data_global _publ_contact_author_name 'Martin Lutz' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'm.lutz@chem.uu.nl' _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' _publ_section_title ; 3H-Benzophosphepine Complexes: Versatile Phosphinidene Precursors ; loop_ _publ_author_name _publ_author_address 'Borst, Mark L. G.' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Bulo, Rosa E.' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Gibney, Daniele J.' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Alem, Yonathan' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'de Kanter, Franciscus J. J.' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Ehlers, Andreas W.' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Schakel, Marius' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Lammertsma, Koop' ; Vrije Universiteit Faculty of Sciences Department of Chemistry De Boelelaan 1083 1081 HV Amsterdam The Netherlands ; data_s3428a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 O10 P2 W2' _chemical_formula_sum 'C22 H16 O10 P2 W2' _chemical_formula_weight 869.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7509(4) _cell_length_b 14.9157(8) _cell_length_c 26.1982(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.038(2) _cell_angle_gamma 90.00 _cell_volume 2636.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 235 _cell_measurement_theta_min 4.12 _cell_measurement_theta_max 22.86 _exptl_crystal_description needle _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 8.892 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.59 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49511 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6046 _reflns_number_gt 5436 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Dirax' _computing_data_reduction 'EvalCCD, sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+2.3897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6046 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0383 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 W1 W 0.089184(15) 0.242815(7) 0.226560(4) 0.01798(4) Uani 1 1 d . . . W2 W 0.434152(15) 0.272019(7) 0.525163(4) 0.01656(3) Uani 1 1 d . . . P1 P 0.21125(10) 0.32175(4) 0.30604(3) 0.01615(13) Uani 1 1 d . . . P2 P 0.31543(10) 0.33276(4) 0.44034(2) 0.01530(13) Uani 1 1 d . . . O11 O -0.0803(4) 0.08401(15) 0.29329(9) 0.0410(6) Uani 1 1 d . . . O12 O 0.5007(3) 0.14067(15) 0.21508(9) 0.0398(6) Uani 1 1 d . . . O13 O 0.2278(3) 0.40232(15) 0.15495(9) 0.0387(5) Uani 1 1 d . . . O14 O -0.3085(3) 0.35250(16) 0.24056(8) 0.0363(5) Uani 1 1 d . . . O15 O -0.0902(3) 0.13899(15) 0.13048(8) 0.0384(5) Uani 1 1 d . . . O21 O 0.2837(4) 0.44724(15) 0.58128(10) 0.0434(6) Uani 1 1 d . . . O22 O 0.8484(3) 0.36290(13) 0.50429(8) 0.0291(5) Uani 1 1 d . . . O23 O 0.6044(3) 0.09404(15) 0.47493(9) 0.0415(6) Uani 1 1 d . . . O24 O 0.0223(3) 0.17403(15) 0.54338(9) 0.0385(6) Uani 1 1 d . . . O25 O 0.6121(3) 0.20422(15) 0.63091(8) 0.0363(5) Uani 1 1 d . . . C11 C 0.4218(4) 0.26947(16) 0.34280(10) 0.0166(5) Uani 1 1 d . . . H11 H 0.5331 0.2587 0.3194 0.020 Uiso 1 1 calc R . . C12 C 0.3451(4) 0.18029(17) 0.36122(10) 0.0174(5) Uani 1 1 d . . . C13 C 0.4257(4) 0.09824(18) 0.34738(11) 0.0252(6) Uani 1 1 d . . . H13 H 0.5346 0.0964 0.3254 0.030 Uiso 1 1 calc R . . C14 C 0.3466(5) 0.01931(19) 0.36577(12) 0.0326(7) Uani 1 1 d . . . H14 H 0.4007 -0.0367 0.3561 0.039 Uiso 1 1 calc R . . C15 C 0.2785(4) 0.43906(17) 0.29687(11) 0.0249(6) Uani 1 1 d . . . H15A H 0.3152 0.4660 0.3300 0.037 Uiso 1 1 calc R . . H15B H 0.1653 0.4715 0.2814 0.037 Uiso 1 1 calc R . . H15C H 0.3911 0.4426 0.2743 0.037 Uiso 1 1 calc R . . C16 C 0.4987(4) 0.32604(17) 0.38886(10) 0.0179(5) Uani 1 1 d . . . H16A H 0.5292 0.3874 0.3770 0.021 Uiso 1 1 calc R . . H16B H 0.6231 0.2992 0.4030 0.021 Uiso 1 1 calc R . . C17 C -0.0159(4) 0.14128(19) 0.27046(11) 0.0255(6) Uani 1 1 d . . . C18 C 0.3534(4) 0.17733(19) 0.21934(11) 0.0251(6) Uani 1 1 d . . . C19 C 0.1831(4) 0.34512(19) 0.18119(11) 0.0250(6) Uani 1 1 d . . . C110 C -0.1676(4) 0.3119(2) 0.23479(10) 0.0240(6) Uani 1 1 d . . . C111 C -0.0238(4) 0.17762(19) 0.16474(11) 0.0250(6) Uani 1 1 d . . . C21 C 0.1063(4) 0.27471(16) 0.40654(10) 0.0168(5) Uani 1 1 d . . . H21 H -0.0051 0.2679 0.4304 0.020 Uiso 1 1 calc R . . C22 C 0.1850(4) 0.18255(17) 0.39346(10) 0.0178(5) Uani 1 1 d . . . C23 C 0.1071(4) 0.10322(18) 0.41230(11) 0.0240(6) Uani 1 1 d . . . H23 H -0.0009 0.1047 0.4346 0.029 Uiso 1 1 calc R . . C24 C 0.1892(5) 0.02170(19) 0.39812(12) 0.0311(7) Uani 1 1 d . . . H24 H 0.1368 -0.0327 0.4108 0.037 Uiso 1 1 calc R . . C25 C 0.2450(4) 0.45061(17) 0.44252(11) 0.0227(6) Uani 1 1 d . . . H25A H 0.2124 0.4719 0.4078 0.034 Uiso 1 1 calc R . . H25B H 0.3555 0.4858 0.4572 0.034 Uiso 1 1 calc R . . H25C H 0.1291 0.4575 0.4637 0.034 Uiso 1 1 calc R . . C26 C 0.0291(4) 0.32381(18) 0.35769(10) 0.0200(5) Uani 1 1 d . . . H26A H -0.0011 0.3869 0.3663 0.024 Uiso 1 1 calc R . . H26B H -0.0956 0.2951 0.3451 0.024 Uiso 1 1 calc R . . C27 C 0.3348(4) 0.3843(2) 0.56049(11) 0.0266(6) Uani 1 1 d . . . C28 C 0.6979(4) 0.33115(17) 0.51225(10) 0.0200(5) Uani 1 1 d . . . C29 C 0.5386(4) 0.1571(2) 0.49165(11) 0.0260(6) Uani 1 1 d . . . C210 C 0.1687(4) 0.20920(19) 0.53689(11) 0.0247(6) Uani 1 1 d . . . C211 C 0.5463(4) 0.22830(18) 0.59281(11) 0.0235(6) 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 W1 0.01762(6) 0.02136(6) 0.01494(6) -0.00173(4) 0.00036(4) 0.00055(4) W2 0.01697(6) 0.01768(6) 0.01501(6) 0.00108(4) 0.00013(4) -0.00241(4) P1 0.0170(3) 0.0160(3) 0.0155(3) 0.0008(2) 0.0010(2) 0.0009(2) P2 0.0168(3) 0.0142(3) 0.0150(3) -0.0005(2) 0.0011(2) -0.0010(2) O11 0.0495(15) 0.0374(13) 0.0356(14) 0.0049(10) -0.0032(11) -0.0223(11) O12 0.0325(13) 0.0384(13) 0.0490(15) 0.0025(11) 0.0091(11) 0.0129(10) O13 0.0436(14) 0.0344(13) 0.0390(14) 0.0120(10) 0.0145(11) 0.0047(10) O14 0.0285(12) 0.0503(14) 0.0304(12) -0.0003(10) 0.0056(9) 0.0134(11) O15 0.0432(14) 0.0414(13) 0.0299(12) -0.0145(10) -0.0077(10) 0.0059(11) O21 0.0468(15) 0.0340(13) 0.0506(16) -0.0147(11) 0.0203(12) -0.0049(11) O22 0.0227(11) 0.0255(11) 0.0399(13) -0.0050(9) 0.0106(9) -0.0041(9) O23 0.0437(14) 0.0301(13) 0.0503(16) -0.0101(10) -0.0033(11) 0.0102(11) O24 0.0289(12) 0.0378(13) 0.0487(15) 0.0138(11) 0.0012(10) -0.0124(10) O25 0.0452(14) 0.0342(12) 0.0286(12) 0.0097(9) -0.0128(10) -0.0124(11) C11 0.0154(13) 0.0184(13) 0.0161(13) 0.0002(9) 0.0030(10) 0.0008(10) C12 0.0172(13) 0.0178(13) 0.0170(13) 0.0008(9) -0.0029(10) 0.0002(10) C13 0.0255(15) 0.0232(14) 0.0271(15) -0.0011(11) 0.0030(12) 0.0038(11) C14 0.044(2) 0.0162(14) 0.0371(18) -0.0010(12) -0.0009(14) 0.0048(13) C15 0.0346(17) 0.0167(13) 0.0235(14) 0.0029(11) 0.0028(12) 0.0013(11) C16 0.0152(13) 0.0205(13) 0.0180(13) 0.0003(10) 0.0007(10) -0.0028(10) C17 0.0261(15) 0.0281(15) 0.0219(15) -0.0063(11) -0.0036(11) -0.0051(12) C18 0.0285(16) 0.0232(14) 0.0236(15) 0.0001(11) 0.0027(12) 0.0008(12) C19 0.0240(15) 0.0285(15) 0.0228(15) -0.0021(12) 0.0035(11) 0.0066(12) C110 0.0235(15) 0.0331(16) 0.0155(13) -0.0007(11) 0.0018(11) -0.0004(12) C111 0.0253(15) 0.0281(15) 0.0216(15) -0.0031(11) 0.0008(11) 0.0042(12) C21 0.0153(13) 0.0194(13) 0.0159(13) -0.0010(9) 0.0029(10) -0.0018(10) C22 0.0194(13) 0.0178(13) 0.0162(13) -0.0019(9) -0.0003(10) -0.0011(10) C23 0.0272(15) 0.0234(14) 0.0216(14) 0.0006(11) 0.0021(11) -0.0088(11) C24 0.0439(19) 0.0169(14) 0.0325(17) 0.0034(12) -0.0009(14) -0.0077(13) C25 0.0267(15) 0.0167(13) 0.0247(15) -0.0015(10) 0.0024(11) -0.0009(11) C26 0.0158(13) 0.0246(14) 0.0195(13) -0.0011(10) 0.0002(10) 0.0022(10) C27 0.0249(15) 0.0295(16) 0.0259(15) -0.0016(12) 0.0083(12) -0.0049(12) C28 0.0238(15) 0.0185(13) 0.0178(13) -0.0032(10) 0.0025(11) 0.0011(11) C29 0.0249(15) 0.0262(16) 0.0268(15) 0.0004(12) -0.0023(12) -0.0019(12) C210 0.0261(15) 0.0259(14) 0.0220(14) 0.0074(11) -0.0013(11) -0.0016(12) C211 0.0254(15) 0.0235(14) 0.0214(14) 0.0025(11) -0.0027(11) -0.0083(11) _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 W1 C111 2.015(3) . ? W1 C110 2.034(3) . ? W1 C17 2.044(3) . ? W1 C18 2.048(3) . ? W1 C19 2.049(3) . ? W1 P1 2.5058(7) . ? W2 C211 2.011(3) . ? W2 C28 2.026(3) . ? W2 C27 2.038(3) . ? W2 C210 2.055(3) . ? W2 C29 2.062(3) . ? W2 P2 2.5048(7) . ? P1 C15 1.826(3) . ? P1 C11 1.860(3) . ? P1 C26 1.861(3) . ? P2 C25 1.822(3) . ? P2 C21 1.854(3) . ? P2 C16 1.865(3) . ? O11 C17 1.138(4) . ? O12 C18 1.144(3) . ? O13 C19 1.143(3) . ? O14 C110 1.143(3) . ? O15 C111 1.145(3) . ? O21 C27 1.145(4) . ? O22 C28 1.147(3) . ? O23 C29 1.134(4) . ? O24 C210 1.137(3) . ? O25 C211 1.136(3) . ? C11 C12 1.513(3) . ? C11 C16 1.547(3) . ? C11 H11 1.0000 . ? C12 C13 1.393(4) . ? C12 C22 1.395(4) . