49(4) . . . . ? O3 C12 Cr C11 -57(4) . . . . ? O3 C12 Cr C15 35(4) . . . . ? O3 C12 Cr C14 48(5) . . . . ? O3 C12 Cr C13 -148(4) . . . . ? O3 C12 Cr P 122(4) . . . . ? O4 C13 Cr C11 -172(100) . . . . ? O4 C13 Cr C15 -25(11) . . . . ? O4 C13 Cr C14 98(11) . . . . ? O4 C13 Cr C12 -81(11) . . . . ? O4 C13 Cr P 12(11) . . . . ? O1 P Cr C11 -87.3(11) . . . . ? C4 P Cr C11 148.7(11) . . . . ? O1 P Cr C15 -171.42(9) . . . . ? C4 P Cr C15 64.56(10) . . . . ? O1 P Cr C14 -81.58(8) . . . . ? C4 P Cr C14 154.41(9) . . . . ? O1 P Cr C12 101.45(9) . . . . ? C4 P Cr C12 -22.57(10) . . . . ? O1 P Cr C13 10.90(9) . . . . ? C4 P Cr C13 -113.11(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.403 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 953772' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_GSTR296 _vrf_REFLT02_GSTR296 ; PROBLEM: The number of reflections greater than the sigma threshold cannot exceed the number of symmetry-independent reflections RESPONSE: The data set was collected from a non-merohedrally twinned crystal. The data set could be detwinned and was refined against the HKLF5-File. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H34 Li O11 P W' _chemical_formula_sum 'C33 H34 Li O11 P W' _chemical_formula_weight 828.36 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' Li Li -0.0003 0.0001 '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' W W -0.8490 6.8722 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.5214(5) _cell_length_b 15.6233(5) _cell_length_c 21.1388(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.504(4) _cell_angle_gamma 90.00 _cell_volume 3378.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9034 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 28.36 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 3.524 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.6199 _exptl_absorpt_correction_T_max 0.8164 _exptl_absorpt_process_details 'STOE XRed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 360 frames, detector distance = 100 mm ; _diffrn_reflns_number 63603 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1392 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6625 _reflns_number_gt 23299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0877P)^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_number_reflns 42056 _refine_ls_number_parameters 535 _refine_ls_number_restraints 248 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.848 _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 C1 C 0.2243(4) 0.2992(3) 0.4427(2) 0.0303(10) Uani 1 1 d . A . C2 C 0.1444(5) 0.2611(3) 0.4883(2) 0.0350(10) Uani 1 1 d . . . C3 C 0.0294(5) 0.2162(3) 0.4657(3) 0.0418(12) Uani 