# 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_Greg1573 _database_code_depnum_ccdc_archive 'CCDC 926024' #TrackingRef 'web_deposit_cif_file_0_Dr.GregorSchnakenburg_1361462579.Gesamtcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H21 O6 P W' _chemical_formula_sum 'C19 H21 O6 P W' _chemical_formula_weight 560.18 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' 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 11.4787(4) _cell_length_b 14.2200(6) _cell_length_c 12.4535(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.477(2) _cell_angle_gamma 90.00 _cell_volume 2019.78(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4372 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 29.13 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 5.830 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.11015 _exptl_absorpt_correction_T_max 0.22242 _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_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13435 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4377 _reflns_number_gt 3888 _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^)+(0.0255P)^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 4377 _refine_ls_number_parameters 249 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0522 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7704(2) -0.0184(2) 0.9299(2) 0.0177(6) Uani 1 1 d . . . C2 C 0.6735(3) -0.0250(2) 1.0044(2) 0.0244(7) Uani 1 1 d . . . H2A H 0.6677 0.0312 1.0505 0.029 Uiso 1 1 calc R . . H2B H 0.5959 -0.0423 0.9667 0.029 Uiso 1 1 calc R . . C3 C 0.7391(3) -0.1070(3) 1.0625(3) 0.0372(9) Uani 1 1 d . . . H3A H 0.6928 -0.1659 1.0601 0.045 Uiso 1 1 calc R . . H3B H 0.7717 -0.0921 1.1376 0.045 Uiso 1 1 calc R . . C4 C 0.8322(3) -0.1055(2) 0.9812(2) 0.0206(6) Uani 1 1 d . . . H4A H 0.9131 -0.0936 1.0150 0.025 Uiso 1 1 calc R . . H4B H 0.8292 -0.1609 0.9328 0.025 Uiso 1 1 calc R . . C5 C 0.8832(2) 0.0075(2) 0.7236(2) 0.0156(6) Uani 1 1 d . . . C6 C 0.9228(2) 0.0986(2) 0.6760(2) 0.0154(6) Uani 1 1 d . . . C7 C 0.8903(2) 0.0969(2) 0.5684(2) 0.0184(6) Uani 1 1 d . . . C8 C 0.8319(2) 0.0077(2) 0.5378(2) 0.0171(6) Uani 1 1 d . . . C9 C 0.8251(2) -0.0447(2) 0.6265(2) 0.0170(6) Uani 1 1 d . . . C10 C 0.9823(3) -0.0475(2) 0.7878(2) 0.0213(6) Uani 1 1 d . . . H10A H 1.0122 -0.0117 0.8523 0.026 Uiso 1 1 calc R . . H10B H 1.0458 -0.0577 0.7426 0.026 Uiso 1 1 calc R . . H10C H 0.9524 -0.1083 0.8095 0.026 Uiso 1 1 calc R . . C11 C 0.9891(3) 0.1726(2) 0.7420(3) 0.0224(6) Uani 1 1 d . . . H11A H 1.0710 0.1531 0.7585 0.027 Uiso 1 1 calc R . . H11B H 0.9541 0.1817 0.8095 0.027 Uiso 1 1 calc R . . H11C H 0.9857 0.2318 0.7013 0.027 Uiso 1 1 calc R . . C12 C 0.9097(3) 0.1735(3) 0.4885(3) 0.0285(7) Uani 1 1 d . . . H12A H 0.9615 0.1502 0.4369 0.034 Uiso 1 1 calc R . . H12B H 0.9459 0.2280 0.5271 0.034 Uiso 1 1 calc R . . H12C H 0.8343 0.1920 0.4494 0.034 Uiso 1 1 calc R . . C13 C 0.7911(3) -0.0197(3) 0.4233(2) 0.0272(7) Uani 1 1 d . . . H13A H 0.8568 -0.0464 0.3897 0.033 Uiso 1 1 calc R . . H13B H 0.7612 0.0359 0.3827 0.033 Uiso 1 1 calc R . . H13C H 0.7285 -0.0666 0.4229 0.033 Uiso 1 1 calc R . . C14 C 0.7711(3) -0.1398(2) 0.6347(3) 0.0277(8) Uani 1 1 d . . . H14A H 0.7054 -0.1357 0.6783 0.033 Uiso 1 1 calc R . . H14B H 0.8300 -0.1836 0.6689 0.033 Uiso 1 1 calc R . . H14C H 0.7427 -0.1625 0.5622 0.033 Uiso 1 1 calc R . . C15 C 0.4456(3) 0.2109(2) 0.6880(2) 0.0236(6) Uani 1 1 d U . . C16 C 0.4959(3) 0.0165(2) 0.7555(2) 0.0200(6) Uani 1 1 d . . . C17 C 0.5747(3) 0.1753(2) 0.8891(2) 0.0212(6) Uani 1 1 d U . . C18 C 0.6947(3) 0.2494(2) 0.7103(2) 0.0204(6) Uani 1 1 d U . . C19 C 0.5866(3) 0.1015(2) 0.5730(2) 0.0200(6) Uani 1 1 d U . . O1 O 0.83305(17) 0.07170(14) 0.92695(15) 0.0199(4) Uani 1 1 d . . . O2 O 0.3627(2) 0.25370(19) 0.6617(2) 0.0440(7) Uani 1 1 d . . . O3 O 0.4466(2) -0.05121(18) 0.76788(16) 0.0329(6) Uani 1 1 d . . . O4 O 0.5613(2) 0.19756(16) 0.97468(17) 0.0340(6) Uani 1 1 d . . . O5 O 0.7526(2) 0.31170(16) 0.69623(19) 0.0319(5) Uani 1 1 d . . . O6 O 0.5748(2) 0.08795(17) 0.48318(16) 0.0300(5) Uani 1 1 d . . . P P 0.76482(6) 0.04447(5) 0.80509(5) 0.01422(15) Uani 1 1 d . . . W W 0.589888(9) 0.135486(8) 0.734031(8) 0.01397(5) 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 0.0215(14) 0.0167(15) 0.0153(13) 0.0014(12) 0.0042(11) -0.0005(12) C2 0.0292(16) 0.0277(18) 0.0179(14) 0.0033(13) 0.0097(13) 0.0050(14) C3 0.0299(18) 0.045(2) 0.038(2) 0.0240(19) 0.0113(16) 0.0062(17) C4 0.0205(15) 0.0223(16) 0.0185(14) 0.0059(13) -0.0006(12) 0.0025(13) C5 0.0175(13) 0.0155(15) 0.0146(12) -0.0006(12) 0.0049(11) 0.0016(11) C6 0.0135(13) 0.0126(14) 0.0210(14) -0.0014(12) 0.0061(11) 0.0005(11) C7 0.0180(14) 0.0180(16) 0.0201(14) 0.0017(13) 0.0071(12) 0.0008(12) C8 0.0139(13) 0.0222(16) 0.0156(13) -0.0025(12) 0.0042(11) 0.0026(12) C9 0.0157(13) 0.0169(15) 0.0195(14) -0.0077(12) 0.0061(11) -0.0003(12) C10 0.0225(15) 0.0205(16) 0.0214(14) 0.0018(13) 0.0045(12) 0.0043(13) C11 0.0233(15) 0.0164(16) 0.0278(15) -0.0024(14) 0.0041(13) -0.0033(13) C12 0.0336(18) 0.0283(19) 0.0247(16) 0.0094(15) 0.0081(14) -0.0008(15) C13 0.0250(16) 0.041(2) 0.0163(13) -0.0065(14) 0.0059(12) 0.0000(15) C14 0.0367(19) 0.0205(18) 0.0265(17) -0.0066(13) 0.0067(15) -0.0046(13) C15 0.0252(13) 0.0255(17) 0.0199(13) -0.0048(12) 0.0024(11) 0.0066(12) C16 0.0221(15) 0.0251(17) 0.0130(13) -0.0016(13) 0.0027(12) -0.0013(14) C17 0.0248(15) 0.0197(16) 0.0196(11) -0.0024(12) 0.0046(11) 0.0039(13) C18 0.0248(13) 0.0147(14) 0.0217(14) 0.0005(11) 0.0029(12) 0.0043(11) C19 0.0223(14) 0.0188(15) 0.0197(12) -0.0024(12) 0.0061(12) 0.0030(12) O1 0.0269(11) 0.0169(11) 0.0156(9) -0.0017(8) 0.0010(8) -0.0015(9) O2 0.0363(14) 0.0497(17) 0.0442(14) -0.0050(13) -0.0032(12) 0.0248(13) O3 0.0404(13) 0.0342(15) 0.0245(12) 0.0041(10) 0.0050(10) -0.0158(12) O4 0.0529(15) 0.0284(14) 0.0229(11) -0.0099(10) 0.0135(11) 0.0000(12) O5 0.0285(12) 0.0193(12) 0.0480(14) 0.0037(11) 0.0050(11) -0.0025(10) O6 0.0374(13) 0.0356(14) 0.0167(10) -0.0039(10) 0.0024(9) 0.0058(11) P 0.0169(3) 0.0137(4) 0.0126(3) 0.0005(3) 0.0039(3) 0.0012(3) W 0.01620(7) 0.01372(8) 0.01252(7) -0.00046(4) 0.00398(5) 0.00250(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 1.472(3) . ? C1 C2 1.530(4) . ? C1 C4 1.531(4) . ? C1 P 1.788(3) . ? C2 C3 1.526(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.553(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C9 1.508(4) . ? C5 C6 1.516(4) . ? C5 C10 1.530(4) . ? C5 P 1.861(3) . ? C6 C7 1.349(4) . ? C6 C11 1.490(4) . ? C7 C8 1.464(4) . ? C7 C12 1.509(4) . ? C8 C9 1.343(4) . ? C8 C13 1.501(4) . ? C9 C14 1.496(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O2 1.146(4) . ? C15 W 2.002(3) . ? C16 O3 1.136(4) . ? C16 W 2.041(3) . ? C17 O4 1.139(3) . ? C17 W 2.039(3) . ? C18 O5 1.132(4) . ? C18 W 2.059(3) . ? C19 O6 1.128(3) . ? C19 W 2.059(3) . ? O1 P 1.673(2) . ? P W 2.4677(7) . ? 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 117.3(2) . . ? O1 C1 C4 120.7(2) . . ? C2 C1 C4 91.8(2) . . ? O1 C1 P 60.84(13) . . ? C2 C1 P 126.9(2) . . ? C4 C1 P 137.5(2) . . ? C3 C2 C1 88.9(2) . . ? C3 C2 H2A 113.8 . . ? C1 C2 H2A 113.8 . . ? C3 C2 H2B 113.8 . . ? C1 C2 H2B 113.8 . . ? H2A C2 H2B 111.1 . . ? C2 C3 C4 91.1(2) . . ? C2 C3 H3A 113.4 . . ? C4 C3 H3A 113.4 . . ? C2 C3 H3B 113.4 . . ? C4 C3 H3B 113.4 . . ? H3A C3 H3B 110.7 . . ? C1 C4 C3 87.9(2) . . ? C1 C4 H4A 114.0 . . ? C3 C4 H4A 114.0 . . ? C1 C4 H4B 114.0 . . ? C3 C4 H4B 114.0 . . ? H4A C4 H4B 111.2 . . ? C9 C5 C6 103.4(2) . . ? C9 C5 C10 113.7(2) . . ? C6 C5 C10 113.8(2) . . ? C9 C5 P 106.97(18) . . ? C6 C5 P 104.00(18) . . ? C10 C5 P 113.92(18) . . ? C7 C6 C11 128.8(3) . . ? C7 C6 C5 108.1(2) . . ? C11 C6 C5 123.0(2) . . ? C6 C7 C8 110.0(3) . . ? C6 C7 C12 126.7(3) . . ? C8 C7 C12 123.4(3) . . ? C9 C8 C7 109.5(2) . . ? C9 C8 C13 126.6(3) . . ? C7 C8 C13 123.9(3) . . ? C8 C9 C14 128.4(3) . . ? C8 C9 C5 109.0(2) . . ? C14 C9 C5 122.7(3) . . ? 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 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 W 179.7(3) . . ? O3 C16 W 178.0(3) . . ? O4 C17 W 177.2(3) . . ? O5 C18 W 179.3(3) . . ? O6 C19 W 173.1(3) . . ? C1 O1 P 68.95(14) . . ? O1 P C1 50.21(12) . . ? O1 P C5 105.31(11) . . ? C1 P C5 112.07(13) . . ? O1 P W 118.86(8) . . ? C1 P W 121.48(9) . . ? C5 P W 124.56(9) . . ? C15 W C17 88.05(12) . . ? C15 W C16 92.83(13) . . ? C17 W C16 90.21(12) . . ? C15 W C19 85.61(12) . . ? C17 W C19 173.55(11) . . ? C16 W C19 88.89(12) . . ? C15 W C18 90.87(12) . . ? C17 W C18 91.78(12) . . ? C16 W C18 175.85(11) . . ? C19 W C18 89.53(12) . . ? C15 W P 175.66(8) . . ? C17 W P 87.66(9) . . ? C16 W P 86.49(9) . . ? C19 W P 98.66(9) . . ? C18 W P 89.95(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -121.9(3) . . . . ? C4 C1 C2 C3 4.3(3) . . . . ? P C1 C2 C3 165.4(3) . . . . ? C1 C2 C3 C4 -4.2(3) . . . . ? O1 C1 C4 C3 119.3(3) . . . . ? C2 C1 C4 C3 -4.2(3) . . . . ? P C1 C4 C3 -161.7(3) . . . . ? C2 C3 C4 C1 4.2(3) . . . . ? C9 C5 C6 C7 0.4(3) . . . . ? C10 C5 C6 C7 124.2(3) . . . . ? P C5 C6 C7 -111.3(2) . . . . ? C9 C5 C6 C11 -178.0(2) . . . . ? C10 C5 C6 C11 -54.1(3) . . . . ? P C5 C6 C11 70.4(3) . . . . ? C11 C6 C7 C8 177.0(3) . . . . ? C5 C6 C7 C8 -1.2(3) . . . . ? C11 C6 C7 C12 -2.9(5) . . . . ? C5 C6 C7 C12 178.9(3) . . . . ? C6 C7 C8 C9 1.8(3) . . . . ? C12 C7 C8 C9 -178.4(3) . . . . ? C6 C7 C8 C13 -176.3(3) . . . . ? C12 C7 C8 C13 3.6(4) . . . . ? C7 C8 C9 C14 178.9(3) . . . . ? C13 C8 C9 C14 -3.1(5) . . . . ? C7 C8 C9 C5 -1.5(3) . . . . ? C13 C8 C9 C5 176.5(3) . . . . ? C6 C5 C9 C8 0.7(3) . . . . ? C10 C5 C9 C8 -123.2(3) . . . . ? P C5 C9 C8 110.1(2) . . . . ? C6 C5 C9 C14 -179.7(3) . . . . ? C10 C5 C9 C14 56.4(3) . . . . ? P C5 C9 C14 -70.2(3) . . . . ? C2 C1 O1 P -119.1(2) . . . . ? C4 C1 O1 P 130.6(2) . . . . ? C1 O1 P C5 -106.20(16) . . . . ? C1 O1 P W 108.48(13) . . . . ? C2 C1 P O1 103.7(3) . . . . ? C4 C1 P O1 -104.8(3) . . . . ? O1 C1 P C5 91.89(16) . . . . ? C2 C1 P C5 -164.4(3) . . . . ? C4 C1 P C5 -13.0(4) . . . . ? O1 C1 P W -103.10(12) . . . . ? C2 C1 P W 0.7(3) . . . . ? C4 C1 P W 152.1(3) . . . . ? C9 C5 P O1 163.25(18) . . . . ? C6 C5 P O1 -87.73(19) . . . . ? C10 C5 P O1 36.7(2) . . . . ? C9 C5 P C1 110.5(2) . . . . ? C6 C5 P C1 -140.50(19) . . . . ? C10 C5 P C1 -16.1(3) . . . . ? C9 C5 P W -54.0(2) . . . . ? C6 C5 P W 55.0(2) . . . . ? C10 C5 P W 179.46(17) . . . . ? O2 C15 W C17 -89(51) . . . . ? O2 C15 W C16 1(51) . . . . ? O2 C15 W C19 89(51) . . . . ? O2 C15 W C18 179(100) . . . . ? O2 C15 W P -80(51) . . . . ? O4 C17 W C15 33(6) . . . . ? O4 C17 W C16 -60(6) . . . . ? O4 C17 W C19 22(6) . . . . ? O4 C17 W C18 124(6) . . . . ? O4 C17 W P -146(6) . . . . ? O3 C16 W C15 173(7) . . . . ? O3 C16 W C17 -99(7) . . . . ? O3 C16 W C19 88(7) . . . . ? O3 C16 W C18 20(8) . . . . ? O3 C16 W P -11(7) . . . . ? O6 C19 W C15 -2(2) . . . . ? O6 C19 W C17 9(3) . . . . ? O6 C19 W C16 91(2) . . . . ? O6 C19 W C18 -93(2) . . . . ? O6 C19 W P 177(2) . . . . ? O5 C18 W C15 -102(24) . . . . ? O5 C18 W C17 170(100) . . . . ? O5 C18 W C16 51(24) . . . . ? O5 C18 W C19 -16(24) . . . . ? O5 C18 W P 82(24) . . . . ? O1 P W C15 -29.1(12) . . . . ? C1 P W C15 29.6(12) . . . . ? C5 P W C15 -167.3(12) . . . . ? O1 P W C17 -19.94(12) . . . . ? C1 P W C17 38.76(15) . . . . ? C5 P W C17 -158.16(14) . . . . ? O1 P W C16 -110.30(11) . . . . ? C1 P W C16 -51.59(14) . . . . ? C5 P W C16 111.49(14) . . . . ? O1 P W C19 161.37(12) . . . . ? C1 P W C19 -139.93(14) . . . . ? C5 P W C19 23.15(14) . . . . ? O1 P W C18 71.84(12) . . . . ? C1 P W C18 130.55(14) . . . . ? C5 P W C18 -66.37(14) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.263 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.128 data_Greg1843 _database_code_depnum_ccdc_archive 'CCDC 926025' #TrackingRef 'web_deposit_cif_file_0_Dr.GregorSchnakenburg_1361462579.Gesamtcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H21 Cr O6 P' _chemical_formula_sum 'C19 H21 Cr O6 P' _chemical_formula_weight 428.33 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' _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 11.5967(5) _cell_length_b 13.9514(6) _cell_length_c 12.2801(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.174(3) _cell_angle_gamma 90.00 _cell_volume 1971.25(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4557 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8912 _exptl_absorpt_correction_T_max 0.9728 _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_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15154 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4679 _reflns_number_gt 3872 _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^)+(0.0510P)^2^+0.6537P] 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 4679 _refine_ls_number_parameters 249 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.012 _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 0.25991(15) 1.01634(12) 0.93135(14) 0.0225(4) Uani 1 1 d . . . C2 C 0.32101(16) 1.10414(13) 0.98645(15) 0.0255(4) Uani 1 1 d . . . H2A H 0.3125 1.1629 0.9410 0.031 Uiso 1 1 calc R . . H2B H 0.4033 1.0929 1.0158 0.031 Uiso 1 1 calc R . . C3 C 0.23604(19) 1.09855(17) 1.07439(19) 0.0407(5) Uani 1 1 d . . . H3A H 0.2728 1.0752 1.1466 0.049 Uiso 1 1 calc R . . H3B H 0.1928 1.1588 1.0824 0.049 Uiso 1 1 calc R . . C4 C 0.16456(17) 1.02178(14) 1.00649(15) 0.0283(4) Uani 1 1 d . . . H4A H 0.1545 0.9618 1.0474 0.034 Uiso 1 1 calc R . . H4B H 0.0891 1.0453 0.9695 0.034 Uiso 1 1 calc R . . C5 C 0.37531(14) 0.99293(12) 0.72602(13) 0.0186(3) Uani 1 1 d . . . C6 C 0.41833(14) 0.90147(12) 0.67799(14) 0.0198(3) Uani 1 1 d . . . C7 C 0.39064(15) 0.90329(12) 0.56813(14) 0.0221(4) Uani 1 1 d . . . C8 C 0.33117(15) 0.99413(13) 0.53596(14) 0.0223(4) Uani 1 1 d . . . C9 C 0.31915(15) 1.04599(12) 0.62638(14) 0.0207(3) Uani 1 1 d . . . C10 C 0.47134(15) 1.04961(12) 0.79398(14) 0.0234(4) Uani 1 1 d . . . H10A H 0.5356 1.0603 0.7505 0.028 Uiso 1 1 calc R . . H10B H 0.4996 1.0134 0.8604 0.028 Uiso 1 1 calc R . . H10C H 0.4405 1.1115 0.8147 0.028 Uiso 1 1 calc R . . C11 C 0.48548(16) 0.82679(13) 0.74638(15) 0.0255(4) Uani 1 1 d . . . H11A H 0.4530 0.8193 0.8158 0.031 Uiso 1 1 calc R . . H11B H 0.5670 0.8465 0.7614 0.031 Uiso 1 1 calc R . . H11C H 0.4805 0.7657 0.7068 0.031 Uiso 1 1 calc R . . C12 C 0.41536(19) 0.82765(15) 0.48781(17) 0.0334(4) Uani 1 1 d . . . H12A H 0.4475 0.7709 0.5276 0.040 Uiso 1 1 calc R . . H12B H 0.4716 0.8522 0.4414 0.040 Uiso 1 1 calc R . . H12C H 0.3431 0.8103 0.4418 0.040 Uiso 1 1 calc R . . C13 C 0.29418(17) 1.02170(15) 0.41904(15) 0.0310(4) Uani 1 1 d . . . H13A H 0.2545 0.9675 0.3799 0.037 Uiso 1 1 calc R . . H13B H 0.3627 1.0391 0.3841 0.037 Uiso 1 1 calc R . . H13C H 0.2411 1.0765 0.4166 0.037 Uiso 1 1 calc R . . C14 C 0.26379(18) 1.14227(13) 0.63342(17) 0.0305(4) Uani 1 1 d . . . H14A H 0.3233 1.1895 