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C24 1.383(5) . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C22 1.517(3) . ? C21 C26 1.549(4) . ? C21 H21 1.0000 . ? C22 C23 1.393(4) . ? C23 C24 1.392(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C111 W1 C110 91.72(11) . . ? C111 W1 C17 88.04(11) . . ? C110 W1 C17 90.09(12) . . ? C111 W1 C18 90.09(11) . . ? C110 W1 C18 177.86(11) . . ? C17 W1 C18 91.11(12) . . ? C111 W1 C19 90.53(12) . . ? C110 W1 C19 88.09(11) . . ? C17 W1 C19 177.65(11) . . ? C18 W1 C19 90.75(11) . . ? C111 W1 P1 176.63(8) . . ? C110 W1 P1 86.00(8) . . ? C17 W1 P1 89.48(8) . . ? C18 W1 P1 92.24(8) . . ? C19 W1 P1 91.88(8) . . ? C211 W2 C28 89.01(11) . . ? C211 W2 C27 89.19(12) . . ? C28 W2 C27 91.35(11) . . ? C211 W2 C210 91.35(11) . . ? C28 W2 C210 178.40(11) . . ? C27 W2 C210 90.22(12) . . ? C211 W2 C29 88.96(11) . . ? C28 W2 C29 88.57(11) . . ? C27 W2 C29 178.15(11) . . ? C210 W2 C29 89.87(12) . . ? C211 W2 P2 176.09(8) . . ? C28 W2 P2 87.12(8) . . ? C27 W2 P2 90.32(9) . . ? C210 W2 P2 92.54(8) . . ? C29 W2 P2 91.52(8) . . ? C15 P1 C11 106.32(13) . . ? C15 P1 C26 104.70(13) . . ? C11 P1 C26 98.23(12) . . ? C15 P1 W1 114.64(9) . . ? C11 P1 W1 117.13(8) . . ? C26 P1 W1 113.93(9) . . ? C25 P2 C21 105.68(12) . . ? C25 P2 C16 104.78(13) . . ? C21 P2 C16 98.21(12) . . ? C25 P2 W2 113.38(9) . . ? C21 P2 W2 117.96(8) . . ? C16 P2 W2 115.00(8) . . ? C12 C11 C16 109.9(2) . . ? C12 C11 P1 105.66(17) . . ? C16 C11 P1 113.85(17) . . ? C12 C11 H11 109.1 . . ? C16 C11 H11 109.1 . . ? P1 C11 H11 109.1 . . ? C13 C12 C22 119.8(2) . . ? C13 C12 C11 123.2(2) . . ? C22 C12 C11 116.9(2) . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C24 C14 C13 120.3(3) . . ? C24 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 P2 112.37(17) . . ? C11 C16 H16A 109.1 . . ? P2 C16 H16A 109.1 . . ? C11 C16 H16B 109.1 . . ? P2 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? O11 C17 W1 177.1(3) . . ? O12 C18 W1 179.7(3) . . ? O13 C19 W1 177.2(3) . . ? O14 C110 W1 177.7(3) . . ? O15 C111 W1 178.2(3) . . ? C22 C21 C26 110.6(2) . . ? C22 C21 P2 105.32(17) . . ? C26 C21 P2 113.71(17) . . ? C22 C21 H21 109.0 . . ? C26 C21 H21 109.0 . . ? P2 C21 H21 109.0 . . ? C23 C22 C12 120.3(2) . . ? C23 C22 C21 123.4(2) . . ? C12 C22 C21 116.3(2) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C14 C24 C23 120.5(3) . . ? C14 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? P2 C25 H25A 109.5 . . ? P2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 P1 112.41(18) . . ? C21 C26 H26A 109.1 . . ? P1 C26 H26A 109.1 . . ? C21 C26 H26B 109.1 . . ? P1 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? O21 C27 W2 178.0(3) . . ? O22 C28 W2 178.4(2) . . ? O23 C29 W2 176.4(3) . . ? O24 C210 W2 179.6(3) . . ? O25 C211 W2 179.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C110 W1 P1 C15 -75.60(13) . . . . ? C17 W1 P1 C15 -165.73(14) . . . . ? C18 W1 P1 C15 103.18(13) . . . . ? C19 W1 P1 C15 12.35(13) . . . . ? C110 W1 P1 C11 158.79(12) . . . . ? C17 W1 P1 C11 68.66(13) . . . . ? C18 W1 P1 C11 -22.43(12) . . . . ? C19 W1 P1 C11 -113.26(12) . . . . ? C110 W1 P1 C26 45.00(12) . . . . ? C17 W1 P1 C26 -45.13(13) . . . . ? C18 W1 P1 C26 -136.22(12) . . . . ? C19 W1 P1 C26 132.95(12) . . . . ? C28 W2 P2 C25 -79.77(13) . . . . ? C27 W2 P2 C25 11.57(13) . . . . ? C210 W2 P2 C25 101.80(13) . . . . ? C29 W2 P2 C25 -168.27(13) . . . . ? C28 W2 P2 C21 155.98(12) . . . . ? C27 W2 P2 C21 -112.68(12) . . . . ? C210 W2 P2 C21 -22.45(13) . . . . ? C29 W2 P2 C21 67.49(12) . . . . ? C28 W2 P2 C16 40.77(12) . . . . ? C27 W2 P2 C16 132.11(12) . . . . ? C210 W2 P2 C16 -137.66(12) . . . . ? C29 W2 P2 C16 -47.72(12) . . . . ? C15 P1 C11 C12 166.48(18) . . . . ? C26 P1 C11 C12 58.44(19) . . . . ? W1 P1 C11 C12 -63.87(18) . . . . ? C15 P1 C11 C16 45.8(2) . . . . ? C26 P1 C11 C16 -62.2(2) . . . . ? W1 P1 C11 C16 175.46(14) . . . . ? C16 C11 C12 C13 -118.3(3) . . . . ? P1 C11 C12 C13 118.5(2) . . . . ? C16 C11 C12 C22 62.0(3) . . . . ? P1 C11 C12 C22 -61.2(3) . . . . ? C22 C12 C13 C14 -0.1(4) . . . . ? C11 C12 C13 C14 -179.8(3) . . . . ? C12 C13 C14 C24 -0.6(5) . . . . ? C12 C11 C16 P2 -50.2(2) . . . . ? P1 C11 C16 P2 68.0(2) . . . . ? C25 P2 C16 C11 -114.63(19) . . . . ? C21 P2 C16 C11 -5.9(2) . . . . ? W2 P2 C16 C11 120.22(16) . . . . ? C25 P2 C21 C22 166.62(17) . . . . ? C16 P2 C21 C22 58.67(19) . . . . ? W2 P2 C21 C22 -65.39(18) . . . . ? C25 P2 C21 C26 45.4(2) . . . . ? C16 P2 C21 C26 -62.6(2) . . . . ? W2 P2 C21 C26 173.35(15) . . . . ? C13 C12 C22 C23 0.7(4) . . . . ? C11 C12 C22 C23 -179.5(2) . . . . ? C13 C12 C22 C21 -180.0(2) . . . . ? C11 C12 C22 C21 -0.2(3) . . . . ? C26 C21 C22 C23 -119.1(3) . . . . ? P2 C21 C22 C23 117.6(2) . . . . ? C26 C21 C22 C12 61.5(3) . . . . ? P2 C21 C22 C12 -61.7(3) . . . . ? C12 C22 C23 C24 -0.7(4) . . . . ? C21 C22 C23 C24 180.0(3) . . . . ? C13 C14 C24 C23 0.6(5) . . . . ? C22 C23 C24 C14 0.1(4) . . . . ? C22 C21 C26 P1 -49.7(3) . . . . ? P2 C21 C26 P1 68.5(2) . . . . ? C15 P1 C26 C21 -115.65(19) . . . . ? C11 P1 C26 C21 -6.3(2) . . . . ? W1 P1 C26 C21 118.33(16) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.576 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.106 #===END data_s3248a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Mo2 O10 P2' _chemical_formula_sum 'C32 H20 Mo2 O10 P2' _chemical_formula_weight 818.30 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 9.0413(1) _cell_length_b 21.6707(3) _cell_length_c 17.8474(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.9773(5) _cell_angle_gamma 90.00 _cell_volume 3242.75(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 45996 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38814 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.24 _reflns_number_total 5864 _reflns_number_gt 4137 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000, SortAV' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5864 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 Mo1 Mo 0.37803(4) 0.040712(13) 0.172092(19) 0.02884(11) Uani 1 1 d . . . Mo2 Mo 0.99730(4) 0.296568(13) 0.289246(18) 0.02578(10) Uani 1 1 d . . . P1 P 0.62099(11) 0.10789(4) 0.20838(6) 0.0255(2) Uani 1 1 d . . . P2 P 0.96081(11) 0.19029(4) 0.33755(5) 0.0243(2) Uani 1 1 d . . . O1 O 0.1768(3) 0.16342(13) 0.15664(17) 0.0494(7) Uani 1 1 d . . . O2 O 0.3407(3) 0.04424(11) -0.01362(17) 0.0443(7) Uani 1 1 d . . . O3 O 0.5981(3) -0.07854(13) 0.19652(18) 0.0523(8) Uani 1 1 d . . . O4 O 0.3943(4) 0.02525(14) 0.35206(19) 0.0638(9) Uani 1 1 d . . . O5 O 0.0583(4) -0.03457(13) 0.1117(2) 0.0616(9) Uani 1 1 d . . . O6 O 1.1281(4) 0.34058(12) 0.47299(17) 0.0495(8) Uani 1 1 d . . . O7 O 1.3486(3) 0.26301(13) 0.30155(17) 0.0492(8) Uani 1 1 d . . . O8 O 0.8758(3) 0.25981(13) 0.10388(17) 0.0500(8) Uani 1 1 d . . . O9 O 0.6568(3) 0.34351(12) 0.27551(17) 0.0478(7) Uani 1 1 d . . . O10 O 1.0259(4) 0.43258(13) 0.23448(19) 0.0586(9) Uani 1 1 d . . . C1 C 0.8182(4) 0.07580(15) 0.2712(2) 0.0257(8) Uani 1 1 d . . . H1 H 0.830(4) 0.0399(14) 0.2467(18) 0.024(9) Uiso 1 1 d . . . C2 C 0.8064(4) 0.06360(15) 0.3524(2) 0.0270(8) Uani 1 1 d . . . C3 C 0.8158(4) 0.00508(16) 0.3861(2) 0.0346(9) Uani 1 1 d . . . H3 H 0.8316 -0.0302 0.3584 0.041 Uiso 1 1 calc R . . C4 C 0.8022(5) -0.00133(18) 0.4601(2) 0.0438(11) Uani 1 1 d . . . H4 H 0.8109 -0.0411 0.4837 0.053 Uiso 1 1 calc R . . C5 C 0.7761(5) 0.04919(18) 0.5003(2) 0.0453(11) Uani 1 1 d . . . H5 H 0.7651 0.0441 0.5509 0.054 Uiso 1 1 calc R . . C6 C 