1 1 d . . . H3A H -0.0010 0.2070 0.4202 0.050 Uiso 1 1 calc R . . C4 C -0.0420(6) 0.1847(4) 0.5075(3) 0.0524(14) Uani 1 1 d . . . H4A H -0.1204 0.1536 0.4911 0.063 Uiso 1 1 calc R . . C5 C 0.0012(6) 0.1985(4) 0.5735(3) 0.0571(16) Uani 1 1 d . . . H5A H -0.0470 0.1761 0.6025 0.068 Uiso 1 1 calc R . . C6 C 0.1127(6) 0.2441(4) 0.5972(3) 0.0550(15) Uani 1 1 d . . . H6A H 0.1413 0.2544 0.6426 0.066 Uiso 1 1 calc R . . C7 C 0.1842(5) 0.2753(4) 0.5546(2) 0.0446(12) Uani 1 1 d . . . H7A H 0.2618 0.3070 0.5713 0.053 Uiso 1 1 calc R . . C8 C 0.3701(5) 0.3024(3) 0.4772(2) 0.0315(10) Uani 1 1 d . . . C9 C 0.4392(5) 0.2272(3) 0.4924(2) 0.0371(11) Uani 1 1 d . . . H9A H 0.3938 0.1745 0.4823 0.044 Uiso 1 1 calc R . . C10 C 0.5710(5) 0.2247(4) 0.5214(2) 0.0434(13) Uani 1 1 d . . . H10A H 0.6149 0.1714 0.5304 0.052 Uiso 1 1 calc R . . C11 C 0.6377(5) 0.2999(4) 0.5370(3) 0.0542(15) Uani 1 1 d . . . H11A H 0.7292 0.2996 0.5553 0.065 Uiso 1 1 calc R . . C12 C 0.5710(7) 0.3747(4) 0.5259(3) 0.0660(19) Uani 1 1 d . . . H12A H 0.6154 0.4269 0.5394 0.079 Uiso 1 1 calc R . . C13 C 0.4383(6) 0.3765(3) 0.4952(3) 0.0555(16) Uani 1 1 d . . . H13A H 0.3946 0.4299 0.4867 0.067 Uiso 1 1 calc R . . C14 C 0.1697(4) 0.3879(3) 0.4181(2) 0.0324(10) Uani 1 1 d . . . C15 C 0.0626(5) 0.4242(4) 0.4339(3) 0.0470(13) Uani 1 1 d . . . H15A H 0.0193 0.3938 0.4617 0.056 Uiso 1 1 calc R . . C16 C 0.0153(6) 0.5042(4) 0.4105(3) 0.0556(15) Uani 1 1 d . . . H16A H -0.0577 0.5283 0.4234 0.067 Uiso 1 1 calc R . . C17 C 0.0737(5) 0.5483(3) 0.3689(3) 0.0510(14) Uani 1 1 d . . . H17A H 0.0405 0.6023 0.3521 0.061 Uiso 1 1 calc R . . C18 C 0.1800(6) 0.5137(3) 0.3521(3) 0.0455(13) Uani 1 1 d . . . H18A H 0.2204 0.5434 0.3228 0.055 Uiso 1 1 calc R . . C19 C 0.2292(5) 0.4358(3) 0.3774(2) 0.0398(10) Uani 1 1 d . . . H19A H 0.3060 0.4141 0.3667 0.048 Uiso 1 1 calc R . . C20 C 0.0340(6) 0.3104(4) 0.2723(3) 0.0572(16) Uani 1 1 d . . . H20A H 0.1134 0.3221 0.2570 0.069 Uiso 1 1 calc R . . H20B H 0.0011 0.3639 0.2866 0.069 Uiso 1 1 calc R . . H20C H -0.0327 0.2856 0.2367 0.069 Uiso 1 1 calc R . . C29 C 0.2253(4) -0.0636(4) 0.3518(2) 0.0393(10) Uani 1 1 d . . . C30 C 0.2211(5) 0.0844(3) 0.2733(3) 0.0377(11) Uani 1 1 d . . . C31 C 0.0167(5) 0.0599(4) 0.3421(2) 0.0452(12) Uani 1 1 d . . . C32 C 0.2136(5) 0.0432(3) 0.4627(3) 0.0421(12) Uani 1 1 d . . . C33 C 0.4175(5) 0.0659(4) 0.3916(2) 0.0433(11) Uani 1 1 d . . . Li Li 0.4431(8) 0.2981(5) 0.2977(4) 0.0387(18) Uani 1 1 d . . . O1 O 0.0630(3) 0.2523(2) 0.32469(15) 0.0400(8) Uani 1 1 d . A . O2 O 0.3070(3) 0.2652(2) 0.33085(15) 0.0347(7) Uani 1 1 d . A . O7 O 0.2308(3) -0.1356(2) 0.34104(17) 0.0427(8) Uani 1 1 d . . . O8 O 0.2245(4) 0.0961(2) 0.22020(17) 0.0500(9) Uani 