0.6600 0.037 Uiso 1 1 calc R . . H14C H 0.2052 1.1391 0.6843 0.037 Uiso 1 1 calc R . . H14B H 0.2266 1.1613 0.5606 0.037 Uiso 1 1 calc R . . C17 C 0.00548(16) 0.97672(13) 0.75202(14) 0.0232(3) Uani 1 1 d U . . C16 C 0.07775(16) 0.82385(13) 0.87586(15) 0.0246(4) Uani 1 1 d U . . C18 C 0.09392(15) 0.89993(12) 0.58129(14) 0.0226(3) Uani 1 1 d U . . C19 C 0.19111(16) 0.75780(13) 0.71010(15) 0.0242(4) Uani 1 1 d U . . C15 C -0.03852(17) 0.79339(13) 0.68449(15) 0.0264(4) Uani 1 1 d U . . Cr Cr 0.09419(2) 0.865110(18) 0.73184(2) 0.01832(9) Uani 1 1 d U . . O1 O 0.32331(11) 0.92400(9) 0.92909(10) 0.0243(3) Uani 1 1 d . . . O2 O -0.11998(13) 0.74935(11) 0.65552(13) 0.0407(4) Uani 1 1 d . . . O3 O 0.06257(14) 0.79761(10) 0.96109(11) 0.0372(3) Uani 1 1 d . . . O4 O -0.04642(13) 1.04473(10) 0.76437(11) 0.0344(3) Uani 1 1 d U . . O5 O 0.08153(12) 0.91579(10) 0.48974(10) 0.0322(3) Uani 1 1 d U . . O6 O 0.24660(12) 0.69259(10) 0.69635(13) 0.0353(3) Uani 1 1 d U . . P P 0.25635(4) 0.95296(3) 0.80454(3) 0.01737(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0249(9) 0.0224(8) 0.0201(8) -0.0013(7) 0.0027(7) -0.0010(7) C2 0.0263(9) 0.0248(9) 0.0247(9) -0.0038(7) 0.0009(7) -0.0016(7) C3 0.0387(12) 0.0467(13) 0.0387(11) -0.0214(10) 0.0134(10) -0.0102(10) C4 0.0308(10) 0.0313(10) 0.0237(9) -0.0053(7) 0.0069(7) -0.0045(8) C5 0.0200(8) 0.0170(8) 0.0192(8) 0.0013(6) 0.0039(6) -0.0001(6) C6 0.0188(8) 0.0177(8) 0.0234(8) 0.0002(6) 0.0045(7) 0.0002(6) C7 0.0202(8) 0.0227(8) 0.0242(8) -0.0021(7) 0.0059(7) -0.0023(7) C8 0.0191(8) 0.0271(9) 0.0210(8) 0.0035(7) 0.0036(7) -0.0018(7) C9 0.0202(8) 0.0194(8) 0.0229(8) 0.0055(6) 0.0043(7) 0.0001(7) C10 0.0235(9) 0.0215(9) 0.0256(9) -0.0021(7) 0.0049(7) -0.0055(7) C11 0.0245(9) 0.0213(9) 0.0304(9) 0.0021(7) 0.0020(7) 0.0043(7) C12 0.0369(11) 0.0341(11) 0.0299(10) -0.0104(8) 0.0079(8) 0.0014(9) C13 0.0288(10) 0.0422(11) 0.0222(9) 0.0061(8) 0.0046(7) 0.0010(9) C14 0.0362(11) 0.0224(9) 0.0331(10) 0.0055(8) 0.0054(8) 0.0057(8) C17 0.0234(9) 0.0281(9) 0.0180(8) 0.0006(7) 0.0017(6) -0.0005(7) C16 0.0258(9) 0.0220(9) 0.0259(8) 0.0009(7) 0.0029(7) -0.0035(7) C18 0.0223(9) 0.0205(8) 0.0249(8) -0.0013(7) 0.0029(7) -0.0028(7) C19 0.0242(9) 0.0219(8) 0.0259(9) -0.0001(7) 0.0013(7) -0.0049(6) C15 0.0279(9) 0.0258(9) 0.0256(9) 0.0033(7) 0.0038(7) -0.0037(7) Cr 0.01965(15) 0.01739(15) 0.01789(15) 0.00032(10) 0.00228(11) -0.00224(10) O1 0.0293(7) 0.0242(6) 0.0190(6) -0.0007(5) 0.0009(5) -0.0012(5) O2 0.0324(8) 0.0438(9) 0.0443(9) 0.0011(7) -0.0020(7) -0.0156(7) O3 0.0521(9) 0.0326(8) 0.0282(7) 0.0080(6) 0.0096(6) -0.0044(7) O4 0.0368(8) 0.0364(8) 0.0295(7) -0.0027(6) 0.0022(6) 0.0123(6) O5 0.0368(8) 0.0370(8) 0.0222(6) 0.0031(6) 0.0015(6) -0.0071(6) O6 0.0326(8) 0.0230(7) 0.0499(9) -0.0035(6) 0.0029(7) 0.0019(6) P 0.0198(2) 0.0158(2) 0.0165(2) -0.00006(15) 0.00216(16) -0.00054(16) _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 1.485(2) . ? C1 C4 1.528(2) . ? C1 C2 1.530(2) . ? C1 P 1.7868(17) . ? C2 C3 1.552(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.535(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C9 1.507(2) . ? C5 C6 1.516(2) . ? C5 C10 1.526(2) . ? C5 P 1.8644(16) . ? C6 C7 1.347(2) . ? C6 C11 1.495(2) . ? C7 C8 1.473(2) . ? C7 C12 1.496(2) . ? C8 C9 1.347(2) . ? C8 C13 1.497(2) . ? C9 C14 1.496(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C17 O4 1.144(2) . ? C17 Cr 1.8994(19) . ? C16 O3 1.143(2) . ? C16 Cr 1.8920(18) . ? C18 O5 1.137(2) . ? C18 Cr 1.9112(18) . ? C19 O6 1.139(2) . ? C19 Cr 1.9107(19) . ? C15 O2 1.146(2) . ? C15 Cr 1.8666(19) . ? Cr P 2.3273(5) . ? O1 P 1.6760(13) . ? 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 C4 116.85(14) . . ? O1 C1 C2 119.98(14) . . ? C4 C1 C2 91.33(13) . . ? O1 C1 P 60.80(8) . . ? C4 C1 P 127.68(13) . . ? C2 C1 P 137.79(13) . . ? C1 C2 C3 88.18(14) . . ? C1 C2 H2A 114.0 . . ? C3 C2 H2A 114.0 . . ? C1 C2 H2B 114.0 . . ? C3 C2 H2B 114.0 . . ? H2A C2 H2B 111.2 . . ? C4 C3 C2 90.22(14) . . ? C4 C3 H3A 113.6 . . ? C2 C3 H3A 113.6 . . ? C4 C3 H3B 113.6 . . ? C2 C3 H3B 113.6 . . ? H3A C3 H3B 110.9 . . ? C1 C4 C3 88.87(14) . . ? C1 C4 H4A 113.8 . . ? C3 C4 H4A 113.8 . . ? C1 C4 H4B 113.8 . . ? C3 C4 H4B 113.8 . . ? H4A C4 H4B 111.1 . . ? C9 C5 C6 103.15(13) . . ? C9 C5 C10 113.66(14) . . ? C6 C5 C10 113.30(14) . . ? C9 C5 P 107.11(11) . . ? C6 C5 P 104.48(11) . . ? C10 C5 P 114.12(11) . . ? C7 C6 C11 128.18(16) . . ? C7 C6 C5 108.95(15) . . ? C11 C6 C5 122.80(15) . . ? C6 C7 C8 109.25(15) . . ? C6 C7 C12 127.25(17) . . ? C8 C7 C12 123.49(16) . . ? C9 C8 C7 109.53(15) . . ? C9 C8 C13 127.31(17) . . ? C7 C8 C13 123.15(16) . . ? C8 C9 C14 128.26(16) . . ? C8 C9 C5 109.07(14) . . ? C14 C9 C5 122.64(15) . . ? 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 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? O4 C17 Cr 178.96(16) . . ? O3 C16 Cr 176.75(17) . . ? O5 C18 Cr 172.11(16) . . ? O6 C19 Cr 178.38(16) . . ? O2 C15 Cr 179.9(2) . . ? C15 Cr C16 87.29(8) . . ? C15 Cr C17 92.36(8) . . ? C16 Cr C17 90.46(8) . . ? C15 Cr C19 90.74(8) . . ? C16 Cr C19 91.26(8) . . ? C17 Cr C19 176.52(8) . . ? C15 Cr C18 86.17(8) . . ? C16 Cr C18 173.41(8) . . ? C17 Cr C18 88.99(7) . . ? C19 Cr C18 89.65(8) . . ? C15 Cr P 175.62(6) . . ? C16 Cr P 88.42(6) . . ? C17 Cr P 86.74(6) . . ? C19 Cr P 90.28(5) . . ? C18 Cr P 98.10(5) . . ? C1 O1 P 68.53(8) . . ? O1 P C1 50.67(7) . . ? O1 P C5 104.82(7) . . ? C1 P C5 111.38(8) . . ? O1 P Cr 118.90(5) . . ? C1 P Cr 121.64(6) . . ? C5 P Cr 125.01(5) . . ? 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 -113.41(17) . . . . ? C4 C1 C2 C3 8.92(16) . . . . ? P C1 C2 C3 168.26(19) . . . . ? C1 C2 C3 C4 -8.88(16) . . . . ? O1 C1 C4 C3 115.87(17) . . . . ? C2 C1 C4 C3 -9.02(16) . . . . ? P C1 C4 C3 -171.59(16) . . . . ? C2 C3 C4 C1 8.89(16) . . . . ? C9 C5 C6 C7 0.13(18) . . . . ? C10 C5 C6 C7 -123.20(16) . . . . ? P C5 C6 C7 112.00(13) . . . . ? C9 C5 C6 C11 177.32(15) . . . . ? C10 C5 C6 C11 54.0(2) . . . . ? P C5 C6 C11 -70.81(18) . . . . ? C11 C6 C7 C8 -175.89(16) . . . . ? C5 C6 C7 C8 1.11(19) . . . . ? C11 C6 C7 C12 3.5(3) . . . . ? C5 C6 C7 C12 -179.49(17) . . . . ? C6 C7 C8 C9 -2.1(2) . . . . ? C12 C7 C8 C9 178.47(17) . . . . ? C6 C7 C8 C13 176.63(16) . . . . ? C12 C7 C8 C13 -2.8(3) . . . . ? C7 C8 C9 C14 -179.68(17) . . . . ? C13 C8 C9 C14 1.7(3) . . . . ? C7 C8 C9 C5 2.14(19) . . . . ? C13 C8 C9 C5 -176.52(16) . . . . ? C6 C5 C9 C8 -1.43(18) . . . . ? C10 C5 C9 C8 121.65(16) . . . . ? P C5 C9 C8 -111.35(14) . . . . ? C6 C5 C9 C14 -179.73(16) . . . . ? C10 C5 C9 C14 -56.6(2) . . . . ? P C5 C9 C14 70.35(18) . . . . ? O2 C15 Cr C16 6(100) . . . . ? O2 C15 Cr C17 -84(100) . . . . ? O2 C15 Cr C19 97(100) . . . . ? O2 C15 Cr C18 -173(100) . . . . ? O2 C15 Cr P -6(100) . . . . ? O3 C16 Cr C15 -15(3) . . . . ? O3 C16 Cr C17 77(3) . . . . ? O3 C16 Cr C19 -106(3) . . . . ? O3 C16 Cr C18 -8(3) . . . . ? O3 C16 Cr P 164(3) . . . . ? O4 C17 Cr C15 -169(100) . . . . ? O4 C17 Cr C16 104(8) . . . . ? O4 C17 Cr C19 -16(9) . . . . ? O4 C17 Cr C18 -83(8) . . . . ? O4 C17 Cr P 15(8) . . . . ? O6 C19 Cr C15 -1(6) . . . . ? O6 C19 Cr C16 87(6) . . . . ? O6 C19 Cr C17 -154(5) . . . . ? O6 C19 Cr C18 -87(6) . . . . ? O6 C19 Cr P 175(100) . . . . ? O5 C18 Cr C15 9.4(12) . . . . ? O5 C18 Cr C16 2.3(17) . . . . ? O5 C18 Cr C17 -83.0(12) . . . . ? O5 C18 Cr C19 100.2(12) . . . . ? O5 C18 Cr P -169.6(12) . . . . ? C4 C1 O1 P 120.13(15) . . . . ? C2 C1 O1 P -131.09(15) . . . . ? C1 O1 P C5 105.72(10) . . . . ? C1 O1 P Cr -108.80(8) . . . . ? C4 C1 P O1 -102.83(18) . . . . ? C2 C1 P O1 103.6(2) . . . . ? O1 C1 P C5 -91.96(9) . . . . ? C4 C1 P C5 165.21(15) . . . . ? C2 C1 P C5 11.7(2) . . . . ? O1 C1 P Cr 103.24(8) . . . . ? C4 C1 P Cr 0.41(19) . . . . ? C2 C1 P Cr -153.12(17) . . . . ? C9 C5 P O1 -164.03(11) . . . . ? C6 C5 P O1 86.99(12) . . . . ? C10 C5 P O1 -37.30(14) . . . . ? C9 C5 P C1 -110.93(12) . . . . ? C6 C5 P C1 140.08(11) . . . . ? C10 C5 P C1 15.79(15) . . . . ? C9 C5 P Cr 53.26(13) . . . . ? C6 C5 P Cr -55.73(13) . . . . ? C10 C5 P Cr 179.98(9) . . . . ? C15 Cr P O1 32.0(8) . . . . ? C16 Cr P O1 19.71(8) . . . . ? C17 Cr P O1 110.26(7) . . . . ? C19 Cr P O1 -71.53(7) . . . . ? C18 Cr P O1 -161.22(7) . . . . ? C15 Cr P C1 -27.3(8) . . . . ? C16 Cr P C1 -39.61(9) . . . . ? C17 Cr P C1 50.94(9) . . . . ? C19 Cr P C1 -130.86(9) . . . . ? C18 Cr P C1 139.45(9) . . . . ? C15 Cr P C5 170.0(8) . . . . ? C16 Cr P C5 157.73(9) . . . . ? C17 Cr P C5 -111.72(8) . . . . ? C19 Cr P C5 66.48(9) . . . . ? C18 Cr P C5 -23.21(9) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.807 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.060 data_Greg1852 _database_code_depnum_ccdc_archive 'CCDC 926026' #TrackingRef 'web_deposit_cif_file_0_Dr.GregorSchnakenburg_1361462579.Gesamtcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H21 Mo O6 P' _chemical_formula_sum 'C19 H21 Mo O6 P' _chemical_formula_weight 472.27 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' _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 11.4412(3) _cell_length_b 14.2800(4) _cell_length_c 12.4894(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.323(2) _cell_angle_gamma 90.00 _cell_volume 2028.11(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14931 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 29.53 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8218 _exptl_absorpt_correction_T_max 0.9419 _exptl_absorpt_process_details 'STOE X-RED (STOE&CIE, 2008)' _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 ; 750 frames, detector distance = 100 mm ; _diffrn_reflns_number 17135 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4889 _reflns_number_gt 4295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA (STOE&CIE, 2008)' _computing_cell_refinement 'STOE X-AREA (STOE&CIE, 2008)' _computing_data_reduction 'STOE X-RED (STOE&CIE, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2.1c (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (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^)+(0.0364P)^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 4889 _refine_ls_number_parameters 249 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.068 _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 0.22746(14) 1.01888(11) 0.57068(12) 0.0208(3) Uani 1 1 d . . . C2 C 0.32406(16) 1.02557(12) 0.49597(14) 0.0275(3) Uani 1 1 d . . . H2A H 0.3272 0.9712 0.4472 0.033 Uiso 1 1 calc R . . H2B H 0.4028 1.0397 0.5337 0.033 Uiso 1 1 calc R . . C3 C 0.26109(17) 1.11108(15) 0.44250(18) 0.0394(4) Uani 1 1 d U . . H3A H 0.2296 1.1003 0.3665 0.047 Uiso 1 1 calc R . . H3B H 0.3089 1.1690 0.4496 0.047 Uiso 1 1 calc R . . C4 C 0.16617(15) 1.10656(12) 0.52134(13) 0.0244(3) Uani 1 1 d . . . H4A H 0.1676 1.1604 0.5714 0.029 Uiso 1 1 calc R . . H4B H 0.0857 1.0950 0.4859 0.029 Uiso 1 1 calc R . . C5 C 0.11430(13) 0.99240(10) 0.77612(12) 0.0178(3) Uani 1 1 d . . . C6 C 0.07615(13) 0.90160(10) 0.82466(12) 0.0191(3) Uani 1 1 d . . . C7 C 0.10950(13) 0.90258(11) 0.93154(12) 0.0206(3) Uani 1 1 d . . . C8 C 0.16809(13) 0.99219(11) 0.96177(12) 0.0209(3) Uani 1 1 d . . . C9 C 0.17321(13) 1.04447(10) 0.87247(12) 0.0204(3) Uani 1 1 d . . . C11 C 0.00864(15) 0.82738(11) 0.75929(14) 0.0254(3) Uani 1 1 d . . . H11A H 0.0129 0.7684 0.7997 0.038 Uiso 1 1 calc R . . H11B H 0.0426 0.8185 0.6913 0.038 Uiso 1 1 calc R . . H11C H -0.0737 0.8467 0.7441 0.038 Uiso 1 1 calc R . . C10 C 0.01356(14) 1.04604(11) 0.71237(13) 0.0239(3) Uani 1 1 d . . . H10A H -0.0504 1.0551 0.7575 0.036 Uiso 1 1 calc R . . H10B H -0.0155 1.0102 0.6480 0.036 Uiso 1 1 calc R . . H10C H 0.0421 1.1072 0.6909 0.036 Uiso 1 1 calc R . . C12 C 0.09148(17) 0.82668(13) 1.01122(15) 0.0313(4) Uani 1 1 d . . . H12A H 0.0380 0.8490 1.0618 0.047 Uiso 1 1 calc R . . H12B H 0.1673 0.8099 1.0509 0.047 Uiso 1 1 calc R . . H12C H 0.0574 0.7715 0.9729 0.047 Uiso 1 1 calc R . . C13 C 0.21013(16) 1.01951(13) 1.07527(14) 0.0299(4) Uani 1 1 d . . . H13A H 0.2733 1.0659 1.0751 0.045 Uiso 1 1 calc R . . H13B H 0.2399 0.9640 1.1156 0.045 Uiso 1 1 calc R . . H13C H 0.1448 1.0466 1.1094 0.045 Uiso 1 1 calc R . . C14 C 0.22553(17) 1.13988(12) 0.86422(16) 0.0313(4) Uani 1 1 d . . . H14A H 0.1636 1.1844 0.8382 0.047 Uiso 1 1 calc R . . H14B H 0.2853 1.1381 0.8137 0.047 Uiso 1 1 calc R . . H14C H 0.2620 1.1596 0.9353 0.047 Uiso 1 1 calc R . . C15 C 0.55543(15) 0.79015(12) 0.80982(14) 0.0284(3) Uani 1 1 d . . . C16 C 0.41308(14) 0.89743(11) 0.92565(13) 0.0219(3) Uani 1 1 d . . . C17 C 0.30490(14) 0.75022(11) 0.78861(13) 0.0237(3) Uani 1 1 d . . . C18 C 0.42401(15) 0.82559(11) 0.60946(13) 0.0248(3) Uani 1 1 d . . . C19 C 0.50407(14) 0.98376(12) 0.74367(13) 0.0236(3) Uani 1 1 d U . . Mo Mo 0.409497(11) 0.864556(8) 0.764854(10) 0.01693(5) Uani 1 1 d U . . O1 O 0.16406(10) 0.92925(7) 0.57338(9) 0.0227(2) Uani 1 1 d . . . O2 O 0.63846(13) 0.74795(11) 0.83572(13) 0.0473(4) Uani 1 1 d U . . O3 O 0.42683(12) 0.91040(9) 1.01589(10) 0.0330(3) Uani 1 1 d . . . O4 O 0.24739(12) 0.68821(9) 0.80293(12) 0.0354(3) Uani 1 1 d . . . O5 O 0.43719(13) 0.80395(9) 0.52381(11) 0.0376(3) Uani 1 1 d . . . O6 O 0.55371(13) 1.05117(10) 0.73173(11) 0.0371(3) Uani 1 1 d . . . P P 0.23314(3) 0.95559(3) 0.69500(3) 0.01668(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0240(7) 0.0193(7) 0.0188(7) 0.0016(6) 0.0000(6) 0.0007(6) C2 0.0309(8) 0.0294(8) 0.0229(8) 0.0060(7) 0.0071(7) 0.0041(7) C3 0.0322(9) 0.0437(10) 0.0431(10) 0.0219(8) 0.0080(8) 0.0056(7) C4 0.0247(8) 0.0237(7) 0.0235(8) 0.0053(6) -0.0029(6) 0.0021(6) C5 0.0182(6) 0.0164(6) 0.0189(7) -0.0009(5) 0.0021(5) 0.0008(5) C6 0.0170(6) 0.0176(6) 0.0228(7) -0.0001(6) 0.0028(5) 0.0013(5) C7 0.0178(7) 0.0214(7) 0.0229(7) 0.0014(6) 0.0041(6) 0.0008(6) C8 0.0175(6) 0.0247(7) 0.0206(7) -0.0037(6) 0.0021(6) 0.0013(6) C9 0.0197(7) 0.0195(7) 0.0221(7) -0.0050(6) 0.0031(6) -0.0005(5) C11 0.0240(7) 0.0214(7) 0.0302(8) -0.0024(7) -0.0001(6) -0.0038(6) C10 0.0221(7) 0.0233(7) 0.0261(8) 0.0020(6) 0.0012(6) 0.0069(6) C12 0.0373(9) 0.0297(9) 0.0273(9) 0.0071(7) 0.0058(7) -0.0016(7) C13 0.0276(8) 0.0406(10) 0.0213(8) -0.0076(7) 0.0024(6) -0.0008(7) C14 0.0370(9) 0.0229(8) 0.0341(9) -0.0057(7) 0.0048(7) -0.0068(7) C15 0.0275(8) 0.0302(8) 0.0268(8) -0.0041(7) -0.0001(7) 0.0081(7) C16 0.0233(7) 0.0200(7) 0.0222(8) -0.0009(6) 0.0018(6) 0.0026(6) C17 0.0230(7) 0.0198(7) 0.0277(8) 0.0011(6) 0.0001(6) 0.0040(6) C18 0.0276(8) 0.0213(7) 0.0254(8) -0.0027(6) 0.0026(6) 0.0018(6) C19 0.0231(7) 0.0292(8) 0.0183(7) -0.0006(6) 0.0009(6) -0.0023(6) Mo 0.01763(7) 0.01614(7) 0.01679(7) -0.00070(5) 0.00087(4) 0.00255(4) O1 0.0286(6) 0.0196(5) 0.0187(5) -0.0008(4) -0.0022(4) -0.0015(4) O2 0.0370(7) 0.0536(8) 0.0491(8) -0.0060(7) -0.0052(6) 0.0238(7) O3 0.0387(7) 0.0379(7) 0.0216(6) -0.0038(5) -0.0004(5) 0.0062(6) O4 0.0316(7) 0.0239(6) 0.0503(8) 0.0038(6) 0.0021(6) -0.0022(5) O5 0.0523(8) 0.0347(7) 0.0267(6) -0.0091(6) 0.0086(6) 0.0011(6) O6 0.0414(7) 0.0379(7) 0.0318(7) 0.0029(6) 0.0024(6) -0.0168(6) P 0.01840(17) 0.01547(16) 0.01590(17) 0.00028(13) 0.00069(14) 0.00137(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 1.4734(18) . ? C1 C2 1.526(2) . ? C1 C4 1.531(2) . ? C1 P 1.7915(16) . ? C2 C3 1.533(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.546(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C9 1.509(2) . ? C5 C6 1.516(2) . ? C5 C10 1.532(2) . ? C5 P 1.8588(14) . ? C6 C7 1.347(2) . ? C6 C11 1.499(2) . ? C7 C8 1.474(2) . ? C7 C12 1.501(2) . ? C8 C9 1.349(2) . ? C8 C13 1.498(2) . ? C9 C14 1.496(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O2 1.141(2) . ? C15 Mo 2.0064(17) . ? C16 O3 1.136(2) . ? C16 Mo 2.0584(16) . ? C17 O4 1.129(2) . ? C17 Mo 2.0650(16) . ? C18 O5 1.139(2) . ? C18 Mo 2.0432(16) . ? C19 O6 1.136(2) . ? C19 Mo 2.0497(16) . ? Mo P 2.4768(4) . ? O1 P 1.6760(12) . ? 