0.7659(5) 0.10707(17) 0.4670(2) 0.0390(10) Uani 1 1 d . . . H6 H 0.7486 0.1419 0.4950 0.047 Uiso 1 1 calc R . . C7 C 0.7805(4) 0.11488(15) 0.3932(2) 0.0264(8) Uani 1 1 d . . . C8 C 0.7712(4) 0.17613(16) 0.3530(2) 0.0267(8) Uani 1 1 d . . . H8 H 0.750(4) 0.2083(14) 0.3846(18) 0.023(9) Uiso 1 1 d . . . C9 C 0.6330(5) 0.17801(17) 0.2700(2) 0.0300(9) Uani 1 1 d . . . H9A H 0.546(4) 0.1797(13) 0.2813(18) 0.019(9) Uiso 1 1 d . . . H9B H 0.637(3) 0.2139(14) 0.2394(17) 0.015(8) Uiso 1 1 d . . . C10 C 0.9556(5) 0.11951(17) 0.2774(2) 0.0270(8) Uani 1 1 d . . . H10A H 1.053(4) 0.1004(15) 0.301(2) 0.033(10) Uiso 1 1 d . . . H10B H 0.948(3) 0.1339(12) 0.2272(18) 0.010(8) Uiso 1 1 d . . . C11 C 0.6406(4) 0.13654(15) 0.1163(2) 0.0291(9) Uani 1 1 d . . . C12 C 0.5444(5) 0.18567(16) 0.0751(2) 0.0364(9) Uani 1 1 d . . . H12 H 0.4825 0.2074 0.0993 0.044 Uiso 1 1 calc R . . C13 C 0.5384(5) 0.20284(17) -0.0002(2) 0.0436(10) Uani 1 1 d . . . H13 H 0.4716 0.2359 -0.0282 0.052 Uiso 1 1 calc R . . C14 C 0.6296(5) 0.17184(18) -0.0347(2) 0.0459(11) Uani 1 1 d . . . H14 H 0.6264 0.1839 -0.0864 0.055 Uiso 1 1 calc R . . C15 C 0.7259(5) 0.12324(18) 0.0055(2) 0.0439(11) Uani 1 1 d . . . H15 H 0.7888 0.1021 -0.0187 0.053 Uiso 1 1 calc R . . C16 C 0.7309(4) 0.10538(16) 0.0806(2) 0.0341(9) Uani 1 1 d . . . H16 H 0.7962 0.0717 0.1078 0.041 Uiso 1 1 calc R . . C17 C 0.2486(4) 0.11919(18) 0.1609(2) 0.0345(9) Uani 1 1 d . . . C18 C 0.3559(4) 0.04460(15) 0.0535(3) 0.0337(9) Uani 1 1 d . . . C19 C 0.5187(5) -0.03679(17) 0.1870(2) 0.0359(9) Uani 1 1 d . . . C20 C 0.3922(5) 0.03218(17) 0.2881(3) 0.0422(10) Uani 1 1 d . . . C21 C 0.1757(5) -0.00812(18) 0.1350(3) 0.0412(10) Uani 1 1 d . . . C22 C 1.1185(4) 0.17373(15) 0.4354(2) 0.0299(9) Uani 1 1 d . . . C23 C 1.1030(5) 0.19099(17) 0.5071(2) 0.0390(10) Uani 1 1 d . . . H23 H 1.0067 0.2093 0.5059 0.047 Uiso 1 1 calc R . . C24 C 1.2272(6) 0.1815(2) 0.5801(3) 0.0539(12) Uani 1 1 d . . . H24 H 1.2150 0.1933 0.6288 0.065 Uiso 1 1 calc R . . C25 C 1.3671(6) 0.1556(2) 0.5836(3) 0.0583(13) Uani 1 1 d . . . H25 H 1.4510 0.1489 0.6343 0.070 Uiso 1 1 calc R . . C26 C 1.3861(5) 0.13922(19) 0.5134(3) 0.0519(12) Uani 1 1 d . . . H26 H 1.4838 0.1217 0.5154 0.062 Uiso 1 1 calc R . . C27 C 1.2619(4) 0.14842(16) 0.4394(2) 0.0360(9) Uani 1 1 d . . . H27 H 1.2756 0.1372 0.3910 0.043 Uiso 1 1 calc R . . C28 C 1.0835(5) 0.32437(16) 0.4080(2) 0.0330(9) Uani 1 1 d . . . C29 C 1.2228(5) 0.27380(17) 0.2978(2) 0.0322(9) Uani 1 1 d . . . C30 C 0.9158(4) 0.27096(17) 0.1711(2) 0.0335(9) Uani 1 1 d . . . C31 C 0.7780(5) 0.32480(16) 0.2801(2) 0.0315(9) Uani 1 1 d . . . C32 C 1.0222(5) 0.38247(18) 0.2555(2) 0.0383(10) 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 Mo1 0.0290(2) 0.02264(18) 0.0362(2) -0.00127(14) 0.01370(17) -0.00444(14) Mo2 0.0272(2) 0.02235(18) 0.02913(19) -0.00009(13) 0.01209(16) -0.00185(14) P1 0.0260(6) 0.0193(5) 0.0314(5) -0.0015(4) 0.0111(5) -0.0011(4) P2 0.0258(6) 0.0231(5) 0.0256(5) -0.0007(4) 0.0115(5) -0.0003(4) O1 0.0479(19) 0.0444(18) 0.059(2) -0.0009(15) 0.0237(17) 0.0093(15) O2 0.0503(19) 0.0448(17) 0.0371(17) -0.0039(14) 0.0156(15) -0.0043(14) O3 0.0444(19) 0.0313(16) 0.077(2) -0.0017(15) 0.0182(17) 0.0030(14) O4 0.069(2) 0.082(2) 0.049(2) 0.0085(18) 0.0321(19) -0.0003(18) O5 0.045(2) 0.062(2) 0.078(2) -0.0062(17) 0.0220(19) -0.0256(17) O6 0.065(2) 0.0416(17) 0.0393(18) -0.0120(14) 0.0161(17) -0.0064(15) O7 0.0302(17) 0.065(2) 0.0539(19) -0.0161(15) 0.0177(16) 0.0004(15) O8 0.054(2) 0.062(2) 0.0330(17) -0.0019(14) 0.0161(16) -0.0202(16) O9 0.0377(18) 0.0490(18) 0.059(2) -0.0043(14) 0.0202(16) 0.0073(15) O10 0.073(2) 0.0307(17) 0.080(2) 0.0131(16) 0.038(2) -0.0056(15) C1 0.032(2) 0.0147(19) 0.032(2) -0.0054(16) 0.0137(18) -0.0013(16) C2 0.024(2) 0.027(2) 0.030(2) 0.0010(16) 0.0097(18) -0.0009(16) C3 0.037(2) 0.027(2) 0.038(2) 0.0004(17) 0.013(2) 0.0017(18) C4 0.051(3) 0.033(2) 0.044(3) 0.014(2) 0.014(2) -0.005(2) C5 0.053(3) 0.050(3) 0.038(2) 0.006(2) 0.024(2) -0.009(2) C6 0.042(3) 0.038(2) 0.042(2) -0.0049(19) 0.022(2) -0.0057(19) C7 0.023(2) 0.030(2) 0.026(2) 0.0001(16) 0.0086(17) -0.0035(16) C8 0.028(2) 0.025(2) 0.032(2) -0.0073(16) 0.0154(19) -0.0001(16) C9 0.026(2) 0.024(2) 0.043(3) -0.0050(18) 0.017(2) -0.0013(17) C10 0.028(2) 0.030(2) 0.023(2) -0.0028(17) 0.0105(19) 0.0007(18) C11 0.033(2) 0.026(2) 0.028(2) -0.0006(16) 0.0100(19) -0.0092(17) C12 0.039(2) 0.032(2) 0.035(2) 0.0019(18) 0.011(2) -0.0049(19) C13 0.048(3) 0.036(2) 0.037(2) 0.0043(19) 0.003(2) -0.005(2) C14 0.061(3) 0.043(3) 0.030(2) -0.001(2) 0.013(2) -0.021(2) C15 0.059(3) 0.042(3) 0.037(2) -0.010(2) 0.026(2) -0.010(2) C16 0.040(3) 0.028(2) 0.034(2) -0.0011(17) 0.013(2) -0.0047(18) C17 0.030(2) 0.038(2) 0.039(2) -0.0040(19) 0.017(2) -0.0038(19) C18 0.030(2) 0.020(2) 0.050(3) -0.0033(18) 0.014(2) -0.0061(16) C19 0.033(2) 0.028(2) 0.045(3) -0.0048(18) 0.012(2) -0.0105(19) C20 0.035(3) 0.042(2) 0.050(3) 0.000(2) 0.018(2) -0.0043(19) C21 0.038(3) 0.034(2) 0.052(3) 0.001(2) 0.018(2) -0.008(2) C22 0.033(2) 0.0194(18) 0.036(2) 0.0049(16) 0.012(2) -0.0008(16) C23 0.041(3) 0.040(2) 0.033(2) -0.0031(18) 0.010(2) -0.0028(19) C24 0.063(4) 0.055(3) 0.034(3) 0.001(2) 0.008(3) -0.013(3) C25 0.047(3) 0.054(3) 0.048(3) 0.012(2) -0.012(3) -0.012(2) C26 0.034(3) 0.049(3) 0.062(3) 0.012(2) 0.006(3) -0.001(2) C27 0.029(2) 0.037(2) 0.039(2) 0.0047(18) 0.010(2) -0.0008(19) C28 0.034(2) 0.025(2) 0.040(3) 0.0003(18) 0.014(2) 0.0016(17) C29 0.039(3) 0.031(2) 0.028(2) -0.0063(17) 0.015(2) -0.0066(19) C30 0.035(2) 0.031(2) 0.037(2) 0.0057(18) 0.017(2) -0.0048(18) C31 0.037(3) 0.025(2) 0.033(2) -0.0015(17) 0.013(2) -0.0030(18) C32 0.039(3) 0.036(2) 0.043(2) -0.0007(19) 0.019(2) -0.0062(19) _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 Mo1 C21 2.000(4) . ? Mo1 C17 2.031(4) . ? Mo1 C20 2.035(4) . ? Mo1 C18 2.052(4) . ? Mo1 C19 2.063(4) . ? Mo1 P1 2.5099(9) . ? Mo2 C32 1.995(4) . ? Mo2 C31 2.022(4) . ? Mo2 C30 2.033(4) . ? Mo2 C29 2.047(4) . ? Mo2 C28 2.055(4) . ? Mo2 P2 2.5237(9) . ? P1 C11 1.826(3) . ? P1 C1 1.850(4) . ? P1 C9 1.855(4) . ? P2 C22 1.830(4) . ? P2 C8 1.861(3) . ? P2 C10 1.863(4) . ? O1 C17 1.144(4) . ? O2 C18 1.153(4) . ? O3 C19 1.127(4) . ? O4 C20 1.144(4) . ? O5 C21 1.139(4) . ? O6 C28 1.133(4) . ? O7 C29 1.138(4) . ? O8 C30 1.142(4) . ? O9 C31 1.143(4) . ? O10 C32 1.154(4) . ? C1 C2 1.515(5) . ? C1 C10 1.533(5) . ? C1 H1 0.92(3) . ? C2 C3 1.393(5) . ? C2 C7 1.396(5) . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 H4 0.9500 . ? C5 C6 1.376(5) . ? C5 H5 0.9500 . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.496(5) . ? C8 C9 1.541(5) . ? C8 H8 0.96(3) . ? C9 H9A 0.88(3) . ? C9 H9B 0.96(3) . ? C10 H10A 0.92(4) . ? C10 H10B 0.93(3) . ? C11 C16 1.385(5) . ? C11 C12 1.398(5) . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.374(5) . ? C13 H13 0.9500 . ? C14 C15 1.384(6) . ? C14 H14 0.9500 . ? C15 C16 1.380(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C22 C27 1.384(5) . ? C22 C23 1.390(5) . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.364(6) . ? C24 H24 0.9500 . ? C25 C26 1.373(6) . ? C25 H25 0.9500 . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Mo1 C17 89.35(15) . . ? C21 Mo1 C20 89.46(16) . . ? C17 Mo1 C20 89.47(15) . . ? C21 Mo1 C18 87.47(15) . . ? C17 Mo1 C18 91.94(14) . . ? C20 Mo1 C18 176.61(14) . . ? C21 Mo1 C19 93.17(15) . . ? C17 Mo1 C19 177.32(15) . . ? C20 Mo1 C19 89.65(15) . . ? C18 Mo1 C19 89.08(14) . . ? C21 Mo1 P1 175.08(12) . . ? C17 Mo1 P1 87.47(10) . . ? C20 Mo1 P1 94.27(11) . . ? C18 Mo1 P1 88.87(10) . . ? C19 Mo1 P1 90.07(10) . . ? C32 Mo2 C31 84.90(14) . . ? C32 Mo2 C30 88.85(15) . . ? C31 Mo2 C30 92.03(14) . . ? C32 Mo2 C29 91.48(15) . . ? C31 Mo2 C29 176.32(14) . . ? C30 Mo2 C29 88.60(14) . . ? C32 Mo2 C28 89.74(15) . . ? C31 Mo2 C28 88.63(14) . . ? C30 Mo2 C28 178.38(14) . . ? C29 Mo2 C28 90.64(14) . . ? C32 Mo2 P2 176.93(11) . . ? C31 Mo2 P2 93.09(10) . . ? C30 Mo2 P2 93.56(10) . . ? C29 Mo2 P2 90.49(10) . . ? C28 Mo2 P2 87.88(10) . . ? C11 P1 C1 106.09(16) . . ? C11 P1 C9 104.53(17) . . ? C1 P1 C9 96.85(17) . . ? C11 P1 Mo1 109.60(12) . . ? C1 P1 Mo1 119.35(11) . . ? C9 P1 Mo1 118.65(13) . . ? C22 P2 C8 104.97(16) . . ? C22 P2 C10 103.36(17) . . ? C8 P2 C10 97.10(16) . . ? C22 P2 Mo2 110.50(11) . . ? C8 P2 Mo2 116.53(11) . . ? C10 P2 Mo2 122.21(12) . . ? C2 C1 C10 112.6(3) . . ? C2 C1 P1 104.4(2) . . ? C10 C1 P1 112.5(3) . . ? C2 C1 H1 111.7(19) . . ? C10 C1 H1 108.9(19) . . ? P1 C1 H1 107(2) . . ? C3 C2 C7 119.6(3) . . ? C3 C2 C1 123.9(3) . . ? C7 C2 C1 116.5(3) . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C2 119.6(3) . . ? C6 C7 C8 123.9(3) . . ? C2 C7 C8 116.5(3) . . ? C7 C8 C9 111.4(3) . . ? C7 C8 P2 109.1(2) . . ? C9 C8 P2 108.3(2) . . ? C7 C8 H8 110.6(18) . . ? C9 C8 H8 106.2(19) . . ? P2 C8 H8 111.3(18) . . ? C8 C9 P1 113.3(3) . . ? C8 C9 H9A 105(2) . . ? P1 C9 H9A 108(2) . . ? C8 C9 H9B 112.3(18) . . ? P1 C9 H9B 109.5(17) . . ? H9A C9 H9B 109(3) . . ? C1 C10 P2 113.3(2) . . ? C1 C10 H10A 111(2) . . ? P2 C10 H10A 107(2) . . ? C1 C10 H10B 112.0(18) . . ? P2 C10 H10B 104.9(17) . . ? H10A C10 H10B 108(3) . . ? C16 C11 C12 119.2(3) . . ? C16 C11 P1 121.4(3) . . ? C12 C11 P1 118.8(3) . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.0(4) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? O1 C17 Mo1 178.3(3) . . ? O2 C18 Mo1 177.0(3) . . ? O3 C19 Mo1 178.5(4) . . ? O4 C20 Mo1 176.6(4) . . ? O5 C21 Mo1 177.7(4) . . ? C27 C22 C23 118.3(4) . . ? C27 C22 P2 120.5(3) . . ? C23 C22 P2 121.0(3) . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 121.1(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.7(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 119.8(4) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C22 C27 C26 120.9(4) . . ? C22 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? O6 C28 Mo2 178.4(3) . . ? O7 C29 Mo2 177.8(3) . . ? O8 C30 Mo2 175.4(3) . . ? O9 C31 Mo2 176.8(3) . . ? O10 C32 Mo2 175.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Mo1 P1 C11 -83.16(16) . . . . ? C20 Mo1 P1 C11 -172.44(17) . . . . ? C18 Mo1 P1 C11 8.83(16) . . . . ? C19 Mo1 P1 C11 97.91(16) . . . . ? C17 Mo1 P1 C1 154.30(16) . . . . ? C20 Mo1 P1 C1 65.02(17) . . . . ? C18 Mo1 P1 C1 -113.70(16) . . . . ? C19 Mo1 P1 C1 -24.63(17) . . . . ? C17 Mo1 P1 C9 36.71(18) . . . . ? C20 Mo1 P1 C9 -52.57(19) . . . . ? C18 Mo1 P1 C9 128.70(18) . . . . ? C19 Mo1 P1 C9 -142.22(18) . . . . ? C31 Mo2 P2 C22 -122.87(16) . . . . ? C30 Mo2 P2 C22 144.90(16) . . . . ? C29 Mo2 P2 C22 56.27(15) . . . . ? C28 Mo2 P2 C22 -34.35(16) . . . . ? C31 Mo2 P2 C8 -3.21(16) . . . . ? C30 Mo2 P2 C8 -95.44(17) . . . . ? C29 Mo2 P2 C8 175.93(16) . . . . ? C28 Mo2 P2 C8 85.31(17) . . . . ? C31 Mo2 P2 C10 115.33(19) . . . . ? C30 Mo2 P2 C10 23.10(19) . . . . ? C29 Mo2 P2 C10 -65.53(18) . . . . ? C28 Mo2 P2 C10 -156.16(19) . . . . ? C11 P1 C1 C2 169.8(2) . . . . ? C9 P1 C1 C2 62.5(2) . . . . ? Mo1 P1 C1 C2 -65.9(2) . . . . ? C11 P1 C1 C10 47.4(3) . . . . ? C9 P1 C1 C10 -59.9(3) . . . . ? Mo1 P1 C1 C10 171.69(19) . . . . ? C10 C1 C2 C3 -121.5(4) . . . . ? P1 C1 C2 C3 116.2(3) . . . . ? C10 C1 C2 C7 60.2(4) . . . . ? P1 C1 C2 C7 -62.1(3) . . . . ? C7 C2 C3 C4 -1.1(5) . . . . ? C1 C2 C3 C4 -179.4(3) . . . . ? C2 C3 C4 C5 1.3(6) . . . . ? C3 C4 C5 C6 -1.0(6) . . . . ? C4 C5 C6 C7 0.4(6) . . . . ? C5 C6 C7 C2 -0.2(6) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? C3 C2 C7 C6 0.5(5) . . . . ? C1 C2 C7 C6 178.9(3) . . . . ? C3 C2 C7 C8 -179.8(3) . . . . ? C1 C2 C7 C8 -1.4(5) . . . . ? C6 C7 C8 C9 -119.8(4) . . . . ? C2 C7 C8 C9 60.6(4) . . . . ? C6 C7 C8 P2 120.7(3) . . . . ? C2 C7 C8 P2 -58.9(4) . . . . ? C22 P2 C8 C7 -48.9(3) . . . . ? C10 P2 C8 C7 57.0(3) . . . . ? Mo2 P2 C8 C7 -171.46(19) . . . . ? C22 P2 C8 C9 -170.3(2) . . . . ? C10 P2 C8 C9 -64.4(3) . . . . ? Mo2 P2 C8 C9 67.1(2) . . . . ? C7 C8 C9 P1 -44.9(4) . . . . ? P2 C8 C9 P1 75.1(3) . . . . ? C11 P1 C9 C8 -121.0(3) . . . . ? C1 P1 C9 C8 -12.4(3) . . . . ? Mo1 P1 C9 C8 116.5(2) . . . . ? C2 C1 C10 P2 -48.4(4) . . . . ? P1 C1 C10 P2 69.3(3) . . . . ? C22 P2 C10 C1 101.4(3) . . . . ? C8 P2 C10 C1 -5.8(3) . . . . ? Mo2 P2 C10 C1 -133.5(2) . . . . ? C1 P1 C11 C16 37.7(3) . . . . ? C9 P1 C11 C16 139.5(3) . . . . ? Mo1 P1 C11 C16 -92.4(3) . . . . ? C1 P1 C11 C12 -151.6(3) . . . . ? C9 P1 C11 C12 -49.9(3) . . . . ? Mo1 P1 C11 C12 78.3(3) . . . . ? C16 C11 C12 C13 0.3(5) . . . . ? P1 C11 C12 C13 -170.5(3) . . . . ? C11 C12 C13 C14 -0.8(6) . . . . ? C12 C13 C14 C15 0.6(6) . . . . ? C13 C14 C15 C16 0.2(6) . . . . ? C14 C15 C16 C11 -0.7(6) . . . . ? C12 C11 C16 C15 0.5(5) . . . . ? P1 C11 C16 C15 171.1(3) . . . . ? C8 P2 C22 C27 146.3(3) . . . . ? C10 P2 C22 C27 45.0(3) . . . . ? Mo2 P2 C22 C27 -87.3(3) . . . . ? C8 P2 C22 C23 -39.3(3) . . . . ? C10 P2 C22 C23 -140.5(3) . . . . ? Mo2 P2 C22 C23 87.1(3) . . . . ? C27 C22 C23 C24 -1.4(5) . . . . ? P2 C22 C23 C24 -176.0(3) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C23 C24 C25 C26 0.8(6) . . . . ? C24 C25 C26 C27 -0.9(6) . . . . ? C23 C22 C27 C26 1.4(5) . . . . ? P2 C22 C27 C26 176.0(3) . . . . ? C25 C26 C27 C22 -0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.686 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.093 #===END data_s3427a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H20 O10 P2 W2' _chemical_formula_sum 'C38 H20 O10 P2 W2' _chemical_formula_weight 1066.18 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 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 8.0153(3) _cell_length_b 10.6946(4) _cell_length_c 22.3651(5) _cell_angle_alpha 88.441(2) _cell_angle_beta 83.323(2) _cell_angle_gamma 79.194(1) _cell_volume 1870.34(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 104 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 20.40 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 6.287 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.69 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44445 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8531 _reflns_number_gt 6886 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Dirax' _computing_data_reduction 'EvalCCD, sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+3.9486P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 8531 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _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 W1 W 0.26522(2) 0.290385(16) 0.084588(8) 0.02358(5) Uani 1 1 d . . . W2 W 0.04578(2) 0.377310(16) 0.392634(7) 0.02076(5) Uani 1 1 d . . . P1 P 0.50528(14) 0.25088(10) 0.14818(5) 0.0198(2) Uani 1 1 d . . . P2 P 0.30211(14) 0.21676(10) 0.35862(5) 0.0178(2) Uani 1 1 d . . . O11 O 0.3396(5) -0.0084(3) 0.06133(16) 0.0402(9) Uani 1 1 d . . . O12 O 0.4947(6) 0.3390(5) -0.03700(19) 0.0742(14) Uani 1 1 d . . . O13 O 0.2034(5) 0.5853(3) 0.11719(17) 0.0460(10) Uani 1 1 d . . . O14 O 0.0261(5) 0.2517(3) 0.20503(16) 0.0408(9) Uani 1 1 d . . . O15 O -0.0601(6) 0.3386(4) 0.0140(2) 0.0675(14) Uani 1 1 d . . . O21 O 0.2906(5) 0.5588(3) 0.42825(17) 0.0425(9) Uani 1 1 d . . . O22 O 0.0130(4) 0.2391(3) 0.52054(15) 0.0365(8) Uani 1 1 d . . . O23 O -0.1809(5) 0.2106(4) 0.33262(16) 0.0477(10) Uani 1 1 d . . . O24 O 0.0932(5) 0.4887(3) 0.25979(15) 0.0390(9) Uani 1 1 d . . . O25 O -0.2834(5) 0.5814(4) 0.43402(17) 0.0562(12) Uani 1 1 d . . . C11 C 0.5466(5) 0.3538(4) 0.20507(18) 0.0204(9) Uani 1 1 d . . . C12 C 0.4677(5) 0.2627(4) 0.22887(18) 0.0186(9) Uani 1 1 d . . . C13 C 0.6140(5) 0.4669(4) 0.2165(2) 0.0227(9) Uani 1 1 d . . . C14 C 0.6953(6) 0.5281(4) 0.1690(2) 0.0325(11) Uani 1 1 d . . . H14 H 0.7094 0.4946 0.1294 0.039 Uiso 1 1 calc R . . C15 C 0.7559(7) 0.6391(5) 0.1796(3) 0.0468(15) Uani 1 1 d . . . H15 H 0.8121 0.6807 0.1474 0.056 Uiso 1 1 calc R . . C16 C 0.7338(7) 0.6874(5) 0.2368(3) 0.0513(17) Uani 1 1 d . . . H16 H 0.7747 0.7629 0.2439 0.062 Uiso 1 1 calc R . . C17 C 0.6529(7) 0.6278(5) 0.2842(3) 0.0446(15) Uani 1 1 d . . . H17 H 0.6376 0.6628 0.3235 0.054 Uiso 1 1 calc R . . C18 C 0.5939(6) 0.5168(4) 0.2746(2) 0.0316(11) Uani 1 1 d . . . H18 H 0.5400 0.4750 0.3073 0.038 Uiso 1 1 calc R . . C19 C 0.6923(5) 0.1241(4) 0.13315(19) 0.0214(9) Uani 1 1 d . . . C110 C 0.7349(6) 0.0715(4) 0.0760(2) 0.0307(11) Uani 1 1 d . . . H110 H 0.6728 0.1062 0.0439 0.037 