1 1 d . . . O9 O -0.0940(3) 0.0582(3) 0.3279(2) 0.0605(10) Uani 1 1 d . . . O10 O 0.2130(4) 0.0305(3) 0.5157(2) 0.0595(11) Uani 1 1 d . . . O11 O 0.5278(3) 0.0653(3) 0.40334(19) 0.0578(10) Uani 1 1 d . . . P P 0.21017(13) 0.22759(7) 0.36546(7) 0.0313(2) Uani 1 1 d . . . W W 0.216734(19) 0.062488(13) 0.367266(10) 0.03327(6) Uani 1 1 d . A . O3 O 0.5883(6) 0.2126(4) 0.2930(3) 0.0402(16) Uani 0.574(7) 1 d PU A 1 O4 O 0.5943(7) 0.3640(5) 0.3557(3) 0.0534(19) Uani 0.574(7) 1 d PU A 1 C22 C 0.7179(14) 0.3251(9) 0.3558(6) 0.060(3) Uani 0.574(7) 1 d PU A 1 H22A H 0.7824 0.3384 0.3968 0.072 Uiso 0.574(7) 1 calc PR A 1 H22B H 0.7519 0.3468 0.3189 0.072 Uiso 0.574(7) 1 calc PR A 1 O5 O 0.4076(7) 0.4314(4) 0.2593(4) 0.0481(17) Uani 0.574(7) 1 d PU A 1 C24 C 0.5271(11) 0.4741(7) 0.2734(6) 0.049(2) Uani 0.574(7) 1 d PDU A 1 H24A H 0.5144 0.5362 0.2649 0.059 Uiso 0.574(7) 1 calc PR A 1 H24B H 0.5854 0.4515 0.2467 0.059 Uiso 0.574(7) 1 calc PR A 1 C25 C 0.3655(15) 0.4293(14) 0.1960(10) 0.053(3) Uani 0.574(7) 1 d PDU A 1 H25A H 0.3849 0.4854 0.1786 0.064 Uiso 0.574(7) 1 calc PR A 1 H25B H 0.2692 0.4232 0.1859 0.064 Uiso 0.574(7) 1 calc PR A 1 C26 C 0.4193(9) 0.3604(7) 0.1594(4) 0.045(2) Uani 0.574(7) 1 d PDU A 1 H26A H 0.3660 0.3554 0.1143 0.054 Uiso 0.574(7) 1 calc PR A 1 H26B H 0.5107 0.3732 0.1580 0.054 Uiso 0.574(7) 1 calc PR A 1 O6 O 0.4126(7) 0.2838(5) 0.1947(3) 0.0436(17) Uani 0.574(7) 1 d PDU A 1 C28 C 0.6248(11) 0.2183(7) 0.2325(5) 0.044(2) Uani 0.574(7) 1 d PU A 1 H28A H 0.6817 0.1702 0.2262 0.052 Uiso 0.574(7) 1 calc PR A 1 H28B H 0.6685 0.2733 0.2278 0.052 Uiso 0.574(7) 1 calc PR A 1 C21 C 0.6955(14) 0.2327(11) 0.3496(6) 0.049(3) Uani 0.574(7) 1 d PU A 1 H21A H 0.6734 0.2106 0.3896 0.059 Uiso 0.574(7) 1 calc PR A 1 H21B H 0.7765 0.2039 0.3448 0.059 Uiso 0.574(7) 1 calc PR A 1 C23 C 0.5839(15) 0.4572(9) 0.3454(8) 0.051(3) Uani 0.574(7) 1 d PU A 1 H23A H 0.6714 0.4839 0.3591 0.061 Uiso 0.574(7) 1 calc PR A 1 H23B H 0.5266 0.4822 0.3715 0.061 Uiso 0.574(7) 1 calc PR A 1 C27 C 0.4752(15) 0.2120(11) 0.1816(11) 0.041(3) Uani 0.574(7) 1 d PDU A 1 H27A H 0.4818 0.2112 0.1357 0.049 Uiso 0.574(7) 1 calc PR A 1 H27B H 0.4287 0.1598 0.1904 0.049 Uiso 0.574(7) 1 calc PR A 1 O5S O 0.4883(9) 0.4352(6) 0.3131(4) 0.048(2) Uani 0.426(7) 1 d PU A 2 C26S C 0.4517(13) 0.3050(9) 0.1666(7) 0.040(3) Uani 0.426(7) 1 d PU A 2 H26C H 0.5260 0.3443 0.1675 0.048 Uiso 0.426(7) 1 calc PR A 2 H26D H 0.3969 0.3049 0.1217 0.048 Uiso 0.426(7) 1 calc PR A 2 O6S O 0.3764(8) 0.3379(6) 0.2087(4) 0.041(2) Uani 0.426(7) 1 d PU A 2 C28S C 0.6727(14) 0.2092(9) 0.2648(7) 0.045(3) Uani 0.426(7) 1 d PU A 2 H28C H 0.7129 0.1561 0.2531 0.054 Uiso 0.426(7) 1 calc PR A 2 H28D H 0.6994 0.2573 0.2403 0.054 