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 117.38(13) . . ? O1 C1 C4 120.98(13) . . ? C2 C1 C4 91.90(12) . . ? O1 C1 P 60.85(7) . . ? C2 C1 P 127.01(12) . . ? C4 C1 P 137.11(12) . . ? C1 C2 C3 88.79(13) . . ? C1 C2 H2A 113.8 . . ? C3 C2 H2A 113.8 . . ? C1 C2 H2B 113.8 . . ? C3 C2 H2B 113.8 . . ? H2A C2 H2B 111.1 . . ? C2 C3 C4 91.07(13) . . ? C2 C3 H3A 113.5 . . ? C4 C3 H3A 113.5 . . ? C2 C3 H3B 113.5 . . ? C4 C3 H3B 113.5 . . ? H3A C3 H3B 110.8 . . ? C1 C4 C3 88.15(13) . . ? C1 C4 H4A 114.0 . . ? C3 C4 H4A 114.0 . . ? C1 C4 H4B 114.0 . . ? C3 C4 H4B 114.0 . . ? H4A C4 H4B 111.2 . . ? C9 C5 C6 103.04(12) . . ? C9 C5 C10 114.36(12) . . ? C6 C5 C10 113.73(13) . . ? C9 C5 P 106.54(10) . . ? C6 C5 P 103.67(9) . . ? C10 C5 P 114.32(10) . . ? C7 C6 C11 128.28(14) . . ? C7 C6 C5 108.96(13) . . ? C11 C6 C5 122.73(14) . . ? C6 C7 C8 109.50(13) . . ? C6 C7 C12 127.22(15) . . ? C8 C7 C12 123.28(15) . . ? C9 C8 C7 109.18(14) . . ? C9 C8 C13 126.86(15) . . ? C7 C8 C13 123.92(14) . . ? C8 C9 C14 127.95(15) . . ? C8 C9 C5 109.30(13) . . ? C14 C9 C5 122.74(14) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 Mo 179.79(17) . . ? O3 C16 Mo 172.28(14) . . ? O4 C17 Mo 179.05(15) . . ? O5 C18 Mo 177.07(15) . . ? O6 C19 Mo 178.13(15) . . ? C15 Mo C18 88.25(7) . . ? C15 Mo C19 92.35(7) . . ? C18 Mo C19 90.24(6) . . ? C15 Mo C16 85.47(7) . . ? C18 Mo C16 173.64(6) . . ? C19 Mo C16 89.00(6) . . ? C15 Mo C17 91.07(7) . . ? C18 Mo C17 91.73(7) . . ? C19 Mo C17 176.10(6) . . ? C16 Mo C17 89.41(6) . . ? C15 Mo P 175.62(5) . . ? C18 Mo P 87.51(5) . . ? C19 Mo P 86.55(5) . . ? C16 Mo P 98.74(4) . . ? C17 Mo P 90.18(4) . . ? C1 O1 P 68.99(8) . . ? O1 P C1 50.15(6) . . ? O1 P C5 104.90(6) . . ? C1 P C5 111.77(7) . . ? O1 P Mo 119.08(4) . . ? C1 P Mo 121.36(5) . . ? C5 P Mo 124.95(5) . . ? 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 124.48(15) . . . . ? C4 C1 C2 C3 -2.19(15) . . . . ? P C1 C2 C3 -162.76(14) . . . . ? C1 C2 C3 C4 2.17(14) . . . . ? O1 C1 C4 C3 -121.66(16) . . . . ? C2 C1 C4 C3 2.17(14) . . . . ? P C1 C4 C3 159.20(17) . . . . ? C2 C3 C4 C1 -2.16(14) . . . . ? C9 C5 C6 C7 -0.42(15) . . . . ? C10 C5 C6 C7 -124.76(14) . . . . ? P C5 C6 C7 110.50(12) . . . . ? C9 C5 C6 C11 177.67(13) . . . . ? C10 C5 C6 C11 53.32(18) . . . . ? P C5 C6 C11 -71.41(15) . . . . ? C11 C6 C7 C8 -176.67(14) . . . . ? C5 C6 C7 C8 1.27(16) . . . . ? C11 C6 C7 C12 3.0(3) . . . . ? C5 C6 C7 C12 -179.08(15) . . . . ? C6 C7 C8 C9 -1.75(17) . . . . ? C12 C7 C8 C9 178.59(15) . . . . ? C6 C7 C8 C13 176.26(14) . . . . ? C12 C7 C8 C13 -3.4(2) . . . . ? C7 C8 C9 C14 -179.54(15) . . . . ? C13 C8 C9 C14 2.5(3) . . . . ? C7 C8 C9 C5 1.43(17) . . . . ? C13 C8 C9 C5 -176.50(14) . . . . ? C6 C5 C9 C8 -0.67(15) . . . . ? C10 C5 C9 C8 123.26(14) . . . . ? P C5 C9 C8 -109.44(12) . . . . ? C6 C5 C9 C14 -179.76(14) . . . . ? C10 C5 C9 C14 -55.83(19) . . . . ? P C5 C9 C14 71.47(16) . . . . ? O2 C15 Mo C18 169(100) . . . . ? O2 C15 Mo C19 79(74) . . . . ? O2 C15 Mo C16 -10(74) . . . . ? O2 C15 Mo C17 -99(100) . . . . ? O2 C15 Mo P 154(100) . . . . ? O5 C18 Mo C15 -34(3) . . . . ? O5 C18 Mo C19 59(3) . . . . ? O5 C18 Mo C16 -24(3) . . . . ? O5 C18 Mo C17 -125(3) . . . . ? O5 C18 Mo P 145(3) . . . . ? O6 C19 Mo C15 -168(4) . . . . ? O6 C19 Mo C18 104(4) . . . . ? O6 C19 Mo C16 -83(4) . . . . ? O6 C19 Mo C17 -17(5) . . . . ? O6 C19 Mo P 16(4) . . . . ? O3 C16 Mo C15 5.6(11) . . . . ? O3 C16 Mo C18 -3.7(15) . . . . ? O3 C16 Mo C19 -86.9(11) . . . . ? O3 C16 Mo C17 96.7(11) . . . . ? O3 C16 Mo P -173.2(11) . . . . ? O4 C17 Mo C15 101(9) . . . . ? O4 C17 Mo C18 -171(100) . . . . ? O4 C17 Mo C19 -50(10) . . . . ? O4 C17 Mo C16 16(9) . . . . ? O4 C17 Mo P -83(9) . . . . ? C2 C1 O1 P 119.16(14) . . . . ? C4 C1 O1 P -130.07(14) . . . . ? C1 O1 P C5 106.12(9) . . . . ? C1 O1 P Mo -108.15(7) . . . . ? C2 C1 P O1 -103.83(16) . . . . ? C4 C1 P O1 105.40(19) . . . . ? O1 C1 P C5 -91.57(8) . . . . ? C2 C1 P C5 164.60(14) . . . . ? C4 C1 P C5 13.83(19) . . . . ? O1 C1 P Mo 103.46(7) . . . . ? C2 C1 P Mo -0.37(17) . . . . ? C4 C1 P Mo -151.14(15) . . . . ? C9 C5 P O1 -162.78(9) . . . . ? C6 C5 P O1 88.90(10) . . . . ? C10 C5 P O1 -35.45(12) . . . . ? C9 C5 P C1 -110.20(11) . . . . ? C6 C5 P C1 141.48(10) . . . . ? C10 C5 P C1 17.13(13) . . . . ? C9 C5 P Mo 54.13(11) . . . . ? C6 C5 P Mo -54.19(11) . . . . ? C10 C5 P Mo -178.55(9) . . . . ? C15 Mo P O1 34.6(7) . . . . ? C18 Mo P O1 19.83(7) . . . . ? C19 Mo P O1 110.23(6) . . . . ? C16 Mo P O1 -161.32(6) . . . . ? C17 Mo P O1 -71.89(7) . . . . ? C15 Mo P C1 -24.1(7) . . . . ? C18 Mo P C1 -38.86(8) . . . . ? C19 Mo P C1 51.53(8) . . . . ? C16 Mo P C1 139.98(8) . . . . ? C17 Mo P C1 -130.59(8) . . . . ? C15 Mo P C5 173.0(7) . . . . ? C18 Mo P C5 158.22(7) . . . . ? C19 Mo P C5 -111.38(7) . . . . ? C16 Mo P C5 -22.93(7) . . . . ? C17 Mo P C5 66.50(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.304 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.064 data_2056 _database_code_depnum_ccdc_archive 'CCDC 926027' #TrackingRef 'web_deposit_cif_file_0_Dr.GregorSchnakenburg_1361462579.Gesamtcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H23 O6 P W' _chemical_formula_sum 'C20 H23 O6 P W' _chemical_formula_weight 574.20 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 8.9261(3) _cell_length_b 15.2902(6) _cell_length_c 15.7122(5) _cell_angle_alpha 96.922(2) _cell_angle_beta 93.6438(18) _cell_angle_gamma 91.033(2) _cell_volume 2123.78(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7395 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 5.547 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.2400 _exptl_absorpt_correction_T_max 0.6653 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _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 'fine slicing \f and \w scans' _diffrn_detector_area_resol_mean 8.33333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24591 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9177 _reflns_number_gt 7045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker AXS, 2011)' _computing_cell_refinement 'Bruker SAINT (Bruker AXS, 2011)' _computing_data_reduction 'Bruker SAINT (Bruker AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0402P)^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 9177 _refine_ls_number_parameters 515 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.012 _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 0.9473(6) 0.8228(4) 0.3565(3) 0.0212(12) Uani 1 1 d . . . C2 C 0.9025(6) 0.8152(4) 0.4472(3) 0.0229(12) Uani 1 1 d . . . H2A H 0.7922 0.8081 0.4487 0.028 Uiso 1 1 calc R . . H2B H 0.9376 0.8676 0.4873 0.028 Uiso 1 1 calc R . . C3 C 0.9820(6) 0.7323(4) 0.4698(4) 0.0304(14) Uani 1 1 d . . . H3A H 0.9928 0.7312 0.5327 0.036 Uiso 1 1 calc R . . H3B H 0.9269 0.6783 0.4427 0.036 Uiso 1 1 calc R . . C4 C 1.1337(6) 0.7412(4) 0.4330(4) 0.0298(14) Uani 1 1 d . . . H4A H 1.1809 0.6831 0.4227 0.036 Uiso 1 1 calc R . . H4B H 1.2019 0.7814 0.4725 0.036 Uiso 1 1 calc R . . C5 C 1.0996(6) 0.7793(4) 0.3481(3) 0.0232(13) Uani 1 1 d . . . H5A H 1.1781 0.8232 0.3393 0.028 Uiso 1 1 calc R . . H5B H 1.0947 0.7319 0.2991 0.028 Uiso 1 1 calc R . . C6 C 0.9493(6) 0.9076(3) 0.1898(3) 0.0182(11) Uani 1 1 d . . . C7 C 0.8248(6) 0.9079(4) 0.1193(3) 0.0227(12) Uani 1 1 d . . . C8 C 0.8284(6) 0.9865(4) 0.0884(3) 0.0209(12) Uani 1 1 d . . . C9 C 0.9477(6) 1.0435(4) 0.1363(3) 0.0211(12) Uani 1 1 d . . . C10 C 1.0167(6) 0.9996(4) 0.1965(3) 0.0214(12) Uani 1 1 d . . . C11 C 1.0601(7) 0.8379(4) 0.1630(3) 0.0337(15) Uani 1 1 d . . . H11A H 1.0897 0.8445 0.1051 0.040 Uiso 1 1 calc R . . H11B H 1.0135 0.7794 0.1632 0.040 Uiso 1 1 calc R . . H11C H 1.1490 0.8445 0.2033 0.040 Uiso 1 1 calc R . . C12 C 0.7285(7) 0.8275(4) 0.0873(4) 0.0357(15) Uani 1 1 d . . . H12A H 0.6725 0.8099 0.1345 0.043 Uiso 1 1 calc R . . H12B H 0.7924 0.7793 0.0661 0.043 Uiso 1 1 calc R . . H12C H 0.6578 0.8409 0.0406 0.043 Uiso 1 1 calc R . . C13 C 0.7335(6) 1.0137(4) 0.0144(3) 0.0324(15) Uani 1 1 d . . . H13A H 0.6578 0.9673 -0.0058 0.039 Uiso 1 1 calc R . . H13B H 0.7972 1.0229 -0.0325 0.039 Uiso 1 1 calc R . . H13C H 0.6834 1.0686 0.0330 0.039 Uiso 1 1 calc R . . C14 C 0.9837(7) 1.1345(4) 0.1164(4) 0.0307(14) Uani 1 1 d . . . H14A H 0.8968 1.1717 0.1261 0.037 Uiso 1 1 calc R . . H14B H 1.0079 1.1319 0.0562 0.037 Uiso 1 1 calc R . . H14C H 1.0700 1.1593 0.1537 0.037 Uiso 1 1 calc R . . C15 C 1.1448(6) 1.0311(4) 0.2613(3) 0.0287(14) Uani 1 1 d . . . H15C H 1.2009 1.0791 0.2405 0.034 Uiso 1 1 calc R . . H15B H 1.2119 0.9822 0.2690 0.034 Uiso 1 1 calc R . . H15A H 1.1046 1.0525 0.3164 0.034 Uiso 1 1 calc R . . C16 C 0.4981(6) 1.0826(4) 0.3834(3) 0.0214(12) Uani 1 1 d U . . C17 C 0.7609(6) 1.0167(4) 0.4612(4) 0.0235(12) Uani 1 1 d . . . C18 C 0.5381(6) 0.8963(4) 0.3746(3) 0.0222(11) Uani 1 1 d U . . C19 C 0.5436(6) 0.9793(4) 0.2226(4) 0.0269(13) Uani 1 1 d . . . C20 C 0.7723(6) 1.1079(4) 0.3102(3) 0.0228(12) Uani 1 1 d . . . C21 C 0.6547(7) 1.4125(4) 0.0659(4) 0.0335(15) Uani 1 1 d . . . C22 C 0.5756(7) 1.3380(4) 0.0079(3) 0.0299(14) Uani 1 1 d . . . H22A H 0.4916 1.3598 -0.0273 0.036 Uiso 1 1 calc R . . H22B H 0.5358 1.2931 0.0417 0.036 Uiso 1 1 calc R . . C23 C 0.6973(7) 1.2999(4) -0.0486(4) 0.0391(16) Uani 1 1 d . . . H23A H 0.7596 1.2584 -0.0189 0.047 Uiso 1 1 calc R . . H23B H 0.6529 1.2688 -0.1036 0.047 Uiso 1 1 calc R . . C24 C 0.7882(8) 1.3796(5) -0.0631(4) 0.0445(19) Uani 1 1 d . . . H24A H 0.7377 1.4109 -0.1080 0.053 Uiso 1 1 calc R . . H24B H 0.8894 1.3629 -0.0807 0.053 Uiso 1 1 calc R . . C25 C 0.7983(6) 1.4377(4) 0.0253(3) 0.0311(14) Uani 1 1 d . . . H25B H 0.8888 1.4244 0.0608 0.037 Uiso 1 1 calc R . . H25A H 0.8010 1.5012 0.0180 0.037 Uiso 1 1 calc R . . C26 C 0.7340(6) 1.5206(4) 0.2408(3) 0.0279(13) Uani 1 1 d . . . C27 C 0.6327(6) 1.5846(4) 0.2899(4) 0.0269(13) Uani 1 1 d . . . C28 C 0.6519(6) 1.5775(4) 0.3731(4) 0.0252(13) Uani 1 1 d . . . C29 C 0.7593(6) 1.5087(4) 0.3878(4) 0.0265(13) Uani 1 1 d . . . C30 C 0.8082(6) 1.4751(4) 0.3117(4) 0.0286(13) Uani 1 1 d . . . C31 C 0.8442(8) 1.5717(5) 0.1935(4) 0.0467(18) Uani 1 1 d . . . H31A H 0.8833 1.6239 0.2313 0.056 Uiso 1 1 calc R . . H31B H 0.7923 1.5902 0.1420 0.056 Uiso 1 1 calc R . . H31C H 0.9275 1.5339 0.1767 0.056 Uiso 1 1 calc R . . C32 C 0.5361(7) 1.6492(4) 0.2461(4) 0.0418(17) Uani 1 1 d . . . H32A H 0.4831 1.6184 0.1943 0.050 Uiso 1 1 calc R . . H32B H 0.6001 1.6967 0.2303 0.050 Uiso 1 1 calc R . . H32C H 0.4629 1.6742 0.2855 0.050 Uiso 1 1 calc R . . C33 C 0.5779(7) 1.6279(5) 0.4467(4) 0.0429(17) Uani 1 1 d . . . H33A H 0.4971 1.6630 0.4241 0.051 Uiso 1 1 calc R . . H33B H 0.6524 1.6671 0.4815 0.051 Uiso 1 1 calc R . . H33C H 0.5361 1.5864 0.4824 0.051 Uiso 1 1 calc R . . C34 C 0.8040(7) 1.4845(5) 0.4747(4) 0.0441(18) Uani 1 1 d . . . H34A H 0.7153 1.4634 0.5006 0.053 Uiso 1 1 calc R . . H34B H 0.8481 1.5364 0.5111 0.053 Uiso 1 1 calc R . . H34C H 0.8780 1.4380 0.4697 0.053 Uiso 1 1 calc R . . C35 C 0.9184(7) 1.4026(5) 0.2929(5) 0.053(2) Uani 1 1 d . . . H35C H 0.9493 1.3786 0.3462 0.063 Uiso 1 1 calc R . . H35A H 1.0067 1.4264 0.2687 0.063 Uiso 1 1 calc R . . H35B H 0.8706 1.3556 0.2516 0.063 Uiso 1 1 calc R . . C36 C 0.2569(6) 1.2874(4) 0.2961(3) 0.0237(13) Uani 1 1 d . . . C37 C 0.4840(7) 1.2352(4) 0.1841(3) 0.0262(12) Uani 1 1 d U . . C38 C 0.2716(6) 1.3608(4) 0.1375(4) 0.0275(13) Uani 1 1 d . . . C39 C 0.3330(6) 1.4681(4) 0.2968(3) 0.0244(12) Uani 1 1 d . . . C40 C 0.5576(6) 1.3304(4) 0.3435(3) 0.0218(12) Uani 1 1 d . . . O1 O 0.8280(4) 0.7875(2) 0.2897(2) 0.0235(9) Uani 1 1 d . . . O2 O 0.4084(4) 1.1301(3) 0.4076(3) 0.0353(10) Uani 1 1 d . . . O3 O 0.8141(5) 1.0276(3) 0.5305(2) 0.0344(10) Uani 1 1 d . . . O4 O 0.4672(4) 0.8402(3) 0.3943(3) 0.0353(10) Uani 1 1 d . . . O5 O 0.4727(4) 0.9646(3) 0.1588(3) 0.0379(11) Uani 1 1 d . . . O6 O 0.8295(5) 1.1725(3) 0.2980(3) 0.0367(11) Uani 1 1 d . . . O7 O 0.5469(5) 1.4885(3) 0.0881(3) 0.0398(11) Uani 1 1 d . . . O8 O 0.1663(4) 1.2524(3) 0.3288(3) 0.0352(10) Uani 1 1 d . . . O9 O 0.5187(6) 1.1677(3) 0.1520(3) 0.0459(12) Uani 1 1 d . . . O10 O 0.1875(5) 1.3630(3) 0.0788(3) 0.0443(12) Uani 1 1 d . . . O11 O 0.2773(5) 1.5310(3) 0.3241(3) 0.0372(11) Uani 1 1 d . . . O12 O 0.6326(4) 1.3096(3) 0.3991(2) 0.0315(10) Uani 1 1 d . . . P1 P 0.85437(14) 0.89598(9) 0.29037(8) 0.0168(3) Uani 1 1 d . . . P2 P 0.60392(19) 1.43917(11) 0.17515(10) 0.0328(4) Uani 1 1 d . . . W1 W 0.65838(2) 0.999691(14) 0.340531(12) 0.01691(7) Uani 1 1 d U . . W2 W 0.41522(2) 1.352301(14) 0.241324(13) 0.01951(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 0.018(3) 0.026(3) 0.022(3) 0.007(2) 0.007(2) 0.003(2) C2 0.020(3) 0.030(3) 0.021(3) 0.008(2) 0.007(2) 0.005(3) C3 0.029(3) 0.041(4) 0.025(3) 0.017(3) 0.005(3) 0.001(3) C4 0.023(3) 0.037(4) 0.032(3) 0.012(3) 0.004(3) 0.009(3) C5 0.018(3) 0.033(3) 0.020(3) 0.008(2) 0.003(2) 0.005(3) C6 0.020(3) 0.024(3) 0.012(2) 0.003(2) 0.007(2) 0.004(2) C7 0.026(3) 0.030(3) 0.011(3) -0.001(2) 0.003(2) 0.002(3) C8 0.023(3) 0.026(3) 0.013(3) 0.000(2) 0.003(2) 0.002(2) C9 0.021(3) 0.027(3) 0.016(3) 0.003(2) 0.010(2) 0.002(2) C10 0.021(3) 0.031(3) 0.013(3) 0.005(2) 0.007(2) 0.004(3) C11 0.043(4) 0.039(4) 0.022(3) 0.007(3) 0.015(3) 0.016(3) C12 0.042(4) 0.040(4) 0.024(3) 0.001(3) 0.005(3) -0.008(3) C13 0.028(3) 0.049(4) 0.020(3) 0.006(3) 0.001(2) 0.006(3) C14 0.038(3) 0.029(3) 0.027(3) 0.011(3) 0.006(3) -0.002(3) C15 0.018(3) 0.046(4) 0.022(3) 0.006(3) 0.000(2) -0.003(3) C16 0.020(3) 0.024(3) 0.020(3) 0.006(2) 0.002(2) 0.002(2) C17 0.021(3) 0.026(3) 0.024(3) 0.003(2) 0.005(2) -0.001(2) C18 0.014(3) 0.025(3) 0.028(3) 0.002(2) 0.002(2) 0.001(2) C19 0.016(3) 0.038(4) 0.028(3) 0.007(3) 0.005(2) 0.006(3) C20 0.018(3) 0.028(3) 0.022(3) 0.000(2) 0.004(2) 0.006(3) C21 0.045(4) 0.034(4) 0.022(3) 0.002(3) 0.014(3) -0.008(3) C22 0.034(3) 0.034(4) 0.022(3) -0.002(3) 0.007(3) 0.006(3) C23 0.042(4) 0.042(4) 0.032(3) -0.002(3) 0.007(3) 0.009(3) C24 