Uiso 1 1 calc R . . C111 C 0.8685(6) -0.0323(5) 0.0658(2) 0.0368(12) Uani 1 1 d . . . H111 H 0.8968 -0.0680 0.0267 0.044 Uiso 1 1 calc R . . C112 C 0.9603(6) -0.0836(4) 0.1121(2) 0.0342(12) Uani 1 1 d . . . H112 H 1.0518 -0.1539 0.1049 0.041 Uiso 1 1 calc R . . C113 C 0.9172(6) -0.0310(5) 0.1696(2) 0.0336(11) Uani 1 1 d . . . H113 H 0.9798 -0.0657 0.2016 0.040 Uiso 1 1 calc R . . C114 C 0.7837(6) 0.0716(4) 0.1801(2) 0.0268(10) Uani 1 1 d . . . H114 H 0.7543 0.1064 0.2193 0.032 Uiso 1 1 calc R . . C115 C 0.3111(6) 0.0990(5) 0.06890(19) 0.0284(10) Uani 1 1 d . . . C116 C 0.4156(7) 0.3205(5) 0.0074(2) 0.0420(13) Uani 1 1 d . . . C117 C 0.2271(6) 0.4810(5) 0.1047(2) 0.0302(11) Uani 1 1 d . . . C118 C 0.1111(6) 0.2646(4) 0.1618(2) 0.0275(10) Uani 1 1 d . . . C119 C 0.0591(7) 0.3196(5) 0.0392(2) 0.0412(13) Uani 1 1 d . . . C21 C 0.3205(5) 0.1065(4) 0.29795(18) 0.0195(9) Uani 1 1 d . . . C22 C 0.3916(5) 0.2060(4) 0.28083(18) 0.0181(9) Uani 1 1 d . . . C23 C 0.2882(5) -0.0140(4) 0.27857(19) 0.0209(9) Uani 1 1 d . . . C24 C 0.3551(6) -0.0593(4) 0.2208(2) 0.0250(10) Uani 1 1 d . . . H24 H 0.4183 -0.0099 0.1942 0.030 Uiso 1 1 calc R . . C25 C 0.3288(6) -0.1762(4) 0.2026(2) 0.0298(11) Uani 1 1 d . . . H25 H 0.3745 -0.2069 0.1635 0.036 Uiso 1 1 calc R . . C26 C 0.2360(6) -0.2484(4) 0.2410(2) 0.0343(12) Uani 1 1 d . . . H26 H 0.2178 -0.3282 0.2282 0.041 Uiso 1 1 calc R . . C27 C 0.1702(7) -0.2046(4) 0.2980(2) 0.0366(12) Uani 1 1 d . . . H27 H 0.1067 -0.2545 0.3243 0.044 Uiso 1 1 calc R . . C28 C 0.1963(6) -0.0878(4) 0.3173(2) 0.0310(11) Uani 1 1 d . . . H28 H 0.1516 -0.0584 0.3567 0.037 Uiso 1 1 calc R . . C29 C 0.4686(5) 0.1534(4) 0.40593(18) 0.0198(9) Uani 1 1 d . . . C210 C 0.4922(6) 0.2216(4) 0.45536(19) 0.0253(10) Uani 1 1 d . . . H210 H 0.4201 0.3013 0.4648 0.030 Uiso 1 1 calc R . . C211 C 0.6206(6) 0.1736(5) 0.4911(2) 0.0318(11) Uani 1 1 d . . . H211 H 0.6376 0.2214 0.5244 0.038 Uiso 1 1 calc R . . C212 C 0.7238(6) 0.0564(5) 0.4783(2) 0.0338(11) Uani 1 1 d . . . H212 H 0.8113 0.0234 0.5028 0.041 Uiso 1 1 calc R . . C213 C 0.6993(6) -0.0128(5) 0.4296(2) 0.0357(12) Uani 1 1 d . . . H213 H 0.7693 -0.0938 0.4211 0.043 Uiso 1 1 calc R . . C214 C 0.5730(6) 0.0356(4) 0.3934(2) 0.0278(10) Uani 1 1 d . . . H214 H 0.5577 -0.0118 0.3598 0.033 Uiso 1 1 calc R . . C215 C 0.2011(6) 0.4924(4) 0.4175(2) 0.0282(10) Uani 1 1 d . . . C216 C 0.0266(5) 0.2892(4) 0.4749(2) 0.0258(10) Uani 1 1 d . . . C217 C -0.1022(6) 0.2675(5) 0.3568(2) 0.0303(11) Uani 1 1 d . . . C218 C 0.0731(6) 0.4528(4) 0.3079(2) 0.0250(10) Uani 1 1 d . . . C219 C -0.1648(7) 0.5074(5) 0.4189(2) 0.0355(12) 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 W1 0.02699(11) 0.02246(9) 0.02079(10) -0.00171(7) -0.00637(8) -0.00088(8) W2 0.01786(10) 0.02248(9) 0.01977(9) -0.00393(7) -0.00050(7) 0.00136(7) P1 0.0207(6) 0.0205(5) 0.0172(5) -0.0018(4) -0.0005(4) -0.0023(4) P2 0.0171(6) 0.0183(5) 0.0171(5) -0.0018(4) 0.0002(4) -0.0020(4) O11 0.049(2) 0.0280(19) 0.043(2) -0.0115(15) -0.0049(18) -0.0046(17) O12 0.089(4) 0.090(4) 0.036(2) 0.015(2) 0.012(2) -0.012(3) O13 0.061(3) 0.0259(19) 0.049(2) -0.0043(16) -0.0037(19) -0.0039(18) O14 0.037(2) 0.045(2) 0.042(2) -0.0056(17) 0.0065(17) -0.0159(17) O15 0.064(3) 0.062(3) 0.081(3) -0.002(2) -0.051(3) 0.002(2) O21 0.038(2) 0.0330(19) 0.058(2) -0.0141(17) -0.0087(18) -0.0068(17) O22 0.036(2) 0.039(2) 0.0284(18) 0.0050(15) -0.0008(15) 0.0048(16) O23 0.044(2) 0.073(3) 0.036(2) -0.0037(19) -0.0022(18) -0.037(2) O24 0.053(2) 0.0330(19) 0.031(2) 0.0066(15) -0.0025(17) -0.0101(17) O25 0.041(2) 0.073(3) 0.040(2) -0.019(2) -0.0056(18) 0.031(2) C11 0.018(2) 0.021(2) 0.020(2) -0.0018(16) -0.0012(17) 0.0007(17) C12 0.016(2) 0.019(2) 0.019(2) -0.0046(16) -0.0018(17) 0.0013(16) C13 0.018(2) 0.020(2) 0.030(2) 0.0017(17) -0.0070(18) 0.0007(17) C14 0.027(3) 0.027(2) 0.042(3) 0.006(2) -0.004(2) -0.004(2) C15 0.033(3) 0.030(3) 0.081(5) 0.018(3) -0.013(3) -0.013(2) C16 0.046(4) 0.026(3) 0.092(5) 0.006(3) -0.042(4) -0.014(3) C17 0.053(4) 0.026(3) 0.058(4) -0.007(2) -0.033(3) 0.000(2) C18 0.031(3) 0.028(2) 0.036(3) 0.000(2) -0.012(2) -0.002(2) C19 0.015(2) 0.022(2) 0.027(2) -0.0005(17) -0.0010(18) -0.0041(17) C110 0.028(3) 0.032(2) 0.030(3) -0.006(2) -0.001(2) -0.001(2) C111 0.031(3) 0.036(3) 0.040(3) -0.017(2) 0.004(2) -0.001(2) C112 0.020(3) 0.025(2) 0.055(3) -0.002(2) 0.002(2) -0.001(2) C113 0.020(3) 0.037(3) 0.043(3) 0.004(2) -0.009(2) -0.001(2) C114 0.019(2) 0.029(2) 0.032(3) -0.0033(19) -0.0014(19) -0.0032(19) C115 0.029(3) 0.035(3) 0.021(2) -0.0036(19) -0.0039(19) -0.004(2) C116 0.050(4) 0.040(3) 0.034(3) 0.004(2) -0.009(3) -0.001(3) C117 0.030(3) 0.030(3) 0.030(3) 0.001(2) -0.006(2) -0.002(2) C118 0.025(3) 0.022(2) 0.035(3) -0.0022(19) -0.008(2) -0.0022(19) C119 0.047(3) 0.034(3) 0.042(3) -0.008(2) -0.018(3) 0.003(2) C21 0.016(2) 0.019(2) 0.021(2) -0.0028(16) -0.0006(17) 0.0025(17) C22 0.018(2) 0.0167(19) 0.019(2) -0.0042(16) -0.0032(17) 0.0010(16) C23 0.018(2) 0.018(2) 0.026(2) -0.0008(17) -0.0063(18) -0.0005(17) C24 0.023(2) 0.023(2) 0.030(2) -0.0021(18) -0.0040(19) -0.0031(18) C25 0.029(3) 0.022(2) 0.038(3) -0.0096(19) -0.012(2) 0.0021(19) C26 0.040(3) 0.017(2) 0.050(3) -0.003(2) -0.017(2) -0.007(2) C27 0.043(3) 0.026(2) 0.045(3) 0.010(2) -0.010(2) -0.017(2) C28 0.035(3) 0.027(2) 0.032(3) 0.0005(19) -0.003(2) -0.007(2) C29 0.018(2) 0.022(2) 0.019(2) 0.0024(16) -0.0005(17) -0.0052(17) C210 0.022(2) 0.030(2) 0.022(2) -0.0021(18) -0.0023(19) -0.0024(19) C211 0.028(3) 0.043(3) 0.027(2) -0.004(2) -0.009(2) -0.008(2) C212 0.023(3) 0.038(3) 0.041(3) 0.010(2) -0.012(2) -0.003(2) C213 0.033(3) 0.026(2) 0.046(3) 0.004(2) -0.012(2) 0.003(2) C214 0.029(3) 0.021(2) 0.033(3) -0.0022(18) -0.008(2) -0.0021(19) C215 0.027(3) 0.024(2) 0.030(2) -0.0073(19) -0.001(2) 0.003(2) C216 0.015(2) 0.029(2) 0.029(2) -0.0049(19) 0.0014(18) 0.0051(18) C217 0.020(2) 0.043(3) 0.027(2) 0.004(2) 0.005(2) -0.008(2) C218 0.026(3) 0.017(2) 0.031(3) -0.0039(18) -0.001(2) -0.0026(18) C219 0.034(3) 0.045(3) 0.022(2) -0.007(2) -0.006(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C119 2.010(5) . ? W1 C116 2.042(6) . ? W1 C115 2.044(5) . ? W1 C118 2.046(5) . ? W1 C117 2.059(5) . ? W1 P1 2.4905(11) . ? W2 C219 2.016(5) . ? W2 C215 2.036(5) . ? W2 C218 2.044(5) . ? W2 C216 2.047(5) . ? W2 C217 2.055(5) . ? W2 P2 2.4765(10) . ? P1 C12 1.799(4) . ? P1 C11 1.803(4) . ? P1 C19 1.828(4) . ? P2 C21 1.797(4) . ? P2 C22 1.801(4) . ? P2 C29 1.819(4) . ? O11 C115 1.141(5) . ? O12 C116 1.147(6) . ? O13 C117 1.132(5) . ? O14 C118 1.138(5) . ? O15 C119 1.148(6) . ? O21 C215 1.148(5) . ? O22 C216 1.144(5) . ? O23 C217 1.141(6) . ? O24 C218 1.136(5) . ? O25 C219 1.141(6) . ? C11 C12 1.325(6) . ? C11 C13 1.454(6) . ? C12 C22 1.423(6) . ? C13 C14 1.395(6) . ? C13 C18 1.398(6) . ? C14 C15 1.400(7) . ? C14 H14 0.9500 . ? C15 C16 1.373(8) . ? C15 H15 0.9500 . ? C16 C17 1.382(8) . ? C16 H16 0.9500 . ? C17 C18 1.388(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C110 1.390(6) . ? C19 C114 1.394(6) . ? C110 C111 1.393(6) . ? C110 H110 0.9500 . ? C111 C112 1.381(7) . ? C111 H111 0.9500 . ? C112 C113 1.397(7) . ? C112 H112 0.9500 . ? C113 C114 1.386(6) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C21 C22 1.326(6) . ? C21 C23 1.448(6) . ? C23 C28 1.396(6) . ? C23 C24 1.402(6) . ? C24 C25 1.386(6) . ? C24 H24 0.9500 . ? C25 C26 1.386(7) . ? C25 H25 0.9500 . ? C26 C27 1.380(7) . ? C26 H26 0.9500 . ? C27 C28 1.392(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C214 1.391(6) . ? C29 C210 1.391(6) . ? C210 C211 1.391(6) . ? C210 H210 0.9500 . ? C211 C212 1.383(7) . ? C211 H211 0.9500 . ? C212 C213 1.386(7) . ? C212 H212 0.9500 . ? C213 C214 1.387(6) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C119 W1 C116 90.0(2) . . ? C119 W1 C115 92.21(19) . . ? C116 W1 C115 91.1(2) . . ? C119 W1 C118 89.3(2) . . ? C116 W1 C118 178.60(19) . . ? C115 W1 C118 90.13(18) . . ? C119 W1 C117 90.93(19) . . ? C116 W1 C117 90.2(2) . . ? C115 W1 C117 176.59(17) . . ? C118 W1 C117 88.60(18) . . ? C119 W1 P1 175.41(17) . . ? C116 W1 P1 94.58(15) . . ? C115 W1 P1 87.60(13) . . ? C118 W1 P1 86.11(13) . . ? C117 W1 P1 89.16(13) . . ? C219 W2 C215 91.5(2) . . ? C219 W2 C218 93.21(18) . . ? C215 W2 C218 88.08(18) . . ? C219 W2 C216 90.41(18) . . ? C215 W2 C216 93.84(18) . . ? C218 W2 C216 175.85(16) . . ? C219 W2 C217 90.2(2) . . ? C215 W2 C217 172.95(18) . . ? C218 W2 C217 85.00(18) . . ? C216 W2 C217 92.98(18) . . ? C219 W2 P2 178.92(13) . . ? C215 W2 P2 89.26(12) . . ? C218 W2 P2 86.08(12) . . ? C216 W2 P2 90.27(12) . . ? C217 W2 P2 88.94(13) . . ? C12 P1 C11 43.18(18) . . ? C12 P1 C19 105.15(19) . . ? C11 P1 C19 108.50(19) . . ? C12 P1 W1 121.51(14) . . ? C11 P1 W1 127.29(14) . . ? C19 P1 W1 123.23(14) . . ? C21 P2 C22 43.27(18) . . ? C21 P2 C29 106.99(19) . . ? C22 P2 C29 109.22(19) . . ? C21 P2 W2 125.89(14) . . ? C22 P2 W2 121.40(13) . . ? C29 P2 W2 123.84(14) . . ? C12 C11 C13 146.1(4) . . ? C12 C11 P1 68.2(2) . . ? C13 C11 P1 145.5(3) . . ? C11 C12 C22 148.9(4) . . ? C11 C12 P1 68.6(3) . . ? C22 C12 P1 142.4(3) . . ? C14 C13 C18 119.7(4) . . ? C14 C13 C11 119.8(4) . . ? C18 C13 C11 120.5(4) . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.6(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.9(5) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 119.7(5) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C110 C19 C114 119.4(4) . . ? C110 C19 P1 120.2(3) . . ? C114 C19 P1 120.2(3) . . ? C19 C110 C111 120.1(4) . . ? C19 C110 H110 119.9 . . ? C111 C110 H110 119.9 . . ? C112 C111 C110 120.6(5) . . ? C112 C111 H111 119.7 . . ? C110 C111 H111 119.7 . . ? C111 C112 C113 119.4(4) . . ? C111 C112 H112 120.3 . . ? C113 C112 H112 120.3 . . ? C114 C113 C112 120.3(4) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C113 C114 C19 120.3(4) . . ? C113 C114 H114 119.9 . . ? C19 C114 H114 119.9 . . ? O11 C115 W1 178.2(4) . . ? O12 C116 W1 177.4(5) . . ? O13 C117 W1 178.1(5) . . ? O14 C118 W1 179.0(4) . . ? O15 C119 W1 178.5(5) . . ? C22 C21 C23 144.3(4) . . ? C22 C21 P2 68.5(2) . . ? C23 C21 P2 147.2(3) . . ? C21 C22 C12 141.6(4) . . ? C21 C22 P2 68.2(2) . . ? C12 C22 P2 149.7(3) . . ? C28 C23 C24 119.5(4) . . ? C28 C23 C21 120.9(4) . . ? C24 C23 C21 119.6(4) . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.3(5) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 119.8(5) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C214 C29 C210 119.2(4) . . ? C214 C29 P2 120.4(3) . . ? C210 C29 P2 120.4(3) . . ? C211 C210 C29 120.4(4) . . ? C211 C210 H210 119.8 . . ? C29 C210 H210 119.8 . . ? C212 C211 C210 120.1(4) . . ? C212 C211 H211 120.0 . . ? C210 C211 H211 120.0 . . ? C211 C212 C213 119.8(4) . . ? C211 C212 H212 120.1 . . ? C213 C212 H212 120.1 . . ? C212 C213 C214 120.2(4) . . ? C212 C213 H213 119.9 . . ? C214 C213 H213 119.9 . . ? C213 C214 C29 120.3(4) . . ? C213 C214 H214 119.8 . . ? C29 C214 H214 119.8 . . ? O21 C215 W2 176.2(4) . . ? O22 C216 W2 178.6(4) . . ? O23 C217 W2 174.6(4) . . ? O24 C218 W2 176.4(4) . . ? O25 C219 W2 179.6(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 C116 W1 P1 C12 161.0(2) . . . . ? C115 W1 P1 C12 -108.1(2) . . . . ? C118 W1 P1 C12 -17.8(2) . . . . ? C117 W1 P1 C12 70.9(2) . . . . ? C116 W1 P1 C11 108.5(2) . . . . ? C115 W1 P1 C11 -160.6(2) . . . . ? C118 W1 P1 C11 -70.3(2) . . . . ? C117 W1 P1 C11 18.3(2) . . . . ? C116 W1 P1 C19 -58.8(2) . . . . ? C115 W1 P1 C19 32.1(2) . . . . ? C118 W1 P1 C19 122.4(2) . . . . ? C117 W1 P1 C19 -149.0(2) . . . . ? C215 W2 P2 C21 -149.1(2) . . . . ? C218 W2 P2 C21 -60.9(2) . . . . ? C216 W2 P2 C21 117.1(2) . . . . ? C217 W2 P2 C21 24.1(2) . . . . ? C215 W2 P2 C22 -96.7(2) . . . . ? C218 W2 P2 C22 -8.6(2) . . . . ? C216 W2 P2 C22 169.4(2) . . . . ? C217 W2 P2 C22 76.4(2) . . . . ? C215 W2 P2 C29 54.1(2) . . . . ? C218 W2 P2 C29 142.3(2) . . . . ? C216 W2 P2 C29 -39.7(2) . . . . ? C217 W2 P2 C29 -132.7(2) . . . . ? C19 P1 C11 C12 -92.6(3) . . . . ? W1 P1 C11 C12 98.5(2) . . . . ? C12 P1 C11 C13 -176.8(7) . . . . ? C19 P1 C11 C13 90.6(6) . . . . ? W1 P1 C11 C13 -78.2(6) . . . . ? C13 C11 C12 C22 -0.4(13) . . . . ? P1 C11 C12 C22 -177.1(7) . . . . ? C13 C11 C12 P1 176.7(7) . . . . ? C19 P1 C12 C11 101.1(3) . . . . ? W1 P1 C12 C11 -112.7(2) . . . . ? C11 P1 C12 C22 177.6(6) . . . . ? C19 P1 C12 C22 -81.4(5) . . . . ? W1 P1 C12 C22 64.9(5) . . . . ? C12 C11 C13 C14 178.6(6) . . . . ? P1 C11 C13 C14 -6.8(8) . . . . ? C12 C11 C13 C18 -3.2(9) . . . . ? P1 C11 C13 C18 171.4(4) . . . . ? C18 C13 C14 C15 -0.1(7) . . . . ? C11 C13 C14 C15 178.2(4) . . . . ? C13 C14 C15 C16 -0.5(7) . . . . ? C14 C15 C16 C17 0.2(8) . . . . ? C15 C16 C17 C18 0.6(8) . . . . ? C16 C17 C18 C13 -1.1(7) . . . . ? C14 C13 C18 C17 0.8(7) . . . . ? C11 C13 C18 C17 -177.4(4) . . . . ? C12 P1 C19 C110 166.3(4) . . . . ? C11 P1 C19 C110 -148.6(4) . . . . ? W1 P1 C19 C110 20.8(4) . . . . ? C12 P1 C19 C114 -7.7(4) . . . . ? C11 P1 C19 C114 37.4(4) . . . . ? W1 P1 C19 C114 -153.3(3) . . . . ? C114 C19 C110 C111 -0.5(7) . . . . ? P1 C19 C110 C111 -174.6(4) . . . . ? C19 C110 C111 C112 -0.2(8) . . . . ? C110 C111 C112 C113 0.4(8) . . . . ? C111 C112 C113 C114 0.0(7) . . . . ? C112 C113 C114 C19 -0.7(7) . . . . ? C110 C19 C114 C113 0.9(7) . . . . ? P1 C19 C114 C113 175.0(4) . . . . ? C29 P2 C21 C22 -100.2(3) . . . . ? W2 P2 C21 C22 99.8(2) . . . . ? C22 P2 C21 C23 177.6(7) . . . . ? C29 P2 C21 C23 77.4(6) . . . . ? W2 P2 C21 C23 -82.6(6) . . . . ? C23 C21 C22 C12 9.2(11) . . . . ? P2 C21 C22 C12 -173.1(6) . . . . ? C23 C21 C22 P2 -177.8(7) . . . . ? C11 C12 C22 C21 -176.1(6) . . . . ? P1 C12 C22 C21 8.3(9) . . . . ? C11 C12 C22 P2 16.8(12) . . . . ? P1 C12 C22 P2 -158.9(4) . . . . ? C29 P2 C22 C21 94.6(3) . . . . ? W2 P2 C22 C21 -110.7(2) . . . . ? C21 P2 C22 C12 171.5(8) . . . . ? C29 P2 C22 C12 -93.9(6) . . . . ? W2 P2 C22 C12 60.8(7) . . . . ? C22 C21 C23 C28 -178.6(6) . . . . ? P2 C21 C23 C28 5.2(8) . . . . ? C22 C21 C23 C24 3.5(9) . . . . ? P2 C21 C23 C24 -172.7(4) . . . . ? C28 C23 C24 C25 0.3(6) . . . . ? C21 C23 C24 C25 178.2(4) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C24 C25 C26 C27 -0.4(7) . . . . ? C25 C26 C27 C28 0.0(7) . . . . ? C26 C27 C28 C23 0.6(7) . . . . ? C24 C23 C28 C27 -0.7(7) . . . . ? C21 C23 C28 C27 -178.6(4) . . . . ? C21 P2 C29 C214 -3.7(4) . . . . ? C22 P2 C29 C214 -49.3(4) . . . . ? W2 P2 C29 C214 156.8(3) . . . . ? C21 P2 C29 C210 176.8(4) . . . . ? C22 P2 C29 C210 131.2(4) . . . . ? W2 P2 C29 C210 -22.7(4) . . . . ? C214 C29 C210 C211 1.2(7) . . . . ? P2 C29 C210 C211 -179.3(4) . . . . ? C29 C210 C211 C212 -1.2(7) . . . . ? C210 C211 C212 C213 0.3(8) . . . . ? C211 C212 C213 C214 0.7(8) . . . . ? C212 C213 C214 C29 -0.7(8) . . . . ? C210 C29 C214 C213 -0.2(7) . . . . ? P2 C29 C214 C213 -179.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.104 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.133 #===END data_s3425a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 O10 P2 W2' _chemical_formula_sum 'C32 H18 O10 P2 W2' _chemical_formula_weight 992.10 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 10.4762(1) _cell_length_b 11.3603(1) _cell_length_c 14.8964(1) _cell_angle_alpha 103.5604(4) _cell_angle_beta 99.8561(5) _cell_angle_gamma 103.9820(4) _cell_volume 1622.87(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 66538 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 7.237 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.27 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47067 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7450 _reflns_number_gt 7010 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000, denzox, sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0073P)^2^+1.6246P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7450 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0173 _refine_ls_R_factor_gt 0.0155 _refine_ls_wR_factor_ref 0.0339 _refine_ls_wR_factor_gt 0.0334 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.002 _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 W1 W 0.278151(9) 0.173784(8) -0.060894(6) 0.01850(3) Uani 1 1 d . . . W2 W 0.115912(8) 0.231261(8) 0.408442(6) 0.01666(3) Uani 1 1 d . . . P1 P 0.35567(6) 0.23847(5) 0.11422(4) 0.01725(11) Uani 