Uiso 0.426(7) 1 calc PR A 2 O3S O 0.5312(8) 0.2011(5) 0.2483(4) 0.033(2) Uani 0.426(7) 1 d PU A 2 O4S O 0.6420(10) 0.2962(7) 0.3531(4) 0.048(2) Uani 0.426(7) 1 d PU A 2 C22S C 0.7035(16) 0.3766(10) 0.3485(7) 0.056(3) Uani 0.426(7) 1 d PU A 2 H22C H 0.7205 0.3839 0.3047 0.067 Uiso 0.426(7) 1 calc PR A 2 H22D H 0.7878 0.3802 0.3812 0.067 Uiso 0.426(7) 1 calc PR A 2 C25S C 0.343(2) 0.4269(19) 0.1987(14) 0.046(4) Uani 0.426(7) 1 d PU A 2 H25C H 0.2607 0.4410 0.2114 0.056 Uiso 0.426(7) 1 calc PR A 2 H25D H 0.3366 0.4448 0.1531 0.056 Uiso 0.426(7) 1 calc PR A 2 C24S C 0.4700(18) 0.4687(12) 0.2483(8) 0.050(3) Uani 0.426(7) 1 d PU A 2 H24C H 0.5491 0.4568 0.2320 0.060 Uiso 0.426(7) 1 calc PR A 2 H24D H 0.4589 0.5315 0.2495 0.060 Uiso 0.426(7) 1 calc PR A 2 C21S C 0.715(2) 0.2244(15) 0.3321(9) 0.048(4) Uani 0.426(7) 1 d PU A 2 H21C H 0.8097 0.2381 0.3428 0.057 Uiso 0.426(7) 1 calc PR A 2 H21D H 0.7027 0.1719 0.3562 0.057 Uiso 0.426(7) 1 calc PR A 2 C23S C 0.6152(19) 0.4413(16) 0.3605(10) 0.051(4) Uani 0.426(7) 1 d PU A 2 H23C H 0.6537 0.4985 0.3574 0.061 Uiso 0.426(7) 1 calc PR A 2 H23D H 0.6019 0.4345 0.4050 0.061 Uiso 0.426(7) 1 calc PR A 2 C27S C 0.503(2) 0.2191(15) 0.1821(14) 0.039(4) Uani 0.426(7) 1 d PU A 2 H27C H 0.4387 0.1770 0.1588 0.047 Uiso 0.426(7) 1 calc PR A 2 H27D H 0.5840 0.2124 0.1661 0.047 Uiso 0.426(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(2) 0.034(3) 0.029(2) -0.0003(19) 0.0094(18) 0.0031(19) C2 0.031(2) 0.040(3) 0.035(2) 0.004(2) 0.0103(19) 0.006(2) C3 0.031(3) 0.052(3) 0.046(3) -0.002(2) 0.017(2) 0.004(2) C4 0.038(3) 0.060(4) 0.065(4) 0.006(3) 0.024(3) 0.004(3) C5 0.046(3) 0.081(4) 0.051(3) 0.018(3) 0.026(3) 0.010(3) C6 0.046(3) 0.081(4) 0.042(3) 0.007(3) 0.018(3) 0.015(3) C7 0.038(3) 0.059(3) 0.040(3) 0.000(2) 0.013(2) 0.009(2) C8 0.033(3) 0.035(3) 0.027(2) -0.0015(19) 0.0077(19) 0.001(2) C9 0.034(3) 0.042(3) 0.035(3) -0.004(2) 0.006(2) 0.002(2) C10 0.038(3) 0.058(4) 0.031(3) -0.003(2) 0.002(2) 0.012(3) C11 0.034(3) 0.078(4) 0.047(3) 0.014(3) 0.002(2) -0.004(3) C12 0.062(4) 0.050(4) 0.066(4) 0.017(3) -0.026(3) -0.028(3) C13 0.061(4) 0.034(3) 0.058(4) 0.005(2) -0.015(3) -0.006(3) C14 0.031(2) 0.037(3) 0.028(2) -0.0011(19) 0.0054(19) 0.005(2) C15 0.045(3) 0.048(3) 0.050(3) 0.003(3) 0.017(2) 0.004(3) C16 0.049(3) 0.051(3) 0.068(4) 0.002(3) 0.017(3) 0.021(3) C17 0.042(3) 0.036(3) 0.070(4) 0.007(3) 0.003(3) 0.007(2) C18 0.048(3) 0.041(3) 0.043(3) 0.001(2) 0.001(2) 0.000(2) C19 0.044(3) 0.037(2) 0.038(3) -0.005(3) 0.008(2) 0.002(3) C20 0.044(3) 0.080(4) 0.043(3) 0.012(3) 0.001(2) 0.006(3) C29 0.033(2) 0.047(3) 0.039(3) 0.000(3) 0.0111(19) -0.002(3) C30 0.034(3) 0.032(3) 0.045(3) -0.004(2) 0.006(2) -0.003(2) C31 0.046(3) 0.041(3) 