0.050(4) 0.062(5) 0.023(3) 0.000(3) 0.019(3) 0.019(4) C25 0.026(3) 0.044(4) 0.026(3) 0.008(3) 0.010(3) 0.002(3) C26 0.032(3) 0.029(3) 0.023(3) 0.004(3) 0.010(3) -0.009(3) C27 0.025(3) 0.024(3) 0.029(3) 0.002(3) -0.007(2) -0.003(3) C28 0.018(3) 0.026(3) 0.030(3) -0.006(2) 0.002(2) -0.004(2) C29 0.022(3) 0.025(3) 0.033(3) 0.010(3) -0.003(2) -0.009(3) C30 0.013(3) 0.024(3) 0.048(4) 0.000(3) 0.005(3) -0.001(2) C31 0.057(4) 0.043(4) 0.039(4) -0.001(3) 0.015(3) -0.025(4) C32 0.044(4) 0.030(4) 0.051(4) 0.015(3) -0.014(3) -0.007(3) C33 0.033(3) 0.043(4) 0.049(4) -0.013(3) 0.016(3) -0.013(3) C34 0.043(4) 0.053(5) 0.038(4) 0.026(3) -0.016(3) -0.019(3) C35 0.026(3) 0.038(4) 0.092(6) -0.003(4) 0.008(4) 0.003(3) C36 0.018(3) 0.027(3) 0.026(3) 0.001(3) 0.001(2) 0.007(3) C37 0.036(3) 0.024(3) 0.020(3) 0.004(2) 0.002(2) -0.001(3) C38 0.031(3) 0.025(3) 0.027(3) 0.003(3) 0.004(3) 0.006(3) C39 0.023(3) 0.025(3) 0.025(3) 0.001(2) 0.001(2) -0.003(3) C40 0.022(3) 0.021(3) 0.024(3) 0.002(2) 0.007(2) 0.000(2) O1 0.024(2) 0.024(2) 0.023(2) 0.0041(17) 0.0000(16) -0.0008(17) O2 0.023(2) 0.042(3) 0.041(2) 0.003(2) 0.0087(19) 0.015(2) O3 0.038(2) 0.041(3) 0.024(2) 0.0021(19) -0.0011(19) 0.005(2) O4 0.026(2) 0.036(3) 0.046(3) 0.011(2) 0.009(2) -0.007(2) O5 0.026(2) 0.060(3) 0.028(2) 0.005(2) -0.0025(19) 0.007(2) O6 0.038(2) 0.025(3) 0.050(3) 0.007(2) 0.022(2) 0.003(2) O7 0.047(3) 0.041(3) 0.033(2) 0.010(2) 0.005(2) 0.010(2) O8 0.026(2) 0.036(3) 0.047(3) 0.012(2) 0.013(2) 0.003(2) O9 0.069(3) 0.030(3) 0.039(3) 0.000(2) 0.009(2) 0.012(3) O10 0.041(3) 0.059(3) 0.032(2) 0.010(2) -0.009(2) 0.005(2) O11 0.032(2) 0.035(3) 0.044(3) -0.004(2) 0.007(2) 0.003(2) O12 0.034(2) 0.035(3) 0.027(2) 0.0093(19) 0.0008(19) 0.007(2) P1 0.0159(6) 0.0204(7) 0.0147(6) 0.0029(6) 0.0034(5) 0.0021(6) P2 0.0404(9) 0.0343(10) 0.0234(8) 0.0003(7) 0.0105(7) -0.0112(8) W1 0.01382(11) 0.02195(13) 0.01577(12) 0.00392(9) 0.00340(8) 0.00265(9) W2 0.01981(12) 0.02121(14) 0.01806(12) 0.00361(9) 0.00338(9) 0.00004(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.492(6) . ? C1 C2 1.522(7) . ? C1 C5 1.530(6) . ? C1 P1 1.796(5) . ? C2 C3 1.530(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.533(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.507(7) . ? C6 C10 1.509(8) . ? C6 C7 1.519(7) . ? C6 P1 1.866(5) . ? C7 C8 1.349(7) . ? C7 C12 1.504(8) . ? C8 C9 1.473(8) . ? C8 C13 1.499(7) . ? C9 C10 1.349(7) . ? C9 C14 1.495(8) . ? C10 C15 1.514(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 O2 1.143(6) . ? C16 W1 2.022(5) . ? C17 O3 1.151(6) . ? C17 W1 2.038(6) . ? C18 O4 1.141(7) . ? C18 W1 2.038(6) . ? C19 O5 1.147(7) . ? C19 W1 2.046(6) . ? C20 O6 1.146(7) . ? C20 W1 2.047(6) . ? C21 C22 1.506(9) . ? C21 C25 1.532(8) . ? C21 O7 1.544(7) . ? C21 P2 1.804(6) . ? C22 C23 1.526(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.500(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.553(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25B 0.9900 . ? C25 H25A 0.9900 . ? C26 C30 1.508(8) . ? C26 C27 1.520(8) . ? C26 C31 1.529(8) . ? C26 P2 1.857(6) . ? C27 C28 1.327(7) . ? C27 C32 1.519(7) . ? C28 C29 1.465(7) . ? C28 C33 1.506(8) . ? C29 C30 1.345(8) . ? C29 C34 1.490(7) . ? C30 C35 1.510(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 O8 1.144(7) . ? C36 W2 2.008(6) . ? C37 O9 1.149(7) . ? C37 W2 2.028(6) . ? C38 O10 1.155(6) . ? C38 W2 2.028(6) . ? C39 O11 1.141(6) . ? C39 W2 2.046(6) . ? C40 O12 1.147(6) . ? C40 W2 2.046(5) . ? O1 P1 1.669(4) . ? O7 P2 1.696(4) . ? P1 W1 2.4840(12) . ? P2 W2 2.4813(16) . ? 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 112.4(4) . . ? O1 C1 C5 114.9(4) . . ? C2 C1 C5 106.7(4) . . ? O1 C1 P1 60.2(2) . . ? C2 C1 P1 121.6(3) . . ? C5 C1 P1 129.7(4) . . ? C1 C2 C3 103.1(4) . . ? C1 C2 H2A 111.1 . . ? C3 C2 H2A 111.1 . . ? C1 C2 H2B 111.1 . . ? C3 C2 H2B 111.1 . . ? H2A C2 H2B 109.1 . . ? C4 C3 C2 102.8(4) . . ? C4 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? C3 C4 C5 104.7(4) . . ? C3 C4 H4A 110.8 . . ? C5 C4 H4A 110.8 . . ? C3 C4 H4B 110.8 . . ? C5 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C1 C5 C4 105.5(4) . . ? C1 C5 H5A 110.6 . . ? C4 C5 H5A 110.6 . . ? C1 C5 H5B 110.6 . . ? C4 C5 H5B 110.6 . . ? H5A C5 H5B 108.8 . . ? C11 C6 C10 112.4(5) . . ? C11 C6 C7 109.4(4) . . ? C10 C6 C7 103.0(4) . . ? C11 C6 P1 116.5(3) . . ? C10 C6 P1 108.4(3) . . ? C7 C6 P1 106.1(3) . . ? C8 C7 C12 128.6(5) . . ? C8 C7 C6 108.8(5) . . ? C12 C7 C6 122.3(5) . . ? C7 C8 C9 109.6(4) . . ? C7 C8 C13 127.2(5) . . ? C9 C8 C13 123.1(5) . . ? C10 C9 C8 109.2(5) . . ? C10 C9 C14 127.8(5) . . ? C8 C9 C14 123.0(5) . . ? C9 C10 C6 109.4(5) . . ? C9 C10 C15 128.5(5) . . ? C6 C10 C15 122.1(4) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15C 109.5 . . ? C10 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C10 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? O2 C16 W1 179.4(5) . . ? O3 C17 W1 177.5(5) . . ? O4 C18 W1 177.9(4) . . ? O5 C19 W1 175.5(5) . . ? O6 C20 W1 174.4(5) . . ? C22 C21 C25 108.5(5) . . ? C22 C21 O7 111.0(5) . . ? C25 C21 O7 115.6(5) . . ? C22 C21 P2 120.6(4) . . ? C25 C21 P2 128.8(5) . . ? O7 C21 P2 60.3(2) . . ? C21 C22 C23 104.0(5) . . ? C21 C22 H22A 110.9 . . ? C23 C22 H22A 110.9 . . ? C21 C22 H22B 110.9 . . ? C23 C22 H22B 110.9 . . ? H22A C22 H22B 109.0 . . ? C24 C23 C22 103.5(5) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.0 . . ? C23 C24 C25 104.3(5) . . ? C23 C24 H24A 110.9 . . ? C25 C24 H24A 110.9 . . ? C23 C24 H24B 110.9 . . ? C25 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? C21 C25 C24 103.5(5) . . ? C21 C25 H25B 111.1 . . ? C24 C25 H25B 111.1 . . ? C21 C25 H25A 111.1 . . ? C24 C25 H25A 111.1 . . ? H25B C25 H25A 109.0 . . ? C30 C26 C27 102.1(4) . . ? C30 C26 C31 113.6(5) . . ? C27 C26 C31 109.5(5) . . ? C30 C26 P2 107.6(4) . . ? C27 C26 P2 105.0(4) . . ? C31 C26 P2 117.6(4) . . ? C28 C27 C32 128.1(5) . . ? C28 C27 C26 109.2(5) . . ? C32 C27 C26 122.5(5) . . ? C27 C28 C29 110.2(5) . . ? C27 C28 C33 128.7(5) . . ? C29 C28 C33 121.1(5) . . ? C30 C29 C28 108.7(5) . . ? C30 C29 C34 128.1(5) . . ? C28 C29 C34 123.2(5) . . ? C29 C30 C26 109.7(4) . . ? C29 C30 C35 128.9(5) . . ? C26 C30 C35 121.4(5) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35C 109.5 . . ? C30 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O8 C36 W2 178.1(5) . . ? O9 C37 W2 177.8(5) . . ? O10 C38 W2 177.7(5) . . ? O11 C39 W2 174.9(5) . . ? O12 C40 W2 173.2(5) . . ? C1 O1 P1 69.0(3) . . ? C21 O7 P2 67.5(2) . . ? O1 P1 C1 50.8(2) . . ? O1 P1 C6 104.7(2) . . ? C1 P1 C6 113.4(2) . . ? O1 P1 W1 120.45(14) . . ? C1 P1 W1 123.84(17) . . ? C6 P1 W1 121.17(15) . . ? O7 P2 C21 52.2(2) . . ? O7 P2 C26 105.1(2) . . ? C21 P2 C26 113.8(3) . . ? O7 P2 W2 118.13(18) . . ? C21 P2 W2 123.1(2) . . ? C26 P2 W2 121.79(18) . . ? C16 W1 C18 89.7(2) . . ? C16 W1 C17 88.5(2) . . ? C18 W1 C17 88.7(2) . . ? C16 W1 C19 89.7(2) . . ? C18 W1 C19 88.1(2) . . ? C17 W1 C19 176.3(2) . . ? C16 W1 C20 87.3(2) . . ? C18 W1 C20 176.98(19) . . ? C17 W1 C20 90.5(2) . . ? C19 W1 C20 92.7(2) . . ? C16 W1 P1 178.80(14) . . ? C18 W1 P1 89.27(14) . . ? C17 W1 P1 90.75(15) . . ? C19 W1 P1 90.97(15) . . ? C20 W1 P1 93.63(14) . . ? C36 W2 C37 89.1(2) . . ? C36 W2 C38 90.4(2) . . ? C37 W2 C38 89.2(2) . . ? C36 W2 C40 86.8(2) . . ? C37 W2 C40 85.8(2) . . ? C38 W2 C40 174.3(2) . . ? C36 W2 C39 88.6(2) . . ? C37 W2 C39 176.6(2) . . ? C38 W2 C39 88.3(2) . . ? C40 W2 C39 96.5(2) . . ? C36 W2 P2 177.21(15) . . ? C37 W2 P2 93.55(17) . . ? C38 W2 P2 88.81(17) . . ? C40 W2 P2 94.30(16) . . ? C39 W2 P2 88.72(16) . . ? 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 99.3(5) . . . . ? C5 C1 C2 C3 -27.6(6) . . . . ? P1 C1 C2 C3 167.1(4) . . . . ? C1 C2 C3 C4 40.6(6) . . . . ? C2 C3 C4 C5 -38.4(6) . . . . ? O1 C1 C5 C4 -121.2(5) . . . . ? C2 C1 C5 C4 4.1(6) . . . . ? P1 C1 C5 C4 167.9(5) . . . . ? C3 C4 C5 C1 21.3(6) . . . . ? C11 C6 C7 C8 -116.7(5) . . . . ? C10 C6 C7 C8 3.1(5) . . . . ? P1 C6 C7 C8 116.8(4) . . . . ? C11 C6 C7 C12 57.8(6) . . . . ? C10 C6 C7 C12 177.6(5) . . . . ? P1 C6 C7 C12 -68.6(5) . . . . ? C12 C7 C8 C9 -176.1(5) . . . . ? C6 C7 C8 C9 -2.0(6) . . . . ? C12 C7 C8 C13 1.3(9) . . . . ? C6 C7 C8 C13 175.4(5) . . . . ? C7 C8 C9 C10 0.0(6) . . . . ? C13 C8 C9 C10 -177.5(5) . . . . ? C7 C8 C9 C14 178.4(5) . . . . ? C13 C8 C9 C14 0.8(8) . . . . ? C8 C9 C10 C6 2.0(6) . . . . ? C14 C9 C10 C6 -176.3(5) . . . . ? C8 C9 C10 C15 -179.6(5) . . . . ? C14 C9 C10 C15 2.1(9) . . . . ? C11 C6 C10 C9 114.6(5) . . . . ? C7 C6 C10 C9 -3.1(5) . . . . ? P1 C6 C10 C9 -115.2(4) . . . . ? C11 C6 C10 C15 -63.9(6) . . . . ? C7 C6 C10 C15 178.5(4) . . . . ? P1 C6 C10 C15 66.4(5) . . . . ? C25 C21 C22 C23 19.0(6) . . . . ? O7 C21 C22 C23 147.0(4) . . . . ? P2 C21 C22 C23 -146.0(5) . . . . ? C21 C22 C23 C24 -36.6(6) . . . . ? C22 C23 C24 C25 40.3(6) . . . . ? C22 C21 C25 C24 5.3(6) . . . . ? O7 C21 C25 C24 -120.1(5) . . . . ? P2 C21 C25 C24 168.6(5) . . . . ? C23 C24 C25 C21 -28.1(6) . . . . ? C30 C26 C27 C28 1.8(6) . . . . ? C31 C26 C27 C28 -119.0(6) . . . . ? P2 C26 C27 C28 114.0(5) . . . . ? C30 C26 C27 C32 177.8(5) . . . . ? C31 C26 C27 C32 57.1(7) . . . . ? P2 C26 C27 C32 -70.0(6) . . . . ? C32 C27 C28 C29 -177.7(6) . . . . ? C26 C27 C28 C29 -2.0(7) . . . . ? C32 C27 C28 C33 3.4(11) . . . . ? C26 C27 C28 C33 179.2(6) . . . . ? C27 C28 C29 C30 1.3(7) . . . . ? C33 C28 C29 C30 -179.7(5) . . . . ? C27 C28 C29 C34 -179.6(6) . . . . ? C33 C28 C29 C34 -0.7(9) . . . . ? C28 C29 C30 C26 -0.1(7) . . . . ? C34 C29 C30 C26 -179.1(6) . . . . ? C28 C29 C30 C35 -179.5(6) . . . . ? C34 C29 C30 C35 1.6(11) . . . . ? C27 C26 C30 C29 -0.9(6) . . . . ? C31 C26 C30 C29 116.9(6) . . . . ? P2 C26 C30 C29 -111.1(5) . . . . ? C27 C26 C30 C35 178.5(5) . . . . ? C31 C26 C30 C35 -63.7(8) . . . . ? P2 C26 C30 C35 68.3(6) . . . . ? C2 C1 O1 P1 114.6(4) . . . . ? C5 C1 O1 P1 -123.0(4) . . . . ? C22 C21 O7 P2 114.1(4) . . . . ? C25 C21 O7 P2 -121.8(5) . . . . ? C1 O1 P1 C6 108.5(3) . . . . ? C1 O1 P1 W1 -110.7(2) . . . . ? C2 C1 P1 O1 -99.4(5) . . . . ? C5 C1 P1 O1 98.9(6) . . . . ? O1 C1 P1 C6 -90.2(3) . . . . ? C2 C1 P1 C6 170.4(4) . . . . ? C5 C1 P1 C6 8.7(6) . . . . ? O1 C1 P1 W1 104.0(2) . . . . ? C2 C1 P1 W1 4.5(6) . . . . ? C5 C1 P1 W1 -157.1(4) . . . . ? C11 C6 P1 O1 -36.2(5) . . . . ? C10 C6 P1 O1 -164.2(3) . . . . ? C7 C6 P1 O1 85.8(4) . . . . ? C11 C6 P1 C1 17.1(5) . . . . ? C10 C6 P1 C1 -110.9(4) . . . . ? C7 C6 P1 C1 139.1(4) . . . . ? C11 C6 P1 W1 -176.7(4) . . . . ? C10 C6 P1 W1 55.4(4) . . . . ? C7 C6 P1 W1 -54.6(4) . . . . ? C21 O7 P2 C26 108.6(3) . . . . ? C21 O7 P2 W2 -111.7(3) . . . . ? C22 C21 P2 O7 -98.1(5) . . . . ? C25 C21 P2 O7 100.3(6) . . . . ? C22 C21 P2 C26 170.7(4) . . . . ? C25 C21 P2 C26 9.2(7) . . . . ? O7 C21 P2 C26 -91.2(3) . . . . ? C22 C21 P2 W2 3.8(6) . . . . ? C25 C21 P2 W2 -157.8(4) . . . . ? O7 C21 P2 W2 101.9(3) . . . . ? C30 C26 P2 O7 -170.8(3) . . . . ? C27 C26 P2 O7 80.9(4) . . . . ? C31 C26 P2 O7 -41.0(5) . . . . ? C30 C26 P2 C21 -115.9(4) . . . . ? C27 C26 P2 C21 135.9(4) . . . . ? C31 C26 P2 C21 13.9(6) . . . . ? C30 C26 P2 W2 51.2(4) . . . . ? C27 C26 P2 W2 -57.0(4) . . . . ? C31 C26 P2 W2 -179.0(4) . . . . ? O2 C16 W1 C18 164(100) . . . . ? O2 C16 W1 C17 76(41) . . . . ? O2 C16 W1 C19 -108(41) . . . . ? O2 C16 W1 C20 -15(41) . . . . ? O2 C16 W1 P1 129(37) . . . . ? O4 C18 W1 C16 6(13) . . . . ? O4 C18 W1 C17 95(13) . . . . ? O4 C18 W1 C19 -83(13) . . . . ? O4 C18 W1 C20 21(16) . . . . ? O4 C18 W1 P1 -174(100) . . . . ? O3 C17 W1 C16 15(12) . . . . ? O3 C17 W1 C18 -75(12) . . . . ? O3 C17 W1 C19 -46(14) . . . . ? O3 C17 W1 C20 102(12) . . . . ? O3 C17 W1 P1 -164(12) . . . . ? O5 C19 W1 C16 -75(6) . . . . ? O5 C19 W1 C18 15(6) . . . . ? O5 C19 W1 C17 -13(9) . . . . ? O5 C19 W1 C20 -162(6) . . . . ? O5 C19 W1 P1 104(6) . . . . ? O6 C20 W1 C16 22(5) . . . . ? O6 C20 W1 C18 7(8) . . . . ? O6 C20 W1 C17 -67(5) . . . . ? O6 C20 W1 C19 111(5) . . . . ? O6 C20 W1 P1 -157(5) . . . . ? O1 P1 W1 C16 41(8) . . . . ? C1 P1 W1 C16 -20(8) . . . . ? C6 P1 W1 C16 175(8) . . . . ? O1 P1 W1 C18 5.4(2) . . . . ? C1 P1 W1 C18 -55.4(3) . . . . ? C6 P1 W1 C18 139.8(3) . . . . ? O1 P1 W1 C17 94.0(2) . . . . ? C1 P1 W1 C17 33.2(3) . . . . ? C6 P1 W1 C17 -131.6(3) . . . . ? O1 P1 W1 C19 -82.7(2) . . . . ? C1 P1 W1 C19 -143.5(3) . . . . ? C6 P1 W1 C19 51.7(3) . . . . ? O1 P1 W1 C20 -175.4(2) . . . . ? C1 P1 W1 C20 123.7(3) . . . . ? C6 P1 W1 C20 -41.1(3) . . . . ? O8 C36 W2 C37 162(14) . . . . ? O8 C36 W2 C38 -109(14) . . . . ? O8 C36 W2 C40 76(14) . . . . ? O8 C36 W2 C39 -20(14) . . . . ? O8 C36 W2 P2 -36(16) . . . . ? O9 C37 W2 C36 21(13) . . . . ? O9 C37 W2 C38 -69(13) . . . . ? O9 C37 W2 C40 108(13) . . . . ? O9 C37 W2 C39 -26(15) . . . . ? O9 C37 W2 P2 -158(13) . . . . ? O10 C38 W2 C36 -30(12) . . . . ? O10 C38 W2 C37 59(12) . . . . ? O10 C38 W2 C40 30(13) . . . . ? O10 C38 W2 C39 -119(12) . . . . ? O10 C38 W2 P2 153(12) . . . . ? O12 C40 W2 C36 50(4) . . . . ? O12 C40 W2 C37 -40(4) . . . . ? O12 C40 W2 C38 -10(5) . . . . ? O12 C40 W2 C39 138(4) . . . . ? O12 C40 W2 P2 -133(4) . . . . ? O11 C39 W2 C36 -63(5) . . . . ? O11 C39 W2 C37 -16(8) . . . . ? O11 C39 W2 C38 27(5) . . . . ? O11 C39 W2 C40 -150(5) . . . . ? O11 C39 W2 P2 116(5) . . . . ? O7 P2 W2 C36 -61(3) . . . . ? C21 P2 W2 C36 -123(3) . . . . ? C26 P2 W2 C36 71(3) . . . . ? O7 P2 W2 C37 100.4(2) . . . . ? C21 P2 W2 C37 39.1(3) . . . . ? C26 P2 W2 C37 -126.8(3) . . . . ? O7 P2 W2 C38 11.3(2) . . . . ? C21 P2 W2 C38 -50.0(3) . . . . ? C26 P2 W2 C38 144.1(3) . . . . ? O7 P2 W2 C40 -173.5(2) . . . . ? C21 P2 W2 C40 125.2(3) . . . . ? C26 P2 W2 C40 -40.7(3) . . . . ? O7 P2 W2 C39 -77.1(2) . . . . ? C21 P2 W2 C39 -138.4(3) . . . . ? C26 P2 W2 C39 55.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.275 _refine_diff_density_min -2.443 _refine_diff_density_rms 0.191 data_1954 _database_code_depnum_ccdc_archive 'CCDC 926028' #TrackingRef 'web_deposit_cif_file_0_Dr.GregorSchnakenburg_1361462579.Gesamtcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H25 O6 P W' _chemical_formula_sum 'C21 H25 O6 P W' _chemical_formula_weight 588.23 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 9.1477(3) _cell_length_b 15.6150(5) _cell_length_c 15.7502(5) _cell_angle_alpha 92.816(2) _cell_angle_beta 94.137(2) _cell_angle_gamma 95.524(2) _cell_volume 2229.93(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 20137 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 35.63 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 5.285 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5249 _exptl_absorpt_correction_T_max 0.8164 _exptl_absorpt_process_details 'STOE X-RED (STOE&CIE, 2008)' _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 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 481 frames, detector distance = 100 mm ; _diffrn_reflns_number 21498 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10583 _reflns_number_gt 8466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA (STOE&CIE, 2008)' _computing_cell_refinement 'STOE X-AREA (STOE&CIE, 2008)' _computing_data_reduction 'STOE X-RED (STOE&CIE, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND2.1c (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (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^)+(0.0432P)^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 10583 _refine_ls_number_parameters 533 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.004 _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 0.5528(6) -0.0571(3) 0.3397(3) 0.0349(7) Uani 1 1 d U . . C2 C 0.5480(6) -0.1319(4) 0.3980(4) 0.0405(9) Uani 1 1 d U . . H2A H 0.4858 -0.1199 0.4453 0.049 Uiso 1 1 calc R . . H2B H 0.5032 -0.1850 0.3656 0.049 Uiso 1 1 calc R . . C3 C 0.7000(6) -0.1454(4) 0.4339(4) 0.0401(13) Uani 1 1 d . . . H3A H 0.7545 -0.1688 0.3875 0.048 Uiso 1 1 calc R . . H3B H 0.6915 -0.1894 0.4770 0.048 Uiso 1 1 calc R . . C4 C 0.7889(6) -0.0660(4) 0.4747(3) 0.0366(11) Uani 1 1 d U . . H4A H 0.8932 -0.0776 0.4839 0.044 Uiso 1 1 calc R . . H4B H 0.7528 -0.0524 0.5311 0.044 Uiso 1 1 calc R . . C5 C 0.7795(7) 0.0107(4) 0.4206(4) 0.0508(14) Uani 1 1 d U . . H5A H 0.8174 0.0632 0.4565 0.061 Uiso 1 1 calc R . . H5B H 0.8463 0.0051 0.3744 0.061 Uiso 1 1 calc R . . C6 C 0.6353(6) 0.0239(4) 0.3823(4) 0.0402(9) Uani 1 1 d U . . H6A H 0.6467 0.0679 0.3394 0.048 Uiso 1 1 calc R . . H6B H 0.5761 0.0466 0.4269 0.048 Uiso 1 1 calc R . . C7 C 0.3050(5) -0.1495(3) 0.2159(3) 0.0335(11) Uani 1 1 d U . . C8 C 0.1543(6) -0.1391(3) 0.2433(3) 0.0319(11) Uani 1 1 d . . . C9 C 0.0596(5) -0.1349(3) 0.1736(3) 0.0269(10) Uani 1 1 d . . . C10 C 0.1409(5) -0.1415(3) 0.0977(3) 0.0270(10) Uani 1 1 d . . . C11 C 0.2825(5) -0.1484(3) 0.1201(3) 0.0324(11) Uani 1 1 d . . . C12 C 0.3674(7) -0.2359(4) 0.2360(4) 0.0483(13) Uani 1 1 d U . . H12A H 0.3288 -0.2803 0.1917 0.058 Uiso 1 1 calc R . . H12B H 0.3377 -0.2537 0.2915 0.058 Uiso 1 1 calc R . . H12C H 0.4752 -0.2283 0.2373 0.058 Uiso 1 1 calc R . . C13 C 0.1242(7) -0.1382(4) 0.3346(4) 0.0471(14) Uani 1 1 d U . . H13A H 0.1986 -0.0983 0.3678 0.057 Uiso 1 1 calc R . . H13B H 0.1277 -0.1963 0.3550 0.057 Uiso 1 1 calc R . . H13C H 0.0263 -0.1194 0.3412 0.057 Uiso 1 1 calc R . . C14 C -0.1031(5) -0.1283(4) 0.1700(4) 0.0430(14) Uani 1 1 d . . . H14A H -0.1334 -0.1199 0.2280 0.052 Uiso 1 1 calc R . . H14B H -0.1555 -0.1814 0.1428 0.052 Uiso 1 1 calc R . . H14C H -0.1267 -0.0792 0.1369 0.052 Uiso 1 1 calc R . . C15 C 0.0657(6) -0.1401(4) 0.0092(3) 0.0411(13) Uani 1 1 d . . . H15A H 0.0275 -0.0842 0.0020 0.049 Uiso 1 1 calc R . . H15B H -0.0159 -0.1860 0.0014 0.049 Uiso 1 1 calc R . . H15C H 0.1367 -0.1493 -0.0333 0.049 Uiso 1 1 calc R . . C16 C 0.4086(7) -0.1579(4) 0.0642(4) 0.0480(14) Uani 1 1 d U . . H16A H 0.4552 -0.2100 0.0778 0.058 Uiso 1 1 calc R . . H16B H 0.4813 -0.1074 0.0744 0.058 Uiso 1 1 calc R . . H16C H 0.3708 -0.1623 0.0041 0.058 Uiso 1 1 calc R . . C17 C 0.3307(5) 0.2080(4) 0.1520(4) 0.0399(13) Uani 1 1 d . . . C18 C 0.1474(5) 0.0729(3) 0.2173(3) 0.0318(11) Uani 1 1 d . . . C19 C 0.3238(5) 0.0447(3) 0.0723(3) 0.0334(11) Uani 1 1 d . . . C20 C 0.5838(5) 0.1131(3) 0.1762(3) 0.0226(8) Uani 1 1 d U . . C21 C 0.4047(5) 0.1532(3) 0.3134(3) 0.0275(10) Uani 1 1 d . . . C22 C 0.8077(4) 0.3064(3) 0.3393(3) 0.0185(8) Uani 1 1 d . . . C23 C 0.7611(5) 0.3091(3) 0.4298(3) 0.0218(9) Uani 1 1 d . . . H23A H 0.7127 0.2521 0.4422 0.026 Uiso 1 1 calc R . . H23B H 0.6895 0.3522 0.4363 0.026 Uiso 1 1 calc R . . C24 C 0.8964(5) 0.3330(3) 0.4926(3) 0.0270(10) Uani 1 1 d . . . H24A H 0.8660 0.3325 0.5516 0.032 Uiso 1 1 calc R . . H24B H 0.9394 0.3921 0.4831 0.032 Uiso 1 1 calc R . . C25 C 1.0128(5) 0.2699(3) 0.4816(3) 0.0300(10) Uani 1 1 d . . . H25A H 1.1021 0.2899 0.5193 0.036 Uiso 1 1 calc R . . H25B H 0.9744 0.2125 0.4989 0.036 Uiso 1 1 calc R . . C26 C 1.0539(5) 0.2622(3) 0.3894(3) 0.0281(10) Uani 1 1 d . . . H26A H 1.1206 0.2164 0.3832 0.034 Uiso 1 1 calc R . . H26B H 1.1070 0.3172 0.3749 0.034 Uiso 1 1 calc R . . C27 C 0.9168(5) 0.2410(3) 0.3278(3) 0.0215(9) Uani 1 1 d . . . H27B H 0.9458 0.2402 0.2684 0.026 Uiso 1 1 calc R . . H27A H 0.8699 0.1830 0.3380 0.026 Uiso 1 1 calc R . . C28 C 0.8817(5) 0.4073(3) 0.1802(3) 0.0220(9) Uani 1 1 d . . . C29 C 0.9878(5) 0.4886(3) 0.1917(3) 0.0254(9) Uani 1 1 d . . . C30 C 0.9485(5) 0.5446(3) 0.1334(3) 0.0256(9) Uani 1 1 d . . . C31 C 0.8150(5) 0.5069(3) 0.0824(3) 0.0232(9) Uani 1 1 d . . . C32 C 0.7712(5) 0.4300(3) 0.1098(3) 0.0235(9) Uani 1 1 d . . . C33 C 0.9590(6) 0.3297(4) 0.1509(4) 0.0391(12) Uani 1 1 d U . . H33A H 1.0358 0.3191 0.1946 0.047 Uiso 1 1 calc R . . H33B H 1.0037 0.3416 0.0974 0.047 Uiso 1 1 calc R . . H33C H 0.8870 0.2788 0.1418 0.047 Uiso 1 1 calc R . . C34 C 1.1185(6) 0.4967(5) 0.2560(4) 0.0494(16) Uani 1 1 d . . . H34A H 1.1915 0.4594 0.2371 0.059 Uiso 1 1 calc R . . H34B H 1.0869 0.4795 0.3113 0.059 Uiso 1 1 calc R . . H34C H 1.1625 0.5567 0.2614 0.059 Uiso 1 1 calc R . . C35 C 1.0276(7) 0.6295(4) 0.1173(4) 0.0416(13) Uani 1 1 d U . . H35A H 1.0785 0.6241 0.0649 0.050 Uiso 1 1 calc R . . H35B H 1.0997 0.6478 0.1653 0.050 Uiso 1 1 calc R . . H35C H 0.9566 0.6723 0.1109 0.050 Uiso 1 1 calc R . . C36 C 0.7442(6) 0.5527(4) 0.0113(3) 0.0407(13) Uani 1 1 d . . . H36A H 0.8112 0.5591 -0.0344 0.049 Uiso 1 1 calc R . . H36B H 0.7229 0.6098 0.0328 0.049 Uiso 1 1 calc R . . H36C H 0.6522 0.5191 -0.0111 0.049 Uiso 1 1 calc R . . C37 C 0.6448(7) 0.3665(4) 0.0757(3) 0.0438(14) Uani 1 1 d . . . H37C H 0.6089 0.3821 0.0189 0.053 Uiso 1 1 calc R . . H37A H 0.5652 0.3672 0.1141 0.053 Uiso 1 1 calc R . . H37B H 0.6777 0.3086 0.0717 0.053 Uiso 1 1 calc R . . C38 C 0.5238(6) 0.6076(3) 0.3803(3) 0.0276(9) Uani 1 1 d U . . C39 C 0.5505(5) 0.5441(3) 0.2136(3) 0.0294(10) Uani 1 1 d . . . C40 C 0.4801(5) 0.4275(3) 0.3437(3) 0.0271(10) Uani 1 1 d . . . C41 C 0.7324(5) 0.5174(3) 0.4526(3) 0.0247(9) Uani 1 1 d . . . C42 C 0.8094(5) 0.6163(3) 0.3107(3) 0.0269(10) Uani 1 1 d . . . O1 O 0.5980(4) -0.0738(2) 0.2552(2) 0.0383(7) Uani 1 1 d U . . O2 O 0.3092(5) 0.2740(3) 0.1270(4) 0.0605(13) Uani 1 1 d . . . O3 O 0.0266(4) 0.0661(3) 0.2312(3) 0.0493(11) Uani 1 1 d . . . O4 O 0.3015(5) 0.0248(3) 0.0018(2) 0.0516(11) Uani 1 1 d . . . O5 O 0.7065(4) 0.1236(2) 0.1658(2) 0.0328(8) Uani 1 1 d . . . O6 O 0.4245(4) 0.1892(2) 0.3786(2) 0.0397(9) Uani 1 1 d . . . O7 O 0.6849(3) 0.30180(19) 0.27293(18) 0.0201(6) Uani 1 1 d . . . O8 O 0.4499(5) 0.6541(2) 0.4120(2) 0.0431(9) Uani 1 1 d . . . O9 O 0.4926(4) 0.5622(3) 0.1506(2) 0.0455(10) Uani 1 1 d . . . O10 O 0.3875(4) 0.3752(3) 0.3501(3) 0.0455(10) Uani 1 1 d . . . O11 O 0.7770(4) 0.5202(2) 0.5226(2) 0.0362(8) Uani 1 1 d . . . O12 O 0.8971(5) 0.6717(3) 0.3014(2) 0.0461(10) Uani 1 1 d . . . P1 P 0.42136(13) -0.04771(8) 0.25200(8) 0.0267(3) Uani 1 1 d U . . P2 P 0.77911(11) 0.39905(7) 0.27734(7) 0.0169(2) Uani 1 1 d . . . W1 W 0.365447(18) 0.092960(11) 0.195235(11) 0.02243(5) Uani 1 1 d U . . W2 W 0.646256(18) 0.522352(10) 0.330215(10) 0.01850(5) 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 0.0342(14) 0.0321(16) 0.0377(15) 0.0067(13) -0.0070(12) 0.0039(13) C2 0.0408(19) 0.036(2) 0.044(2) 0.0073(17) -0.0046(17) 0.0035(17) C3 0.036(3) 0.032(3) 0.053(3) 0.019(2) -0.007(2) 0.002(2) C4 0.030(3) 0.041(3) 0.037(3) 0.004(2) -0.010(2) 0.005(2) C5 0.052(2) 0.046(2) 0.053(2) 0.0098(16) -0.0078(17) -0.0001(17) C6 0.042(2) 0.0334(19) 0.043(2) 0.0079(17) -0.0115(17) 0.0017(17) C7 0.029(2) 0.023(2) 0.045(3) 0.001(2) -0.011(2) -0.0070(18) C8 0.033(3) 0.030(3) 0.029(2) 0.006(2) 0.000(2) -0.015(2) C9 0.025(2) 0.023(2) 0.032(2) -0.0006(19) 0.0013(19) -0.0012(18) C10 0.025(2) 0.028(2) 0.027(2) -0.0042(18) 0.0029(18) 0.0009(19) C11 0.026(2) 0.030(3) 0.040(3) -0.012(2) 0.001(2) -0.0009(19) C12 0.051(2) 0.0390(18) 0.054(2) 0.0032(16) -0.0081(17) 0.0066(16) C13 0.049(2) 0.049(2) 0.042(2) 0.0033(16) 0.0051(16) -0.0064(17) C14 0.022(2) 0.050(3) 0.055(3) -0.008(3) 0.005(2) -0.003(2) C15 0.037(3) 0.051(3) 0.031(3) -0.003(2) -0.004(2) -0.010(3) C16 0.043(2) 0.049(2) 0.051(2) -0.0078(17) 0.0067(17) 0.0060(17) C17 0.023(2) 0.039(3) 0.060(3) 0.023(3) 0.009(2) -0.001(2) C18 0.027(2) 0.020(2) 0.049(3) 0.005(2) 0.001(2) 0.0038(19) C19 0.025(2) 0.033(3) 0.041(3) 0.008(2) -0.003(2) -0.004(2) C20 0.0234(16) 0.024(2) 0.021(2) 0.0055(17) -0.0001(16) 0.0016(17) C21 0.022(2) 0.020(2) 0.042(3) 0.006(2) 0.009(2) 0.0007(17) C22 0.0196(19) 0.0158(19) 0.0206(19) 0.0043(15) 0.0044(16) 0.0003(15) C23 0.020(2) 0.026(2) 0.021(2) 0.0056(17) 0.0049(16) 0.0055(17) C24 0.029(2) 0.032(3) 0.022(2) 0.0010(18) 0.0009(18) 0.011(2) C25 0.027(2) 0.036(3) 0.028(2) 0.003(2) -0.0029(19) 0.013(2) C26 0.022(2) 0.032(3) 0.032(2) 0.006(2) 0.0015(19) 0.0091(19) C27 0.023(2) 0.020(2) 0.023(2) 0.0042(16) 0.0037(17) 0.0049(17) C28 0.024(2) 0.023(2) 0.020(2) 0.0043(17) 0.0079(17) 0.0034(17) C29 0.016(2) 0.035(3) 0.024(2) 0.0102(19) 0.0003(17) -0.0037(18) C30 0.024(2) 0.030(2) 0.022(2) 0.0041(18) 0.0016(17) -0.0044(18) C31 0.025(2) 0.029(2) 0.0159(19) 0.0040(17) 0.0016(16) 0.0015(18) C32 0.026(2) 0.030(2) 0.0130(19) 0.0012(16) 0.0022(16) -0.0022(18) C33 0.0437(19) 0.0383(19) 0.0383(18) 0.0063(15) 0.0145(16) 0.0087(16) C34 0.028(3) 0.073(4) 0.043(3) 0.027(3) -0.012(2) -0.013(3) C35 0.044(2) 0.0403(19) 0.0385(19) 0.0072(16) 0.0031(16) -0.0055(16) C36 0.039(3) 0.056(4) 0.029(3) 0.020(2) 0.000(2) 0.004(3) C37 0.049(3) 0.047(3) 0.029(3) 0.000(2) -0.006(2) -0.020(3) C38 0.039(3) 0.023(2) 0.024(2) 0.0056(17) 0.0112(19) 0.0083(18) C39 0.029(2) 0.033(3) 0.027(2) 0.003(2) 0.0018(19) 0.008(2) C40 0.018(2) 0.023(2) 0.043(3) 0.006(2) 0.0039(19) 0.0072(18) C41 0.030(2) 0.022(2) 0.024(2) 0.0026(17) 0.0057(18) 0.0082(18) C42 0.034(2) 0.024(2) 0.023(2) 0.0015(18) 0.0044(19) 0.0008(19) O1 0.0303(11) 0.0394(17) 0.0455(16) 0.0039(14) -0.0010(13) 0.0068(13) O2 0.039(2) 0.043(2) 0.108(4) 0.043(3) 0.016(2) 0.0145(19) O3 0.0258(19) 0.037(2) 0.086(3) -0.003(2) 0.014(2) 0.0043(16) O4 0.051(3) 0.066(3) 0.033(2) 0.005(2) -0.0059(18) -0.013(2) O5 0.0242(17) 0.043(2) 0.0304(17) 0.0002(15) 0.0043(14) 0.0015(15) O6 0.039(2) 0.034(2) 0.046(2) -0.0071(17) 0.0084(17) 0.0041(16) O7 0.0167(14) 0.0197(15) 0.0236(15) 0.0025(12) 0.0007(11) -0.0001(11) O8 0.059(3) 0.032(2) 0.045(2) 0.0126(17) 0.0241(19) 0.0198(18) O9 0.042(2) 0.062(3) 0.035(2) 0.0089(19) -0.0063(17) 0.020(2) O10 0.0230(18) 0.036(2) 0.079(3) 0.011(2) 0.0124(18) 0.0019(16) O11 0.049(2) 0.036(2) 0.0235(17) -0.0011(15) 0.0003(15) 0.0092(17) O12 0.060(3) 0.034(2) 0.040(2) -0.0032(17) 0.0116(19) -0.0204(19) P1 0.0231(5) 0.0182(5) 0.0370(6) 0.0044(5) -0.0082(5) 0.0002(4) P2 0.0165(5) 0.0171(5) 0.0177(5) 0.0031(4) 0.0031(4) 0.0023(4) W1 0.01732(9) 0.01940(9) 0.03102(10) 0.00727(7) 0.00054(7) 0.00212(7) W2 0.01955(9) 0.01726(9) 0.01935(9) 0.00212(6) 0.00238(6) 0.00393(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 1.442(7) . ? C1 C6 1.510(7) . ? C1 C2 1.519(8) . ? C1 P1 1.786(5) . ? C2 C3 1.501(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.504(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.510(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.448(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.495(7) . ? C7 C11 1.509(7) . ? C7 C12 1.552(8) . ? C7 P1 1.866(5) . ? C8 C9 1.357(7) . ? C8 C13 1.483(7) . ? C9 C10 1.458(6) . ? C9 C14 1.499(7) . ? C10 C11 1.334(7) . ? C10 C15 1.511(7) . ? C11 C16 1.515(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O2 1.150(7) . ? C17 W1 1.998(6) . ? C18 O3 1.138(6) . ? C18 W1 2.047(5) . ? C19 O4 1.136(6) . ? C19 W1 2.040(5) . ? C20 O5 1.144(5) . ? C20 W1 2.038(4) . ? C21 O6 1.140(6) . ? C21 W1 2.035(5) . ? C22 O7 1.473(5) . ? C22 C27 1.508(6) . ? C22 C23 1.518(6) . ? C22 P2 1.813(4) . ? C23 C24 1.531(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.533(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.528(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.529(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27B 0.9900 . ? C27 H27A 0.9900 . ? C28 C29 1.517(6) . ? C28 C32 1.524(6) . ? C28 C33 1.529(7) . ? C28 P2 1.856(4) . ? C29 C30 1.352(7) . ? C29 C34 1.501(6) . ? C30 C31 1.468(6) . ? C30 C35 1.490(7) . ? C31 C32 1.331(6) . ? C31 C36 1.500(7) . ? C32 C37 1.499(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 O8 1.158(6) . ? C38 W2 1.990(5) . ? C39 O9 1.151(6) . ? C39 W2 2.035(5) . ? C40 O10 1.133(6) . ? C40 W2 2.047(5) . ? C41 O11 1.145(5) . ? C41 W2 2.037(5) . ? C42 O12 1.144(6) . ? C42 W2 2.041(5) . ? O1 P1 1.702(4) . ? O7 P2 1.668(3) . ? P1 W1 2.4958(12) . ? P2 W2 2.5132(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 111.5(5) . . ? O1 C1 C2 116.8(5) . . ? C6 C1 C2 112.3(4) . . ? O1 C1 P1 62.6(2) . . ? C6 C1 P1 118.8(4) . . ? C2 C1 P1 124.4(4) . . ? C3 C2 C1 110.9(5) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 115.1(5) . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 C5 112.1(4) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 116.9(5) . . ? C6 C5 H5A 108.1 . . ? C4 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? C4 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C1 113.4(5) . . ? C5 C6 H6A 108.9 . . ? C1 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C1 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C11 102.5(4) . . ? C8 C7 C12 116.0(5) . . ? C11 C7 C12 106.9(4) . . ? C8 C7 P1 106.3(3) . . ? C11 C7 P1 106.0(3) . . ? C12 C7 P1 117.6(4) . . ? C9 C8 C13 129.2(5) . . ? C9 C8 C7 109.6(4) . . ? C13 C8 C7 121.2(5) . . ? C8 C9 C10 108.6(4) . . ? C8 C9 C14 128.3(5) . . ? C10 C9 C14 123.1(4) . . ? C11 C10 C9 109.9(4) . . ? C11 C10 C15 128.6(5) . . ? C9 C10 C15 121.6(4) . . ? C10 C11 C7 109.4(4) . . ? C10 C11 C16 129.3(5) . . ? C7 C11 C16 121.3(5) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 W1 179.3(5) . . ? O3 C18 W1 176.4(4) . . ? O4 C19 W1 174.2(5) . . ? O5 C20 W1 179.3(4) . . ? O6 C21 W1 177.7(4) . . ? O7 C22 C27 115.5(3) . . ? O7 C22 C23 114.3(3) . . ? C27 C22 C23 110.7(4) . . ? O7 C22 P2 59.97(19) . . ? C27 C22 P2 128.3(3) . . ? C23 C22 P2 117.2(3) . . ? C22 C23 C24 109.7(3) . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 111.2(4) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 111.6(4) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 111.1(4) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C22 C27 C26 111.0(4) . . ? C22 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? C22 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? H27B C27 H27A 108.0 . . ? C29 C28 C32 102.1(3) . . ? C29 C28 C33 111.4(4) . . ? C32 C28 C33 110.3(4) . . ? C29 C28 P2 107.8(3) . . ? C32 C28 P2 105.8(3) . . ? C33 C28 P2 118.1(3) . . ? C30 C29 C34 129.0(4) . . ? C30 C29 C28 109.2(4) . . ? C34 C29 C28 121.7(4) . . ? C29 C30 C31 109.2(4) . . ? C29 C30 C35 127.6(4) . . ? C31 C30 C35 123.2(4) . . ? C32 C31 C30 109.9(4) . . ? C32 C31 C36 127.8(4) . . ? C30 C31 C36 122.4(4) . . ? C31 C32 C37 129.2(4) . . ? C31 C32 C28 109.5(4) . . ? C37 C32 C28 121.1(4) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37C 109.5 . . ? C32 C37 H37A 109.5 . . ? H37C C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37C C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O8 C38 W2 176.7(4) . . ? O9 C39 W2 174.6(4) . . ? O10 C40 W2 179.1(5) . . ? O11 C41 W2 175.1(4) . . ? O12 C42 W2 176.8(4) . . ? C1 O1 P1 68.7(3) . . ? C22 O7 P2 70.2(2) . . ? O1 P1 C1 48.7(2) . . ? O1 P1 C7 105.2(2) . . ? C1 P1 C7 114.9(2) . . ? O1 P1 W1 118.79(15) . . ? C1 P1 W1 123.52(18) . . ? C7 P1 W1 120.91(16) . . ? O7 P2 C22 49.83(16) . . ? O7 P2 C28 107.97(18) . . ? C22 P2 C28 115.7(2) . . ? O7 P2 W2 115.99(11) . . ? C22 P2 W2 122.86(14) . . ? C28 P2 W2 120.64(15) . . ? C17 W1 C21 87.1(2) . . ? C17 W1 C20 91.02(19) . . ? C21 W1 C20 90.17(17) . . ? C17 W1 C19 87.0(2) . . ? C21 W1 C19 174.2(2) . . ? C20 W1 C19 89.61(18) . . ? C17 W1 C18 89.5(2) . . ? C21 W1 C18 88.6(2) . . ? C20 W1 C18 178.68(18) . . ? C19 W1 C18 91.6(2) . . ? C17 W1 P1 177.15(15) . . ? C21 W1 P1 91.36(14) . . ? C20 W1 P1 86.56(13) . . ? C19 W1 P1 94.45(15) . . ? C18 W1 P1 92.91(14) . . ? C38 W2 C39 88.01(19) . . ? C38 W2 C41 84.12(19) . . ? C39 W2 C41 171.62(18) . . ? C38 W2 C42 92.02(19) . . ? C39 W2 C42 87.96(19) . . ? C41 W2 C42 89.46(18) . . ? C38 W2 C40 88.83(19) . . ? C39 W2 C40 89.5(2) . . ? C41 W2 C40 93.18(19) . . ? C42 W2 C40 177.31(18) . . ? C38 W2 P2 171.90(14) . . ? C39 W2 P2 94.97(14) . . ? C41 W2 P2 93.21(13) . . ? C42 W2 P2 95.61(14) . . ? C40 W2 P2 83.67(13) . . ? 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 77.9(6) . . . . ? C6 C1 C2 C3 -52.7(7) . . . . ? P1 C1 C2 C3 151.7(4) . . . . ? C1 C2 C3 C4 51.2(7) . . . . ? C2 C3 C4 C5 -45.6(7) . . . . ? C3 C4 C5 C6 43.4(8) . . . . ? C4 C5 C6 C1 -46.8(8) . . . . ? O1 C1 C6 C5 -82.2(6) . . . . ? C2 C1 C6 C5 51.1(7) . . . . ? P1 C1 C6 C5 -151.8(5) . . . . ? C11 C7 C8 C9 1.3(5) . . . . ? C12 C7 C8 C9 -114.7(5) . . . . ? P1 C7 C8 C9 112.4(4) . . . . ? C11 C7 C8 C13 179.0(5) . . . . ? C12 C7 C8 C13 62.9(6) . . . . ? P1 C7 C8 C13 -70.0(5) . . . . ? C13 C8 C9 C10 -177.8(5) . . . . ? C7 C8 C9 C10 -0.4(6) . . . . ? C13 C8 C9 C14 -0.2(9) . . . . ? C7 C8 C9 C14 177.2(5) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C14 C9 C10 C11 -178.6(5) . . . . ? C8 C9 C10 C15 179.1(5) . . . . ? C14 C9 C10 C15 1.4(7) . . . . ? C9 C10 C11 C7 1.7(6) . . . . ? C15 C10 C11 C7 -178.2(5) . . . . ? C9 C10 C11 C16 179.2(5) . . . . ? C15 C10 C11 C16 -0.7(9) . . . . ? C8 C7 C11 C10 -1.8(5) . . . . ? C12 C7 C11 C10 120.7(5) . . . . ? P1 C7 C11 C10 -113.1(4) . . . . ? C8 C7 C11 C16 -179.6(5) . . . . ? C12 C7 C11 C16 -57.1(6) . . . . ? P1 C7 C11 C16 69.1(6) . . . . ? O7 C22 C23 C24 -168.0(3) . . . . ? C27 C22 C23 C24 59.5(5) . . . . ? P2 C22 C23 C24 -100.7(4) . . . . ? C22 C23 C24 C25 -56.8(5) . . . . ? C23 C24 C25 C26 54.1(5) . . . . ? C24 C25 C26 C27 -52.9(5) . . . . ? O7 C22 C27 C26 169.0(3) . . . . ? C23 C22 C27 C26 -59.1(5) . . . . ? P2 C22 C27 C26 98.3(4) . . . . ? C25 C26 C27 C22 55.4(5) . . . . ? C32 C28 C29 C30 -3.7(5) . . . . ? C33 C28 C29 C30 114.1(5) . . . . ? P2 C28 C29 C30 -114.8(4) . . . . ? C32 C28 C29 C34 180.0(5) . . . . ? C33 C28 C29 C34 -62.3(6) . . . . ? P2 C28 C29 C34 68.8(5) . . . . ? C34 C29 C30 C31 177.8(5) . . . . ? C28 C29 C30 C31 1.8(5) . . . . ? C34 C29 C30 C35 0.9(9) . . . . ? C28 C29 C30 C35 -175.1(5) . . . . ? C29 C30 C31 C32 1.2(6) . . . . ? C35 C30 C31 C32 178.3(5) . . . . ? C29 C30 C31 C36 -179.2(5) . . . . ? C35 C30 C31 C36 -2.1(7) . . . . ? C30 C31 C32 C37 -177.5(5) . . . . ? C36 C31 C32 C37 2.9(9) . . . . ? C30 C31 C32 C28 -3.6(5) . . . . ? C36 C31 C32 C28 176.8(5) . . . . ? C29 C28 C32 C31 4.4(5) . . . . ? C33 C28 C32 C31 -114.1(4) . . . . ? P2 C28 C32 C31 117.1(4) . . . . ? C29 C28 C32 C37 178.9(4) . . . . ? C33 C28 C32 C37 60.3(6) . . . . ? P2 C28 C32 C37 -68.5(5) . . . . ? C6 C1 O1 P1 -112.2(4) . . . . ? C2 C1 O1 P1 116.8(4) . . . . ? C27 C22 O7 P2 -121.2(3) . . . . ? C23 C22 O7 P2 108.6(3) . . . . ? C1 O1 P1 C7 -110.0(3) . . . . ? C1 O1 P1 W1 110.9(3) . . . . ? C6 C1 P1 O1 100.7(5) . . . . ? C2 C1 P1 O1 -105.1(6) . . . . ? O1 C1 P1 C7 88.7(3) . . . . ? C6 C1 P1 C7 -170.6(4) . . . . ? C2 C1 P1 C7 -16.4(6) . . . . ? O1 C1 P1 W1 -100.8(3) . . . . ? C6 C1 P1 W1 -0.1(5) . . . . ? C2 C1 P1 W1 154.1(4) . . . . ? C8 C7 P1 O1 159.1(3) . . . . ? C11 C7 P1 O1 -92.3(4) . . . . ? C12 C7 P1 O1 27.1(5) . . . . ? C8 C7 P1 C1 107.9(4) . . . . ? C11 C7 P1 C1 -143.4(3) . . . . ? C12 C7 P1 C1 -24.1(5) . . . . ? C8 C7 P1 W1 -62.8(4) . . . . ? C11 C7 P1 W1 45.8(4) . . . . ? C12 C7 P1 W1 165.2(4) . . . . ? C22 O7 P2 C28 108.8(2) . . . . ? C22 O7 P2 W2 -112.23(19) . . . . ? C27 C22 P2 O7 100.1(4) . . . . ? C23 C22 P2 O7 -103.8(4) . . . . ? O7 C22 P2 C28 -92.4(2) . . . . ? C27 C22 P2 C28 7.7(4) . . . . ? C23 C22 P2 C28 163.8(3) . . . . ? O7 C22 P2 W2 97.90(19) . . . . ? C27 C22 P2 W2 -162.0(3) . . . . ? C23 C22 P2 W2 -5.9(4) . . . . ? C29 C28 P2 O7 -170.0(3) . . . . ? C32 C28 P2 O7 81.3(3) . . . . ? C33 C28 P2 O7 -42.8(4) . . . . ? C29 C28 P2 C22 -116.6(3) . . . . ? C32 C28 P2 C22 134.7(3) . . . . ? C33 C28 P2 C22 10.6(4) . . . . ? C29 C28 P2 W2 53.3(3) . . . . ? C32 C28 P2 W2 -55.3(3) . . . . ? C33 C28 P2 W2 -179.4(3) . . . . ? O2 C17 W1 C21 -107(48) . . . . ? O2 C17 W1 C20 163(100) . . . . ? O2 C17 W1 C19 74(48) . . . . ? O2 C17 W1 C18 -18(48) . . . . ? O2 C17 W1 P1 -165(100) . . . . ? O6 C21 W1 C17 16(11) . . . . ? O6 C21 W1 C20 107(11) . . . . ? O6 C21 W1 C19 19(12) . . . . ? O6 C21 W1 C18 -74(11) . . . . ? O6 C21 W1 P1 -167(11) . . . . ? O5 C20 W1 C17 179(100) . . . . ? O5 C20 W1 C21 92(34) . . . . ? O5 C20 W1 C19 -94(34) . . . . ? O5 C20 W1 C18 67(38) . . . . ? O5 C20 W1 P1 1(34) . . . . ? O4 C19 W1 C17 12(5) . . . . ? O4 C19 W1 C21 9(6) . . . . ? O4 C19 W1 C20 -79(5) . . . . ? O4 C19 W1 C18 102(5) . . . . ? O4 C19 W1 P1 -165(5) . . . . ? O3 C18 W1 C17 -42(8) . . . . ? O3 C18 W1 C21 45(8) . . . . ? O3 C18 W1 C20 70(12) . . . . ? O3 C18 W1 C19 -129(8) . . . . ? O3 C18 W1 P1 137(8) . . . . ? O1 P1 W1 C17 -32(4) . . . . ? C1 P1 W1 C17 26(4) . . . . ? C7 P1 W1 C17 -164(4) . . . . ? O1 P1 W1 C21 -89.7(2) . . . . ? C1 P1 W1 C21 -32.3(3) . . . . ? C7 P1 W1 C21 137.6(2) . . . . ? O1 P1 W1 C20 0.4(2) . . . . ? C1 P1 W1 C20 57.8(3) . . . . ? C7 P1 W1 C20 -132.3(2) . . . . ? O1 P1 W1 C19 89.7(2) . . . . ? C1 P1 W1 C19 147.1(3) . . . . ? C7 P1 W1 C19 -42.9(3) . . . . ? O1 P1 W1 C18 -178.4(2) . . . . ? C1 P1 W1 C18 -121.0(3) . . . . ? C7 P1 W1 C18 49.0(3) . . . . ? O8 C38 W2 C39 124(8) . . . . ? O8 C38 W2 C41 -59(8) . . . . ? O8 C38 W2 C42 -148(8) . . . . ? O8 C38 W2 C40 34(8) . . . . ? O8 C38 W2 P2 12(9) . . . . ? O9 C39 W2 C38 15(5) . . . . ? O9 C39 W2 C41 -5(6) . . . . ? O9 C39 W2 C42 -77(5) . . . . ? O9 C39 W2 C40 104(5) . . . . ? O9 C39 W2 P2 -173(5) . . . . ? O11 C41 W2 C38 -20(5) . . . . ? O11 C41 W2 C39 0(6) . . . . ? O11 C41 W2 C42 73(5) . . . . ? O11 C41 W2 C40 -108(5) . . . . ? O11 C41 W2 P2 168(5) . . . . ? O12 C42 W2 C38 1(8) . . . . ? O12 C42 W2 C39 89(8) . . . . ? O12 C42 W2 C41 -83(8) . . . . ? O12 C42 W2 C40 109(8) . . . . ? O12 C42 W2 P2 -176(100) . . . . ? O10 C40 W2 C38 96(28) . . . . ? O10 C40 W2 C39 8(28) . . . . ? O10 C40 W2 C41 -180(100) . . . . ? O10 C40 W2 C42 -12(30) . . . . ? O10 C40 W2 P2 -87(28) . . . . ? O7 P2 W2 C38 24.0(10) . . . . ? C22 P2 W2 C38 -33.4(10) . . . . ? C28 P2 W2 C38 157.4(10) . . . . ? O7 P2 W2 C39 -87.35(19) . . . . ? C22 P2 W2 C39 -144.7(2) . . . . ? C28 P2 W2 C39 46.1(2) . . . . ? O7 P2 W2 C41 94.45(18) . . . . ? C22 P2 W2 C41 37.1(2) . . . . ? C28 P2 W2 C41 -132.1(2) . . . . ? O7 P2 W2 C42 -175.78(18) . . . . ? C22 P2 W2 C42 126.9(2) . . . . ? C28 P2 W2 C42 -42.3(2) . . . . ? O7 P2 W2 C40 1.60(18) . . . . ? C22 P2 W2 C40 -55.8(2) . . . . ? C28 P2 W2 C40 135.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.133 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.138 data_2068f _database_code_depnum_ccdc_archive 'CCDC 926029' #TrackingRef 'web_deposit_cif_file_0_Dr.GregorSchnakenburg_1361462579.Gesamtcif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Li2 O14 P2 W2' _chemical_formula_sum 'C60 H72 Li2 O14 P2 W2' _chemical_formula_weight 1460.70 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 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 12.0282(9) _cell_length_b 13.9181(10) _cell_length_c 20.8583(16) _cell_angle_alpha 94.714(2) _cell_angle_beta 103.892(2) _cell_angle_gamma 113.038(2) _cell_volume 3058.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3717 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 24.94 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 3.873 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8605 _exptl_absorpt_correction_T_max 0.9266 _exptl_absorpt_process_details 'SADABS (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 'fine slicing \f and \w scans' _diffrn_detector_area_resol_mean 8.33333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29053 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 28.00 _reflns_number_total 14653 _reflns_number_gt 9729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker AXS, 2011)' _computing_cell_refinement 'Bruker SAINT (Bruker AXS, 2011)' _computing_data_reduction 'Bruker SAINT (Bruker AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0579P)^2^+6.8077P] 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 14653 _refine_ls_number_parameters 731 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.030 _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 0.3241(8) 0.5036(7) 0.8687(4) 0.035(2) Uani 1 1 d . . . C2 C 0.3624(10) 0.4292(8) 0.8665(5) 0.045(2) Uani 1 1 d U . . H2A H 0.3075 0.3561 0.8489 0.054 Uiso 1 1 calc R . . C3 C 0.5054(10) 0.4715(9) 0.8953(6) 0.057(2) Uani 1 1 d U . . H3A H 0.5464 0.4741 0.8592 0.068 Uiso 1 1 calc R . . H3B H 0.5290 0.4281 0.9266 0.068 Uiso 1 1 calc R . . C4 C 0.5394(11) 0.5833(9) 0.9325(6) 0.058(2) Uani 1 1 d U . . H4A H 0.6225 0.6342 0.9301 0.070 Uiso 1 1 calc R . . H4B H 0.5433 0.5833 0.9804 0.070 Uiso 1 1 calc R . . C5 C 0.4341(9) 0.6136(8) 0.8968(5) 0.048(2) Uani 1 1 d U . . H5A H 0.4157 0.6576 0.9288 0.058 Uiso 1 1 calc R . . H5B H 0.4555 0.6520 0.8604 0.058 Uiso 1 1 calc R . . C6 C 0.0850(8) 0.4896(6) 0.8940(4) 0.0311(19) Uani 1 1 d . . . C7 C 0.1573(9) 0.5969(6) 0.9420(4) 0.0365(19) Uani 1 1 d U . . C8 C 0.0886(8) 0.6533(7) 0.9318(4) 0.034(2) Uani 1 1 d . . . C9 C -0.0356(8) 0.5860(7) 0.8824(4) 0.035(2) Uani 1 1 d . . . C10 C -0.0411(8) 0.4916(7) 0.8614(4) 0.038(2) Uani 1 1 d . . . C11 C 0.2715(10) 0.6216(8) 0.9998(5) 0.052(2) Uani 1 1 d U . . H11A H 0.3000 0.5650 0.9959 0.062 Uiso 1 1 calc R . . H11B H 0.2503 0.6265 1.0421 0.062 Uiso 1 1 calc R . . H11C H 0.3391 0.6897 0.9994 0.062 Uiso 1 1 calc R . . C12 C 0.0739(10) 0.3974(7) 0.9322(5) 0.044(2) Uani 1 1 d . . . H12A H 0.0422 0.4068 0.9703 0.053 Uiso 1 1 calc R . . H12B H 0.1573 0.3973 0.9489 0.053 Uiso 1 1 calc R . . H12C H 0.0151 0.3295 0.9017 0.053 Uiso 1 1 calc R . . C13 C 0.1219(10) 0.7632(7) 0.9673(5) 0.047(3) Uani 1 1 d . . . H13A H 0.2100 0.7950 0.9958 0.056 Uiso 1 1 calc R . . H13B H 0.0661 0.7596 0.9953 0.056 Uiso 1 1 calc R . . H13C H 0.1112 0.8071 0.9339 0.056 Uiso 1 1 calc R . . C14 C -0.1392(10) 0.6226(9) 0.8653(5) 0.055(3) Uani 1 1 d . . . H14A H -0.1089 0.6891 0.8486 0.066 Uiso 1 1 calc R . . H14B H -0.1638 0.6346 0.9057 0.066 Uiso 1 1 calc R . . H14C H -0.2124 0.5680 0.8304 0.066 Uiso 1 1 calc R . . C15 C -0.1463(10) 0.4000(8) 0.8125(5) 0.057(3) Uani 1 1 d U . . H15C H -0.2249 0.4086 0.8069 0.069 Uiso 1 1 calc R . . H15B H -0.1551 0.3343 0.8290 0.069 Uiso 1 1 calc R . . H15A H -0.1288 0.3963 0.7691 0.069 Uiso 1 1 calc R . . C16 C 0.1969(9) 0.6797(8) 0.6641(5) 0.044(2) Uani 1 1 d U . . C17 C 0.0395(8) 0.4680(6) 0.6783(4) 0.0260(17) Uani 1 1 d . . . C18 C 0.0221(10) 0.6386(7) 0.7408(5) 0.041(2) Uani 1 1 d . . . C19 C 0.2806(12) 0.7356(8) 0.8140(6) 0.067(3) Uani 1 1 d U . . C20 C 0.3228(9) 0.5831(6) 0.7305(4) 0.0320(19) Uani 1 1 d . . . C21 C -0.0039(9) -0.0117(8) 0.6563(5) 0.0478(13) Uani 1 1 d DU . . C22 C 0.1030(10) 0.0585(8) 0.6388(6) 0.0564(15) Uani 1 1 d DU . . H22A H 0.1507 0.1235 0.6746 0.068 Uiso 1 1 calc R . . H22B H 0.0730 0.0803 0.5964 0.068 Uiso 1 1 calc R . . C23 C 0.1889(10) 0.0095(8) 0.6300(6) 0.0552(15) Uani 1 1 d DU . . H23A H 0.2074 0.0170 0.5864 0.066 Uiso 1 1 calc R . . H23B H 0.2695 0.0420 0.6670 0.066 Uiso 1 1 calc R . . C24 C 0.1174(11) -0.1015(8) 0.6317(6) 0.0595(15) Uani 1 1 d DU . . H24A H 0.1703 -0.1272 0.6632 0.071 Uiso 1 1 calc R . . H24B H 0.0873 -0.1466 0.5863 0.071 Uiso 1 1 calc R . . C25 C 0.0070(11) -0.1045(9) 0.6554(5) 0.0565(15) Uani 1 1 d U . . H25A H -0.0483 -0.1648 0.6681 0.068 Uiso 1 1 calc R . . C26 C -0.2216(7) 0.0343(6) 0.6046(4) 0.0216(16) Uani 1 1 d . . . C27 C -0.3032(7) -0.0759(6) 0.5616(3) 0.0230(16) Uani 1 1 d . . . C28 C -0.4241(7) -0.1002(6) 0.5588(4) 0.0274(18) Uani 1 1 d . . . C29 C -0.4336(7) -0.0112(6) 0.5962(4) 0.0249(17) Uani 1 1 d . . . C30 C -0.3182(7) 0.0665(6) 0.6234(3) 0.0192(15) Uani 1 1 d . . . C31 C -0.1495(8) 0.1115(6) 0.5649(4) 0.0268(17) Uani 1 1 d . . . H31A H -0.2101 0.1168 0.5261 0.032 Uiso 1 1 calc R . . H31B H -0.0944 0.0850 0.5491 0.032 Uiso 1 1 calc R . . H31C H -0.0982 0.1819 0.5940 0.032 Uiso 1 1 calc R . . C32 C -0.2576(8) -0.1401(7) 0.5227(4) 0.0327(19) Uani 1 1 d . . . H32A H -0.2634 -0.2032 0.5419 0.039 Uiso 1 1 calc R . . H32B H -0.1694 -0.0967 0.5251 0.039 Uiso 1 1 calc R . . H32C H -0.3101 -0.1623 0.4755 0.039 Uiso 1 1 calc R . . C33 C -0.5387(8) -0.2001(7) 0.5207(4) 0.037(2) Uani 1 1 d . . . H33A H -0.5122 -0.2496 0.4996 0.045 Uiso 1 1 calc R . . H33B H -0.5941 -0.1824 0.4857 0.045 Uiso 1 1 calc R . . H33C H -0.5846 -0.2333 0.5517 0.045 Uiso 1 1 calc R . . C34 C -0.5570(7) -0.0108(7) 0.5988(4) 0.033(2) Uani 1 1 d . . . H34A H -0.6151 -0.0822 0.6013 0.039 Uiso 1 1 calc R . . H34B H -0.5943 0.0098 0.5581 0.039 Uiso 1 1 calc R . . H34C H -0.5424 0.0402 0.6386 0.039 Uiso 1 1 calc R . . C35 C -0.2837(8) 0.1736(6) 0.6655(4) 0.0318(19) Uani 1 1 d . . . H35C H -0.3597 0.1755 0.6740 0.038 Uiso 1 1 calc R . . H35B H -0.2483 0.2301 0.6414 0.038 Uiso 1 1 calc R . . H35A H -0.2210 0.1846 0.7086 0.038 Uiso 1 1 calc R . . C36 C -0.2802(8) -0.1861(6) 0.8205(4) 0.0316(19) Uani 1 1 d . . . C37 C -0.0450(8) -0.0902(6) 0.7996(4) 0.0281(18) Uani 1 1 d . . . C38 C -0.1641(7) 0.0465(6) 0.8193(4) 0.0246(17) Uani 1 1 d . . . C39 C -0.3971(8) -0.1022(6) 0.7290(4) 0.0311(19) Uani 1 1 d . . . C40 C -0.2766(9) -0.2252(7) 0.6842(4) 0.037(2) Uani 1 1 d . . . C41 C 0.2890(10) 0.3453(8) 0.6524(5) 0.0497(15) Uani 1 1 d U . . C42 C 0.3398(10) 0.3942(8) 0.5990(5) 0.0492(14) Uani 1 1 d U . . C43 C 0.4788(10) 0.4137(8) 0.6151(5) 0.0523(15) Uani 1 1 d U . . H43A H 0.5352 0.4900 0.6337 0.063 Uiso 1 1 calc R . . H43B