0.051(3) -0.004(3) 0.016(2) -0.005(3) C32 0.041(3) 0.037(3) 0.048(3) 0.001(2) 0.009(2) 0.001(2) C33 0.039(3) 0.043(3) 0.046(3) -0.013(3) 0.007(2) 0.005(3) Li 0.040(5) 0.042(5) 0.035(4) 0.000(4) 0.012(3) -0.006(4) O1 0.0286(17) 0.048(2) 0.0426(19) 0.0105(16) 0.0055(14) 0.0024(15) O2 0.0331(18) 0.0378(18) 0.0385(18) -0.0014(14) 0.0191(14) -0.0013(14) O7 0.041(2) 0.032(2) 0.056(2) -0.0039(16) 0.0136(16) 0.0047(16) O8 0.053(2) 0.059(2) 0.037(2) -0.0026(17) 0.0101(17) -0.0001(18) O9 0.0268(19) 0.057(2) 0.096(3) -0.005(3) 0.0112(18) -0.004(2) O10 0.069(3) 0.061(3) 0.051(3) 0.0102(19) 0.020(2) 0.008(2) O11 0.0303(19) 0.064(2) 0.077(3) -0.019(2) 0.0078(17) 0.009(2) P 0.0257(5) 0.0344(6) 0.0346(6) 0.0020(6) 0.0085(4) -0.0002(6) W 0.02783(9) 0.03405(10) 0.03836(9) -0.00191(12) 0.00862(6) 0.00010(11) O3 0.035(3) 0.040(3) 0.048(4) 0.007(3) 0.016(3) 0.004(2) O4 0.048(4) 0.053(4) 0.063(4) -0.008(3) 0.018(3) -0.008(3) C22 0.047(5) 0.058(5) 0.070(6) 0.000(5) 0.001(5) 0.004(5) O5 0.045(3) 0.034(3) 0.076(4) -0.001(3) 0.037(3) -0.003(3) C24 0.051(5) 0.027(4) 0.076(6) -0.004(4) 0.028(5) -0.004(4) C25 0.040(6) 0.043(5) 0.085(6) 0.019(5) 0.034(5) 0.009(5) C26 0.041(4) 0.050(5) 0.046(4) 0.015(4) 0.018(3) 0.006(4) O6 0.047(3) 0.044(4) 0.044(3) 0.009(3) 0.020(3) 0.002(3) C28 0.046(5) 0.041(4) 0.051(5) 0.008(4) 0.028(4) 0.010(4) C21 0.040(5) 0.054(5) 0.051(6) 0.005(5) 0.005(4) 0.011(5) C23 0.051(6) 0.031(5) 0.070(6) -0.013(5) 0.015(5) -0.004(4) C27 0.049(6) 0.038(5) 0.040(5) -0.001(4) 0.021(5) -0.006(4) O5S 0.050(4) 0.043(4) 0.058(4) -0.002(4) 0.026(4) -0.002(4) C26S 0.040(5) 0.035(5) 0.043(5) 0.000(4) 0.008(4) -0.002(4) O6S 0.037(4) 0.041(4) 0.047(4) 0.010(3) 0.017(3) -0.004(3) C28S 0.041(5) 0.042(5) 0.051(5) -0.002(5) 0.010(5) 0.004(4) O3S 0.031(4) 0.028(4) 0.040(4) 0.001(3) 0.006(3) -0.001(3) O4S 0.046(4) 0.050(5) 0.048(4) 0.000(4) 0.010(4) -0.015(4) C22S 0.052(6) 0.054(5) 0.057(5) 0.000(5) 0.006(5) -0.015(5) C25S 0.035(6) 0.044(6) 0.067(6) 0.011(5) 0.024(5) 0.007(5) C24S 0.049(6) 0.044(5) 0.061(6) 0.003(5) 0.022(5) 0.006(5) C21S 0.040(6) 0.047(6) 0.054(6) 0.003(5) 0.007(5) -0.001(5) C23S 0.053(6) 0.048(6) 0.054(6) -0.004(5) 0.016(5) -0.007(5) C27S 0.045(6) 0.032(5) 0.041(5) -0.003(5) 0.011(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C8 1.538(6) . ? C1 C2 1.540(6) . ? C1 C14 1.542(6) . ? C1 P 1.956(4) . ? C2 C3 1.383(7) . ? C2 C7 1.384(7) . ? C3 C4 1.379(7) . ? C3 H3A 0.9500 . ? C4 C5 1.378(8) . ? C4 H4A 0.9500 . ? C5 C6 1.364(8) . ? C5 H5A 0.9500 . ? C6 C7 1.390(7) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.368(7) . ? C8 C9 1.379(7) . ? C9 C10 1.380(7) . ? C9 H9A 0.9500 . ? C10 C11 1.369(8) . ? C10 H10A 0.9500 . ? C11 C12 1.356(9) . ? C11 H11A 0.9500 . ? C12 C13 1.396(9) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.371(7) . ? C14 C19 1.395(7) . ? C15 C16 1.393(8) . ? C15 H15A 0.9500 . ? C16 C17 1.369(8) . ? C16 H16A 0.9500 . ? C17 C18 1.362(8) . ? C17 H17A 0.9500 . ? C18 C19 1.381(7) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 O1 1.410(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C29 O7 1.153(6) . ? C29 W 2.002(6) . ? C30 O8 1.146(6) . ? C30 W 2.027(5) . ? C31 O9 1.132(6) . ? C31 W 2.048(5) . ? C32 O10 1.140(6) . ? C32 W 2.048(6) . ? C33 O11 1.129(6) . ? C33 W 2.054(5) . ? Li O2 1.809(8) . ? Li O6S 1.950(11) . ? Li O4 2.046(11) . ? Li O3 2.049(10) . ? Li O6 2.138(11) . ? Li O4S 2.146(13) . ? Li O3S 2.166(11) . ? Li O5S 2.203(13) . ? Li O5 2.235(11) . ? O1 P 1.632(3) . ? O2 P 1.505(3) . ? P W 2.5804(12) . ? O3 C28 1.421(12) . ? O3 C21 1.474(16) . ? O4 C22 1.436(15) . ? O4 C23 1.472(16) . ? C22 C21 1.46(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O5 C25 1.31(2) . ? O5 C24 1.392(13) . ? C24 C23 1.523(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.510(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O6 1.420(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O6 C27 1.362(15) . ? C28 C27 1.69(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O5S C24S 1.44(2) . ? O5S C23S 1.47(2) . ? C26S O6S 1.419(17) . ? C26S C27S 1.46(3) . ? C26S H26C 0.9900 . ? C26S H26D 0.9900 . ? O6S C25S 1.44(3) . ? C28S C21S 1.41(2) . ? C28S O3S 1.453(17) . ? C28S H28C 0.9900 . ? C28S H28D 0.9900 . ? O3S C27S 1.39(3) . ? O4S C22S 1.427(18) . ? O4S C21S 1.49(2) . ? C22S C23S 1.43(3) . ? C22S H22C 0.9900 . ? C22S H22D 0.9900 . ? C25S C24S 1.63(3) . ? C25S H25C 0.9900 . ? C25S H25D 0.9900 . ? C24S H24C 0.9900 . ? C24S H24D 0.9900 . ? C21S H21C 0.9900 . ? C21S H21D 0.9900 . ? C23S H23C 0.9900 . ? C23S H23D 0.9900 . ? C27S H27C 0.9900 . ? C27S H27D 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 C8 C1 C2 110.2(4) . . ? C8 C1 C14 112.5(4) . . ? C2 C1 C14 110.1(4) . . ? C8 C1 P 106.7(3) . . ? C2 C1 P 110.8(3) . . ? C14 C1 P 106.4(3) . . ? C3 C2 C7 117.7(4) . . ? C3 C2 C1 122.8(4) . . ? C7 C2 C1 119.5(4) . . ? C4 C3 C2 121.5(5) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C5 C4 C3 119.5(6) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C2 C7 C6 121.2(5) . . ? C2 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C13 C8 C9 116.2(5) . . ? C13 C8 C1 124.0(5) . . ? C9 C8 C1 119.8(4) . . ? C8 C9 C10 123.2(5) . . ? C8 C9 H9A 118.4 . . ? C10 C9 H9A 118.4 . . ? C11 C10 C9 119.2(5) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C12 C11 C10 118.9(5) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 121.2(6) . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 119.4 . . ? C8 C13 C12 121.0(6) . . ? C8 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C15 C14 C19 116.3(5) . . ? C15 C14 C1 123.5(4) . . ? C19 C14 C1 120.2(4) . . ? C14 C15 C16 122.0(5) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C14 122.0(5) . . ? C18 C19 H19A 119.0 . . ? C14 C19 H19A 119.0 . . ? O1 C20 H20A 109.5 . . ? O1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O7 C29 W 177.9(4) . . ? O8 C30 W 179.3(4) . . ? O9 C31 W 179.7(6) . . ? O10 C32 W 178.4(4) . . ? O11 C33 W 177.3(5) . . ? O2 Li O6S 109.0(5) . . ? O2 Li O4 119.1(4) . . ? O6S Li O4 118.1(5) . . ? O2 Li O3 120.0(5) . . ? O6S Li O3 105.4(5) . . ? O4 Li O3 82.7(4) . . ? O2 Li O6 114.9(5) . . ? O6S Li O6 27.8(3) . . ? O4 Li O6 125.0(5) . . ? O3 Li O6 79.5(4) . . ? O2 Li O4S 123.0(5) . . ? O6S Li O4S 128.0(5) . . ? O4 Li O4S 32.6(3) . . ? O3 Li O4S 51.3(4) . . ? O6 Li O4S 116.7(5) . . ? O2 Li O3S 117.0(5) . . ? O6S Li O3S 81.7(5) . . ? O4 Li O3S 106.3(5) . . ? O3 Li O3S 27.5(3) . . ? O6 Li O3S 54.2(4) . . ? O4S Li O3S 77.3(4) . . ? O2 Li O5S 112.5(5) . . ? O6S Li O5S 81.3(5) . . ? O4 Li O5S 46.4(4) . . ? O3 Li O5S 120.2(5) . . ? O6 Li O5S 103.1(4) . . ? O4S Li O5S 77.5(5) . . ? O3S Li O5S 130.5(5) . . ? O2 Li O5 109.0(4) . . ? O6S Li O5 50.2(4) . . ? O4 Li O5 77.8(4) . . ? O3 Li O5 130.7(4) . . ? O6 Li O5 75.8(4) . . ? O4S Li O5 105.6(5) . . ? O3S Li O5 122.0(4) . . ? O5S Li O5 32.7(3) . . ? C20 O1 P 124.9(3) . . ? P O2 Li 170.2(4) . . ? O2 P O1 108.48(18) . . ? O2 P C1 104.71(19) . . ? O1 P C1 100.55(18) . . ? O2 P W 112.24(13) . . ? O1 P W 105.26(14) . . ? C1 P W 124.28(14) . . ? C29 W C30 89.67(17) . . ? C29 W C31 91.2(2) . . ? C30 W C31 90.34(19) . . ? C29 W C32 91.55(18) . . ? C30 W C32 178.7(2) . . ? C31 W C32 90.0(2) . . ? C29 W C33 89.1(2) . . ? C30 W C33 89.1(2) . . ? C31 W C33 179.4(2) . . ? C32 W C33 90.5(2) . . ? C29 W P 169.47(12) . . ? C30 W P 79.83(13) . . ? C31 W P 89.65(17) . . ? C32 W P 98.94(14) . . ? C33 W P 90.00(17) . . ? C28 O3 C21 113.7(9) . . ? C28 O3 Li 111.4(6) . . ? C21 O3 Li 105.0(7) . . ? C22 O4 C23 117.0(10) . . ? C22 O4 Li 111.4(8) . . ? C23 O4 Li 112.9(7) . . ? O4 C22 C21 106.9(13) . . ? O4 C22 H22A 110.3 . . ? C21 C22 H22A 110.3 . . ? O4 C22 H22B 110.3 . . ? C21 C22 H22B 110.3 . . ? H22A C22 H22B 108.6 . . ? C25 O5 C24 107.7(11) . . ? C25 O5 Li 109.7(10) . . ? C24 O5 Li 107.7(7) . . ? O5 C24 C23 104.7(10) . . ? O5 C24 H24A 110.8 . . ? C23 C24 H24A 110.8 . . ? O5 C24 H24B 110.8 . . ? C23 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? O5 C25 C26 117.6(15) . . ? O5 C25 H25A 107.9 . . ? C26 C25 H25A 107.9 . . ? O5 C25 H25B 107.9 . . ? C26 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? O6 C26 C25 105.2(12) . . ? O6 C26 H26A 