H 0.4976 0.3913 0.5742 0.063 Uiso 1 1 calc R . . C44 C 0.4961(11) 0.3451(9) 0.6680(6) 0.0567(15) Uani 1 1 d U . . H44A H 0.4893 0.2761 0.6465 0.068 Uiso 1 1 calc R . . H44B H 0.5794 0.3827 0.7027 0.068 Uiso 1 1 calc R . . C45 C 0.3906(10) 0.3288(9) 0.6982(5) 0.0530(15) Uani 1 1 d U . . H45A H 0.3568 0.2556 0.7071 0.064 Uiso 1 1 calc R . . H45B H 0.4232 0.3795 0.7417 0.064 Uiso 1 1 calc R . . C46 C 0.2732(10) 0.4195(8) 0.5489(5) 0.0531(15) Uani 1 1 d U . . C47 C 0.3279(11) 0.4727(9) 0.4983(5) 0.0561(15) Uani 1 1 d U . . H47A H 0.3468 0.4239 0.4700 0.067 Uiso 1 1 calc R . . H47B H 0.4073 0.5370 0.5207 0.067 Uiso 1 1 calc R . . C48 C 0.2286(10) 0.5035(9) 0.4546(6) 0.0599(15) Uani 1 1 d U . . H48A H 0.2406 0.5759 0.4731 0.072 Uiso 1 1 calc R . . H48B H 0.2311 0.4994 0.4074 0.072 Uiso 1 1 calc R . . C49 C 0.1103(11) 0.4212(9) 0.4601(5) 0.0598(15) Uani 1 1 d U . . H49A H 0.0844 0.3543 0.4281 0.072 Uiso 1 1 calc R . . H49B H 0.0417 0.4452 0.4491 0.072 Uiso 1 1 calc R . . C50 C 0.1338(10) 0.4028(9) 0.5315(5) 0.0546(16) Uani 1 1 d U . . H50A H 0.0773 0.3298 0.5338 0.066 Uiso 1 1 calc R . . H50B H 0.1230 0.4550 0.5617 0.066 Uiso 1 1 calc R . . C51 C 0.1981(7) 0.1454(6) 0.9160(4) 0.0243(16) Uani 1 1 d . . . C52 C 0.3033(7) 0.1144(6) 0.9351(4) 0.0252(17) Uani 1 1 d . . . C53 C 0.3067(7) 0.0797(7) 1.0023(4) 0.0285(18) Uani 1 1 d . . . H53A H 0.3701 0.1383 1.0398 0.034 Uiso 1 1 calc R . . H53B H 0.3270 0.0173 1.0033 0.034 Uiso 1 1 calc R . . C54 C 0.1718(8) 0.0507(6) 1.0070(4) 0.0309(19) Uani 1 1 d . . . H54A H 0.1143 -0.0238 0.9840 0.037 Uiso 1 1 calc R . . H54B H 0.1716 0.0601 1.0545 0.037 Uiso 1 1 calc R . . C55 C 0.1331(8) 0.1297(7) 0.9709(4) 0.0331(19) Uani 1 1 d . . . H55B H 0.0401 0.1000 0.9513 0.040 Uiso 1 1 calc R . . H55A H 0.1624 0.1979 1.0024 0.040 Uiso 1 1 calc R . . C56 C 0.3780(9) 0.1122(7) 0.8985(5) 0.0371(13) Uani 1 1 d U . . C57 C 0.3736(9) 0.1404(7) 0.8292(4) 0.0383(13) Uani 1 1 d U . . H57A H 0.4137 0.2185 0.8325 0.046 Uiso 1 1 calc R . . H57B H 0.2853 0.1113 0.7995 0.046 Uiso 1 1 calc R . . C58 C 0.4488(9) 0.0875(8) 0.8031(5) 0.0414(13) Uani 1 1 d U . . H58A H 0.3935 0.0123 0.7810 0.050 Uiso 1 1 calc R . . H58B H 0.4873 0.1256 0.7704 0.050 Uiso 1 1 calc R . . C59 C 0.5490(9) 0.0948(8) 0.8644(4) 0.0412(13) Uani 1 1 d U . . H59A H 0.6214 0.1658 0.8768 0.049 Uiso 1 1 calc R . . H59B H 0.5798 0.0397 0.8570 0.049 Uiso 1 1 calc R . . C60 C 0.4821(9) 0.0760(7) 0.9189(4) 0.0387(13) Uani 1 1 d U . . H60A H 0.4465 -0.0004 0.9215 0.046 Uiso 1 1 calc R . . H60B H 0.5418 0.1177 0.9634 0.046 Uiso 1 1 calc R . . O1 O 0.0942(5) 0.3603(4) 0.7928(2) 0.0200(11) Uani 1 1 d . . . O2 O 0.2197(7) 0.7152(6) 0.6174(4) 0.0540(18) Uani 1 1 d U . . O3 O -0.0369(6) 0.3886(5) 0.6449(3) 0.0410(15) Uani 1 1 d . . . O4 O -0.0635(7) 0.6598(6) 0.7341(4) 0.0560(19) Uani 1 1 d U . . O5 O 0.3371(8) 0.8091(5) 0.8564(4) 0.076(2) Uani 1 1 d U . . O6 O 0.4117(6) 0.5774(5) 0.7237(3) 0.0504(18) Uani 1 1 d . . . O7 O -0.0287(5) 0.1486(4) 0.7201(2) 0.0207(11) Uani 1 1 d . . . O8 O -0.3128(6) -0.2399(5) 0.8581(3) 0.0425(16) Uani 1 1 d . . . O9 O 0.0502(6) -0.0925(5) 0.8264(3) 0.0479(17) Uani 1 1 d . . . O10 O -0.1334(5) 0.1296(4) 0.8513(3) 0.0316(13) Uani 1 1 d . . . O11 O -0.4991(6) -0.1153(6) 0.7191(3) 0.0472(17) Uani 1 1 d . . . O12 O -0.3160(7) -0.2993(5) 0.6437(3) 0.0531(19) Uani 1 1 d . . . O13 O 0.1765(6) 0.3238(5) 0.6553(3) 0.0457(16) Uani 1 1 d U . . O14 O 0.1652(5) 0.1779(4) 0.8656(3) 0.0273(12) Uani 1 1 d . . . P1 P 0.16136(19) 0.48103(15) 0.82550(10) 0.0243(4) Uani 1 1 d . . . P2 P -0.11219(18) 0.02928(15) 0.68445(9) 0.0192(4) Uani 1 1 d U . . W1 W 0.16936(3) 0.60391(2) 0.740280(17) 0.03042(11) Uani 1 1 d . . . W2 W -0.21655(3) -0.09213(2) 0.758086(15) 0.02081(9) Uani 1 1 d . . . Li1 Li 0.0599(13) 0.2840(11) 0.7050(7) 0.029(3) Uani 1 1 d U . . Li2 Li 0.0506(12) 0.2237(9) 0.8108(6) 0.022(3) 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 0.031(5) 0.029(4) 0.032(4) 0.010(4) 0.004(4) 0.001(4) C2 0.051(3) 0.058(6) 0.040(5) 0.024(5) 0.021(4) 0.032(5) C3 0.053(3) 0.060(3) 0.057(3) 0.0146(18) 0.0149(19) 0.024(2) C4 0.056(3) 0.058(3) 0.058(3) 0.0164(18) 0.015(2) 0.021(2) C5 0.046(3) 0.048(3) 0.047(3) 0.0139(19) 0.0131(19) 0.017(2) C6 0.037(5) 0.019(4) 0.034(4) 0.001(3) 0.013(4) 0.009(4) C7 0.048(5) 0.026(4) 0.039(5) 0.005(4) 0.012(3) 0.020(4) C8 0.027(5) 0.033(5) 0.042(5) 0.008(4) 0.009(4) 0.013(4) C9 0.031(5) 0.043(5) 0.037(5) 0.012(4) 0.015(4) 0.018(4) C10 0.023(5) 0.045(5) 0.038(5) 0.002(4) 0.014(4) 0.005(4) C11 0.051(3) 0.053(3) 0.050(3) 0.0071(19) 0.0099(18) 0.025(2) C12 0.071(7) 0.045(5) 0.038(5) 0.016(4) 0.030(5) 0.036(5) C13 0.056(7) 0.029(5) 0.064(7) 0.002(4) 0.025(5) 0.024(5) C14 0.042(6) 0.085(8) 0.049(6) 0.016(6) 0.014(5) 0.038(6) C15 0.055(3) 0.060(3) 0.057(3) 0.0073(19) 0.019(2) 0.023(2) C16 0.045(3) 0.042(3) 0.045(3) 0.0119(19) 0.0122(19) 0.0185(19) C17 0.031(5) 0.019(4) 0.029(4) 0.010(3) 0.012(4) 0.009(4) C18 0.055(6) 0.038(5) 0.041(5) 0.018(4) 0.015(5) 0.029(5) C19 0.083(6) 0.023(4) 0.073(5) 0.001(4) 0.000(5) 0.016(4) C20 0.034(5) 0.030(4) 0.039(5) 0.007(4) 0.015(4) 0.018(4) C21 0.0490(19) 0.054(2) 0.057(2) 0.0086(17) 0.0263(17) 0.0338(17) C22 0.0548(19) 0.0585(19) 0.0620(19) 0.0083(14) 0.0214(15) 0.0287(14) C23 0.054(2) 0.059(2) 0.061(2) 0.0090(17) 0.0236(18) 0.0305(18) C24 0.0584(19) 0.0610(19) 0.0636(19) 0.0107(14) 0.0220(14) 0.0279(14) C25 0.0559(18) 0.0590(19) 0.0610(19) 0.0115(14) 0.0220(14) 0.0283(14) C26 0.022(4) 0.026(4) 0.026(4) 0.005(3) 0.013(3) 0.015(3) C27 0.028(4) 0.022(4) 0.017(3) 0.004(3) 0.007(3) 0.009(3) C28 0.025(4) 0.038(5) 0.017(4) 0.004(3) 0.006(3) 0.012(4) C29 0.024(4) 0.032(4) 0.021(4) 0.009(3) 0.005(3) 0.014(4) C30 0.017(4) 0.028(4) 0.016(3) 0.003(3) 0.005(3) 0.014(3) C31 0.029(4) 0.028(4) 0.026(4) 0.006(3) 0.011(3) 0.013(4) C32 0.040(5) 0.035(5) 0.030(4) 0.002(4) 0.016(4) 0.021(4) C33 0.035(5) 0.035(5) 0.036(5) 0.008(4) 0.011(4) 0.009(4) C34 0.015(4) 0.050(5) 0.034(5) 0.005(4) 0.010(4) 0.015(4) C35 0.029(5) 0.032(4) 0.038(5) 0.003(4) 0.007(4) 0.020(4) C36 0.034(5) 0.026(4) 0.028(4) 0.003(3) 0.005(4) 0.009(4) C37 0.032(5) 0.020(4) 0.034(4) 0.007(3) 0.011(4) 0.012(4) C38 0.023(4) 0.021(4) 0.031(4) 0.012(3) 0.008(3) 0.009(3) C39 0.025(5) 0.031(4) 0.029(4) 0.006(3) 0.011(4) 0.001(4) C40 0.050(6) 0.023(4) 0.038(5) 0.008(4) 0.018(4) 0.012(4) C41 0.052(2) 0.050(2) 0.053(2) 0.0129(18) 0.0184(19) 0.0246(19) C42 0.0516(19) 0.0491(19) 0.0506(19) 0.0106(15) 0.0195(15) 0.0227(15) C43 0.055(2) 0.051(2) 0.054(2) 0.0114(18) 0.0179(18) 0.0239(18) C44 0.057(2) 0.0558(19) 0.0571(19) 0.0132(15) 0.0165(15) 0.0233(15) C45 0.054(2) 0.053(2) 0.056(2) 0.0136(19) 0.0169(19) 0.0245(19) C46 0.055(2) 0.054(2) 0.054(2) 0.0111(18) 0.0192(19) 0.0253(19) C47 0.0566(19) 0.0571(19) 0.0559(19) 0.0114(14) 0.0180(14) 0.0245(14) C48 0.0591(19) 0.0603(19) 0.0582(19) 0.0136(14) 0.0173(14) 0.0230(14) C49 0.0589(19) 0.0602(19) 0.0580(19) 0.0134(14) 0.0175(14) 0.0226(14) C50 0.056(2) 0.056(2) 0.055(2) 0.0132(18) 0.0185(19) 0.0248(19) C51 0.025(4) 0.025(4) 0.023(4) 0.009(3) 0.007(3) 0.010(3) C52 0.023(4) 0.025(4) 0.026(4) 0.008(3) 0.010(3) 0.007(3) C53 0.023(4) 0.037(5) 0.026(4) 0.013(3) 0.006(3) 0.013(4) C54 0.027(5) 0.031(4) 0.032(4) 0.009(4) 0.010(4) 0.008(4) C55 0.030(5) 0.033(5) 0.033(4) 0.006(4) 0.004(4) 0.012(4) C56 0.037(2) 0.039(2) 0.039(2) 0.0081(18) 0.0109(18) 0.0202(18) C57 0.037(2) 0.042(2) 0.040(2) 0.0079(19) 0.0131(19) 0.0212(19) C58 0.039(2) 0.046(2) 0.042(2) 0.0064(18) 0.0133(18) 0.0208(18) C59 0.0392(18) 0.0443(17) 0.0419(17) 0.0057(14) 0.0125(14) 0.0199(14) C60 0.0378(18) 0.0405(17) 0.0403(17) 0.0070(14) 0.0108(14) 0.0199(13) O1 0.020(3) 0.017(2) 0.026(3) 0.005(2) 0.009(2) 0.010(2) O2 0.055(2) 0.054(2) 0.054(2) 0.0161(18) 0.0170(18) 0.0227(18) O3 0.037(4) 0.035(4) 0.043(4) 0.008(3) 0.009(3) 0.009(3) O4 0.058(3) 0.057(2) 0.057(2) 0.0147(18) 0.0173(18) 0.0282(18) O5 0.092(6) 0.027(3) 0.077(5) -0.002(3) 0.000(4) 0.010(4) O6 0.040(4) 0.045(4) 0.059(4) 0.001(3) 0.016(4) 0.011(3) O7 0.020(3) 0.024(3) 0.023(3) 0.006(2) 0.010(2) 0.012(2) O8 0.048(4) 0.043(4) 0.039(4) 0.019(3) 0.021(3) 0.015(3) O9 0.035(4) 0.049(4) 0.059(4) 0.014(3) 0.003(3) 0.023(3) O10 0.037(3) 0.022(3) 0.031(3) -0.001(2) 0.007(3) 0.010(3) O11 0.025(4) 0.072(5) 0.042(4) 0.023(3) 0.012(3) 0.015(3) O12 0.077(5) 0.026(3) 0.045(4) -0.006(3) 0.021(4) 0.012(3) O13 0.046(2) 0.045(2) 0.048(2) 0.0098(16) 0.0230(17) 0.0161(16) O14 0.024(3) 0.035(3) 0.027(3) 0.014(2) 0.007(2) 0.016(3) P1 0.0221(11) 0.0176(9) 0.0300(10) 0.0059(8) 0.0053(9) 0.0064(8) P2 0.0201(10) 0.0192(9) 0.0202(9) 0.0043(7) 0.0082(8) 0.0089(8) W1 0.0344(2) 0.01989(17) 0.0354(2) 0.00935(14) 0.00886(16) 0.00995(15) W2 0.02287(18) 0.01884(16) 0.02057(16) 0.00460(12) 0.00799(13) 0.00767(13) Li1 0.029(3) 0.030(3) 0.029(3) 0.005(2) 0.010(2) 0.012(2) Li2 0.022(3) 0.022(3) 0.023(3) 0.0046(19) 0.006(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.289(13) . ? C1 C5 1.527(12) . ? C1 P1 1.835(9) . ? C2 C3 1.523(14) . ? C2 H2A 0.9500 . ? C3 C4 1.529(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.534(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.520(11) . ? C6 C10 1.519(13) . ? C6 C12 1.545(12) . ? C6 P1 1.893(8) . ? C7 C8 1.340(12) . ? C7 C11 1.492(13) . ? C8 C9 1.476(12) . ? C8 C13 1.497(11) . ? C9 C10 1.321(12) . ? C9 C14 1.501(13) . ? C10 C15 1.474(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 O2 1.170(11) . ? C16 W1 2.000(10) . ? C17 O3 1.151(9) . ? C17 W1 2.001(8) . ? C17 Li1 2.756(16) . ? C18 O4 1.159(11) . ? C18 W1 2.012(10) . ? C19 O5 1.144(12) . ? C19 W1 2.035(10) . ? C20 O6 1.143(10) . ? C20 W1 2.030(9) . ? C21 C25 1.348(14) . ? C21 C22 1.430(12) . ? C21 P2 1.805(9) . ? C22 C23 1.480(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.454(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.512(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9500 . ? C26 C27 1.515(10) . ? C26 C30 1.518(10) . ? C26 C31 1.534(10) . ? C26 P2 1.884(8) . ? C27 C28 1.343(11) . ? C27 C32 1.495(10) . ? C28 C29 1.465(11) . ? C28 C33 1.503(11) . ? C29 C30 1.328(10) . ? C29 C34 1.502(11) . ? C30 C35 1.514(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35C 0.9800 . ? C35 H35B 0.9800 . ? C35 H35A 0.9800 . ? C36 O8 1.160(10) . ? C36 W2 1.992(8) . ? C37 O9 1.161(10) . ? C37 W2 2.025(9) . ? C38 O10 1.157(9) . ? C38 W2 2.002(8) . ? C39 O11 1.132(10) . ? C39 W2 2.054(9) . ? C40 O12 1.132(10) . ? C40 W2 2.068(8) . ? C41 O13 1.284(12) . ? C41 C45 1.469(15) . ? C41 C42 1.485(14) . ? C42 C46 1.318(14) . ? C42 C43 1.529(14) . ? C43 C44 1.547(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.496(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.475(14) . ? C46 C50 1.544(15) . ? C47 C48 1.543(15) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.474(14) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.511(14) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O14 1.219(9) . ? C51 C52 1.470(11) . ? C51 C55 1.520(11) . ? C52 C56 1.319(12) . ? C52 C53 1.516(10) . ? C53 C54 1.541(11) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.536(12) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55B 0.9900 . ? C55 H55A 0.9900 . ? C56 C60 1.508(12) . ? C56 C57 1.523(12) . ? C57 C58 1.533(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.497(13) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.526(12) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? O1 P1 1.557(5) . ? O1 Li2 1.861(13) . ? O1 Li1 1.905(14) . ? O3 Li1 2.444(16) . ? O7 P2 1.566(5) . ? O7 Li1 1.863(15) . ? O7 Li2 1.900(13) . ? O10 Li2 2.476(14) . ? O13 Li1 1.880(15) . ? O14 Li2 1.914(14) . ? P1 W1 2.559(2) . ? P2 W2 2.5461(19) . ? Li1 Li2 2.438(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 C2 C1 C5 112.0(9) . . ? C2 C1 P1 122.5(7) . . ? C5 C1 P1 124.1(7) . . ? C1 C2 C3 112.5(10) . . ? C1 C2 H2A 123.8 . . ? C3 C2 H2A 123.8 . . ? C2 C3 C4 101.2(9) . . ? C2 C3 H3A 111.5 . . ? C4 C3 H3A 111.5 . . ? C2 C3 H3B 111.5 . . ? C4 C3 H3B 111.5 . . ? H3A C3 H3B 109.4 . . ? C3 C4 C5 105.9(9) . . ? C3 C4 H4A 110.6 . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4B 110.6 . . ? C5 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? C1 C5 C4 100.7(8) . . ? C1 C5 H5A 111.6 . . ? C4 C5 H5A 111.6 . . ? C1 C5 H5B 111.6 . . ? C4 C5 H5B 111.6 . . ? H5A C5 H5B 109.4 . . ? C7 C6 C10 102.3(7) . . ? C7 C6 C12 111.1(7) . . ? C10 C6 C12 113.6(7) . . ? C7 C6 P1 111.3(6) . . ? C10 C6 P1 107.9(6) . . ? C12 C6 P1 110.4(6) . . ? C8 C7 C11 126.7(8) . . ? C8 C7 C6 109.0(8) . . ? C11 C7 C6 123.1(8) . . ? C7 C8 C9 109.0(8) . . ? C7 C8 C13 127.9(8) . . ? C9 C8 C13 122.9(8) . . ? C10 C9 C8 110.1(8) . . ? C10 C9 C14 127.8(9) . . ? C8 C9 C14 122.0(8) . . ? C9 C10 C15 128.7(10) . . ? C9 C10 C6 109.3(8) . . ? C15 C10 C6 122.0(9) . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15C 109.5 . . ? C10 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C10 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? O2 C16 W1 171.2(9) . . ? O3 C17 W1 177.2(7) . . ? O3 C17 Li1 62.3(5) . . ? W1 C17 Li1 116.5(4) . . ? O4 C18 W1 172.8(8) . . ? O5 C19 W1 176.1(12) . . ? O6 C20 W1 175.7(8) . . ? C25 C21 C22 105.2(9) . . ? C25 C21 P2 130.2(8) . . ? C22 C21 P2 124.1(8) . . ? C21 C22 C23 112.8(9) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 103.1(9) . . ? C24 C23 H23A 111.2 . . ? C22 C23 H23A 111.2 . . ? C24 C23 H23B 111.2 . . ? C22 C23 H23B 111.2 . . ? H23A C23 H23B 109.1 . . ? C23 C24 C25 105.4(9) . . ? C23 C24 H24A 110.7 . . ? C25 C24 H24A 110.7 . . ? C23 C24 H24B 110.7 . . ? C25 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? C21 C25 C24 112.2(10) . . ? C21 C25 H25A 123.9 . . ? C24 C25 H25A 123.9 . . ? C27 C26 C30 102.5(6) . . ? C27 C26 C31 111.7(6) . . ? C30 C26 C31 110.9(6) . . ? C27 C26 P2 111.2(5) . . ? C30 C26 P2 108.1(5) . . ? C31 C26 P2 112.0(5) . . ? C28 C27 C32 126.2(7) . . ? C28 C27 C26 108.2(7) . . ? C32 C27 C26 125.1(7) . . ? C27 C28 C29 110.5(7) . . ? C27 C28 C33 127.2(8) . . ? C29 C28 C33 122.2(7) . . ? C30 C29 C28 108.9(7) . . ? C30 C29 C34 127.6(7) . . ? C28 C29 C34 123.4(7) . . ? C29 C30 C35 126.9(7) . . ? C29 C30 C26 109.8(6) . . ? C35 C30 C26 123.3(6) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35C 109.5 . . ? C30 C35 H35B 109.5 . . ? H35C C35 H35B 109.5 . . ? C30 C35 H35A 109.5 . . ? H35C C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? O8 C36 W2 177.5(8) . . ? O9 C37 W2 175.6(7) . . ? O10 C38 W2 175.8(7) . . ? O11 C39 W2 171.2(7) . . ? O12 C40 W2 176.3(9) . . ? O13 C41 C45 129.1(10) . . ? O13 C41 C42 124.1(10) . . ? C45 C41 C42 106.8(9) . . ? C46 C42 C41 123.1(10) . . ? C46 C42 C43 128.1(10) . . ? C41 C42 C43 108.6(9) . . ? C42 C43 C44 104.8(9) . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43B 110.8 . . ? C44 C43 H43B 110.8 . . ? H43A C43 H43B 108.9 . . ? C45 C44 C43 104.1(9) . . ? C45 C44 H44A 110.9 . . ? C43 C44 H44A 110.9 . . ? C45 C44 H44B 110.9 . . ? C43 C44 H44B 110.9 . . ? H44A C44 H44B 108.9 . . ? C41 C45 C44 110.5(9) . . ? C41 C45 H45A 109.6 . . ? C44 C45 H45A 109.6 . . ? C41 C45 H45B 109.6 . . ? C44 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C42 C46 C47 122.1(10) . . ? C42 C46 C50 129.7(10) . . ? C47 C46 C50 108.2(9) . . ? C46 C47 C48 106.9(9) . . ? C46 C47 H47A 110.3 . . ? C48 C47 H47A 110.3 . . ? C46 C47 H47B 110.3 . . ? C48 C47 H47B 110.3 . . ? H47A C47 H47B 108.6 . . ? C49 C48 C47 101.2(9) . . ? C49 C48 H48A 111.5 . . ? C47 C48 H48A 111.5 . . ? C49 C48 H48B 111.5 . . ? C47 C48 H48B 111.5 . . ? H48A C48 H48B 109.4 . . ? C48 C49 C50 108.0(9) . . ? C48 C49 H49A 110.1 . . ? C50 C49 H49A 110.1 . . ? C48 C49 H49B 110.1 . . ? C50 C49 H49B 110.1 . . ? H49A C49 H49B 108.4 . . ? C49 C50 C46 101.2(9) . . ? C49 C50 H50A 111.5 . . ? C46 C50 H50A 111.5 . . ? C49 C50 H50B 111.5 . . ? C46 C50 H50B 111.5 . . ? H50A C50 H50B 109.3 . . ? O14 C51 C52 127.9(7) . . ? O14 C51 C55 124.1(8) . . ? C52 C51 C55 108.0(6) . . ? C56 C52 C51 125.8(8) . . ? C56 C52 C53 125.9(8) . . ? C51 C52 C53 108.3(6) . . ? C52 C53 C54 103.9(6) . . ? C52 C53 H53A 111.0 . . ? C54 C53 H53A 111.0 . . ? C52 C53 H53B 111.0 . . ? C54 C53 H53B 111.0 . . ? H53A C53 H53B 109.0 . . ? C55 C54 C53 103.4(7) . . ? C55 C54 H54A 111.1 . . ? C53 C54 H54A 111.1 . . ? C55 C54 H54B 111.1 . . ? C53 C54 H54B 111.1 . . ? H54A C54 H54B 109.1 . . ? C51 C55 C54 104.1(7) . . ? C51 C55 H55B 110.9 . . ? C54 C55 H55B 110.9 . . ? C51 C55 H55A 110.9 . . ? C54 C55 H55A 110.9 . . ? H55B C55 H55A 108.9 . . ? C52 C56 C60 124.1(8) . . ? C52 C56 C57 127.7(9) . . ? C60 C56 C57 108.2(7) . . ? C56 C57 C58 103.1(8) . . ? C56 C57 H57A 111.1 . . ? C58 C57 H57A 111.1 . . ? C56 C57 H57B 111.1 . . ? C58 C57 H57B 111.1 . . ? H57A C57 H57B 109.1 . . ? C59 C58 C57 105.0(7) . . ? C59 C58 H58A 110.8 . . ? C57 C58 H58A 110.8 . . ? C59 C58 H58B 110.8 . . ? C57 C58 H58B 110.8 . . ? H58A C58 H58B 108.8 . . ? C58 C59 C60 103.9(8) . . ? C58 C59 H59A 111.0 . . ? C60 C59 H59A 111.0 . . ? C58 C59 H59B 111.0 . . ? C60 C59 H59B 111.0 . . ? H59A C59 H59B 109.0 . . ? C56 C60 C59 105.7(8) . . ? C56 C60 H60A 110.6 . . ? C59 C60 H60A 110.6 . . ? C56 C60 H60B 110.6 . . ? C59 C60 H60B 110.6 . . ? H60A C60 H60B 108.7 . . ? P1 O1 Li2 144.1(5) . . ? P1 O1 Li1 133.1(5) . . ? Li2 O1 Li1 80.7(6) . . ? C17 O3 Li1 93.0(6) . . ? P2 O7 Li1 143.5(5) . . ? P2 O7 Li2 135.4(5) . . ? Li1 O7 Li2 80.7(6) . . ? C38 O10 Li2 96.2(6) . . ? C41 O13 Li1 148.3(8) . . ? C51 O14 Li2 149.9(7) . . ? O1 P1 C1 104.2(3) . . ? O1 P1 C6 103.1(3) . . ? C1 P1 C6 106.2(4) . . ? O1 P1 W1 113.9(2) . . ? C1 P1 W1 108.2(3) . . ? C6 P1 W1 120.0(3) . . ? O7 P2 C21 103.8(4) . . ? O7 P2 C26 104.8(3) . . ? C21 P2 C26 104.4(4) . . ? O7 P2 W2 115.2(2) . . ? C21 P2 W2 111.1(3) . . ? C26 P2 W2 116.2(2) . . ? C17 W1 C16 92.8(3) . . ? C17 W1 C18 85.3(4) . . ? C16 W1 C18 90.6(4) . . ? C17 W1 C20 96.3(3) . . ? C16 W1 C20 81.4(4) . . ? C18 W1 C20 171.9(4) . . ? C17 W1 C19 169.7(4) . . ? C16 W1 C19 95.1(4) . . ? C18 W1 C19 88.1(5) . . ? C20 W1 C19 91.3(5) . . ? C17 W1 P1 82.1(2) . . ? C16 W1 P1 165.5(3) . . ? C18 W1 P1 102.5(3) . . ? C20 W1 P1 85.6(3) . . ? C19 W1 P1 91.7(3) . . ? C36 W2 C38 96.8(3) . . ? C36 W2 C37 87.4(3) . . ? C38 W2 C37 90.1(3) . . ? C36 W2 C39 84.1(3) . . ? C38 W2 C39 88.2(3) . . ? C37 W2 C39 171.1(3) . . ? C36 W2 C40 89.7(3) . . ? C38 W2 C40 172.2(3) . . ? C37 W2 C40 94.4(4) . . ? C39 W2 C40 88.2(4) . . ? C36 W2 P2 174.0(3) . . ? C38 W2 P2 82.8(2) . . ? C37 W2 P2 86.5(2) . . ? C39 W2 P2 101.9(2) . . ? C40 W2 P2 91.1(2) . . ? O7 Li1 O13 127.8(8) . . ? O7 Li1 O1 96.8(7) . . ? O13 Li1 O1 122.2(7) . . ? O7 Li1 O3 125.0(7) . . ? O13 Li1 O3 87.0(6) . . ? O1 Li1 O3 95.6(6) . . ? O7 Li1 Li2 50.3(5) . . ? O13 Li1 Li2 137.3(8) . . ? O1 Li1 Li2 48.9(4) . . ? O3 Li1 Li2 131.5(7) . . ? O7 Li1 C17 143.5(7) . . ? O13 Li1 C17 82.6(5) . . ? O1 Li1 C17 77.7(5) . . ? O3 Li1 C17 24.6(2) . . ? Li2 Li1 C17 123.5(6) . . ? O1 Li2 O7 97.0(6) . . ? O1 Li2 O14 124.8(7) . . ? O7 Li2 O14 116.0(7) . . ? O1 Li2 Li1 50.4(5) . . ? O7 Li2 Li1 49.0(4) . . ? O14 Li2 Li1 127.2(7) . . ? O1 Li2 O10 123.4(6) . . ? O7 Li2 O10 95.6(5) . . ? O14 Li2 O10 97.3(5) . . ? Li1 Li2 O10 130.5(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 C5 C1 C2 C3 2.5(12) . . . . ? P1 C1 C2 C3 169.7(7) . . . . ? C1 C2 C3 C4 14.8(11) . . . . ? C2 C3 C4 C5 -25.6(11) . . . . ? C2 C1 C5 C4 -18.6(11) . . . . ? P1 C1 C5 C4 174.4(7) . . . . ? C3 C4 C5 C1 26.8(10) . . . . ? C10 C6 C7 C8 -6.2(10) . . . . ? C12 C6 C7 C8 -127.8(9) . . . . ? P1 C6 C7 C8 108.7(8) . . . . ? C10 C6 C7 C11 161.7(9) . . . . ? C12 C6 C7 C11 40.0(12) . . . . ? P1 C6 C7 C11 -83.4(10) . . . . ? C11 C7 C8 C9 -162.2(9) . . . . ? C6 C7 C8 C9 5.2(10) . . . . ? C11 C7 C8 C13 12.8(16) . . . . ? C6 C7 C8 C13 -179.9(9) . . . . ? C7 C8 C9 C10 -1.8(11) . . . . ? C13 C8 C9 C10 -177.1(8) . . . . ? C7 C8 C9 C14 174.0(9) . . . . ? C13 C8 C9 C14 -1.3(14) . . . . ? C8 C9 C10 C15 -180.0(9) . . . . ? C14 C9 C10 C15 4.5(16) . . . . ? C8 C9 C10 C6 -2.4(10) . . . . ? C14 C9 C10 C6 -177.8(9) . . . . ? C7 C6 C10 C9 5.1(9) . . . . ? C12 C6 C10 C9 125.0(8) . . . . ? P1 C6 C10 C9 -112.3(7) . . . . ? C7 C6 C10 C15 -177.1(8) . . . . ? C12 C6 C10 C15 -57.2(11) . . . . ? P1 C6 C10 C15 65.5(10) . . . . ? C25 C21 C22 C23 -3.2(13) . . . . ? P2 C21 C22 C23 169.1(8) . . . . ? C21 C22 C23 C24 9.5(13) . . . . ? C22 C23 C24 C25 -11.2(12) . . . . ? C22 C21 C25 C24 -4.5(13) . . . . ? P2 C21 C25 C24 -176.2(9) . . . . ? C23 C24 C25 C21 10.5(14) . . . . ? C30 C26 C27 C28 -1.0(8) . . . . ? C31 C26 C27 C28 -119.8(7) . . . . ? P2 C26 C27 C28 114.3(6) . . . . ? C30 C26 C27 C32 172.2(7) . . . . ? C31 C26 C27 C32 53.4(10) . . . . ? P2 C26 C27 C32 -72.5(8) . . . . ? C32 C27 C28 C29 -171.6(7) . . . . ? C26 C27 C28 C29 1.6(9) . . . . ? C32 C27 C28 C33 5.2(14) . . . . ? C26 C27 C28 C33 178.4(8) . . . . ? C27 C28 C29 C30 -1.6(9) . . . . ? C33 C28 C29 C30 -178.6(7) . . . . ? C27 C28 C29 C34 175.9(7) . . . . ? C33 C28 C29 C34 -1.1(12) . . . . ? C28 C29 C30 C35 179.3(7) . . . . ? C34 C29 C30 C35 1.9(13) . . . . ? C28 C29 C30 C26 0.9(9) . . . . ? C34 C29 C30 C26 -176.5(7) . . . . ? C27 C26 C30 C29 0.0(8) . . . . ? C31 C26 C30 C29 119.4(7) . . . . ? P2 C26 C30 C29 -117.5(6) . . . . ? C27 C26 C30 C35 -178.4(7) . . . . ? C31 C26 C30 C35 -59.1(9) . . . . ? P2 C26 C30 C35 64.0(8) . . . . ? O13 C41 C42 C46 -0.4(17) . . . . ? C45 C41 C42 C46 179.7(10) . . . . ? O13 C41 C42 C43 176.5(9) . . . . ? C45 C41 C42 C43 -3.3(11) . . . . ? C46 C42 C43 C44 -167.2(11) . . . . ? C41 C42 C43 C44 16.0(11) . . . . ? C42 C43 C44 C45 -22.1(11) . . . . ? O13 C41 C45 C44 168.6(10) . . . . ? C42 C41 C45 C44 -11.6(12) . . . . ? C43 C44 C45 C41 21.3(12) . . . . ? C41 C42 C46 C47 177.0(9) . . . . ? C43 C42 C46 C47 0.7(18) . . . . ? C41 C42 C46 C50 -2.7(18) . . . . ? C43 C42 C46 C50 -179.0(10) . . . . ? C42 C46 C47 C48 -172.1(10) . . . . ? C50 C46 C47 C48 7.7(12) . . . . ? C46 C47 C48 C49 -27.9(12) . . . . ? C47 C48 C49 C50 38.9(12) . . . . ? C48 C49 C50 C46 -34.2(12) . . . . ? C42 C46 C50 C49 -165.1(11) . . . . ? C47 C46 C50 C49 15.2(11) . . . . ? O14 C51 C52 C56 -3.2(13) . . . . ? C55 C51 C52 C56 176.5(8) . . . . ? O14 C51 C52 C53 179.9(8) . . . . ? C55 C51 C52 C53 -0.4(8) . . . . ? C56 C52 C53 C54 -155.5(8) . . . . ? C51 C52 C53 C54 21.4(8) . . . . ? C52 C53 C54 C55 -33.6(8) . . . . ? O14 C51 C55 C54 158.9(7) . . . . ? C52 C51 C55 C54 -20.8(8) . . . . ? C53 C54 C55 C51 33.4(8) . . . . ? C51 C52 C56 C60 -177.7(8) . . . . ? C53 C52 C56 C60 -1.3(14) . . . . ? C51 C52 C56 C57 -0.1(15) . . . . ? C53 C52 C56 C57 176.4(8) . . . . ? C52 C56 C57 C58 -161.4(9) . . . . ? C60 C56 C57 C58 16.6(10) . . . . ? C56 C57 C58 C59 -33.6(9) . . . . ? C57 C58 C59 C60 37.8(9) . . . . ? C52 C56 C60 C59 -175.9(8) . . . . ? C57 C56 C60 C59 6.1(10) . . . . ? C58 C59 C60 C56 -27.0(9) . . . . ? W1 C17 O3 Li1 -65(16) . . . . ? W2 C38 O10 Li2 -50(9) . . . . ? C45 C41 O13 Li1 11(2) . . . . ? C42 C41 O13 Li1 -168.4(11) . . . . ? C52 C51 O14 Li2 176.8(10) . . . . ? C55 C51 O14 Li2 -2.8(17) . . . . ? Li2 O1 P1 C1 59.7(9) . . . . ? Li1 O1 P1 C1 -96.2(8) . . . . ? Li2 O1 P1 C6 -51.0(9) . . . . ? Li1 O1 P1 C6 153.0(7) . . . . ? Li2 O1 P1 W1 177.3(8) . . . . ? Li1 O1 P1 W1 21.4(8) . . . . ? C2 C1 P1 O1 1.8(9) . . . . ? C5 C1 P1 O1 167.4(7) . . . . ? C2 C1 P1 C6 110.3(8) . . . . ? C5 C1 P1 C6 -84.1(8) . . . . ? C2 C1 P1 W1 -119.7(8) . . . . ? C5 C1 P1 W1 45.9(8) . . . . ? C7 C6 P1 O1 167.6(6) . . . . ? C10 C6 P1 O1 -81.0(6) . . . . ? C12 C6 P1 O1 43.7(7) . . . . ? C7 C6 P1 C1 58.3(7) . . . . ? C10 C6 P1 C1 169.8(6) . . . . ? C12 C6 P1 C1 -65.5(7) . . . . ? C7 C6 P1 W1 -64.5(7) . . . . ? C10 C6 P1 W1 46.9(6) . . . . ? C12 C6 P1 W1 171.6(5) . . . . ? Li1 O7 P2 C21 67.4(10) . . . . ? Li2 O7 P2 C21 -102.8(8) . . . . ? Li1 O7 P2 C26 -41.8(10) . . . . ? Li2 O7 P2 C26 147.9(7) . . . . ? Li1 O7 P2 W2 -170.8(9) . . . . ? Li2 O7 P2 W2 18.9(7) . . . . ? C25 C21 P2 O7 141.1(11) . . . . ? C22 C21 P2 O7 -29.3(11) . . . . ? C25 C21 P2 C26 -109.4(11) . . . . ? C22 C21 P2 C26 80.3(10) . . . . ? C25 C21 P2 W2 16.7(12) . . . . ? C22 C21 P2 W2 -153.7(9) . . . . ? C27 C26 P2 O7 176.0(5) . . . . ? C30 C26 P2 O7 -72.2(5) . . . . ? C31 C26 P2 O7 50.3(5) . . . . ? C27 C26 P2 C21 67.2(6) . . . . ? C30 C26 P2 C21 179.0(5) . . . . ? C31 C26 P2 C21 -58.5(6) . . . . ? C27 C26 P2 W2 -55.5(5) . . . . ? C30 C26 P2 W2 56.3(5) . . . . ? C31 C26 P2 W2 178.7(4) . . . . ? O3 C17 W1 C16 -161(15) . . . . ? Li1 C17 W1 C16 135.0(5) . . . . ? O3 C17 W1 C18 -71(15) . . . . ? Li1 C17 W1 C18 -134.6(5) . . . . ? O3 C17 W1 C20 117(15) . . . . ? Li1 C17 W1 C20 53.3(5) . . . . ? O3 C17 W1 C19 -21(17) . . . . ? Li1 C17 W1 C19 -85(2) . . . . ? O3 C17 W1 P1 33(15) . . . . ? Li1 C17 W1 P1 -31.3(4) . . . . ? O2 C16 W1 C17 -68(6) . . . . ? O2 C16 W1 C18 -153(6) . . . . ? O2 C16 W1 C20 28(6) . . . . ? O2 C16 W1 C19 119(6) . . . . ? O2 C16 W1 P1 1(7) . . . . ? O4 C18 W1 C17 -70(7) . . . . ? O4 C18 W1 C16 22(7) . . . . ? O4 C18 W1 C20 31(8) . . . . ? O4 C18 W1 C19 117(7) . . . . ? O4 C18 W1 P1 -151(7) . . . . ? O6 C20 W1 C17 123(11) . . . . ? O6 C20 W1 C16 31(11) . . . . ? O6 C20 W1 C18 22(12) . . . . ? O6 C20 W1 C19 -64(11) . . . . ? O6 C20 W1 P1 -155(11) . . . . ? O5 C19 W1 C17 -26(17) . . . . ? O5 C19 W1 C16 115(15) . . . . ? O5 C19 W1 C18 24(15) . . . . ? O5 C19 W1 C20 -164(15) . . . . ? O5 C19 W1 P1 -78(15) . . . . ? O1 P1 W1 C17 14.6(3) . . . . ? C1 P1 W1 C17 129.8(4) . . . . ? C6 P1 W1 C17 -108.2(4) . . . . ? O1 P1 W1 C16 -55.8(12) . . . . ? C1 P1 W1 C16 59.4(12) . . . . ? C6 P1 W1 C16 -178.6(11) . . . . ? O1 P1 W1 C18 97.9(4) . . . . ? C1 P1 W1 C18 -146.8(4) . . . . ? C6 P1 W1 C18 -24.9(4) . . . . ? O1 P1 W1 C20 -82.5(3) . . . . ? C1 P1 W1 C20 32.8(4) . . . . ? C6 P1 W1 C20 154.7(4) . . . . ? O1 P1 W1 C19 -173.7(5) . . . . ? C1 P1 W1 C19 -58.4(5) . . . . ? C6 P1 W1 C19 63.5(5) . . . . ? O8 C36 W2 C38 -77(17) . . . . ? O8 C36 W2 C37 13(17) . . . . ? O8 C36 W2 C39 -164(17) . . . . ? O8 C36 W2 C40 108(17) . . . . ? O8 C36 W2 P2 9(19) . . . . ? O10 C38 W2 C36 -165(9) . . . . ? O10 C38 W2 C37 108(9) . . . . ? O10 C38 W2 C39 -81(9) . . . . ? O10 C38 W2 C40 -18(11) . . . . ? O10 C38 W2 P2 21(9) . . . . ? O9 C37 W2 C36 -8(9) . . . . ? O9 C37 W2 C38 89(9) . . . . ? O9 C37 W2 C39 10(11) . . . . ? O9 C37 W2 C40 -98(9) . . . . ? O9 C37 W2 P2 172(9) . . . . ? O11 C39 W2 C36 3(5) . . . . ? O11 C39 W2 C38 -94(5) . . . . ? O11 C39 W2 C37 -15(6) . . . . ? O11 C39 W2 C40 93(5) . . . . ? O11 C39 W2 P2 -177(5) . . . . ? O12 C40 W2 C36 64(12) . . . . ? O12 C40 W2 C38 -83(13) . . . . ? O12 C40 W2 C37 151(12) . . . . ? O12 C40 W2 C39 -20(12) . . . . ? O12 C40 W2 P2 -122(12) . . . . ? O7 P2 W2 C36 -73(2) . . . . ? C21 P2 W2 C36 44(2) . . . . ? C26 P2 W2 C36 163(2) . . . . ? O7 P2 W2 C38 13.3(3) . . . . ? C21 P2 W2 C38 131.0(4) . . . . ? C26 P2 W2 C38 -109.9(3) . . . . ? O7 P2 W2 C37 -77.3(3) . . . . ? C21 P2 W2 C37 40.4(4) . . . . ? C26 P2 W2 C37 159.5(3) . . . . ? O7 P2 W2 C39 99.9(3) . . . . ? C21 P2 W2 C39 -142.4(4) . . . . ? C26 P2 W2 C39 -23.2(3) . . . . ? O7 P2 W2 C40 -171.7(4) . . . . ? C21 P2 W2 C40 -54.0(5) . . . . ? C26 P2 W2 C40 65.2(4) . . . . ? P2 O7 Li1 O13 -48.7(15) . . . . ? Li2 O7 Li1 O13 124.4(11) . . . . ? P2 O7 Li1 O1 170.7(5) . . . . ? Li2 O7 Li1 O1 -16.2(6) . . . . ? P2 O7 Li1 O3 68.9(12) . . . . ? Li2 O7 Li1 O3 -118.0(8) . . . . ? P2 O7 Li1 Li2 -173.1(9) . . . . ? P2 O7 Li1 C17 92.2(13) . . . . ? Li2 O7 Li1 C17 -94.7(11) . . . . ? C41 O13 Li1 O7 -77.7(17) . . . . ? C41 O13 Li1 O1 54.2(19) . . . . ? C41 O13 Li1 O3 148.9(13) . . . . ? C41 O13 Li1 Li2 -8(2) . . . . ? C41 O13 Li1 C17 124.6(14) . . . . ? P1 O1 Li1 O7 -177.5(4) . . . . ? Li2 O1 Li1 O7 16.5(6) . . . . ? P1 O1 Li1 O13 38.8(13) . . . . ? Li2 O1 Li1 O13 -127.1(10) . . . . ? P1 O1 Li1 O3 -51.2(8) . . . . ? Li2 O1 Li1 O3 142.9(6) . . . . ? P1 O1 Li1 Li2 166.0(7) . . . . ? P1 O1 Li1 C17 -34.1(7) . . . . ? Li2 O1 Li1 C17 159.9(5) . . . . ? C17 O3 Li1 O7 145.8(8) . . . . ? C17 O3 Li1 O13 -78.7(7) . . . . ? C17 O3 Li1 O1 43.4(7) . . . . ? C17 O3 Li1 Li2 80.7(9) . . . . ? O3 C17 Li1 O7 -50.7(12) . . . . ? W1 C17 Li1 O7 126.5(10) . . . . ? O3 C17 Li1 O13 99.1(7) . . . . ? W1 C17 Li1 O13 -83.7(6) . . . . ? O3 C17 Li1 O1 -135.6(7) . . . . ? W1 C17 Li1 O1 41.6(6) . . . . ? W1 C17 Li1 O3 177.2(8) . . . . ? O3 C17 Li1 Li2 -117.5(9) . . . . ? W1 C17 Li1 Li2 59.7(9) . . . . ? P1 O1 Li2 O7 -178.6(5) . . . . ? Li1 O1 Li2 O7 -16.2(6) . . . . ? P1 O1 Li2 O14 -50.0(13) . . . . ? Li1 O1 Li2 O14 112.4(9) . . . . ? P1 O1 Li2 Li1 -162.4(9) . . . . ? P1 O1 Li2 O10 79.9(10) . . . . ? Li1 O1 Li2 O10 -117.6(8) . . . . ? P2 O7 Li2 O1 -169.3(4) . . . . ? Li1 O7 Li2 O1 16.6(6) . . . . ? P2 O7 Li2 O14 56.3(10) . . . . ? Li1 O7 Li2 O14 -117.8(8) . . . . ? P2 O7 Li2 Li1 174.1(8) . . . . ? P2 O7 Li2 O10 -44.6(8) . . . . ? Li1 O7 Li2 O10 141.3(6) . . . . ? C51 O14 Li2 O1 115.7(13) . . . . ? C51 O14 Li2 O7 -124.0(12) . . . . ? C51 O14 Li2 Li1 179.1(11) . . . . ? C51 O14 Li2 O10 -24.1(14) . . . . ? O7 Li1 Li2 O1 -158.4(8) . . . . ? O13 Li1 Li2 O1 95.6(11) . . . . ? O3 Li1 Li2 O1 -53.3(8) . . . . ? C17 Li1 Li2 O1 -23.7(6) . . . . ? O13 Li1 Li2 O7 -106.0(12) . . . . ? O1 Li1 Li2 O7 158.4(8) . . . . ? O3 Li1 Li2 O7 105.2(9) . . . . ? C17 Li1 Li2 O7 134.7(9) . . . . ? O7 Li1 Li2 O14 94.0(8) . . . . ? O13 Li1 Li2 O14 -12.0(15) . . . . ? O1 Li1 Li2 O14 -107.6(9) . . . . ? O3 Li1 Li2 O14 -160.8(7) . . . . ? C17 Li1 Li2 O14 -131.3(8) . . . . ? O7 Li1 Li2 O10 -55.0(8) . . . . ? O13 Li1 Li2 O10 -161.0(8) . . . . ? O1 Li1 Li2 O10 103.5(8) . . . . ? O3 Li1 Li2 O10 50.2(12) . . . . ? C17 Li1 Li2 O10 79.8(10) . . . . ? C38 O10 Li2 O1 140.6(8) . . . . ? C38 O10 Li2 O7 38.4(7) . . . . ? C38 O10 Li2 O14 -78.8(7) . . . . ? C38 O10 Li2 Li1 76.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.153 _refine_diff_density_min -1.891 _refine_diff_density_rms 0.197 #END---------------------------------------------------------------------------