110.7 . . ? C25 C26 H26A 110.7 . . ? O6 C26 H26B 110.7 . . ? C25 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? C27 O6 C26 120.2(11) . . ? C27 O6 Li 109.1(10) . . ? C26 O6 Li 115.7(6) . . ? O3 C28 C27 99.3(10) . . ? O3 C28 H28A 111.9 . . ? C27 C28 H28A 111.9 . . ? O3 C28 H28B 111.9 . . ? C27 C28 H28B 111.9 . . ? H28A C28 H28B 109.6 . . ? C22 C21 O3 111.1(11) . . ? C22 C21 H21A 109.4 . . ? O3 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? O3 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O4 C23 C24 108.6(11) . . ? O4 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? O4 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? O6 C27 C28 104.2(11) . . ? O6 C27 H27A 110.9 . . ? C28 C27 H27A 110.9 . . ? O6 C27 H27B 110.9 . . ? C28 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? C24S O5S C23S 121.5(14) . . ? C24S O5S Li 103.7(9) . . ? C23S O5S Li 107.0(11) . . ? O6S C26S C27S 115.2(16) . . ? O6S C26S H26C 108.5 . . ? C27S C26S H26C 108.5 . . ? O6S C26S H26D 108.5 . . ? C27S C26S H26D 108.5 . . ? H26C C26S H26D 107.5 . . ? C26S O6S C25S 114.3(15) . . ? C26S O6S Li 111.2(9) . . ? C25S O6S Li 118.1(12) . . ? C21S C28S O3S 108.8(13) . . ? C21S C28S H28C 109.9 . . ? O3S C28S H28C 109.9 . . ? C21S C28S H28D 109.9 . . ? O3S C28S H28D 109.9 . . ? H28C C28S H28D 108.3 . . ? C27S O3S C28S 100.8(13) . . ? C27S O3S Li 109.3(11) . . ? C28S O3S Li 110.7(8) . . ? C22S O4S C21S 111.7(14) . . ? C22S O4S Li 110.6(9) . . ? C21S O4S Li 110.8(10) . . ? O4S C22S C23S 106.6(15) . . ? O4S C22S H22C 110.4 . . ? C23S C22S H22C 110.4 . . ? O4S C22S H22D 110.4 . . ? C23S C22S H22D 110.4 . . ? H22C C22S H22D 108.6 . . ? O6S C25S C24S 99.1(17) . . ? O6S C25S H25C 112.0 . . ? C24S C25S H25C 112.0 . . ? O6S C25S H25D 112.0 . . ? C24S C25S H25D 112.0 . . ? H25C C25S H25D 109.6 . . ? O5S C24S C25S 112.0(19) . . ? O5S C24S H24C 109.2 . . ? C25S C24S H24C 109.2 . . ? O5S C24S H24D 109.2 . . ? C25S C24S H24D 109.2 . . ? H24C C24S H24D 107.9 . . ? C28S C21S O4S 111.3(16) . . ? C28S C21S H21C 109.4 . . ? O4S C21S H21C 109.4 . . ? C28S C21S H21D 109.4 . . ? O4S C21S H21D 109.4 . . ? H21C C21S H21D 108.0 . . ? C22S C23S O5S 110.9(17) . . ? C22S C23S H23C 109.5 . . ? O5S C23S H23C 109.5 . . ? C22S C23S H23D 109.5 . . ? O5S C23S H23D 109.5 . . ? H23C C23S H23D 108.0 . . ? O3S C27S C26S 113.1(18) . . ? O3S C27S H27C 109.0 . . ? C26S C27S H27C 109.0 . . ? O3S C27S H27D 109.0 . . ? C26S C27S H27D 109.0 . . ? H27C C27S H27D 107.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.166 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.121 #END--------------------------------------------------------------------------- _database_code_depnum_ccdc_archive 'CCDC 953774'