1 1 d . . . P2 P 0.24927(5) 0.32985(5) 0.30733(4) 0.01599(11) Uani 1 1 d . . . O1 O 0.3138(3) -0.0933(2) -0.05214(16) 0.0680(8) Uani 1 1 d . . . O2 O -0.0307(2) 0.0947(2) -0.05392(15) 0.0528(6) Uani 1 1 d . . . O3 O 0.2521(2) 0.45208(18) -0.03700(14) 0.0423(5) Uani 1 1 d . . . O4 O 0.58458(19) 0.2696(2) -0.07482(14) 0.0418(5) Uani 1 1 d . . . O5 O 0.19333(18) 0.09682(16) -0.28536(11) 0.0304(4) Uani 1 1 d . . . O6 O -0.15783(19) 0.20634(19) 0.26515(14) 0.0430(5) Uani 1 1 d . . . O7 O 0.11258(19) -0.04046(16) 0.28549(13) 0.0320(4) Uani 1 1 d . . . O8 O 0.38627(19) 0.24123(19) 0.54930(12) 0.0357(4) Uani 1 1 d . . . O9 O 0.13960(18) 0.51024(17) 0.52775(14) 0.0377(4) Uani 1 1 d . . . O10 O -0.0626(2) 0.1178(2) 0.53575(14) 0.0435(5) Uani 1 1 d . . . C1 C 0.2425(2) 0.2205(2) 0.19503(15) 0.0168(4) Uani 1 1 d . . . H1 H 0.153(2) 0.184(2) 0.1634(16) 0.014(6) Uiso 1 1 d . . . C2 C 0.3286(2) 0.1293(2) 0.18930(15) 0.0177(4) Uani 1 1 d . . . H2 H 0.277(2) 0.048(2) 0.1474(17) 0.020(6) Uiso 1 1 d . . . C3 C 0.4254(2) 0.1145(2) 0.26898(15) 0.0187(4) Uani 1 1 d . . . C4 C 0.4289(2) -0.0108(2) 0.25764(18) 0.0260(5) Uani 1 1 d . . . H4 H 0.3707 -0.0753 0.2033 0.031 Uiso 1 1 calc R . . C5 C 0.5139(3) -0.0436(3) 0.32263(19) 0.0345(6) Uani 1 1 d . . . H5 H 0.5114 -0.1297 0.3139 0.041 Uiso 1 1 calc R . . C6 C 0.6027(3) 0.0494(3) 0.40038(19) 0.0361(6) Uani 1 1 d . . . H6 H 0.6631 0.0283 0.4449 0.043 Uiso 1 1 calc R . . C7 C 0.6023(2) 0.1734(3) 0.41247(17) 0.0286(5) Uani 1 1 d . . . H7 H 0.6656 0.2373 0.4650 0.034 Uiso 1 1 calc R . . C8 C 0.5123(2) 0.2091(2) 0.35047(15) 0.0198(4) Uani 1 1 d . . . C9 C 0.5199(2) 0.3440(2) 0.37981(15) 0.0199(4) Uani 1 1 d . . . H9 H 0.608(2) 0.397(2) 0.4179(17) 0.016(6) Uiso 1 1 d . . . C10 C 0.4261(2) 0.4028(2) 0.36486(15) 0.0193(4) Uani 1 1 d . . . H10 H 0.448(3) 0.491(3) 0.3900(18) 0.026(7) Uiso 1 1 d . . . C11 C 0.5035(2) 0.3725(2) 0.17234(14) 0.0178(4) Uani 1 1 d . . . C12 C 0.4910(2) 0.4952(2) 0.18963(15) 0.0203(4) Uani 1 1 d . . . H12 H 0.4056 0.5079 0.1695 0.024 Uiso 1 1 calc R . . C13 C 0.6041(2) 0.5981(2) 0.23624(16) 0.0240(5) Uani 1 1 d . . . H13 H 0.5956 0.6815 0.2495 0.029 Uiso 1 1 calc R . . C14 C 0.7292(3) 0.5801(2) 0.26356(17) 0.0287(5) Uani 1 1 d . . . H14 H 0.8059 0.6510 0.2967 0.034 Uiso 1 1 calc R . . C15 C 0.7431(2) 0.4591(2) 0.24284(17) 0.0258(5) Uani 1 1 d . . . H15 H 0.8297 0.4474 0.2600 0.031 Uiso 1 1 calc R . . C16 C 0.6302(2) 0.3549(2) 0.19693(16) 0.0214(4) Uani 1 1 d . . . H16 H 0.6397 0.2719 0.1824 0.026 Uiso 1 1 calc R . . C17 C 0.1933(2) 0.4548(2) 0.26933(16) 0.0219(5) Uani 1 1 d . . . C18 C 0.1002(3) 0.4259(2) 0.18301(18) 0.0310(5) Uani 1 1 d . . . H18 H 0.0680 0.3412 0.1427 0.037 Uiso 1 1 calc R . . C19 C 0.0537(3) 0.5192(3) 0.1550(2) 0.0421(7) Uani 1 1 d . . . H19 H -0.0097 0.4983 0.0957 0.050 Uiso 1 1 calc R . . C20 C 0.0991(3) 0.6424(3) 0.2130(2) 0.0427(7) Uani 1 1 d . . . H20 H 0.0672 0.7063 0.1938 0.051 Uiso 1 1 calc R . . C21 C 0.1904(3) 0.6721(3) 0.2987(2) 0.0458(7) Uani 1 1 d . . . H21 H 0.2216 0.7568 0.3390 0.055 Uiso 1 1 calc R . . C22 C 0.2375(3) 0.5791(2) 0.3269(2) 0.0370(6) Uani 1 1 d . . . H22 H 0.3007 0.6008 0.3864 0.044 Uiso 1 1 calc R . . C23 C 0.2988(3) 0.0001(3) -0.05858(18) 0.0377(7) Uani 1 1 d . . . C24 C 0.0808(3) 0.1201(2) -0.05654(17) 0.0307(5) Uani 1 1 d . . . C25 C 0.2624(3) 0.3528(2) -0.04796(16) 0.0256(5) Uani 1 1 d . . . C26 C 0.4768(3) 0.2353(2) -0.06816(17) 0.0278(5) Uani 1 1 d . . . C27 C 0.2231(2) 0.1238(2) -0.20432(16) 0.0233(5) Uani 1 1 d . . . C28 C -0.0590(2) 0.2177(2) 0.31654(17) 0.0248(5) Uani 1 1 d . . . C29 C 0.1126(2) 0.0558(2) 0.33042(16) 0.0219(5) Uani 1 1 d . . . C30 C 0.2894(2) 0.2383(2) 0.49910(16) 0.0235(5) Uani 1 1 d . . . C31 C 0.1291(2) 0.4098(2) 0.48456(16) 0.0235(5) Uani 1 1 d . . . C32 C 0.0029(2) 0.1573(2) 0.48939(17) 0.0265(5) 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 W1 0.02293(5) 0.01678(5) 0.01359(5) 0.00357(3) 0.00232(4) 0.00412(4) W2 0.01760(5) 0.01734(5) 0.01564(5) 0.00605(3) 0.00386(3) 0.00507(3) P1 0.0203(3) 0.0160(3) 0.0145(3) 0.0038(2) 0.0030(2) 0.0051(2) P2 0.0183(3) 0.0141(2) 0.0154(3) 0.0043(2) 0.0035(2) 0.0048(2) O1 0.132(2) 0.0336(12) 0.0412(13) 0.0097(10) 0.0070(14) 0.0404(14) O2 0.0272(11) 0.0762(16) 0.0461(13) 0.0217(12) 0.0063(9) -0.0028(10) O3 0.0651(14) 0.0308(10) 0.0351(11) 0.0103(9) 0.0085(10) 0.0233(10) O4 0.0295(10) 0.0486(12) 0.0439(12) 0.0073(10) 0.0135(9) 0.0081(9) O5 0.0332(10) 0.0319(9) 0.0171(8) 0.0040(7) 0.0023(7) -0.0011(8) O6 0.0318(10) 0.0444(12) 0.0460(12) 0.0124(10) -0.0093(9) 0.0123(9) O7 0.0382(10) 0.0213(9) 0.0364(10) 0.0060(8) 0.0142(8) 0.0073(8) O8 0.0355(10) 0.0499(12) 0.0250(9) 0.0122(8) 0.0018(8) 0.0211(9) O9 0.0242(9) 0.0301(10) 0.0466(11) -0.0080(9) 0.0005(8) 0.0099(8) O10 0.0458(12) 0.0545(13) 0.0463(12) 0.0300(10) 0.0277(10) 0.0177(10) C1 0.0165(10) 0.0150(10) 0.0161(10) 0.0034(8) 0.0011(8) 0.0026(8) C2 0.0201(10) 0.0133(10) 0.0181(10) 0.0031(8) 0.0028(9) 0.0045(8) C3 0.0172(10) 0.0215(11) 0.0200(11) 0.0084(9) 0.0053(8) 0.0074(9) C4 0.0289(12) 0.0209(11) 0.0292(13) 0.0069(10) 0.0067(10) 0.0098(10) C5 0.0422(15) 0.0294(13) 0.0405(15) 0.0159(12) 0.0092(12) 0.0208(12) C6 0.0363(15) 0.0459(16) 0.0338(14) 0.0178(13) 0.0032(12) 0.0236(13) C7 0.0235(12) 0.0371(14) 0.0244(12) 0.0076(11) 0.0013(10) 0.0118(11) C8 0.0172(10) 0.0246(11) 0.0183(11) 0.0066(9) 0.0043(8) 0.0070(9) C9 0.0185(11) 0.0217(11) 0.0148(10) 0.0040(9) 0.0012(9) 0.0006(9) C10 0.0208(11) 0.0169(11) 0.0159(10) 0.0029(9) 0.0029(8) 0.0007(9) C11 0.0219(11) 0.0174(10) 0.0130(10) 0.0041(8) 0.0060(8) 0.0026(8) C12 0.0241(11) 0.0210(11) 0.0183(11) 0.0084(9) 0.0076(9) 0.0067(9) C13 0.0309(12) 0.0198(11) 0.0217(11) 0.0082(9) 0.0084(10) 0.0047(9) C14 0.0308(13) 0.0244(12) 0.0230(12) 0.0067(10) 0.0010(10) -0.0023(10) C15 0.0196(11) 0.0313(13) 0.0263(12) 0.0103(10) 0.0053(9) 0.0051(10) C16 0.0236(11) 0.0208(11) 0.0208(11) 0.0066(9) 0.0072(9) 0.0066(9) C17 0.0234(11) 0.0215(11) 0.0265(12) 0.0109(9) 0.0108(9) 0.0096(9) C18 0.0325(13) 0.0289(13) 0.0325(14) 0.0087(11) 0.0024(11) 0.0148(11) C19 0.0478(17) 0.0464(17) 0.0403(16) 0.0198(14) 0.0035(13) 0.0269(14) C20 0.0536(18) 0.0370(16) 0.0563(19) 0.0268(14) 0.0190(15) 0.0303(14) C21 0.063(2) 0.0213(13) 0.0559(19) 0.0102(13) 0.0132(16) 0.0192(14) C22 0.0497(17) 0.0257(13) 0.0353(15) 0.0061(11) 0.0050(13) 0.0167(12) C23 0.065(2) 0.0269(14) 0.0182(12) 0.0032(10) 0.0034(12) 0.0171(13) C24 0.0308(14) 0.0337(14) 0.0195(12) 0.0084(10) -0.0008(10) -0.0011(11) C25 0.0322(13) 0.0268(13) 0.0173(11) 0.0061(10) 0.0030(10) 0.0099(10) C26 0.0327(14) 0.0275(13) 0.0198(12) 0.0018(10) 0.0047(10) 0.0089(11) C27 0.0244(12) 0.0204(11) 0.0210(12) 0.0045(9) 0.0042(9) 0.0016(9) C28 0.0259(12) 0.0211(11) 0.0274(12) 0.0080(10) 0.0050(10) 0.0071(10) C29 0.0212(11) 0.0224(12) 0.0231(12) 0.0100(10) 0.0062(9) 0.0045(9) C30 0.0292(12) 0.0249(12) 0.0197(11) 0.0082(9) 0.0072(10) 0.0115(10) C31 0.0149(10) 0.0282(13) 0.0234(12) 0.0033(10) 0.0008(9) 0.0061(9) C32 0.0274(12) 0.0307(13) 0.0262(12) 0.0131(10) 0.0092(10) 0.0105(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 W1 C27 2.018(2) . ? W1 C24 2.026(3) . ? W1 C23 2.044(3) . ? W1 C25 2.047(2) . ? W1 C26 2.060(3) . ? W1 P1 2.4681(5) . ? W2 C32 2.011(2) . ? W2 C31 2.038(2) . ? W2 C28 2.040(2) . ? W2 C30 2.043(2) . ? W2 C29 2.047(2) . ? W2 P2 2.4960(5) . ? P1 C11 1.803(2) . ? P1 C1 1.840(2) . ? P1 C2 1.860(2) . ? P2 C10 1.799(2) . ? P2 C1 1.814(2) . ? P2 C17 1.829(2) . ? O1 C23 1.132(3) . ? O2 C24 1.143(3) . ? O3 C25 1.135(3) . ? O4 C26 1.131(3) . ? O5 C27 1.140(3) . ? O6 C28 1.137(3) . ? O7 C29 1.141(3) . ? O8 C30 1.141(3) . ? O9 C31 1.139(3) . ? O10 C32 1.144(3) . ? C1 C2 1.527(3) . ? C1 H1 0.92(2) . ? C2 C3 1.493(3) . ? C2 H2 0.95(3) . ? C3 C4 1.403(3) . ? C3 C8 1.412(3) . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.380(4) . ? C5 H5 0.9500 . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.403(3) . ? C7 H7 0.9500 . ? C8 C9 1.470(3) . ? C9 C10 1.331(3) . ? C9 H9 0.96(2) . ? C10 H10 0.94(3) . ? C11 C16 1.390(3) . ? C11 C12 1.399(3) . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.382(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.391(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.387(3) . ? C17 C18 1.390(3) . ? C18 C19 1.387(4) . ? C18 H18 0.9500 . ? C19 C20 1.379(4) . ? C19 H19 0.9500 . ? C20 C21 1.372(4) . ? C20 H20 0.9500 . ? C21 C22 1.387(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 W1 C24 90.21(9) . . ? C27 W1 C23 93.12(10) . . ? C24 W1 C23 92.09(12) . . ? C27 W1 C25 92.88(9) . . ? C24 W1 C25 87.64(10) . . ? C23 W1 C25 174.00(9) . . ? C27 W1 C26 88.57(9) . . ? C24 W1 C26 177.15(10) . . ? C23 W1 C26 90.55(11) . . ? C25 W1 C26 89.84(10) . . ? C27 W1 P1 177.54(7) . . ? C24 W1 P1 92.24(7) . . ? C23 W1 P1 87.00(7) . . ? C25 W1 P1 87.01(6) . . ? C26 W1 P1 88.97(7) . . ? C32 W2 C31 90.57(10) . . ? C32 W2 C28 88.51(10) . . ? C31 W2 C28 91.85(9) . . ? C32 W2 C30 90.80(9) . . ? C31 W2 C30 89.95(9) . . ? C28 W2 C30 178.08(9) . . ? C32 W2 C29 92.19(9) . . ? C31 W2 C29 176.87(9) . . ? C28 W2 C29 89.69(9) . . ? C30 W2 C29 88.55(9) . . ? C32 W2 P2 177.27(7) . . ? C31 W2 P2 87.54(7) . . ? C28 W2 P2 89.58(7) . . ? C30 W2 P2 91.17(6) . . ? C29 W2 P2 89.74(6) . . ? C11 P1 C1 109.82(9) . . ? C11 P1 C2 110.86(10) . . ? C1 P1 C2 48.74(9) . . ? C11 P1 W1 119.18(7) . . ? C1 P1 W1 124.28(7) . . ? C2 P1 W1 124.59(7) . . ? C10 P2 C1 106.17(10) . . ? C10 P2 C17 104.49(11) . . ? C1 P2 C17 102.36(10) . . ? C10 P2 W2 113.42(7) . . ? C1 P2 W2 114.12(7) . . ? C17 P2 W2 115.11(7) . . ? C2 C1 P2 121.46(15) . . ? C2 C1 P1 66.33(11) . . ? P2 C1 P1 128.77(12) . . ? C2 C1 H1 114.5(14) . . ? P2 C1 H1 107.8(14) . . ? P1 C1 H1 113.0(14) . . ? C3 C2 C1 127.71(19) . . ? C3 C2 P1 130.22(16) . . ? C1 C2 P1 64.93(11) . . ? C3 C2 H2 109.6(14) . . ? C1 C2 H2 110.5(14) . . ? P1 C2 H2 106.6(14) . . ? C4 C3 C8 118.0(2) . . ? C4 C3 C2 113.6(2) . . ? C8 C3 C2 128.41(19) . . ? C5 C4 C3 122.4(2) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 119.7(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 119.0(2) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 122.7(2) . . ? C6 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C3 118.0(2) . . ? C7 C8 C9 114.6(2) . . ? C3 C8 C9 127.41(19) . . ? C10 C9 C8 131.1(2) . . ? C10 C9 H9 115.7(14) . . ? C8 C9 H9 113.1(14) . . ? C9 C10 P2 126.86(18) . . ? C9 C10 H10 120.0(16) . . ? P2 C10 H10 113.0(16) . . ? C16 C11 C12 119.9(2) . . ? C16 C11 P1 120.45(16) . . ? C12 C11 P1 119.60(17) . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.2(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.0(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 119.8(2) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C22 C17 C18 118.2(2) . . ? C22 C17 P2 121.41(19) . . ? C18 C17 P2 120.29(18) . . ? C19 C18 C17 120.7(2) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 119.7(2) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.8(3) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? O1 C23 W1 176.2(2) . . ? O2 C24 W1 177.2(2) . . ? O3 C25 W1 176.9(2) . . ? O4 C26 W1 177.9(2) . . ? O5 C27 W1 179.1(2) . . ? O6 C28 W2 177.9(2) . . ? O7 C29 W2 178.2(2) . . ? O8 C30 W2 179.4(2) . . ? O9 C31 W2 178.4(2) . . ? O10 C32 W2 178.3(2) . . ? 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 C24 W1 P1 C11 -145.49(11) . . . . ? C23 W1 P1 C11 122.53(12) . . . . ? C25 W1 P1 C11 -57.97(11) . . . . ? C26 W1 P1 C11 31.93(11) . . . . ? C24 W1 P1 C1 2.78(11) . . . . ? C23 W1 P1 C1 -89.19(12) . . . . ? C25 W1 P1 C1 90.30(11) . . . . ? C26 W1 P1 C1 -179.80(11) . . . . ? C24 W1 P1 C2 62.82(11) . . . . ? C23 W1 P1 C2 -29.15(12) . . . . ? C25 W1 P1 C2 150.34(11) . . . . ? C26 W1 P1 C2 -119.76(11) . . . . ? C31 W2 P2 C10 74.43(10) . . . . ? C28 W2 P2 C10 166.29(10) . . . . ? C30 W2 P2 C10 -15.47(10) . . . . ? C29 W2 P2 C10 -104.02(10) . . . . ? C31 W2 P2 C1 -163.81(10) . . . . ? C28 W2 P2 C1 -71.94(10) . . . . ? C30 W2 P2 C1 106.29(10) . . . . ? C29 W2 P2 C1 17.75(10) . . . . ? C31 W2 P2 C17 -45.85(11) . . . . ? C28 W2 P2 C17 46.02(11) . . . . ? C30 W2 P2 C17 -135.75(11) . . . . ? C29 W2 P2 C17 135.71(11) . . . . ? C10 P2 C1 C2 46.74(19) . . . . ? C17 P2 C1 C2 156.03(17) . . . . ? W2 P2 C1 C2 -78.93(17) . . . . ? C10 P2 C1 P1 -36.82(17) . . . . ? C17 P2 C1 P1 72.46(16) . . . . ? W2 P2 C1 P1 -162.50(11) . . . . ? C11 P1 C1 C2 -100.79(13) . . . . ? W1 P1 C1 C2 108.42(11) . . . . ? C11 P1 C1 P2 11.47(18) . . . . ? C2 P1 C1 P2 112.27(19) . . . . ? W1 P1 C1 P2 -139.32(11) . . . . ? P2 C1 C2 C3 0.4(3) . . . . ? P1 C1 C2 C3 122.6(2) . . . . ? P2 C1 C2 P1 -122.23(16) . . . . ? C11 P1 C2 C3 -20.7(2) . . . . ? C1 P1 C2 C3 -119.3(2) . . . . ? W1 P1 C2 C3 132.97(17) . . . . ? C11 P1 C2 C1 98.54(13) . . . . ? W1 P1 C2 C1 -107.77(11) . . . . ? C1 C2 C3 C4 145.1(2) . . . . ? P1 C2 C3 C4 -127.6(2) . . . . ? C1 C2 C3 C8 -36.1(3) . . . . ? P1 C2 C3 C8 51.2(3) . . . . ? C8 C3 C4 C5 -0.3(3) . . . . ? C2 C3 C4 C5 178.6(2) . . . . ? C3 C4 C5 C6 -2.2(4) . . . . ? C4 C5 C6 C7 1.4(4) . . . . ? C5 C6 C7 C8 2.0(4) . . . . ? C6 C7 C8 C3 -4.5(4) . . . . ? C6 C7 C8 C9 175.1(2) . . . . ? C4 C3 C8 C7 3.5(3) . . . . ? C2 C3 C8 C7 -175.2(2) . . . . ? C4 C3 C8 C9 -176.0(2) . . . . ? C2 C3 C8 C9 5.3(4) . . . . ? C7 C8 C9 C10 -150.6(2) . . . . ? C3 C8 C9 C10 28.9(4) . . . . ? C8 C9 C10 P2 4.4(4) . . . . ? C1 P2 C10 C9 -51.3(2) . . . . ? C17 P2 C10 C9 -159.0(2) . . . . ? W2 P2 C10 C9 74.8(2) . . . . ? C1 P1 C11 C16 111.77(18) . . . . ? C2 P1 C11 C16 59.56(19) . . . . ? W1 P1 C11 C16 -95.74(17) . . . . ? C1 P1 C11 C12 -70.52(19) . . . . ? C2 P1 C11 C12 -122.73(17) . . . . ? W1 P1 C11 C12 81.97(17) . . . . ? C16 C11 C12 C13 -3.7(3) . . . . ? P1 C11 C12 C13 178.54(16) . . . . ? C11 C12 C13 C14 1.5(3) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C13 C14 C15 C16 -2.0(4) . . . . ? C12 C11 C16 C15 3.1(3) . . . . ? P1 C11 C16 C15 -179.19(17) . . . . ? C14 C15 C16 C11 -0.3(3) . . . . ? C10 P2 C17 C22 -40.3(2) . . . . ? C1 P2 C17 C22 -150.9(2) . . . . ? W2 P2 C17 C22 84.8(2) . . . . ? C10 P2 C17 C18 142.50(19) . . . . ? C1 P2 C17 C18 31.9(2) . . . . ? W2 P2 C17 C18 -92.44(19) . . . . ? C22 C17 C18 C19 0.5(4) . . . . ? P2 C17 C18 C19 177.8(2) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? C19 C20 C21 C22 0.2(5) . . . . ? C20 C21 C22 C17 0.0(5) . . . . ? C18 C17 C22 C21 -0.4(4) . . . . ? P2 C17 C22 C21 -177.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.893 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.077 #===END data_s3426a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H16 Mo2 O10 P2' _chemical_formula_sum 'C32 H16 Mo2 O10 P2' _chemical_formula_weight 814.27 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 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 9.2748(4) _cell_length_b 12.0660(6) _cell_length_c 15.2717(6) _cell_angle_alpha 90.529(2) _cell_angle_beta 98.060(1) _cell_angle_gamma 104.808(2) _cell_volume 1634.16(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 126 _cell_measurement_theta_min 5.47 _cell_measurement_theta_max 20.58 _exptl_crystal_description plate _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36889 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7481 _reflns_number_gt 6402 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Dirax' _computing_data_reduction 'EvalCCD, sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.8718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7481 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Mo1 Mo 0.46661(2) 1.163408(17) 0.211087(13) 0.02273(7) Uani 1 1 d . . . Mo2 Mo 0.26778(2) 0.630866(17) 0.359924(14) 0.02582(7) Uani 1 1 d . . . P1 P 0.19341(7) 1.05267(5) 0.18754(4) 0.02216(13) Uani 1 1 d . . . P2 P 0.01157(7) 0.66155(5) 0.32127(4) 0.02563(14) Uani 1 1 d . . . O1 O 0.4034(3) 1.4106(2) 0.20600(19) 0.0625(7) Uani 1 1 d . . . O2 O 0.4800(2) 1.1832(2) 0.00502(13) 0.0420(5) Uani 1 1 d . . . O3 O 0.5524(3) 0.9229(2) 0.21021(16) 0.0522(6) Uani 1 1 d . . . O4 O 0.4545(3) 1.1695(2) 0.41898(14) 0.0540(6) Uani 1 1 d . . . O5 O 0.8157(2) 1.2828(2) 0.24110(16) 0.0503(6) Uani 1 1 d . . . O6 O 0.1967(4) 0.6168(2) 0.55815(16) 0.0610(7) Uani 1 1 d . . . O7 O 0.1469(3) 0.35920(18) 0.34022(19) 0.0617(7) Uani 1 1 d . . . O8 O 0.3298(3) 0.6507(2) 0.15922(17) 0.0584(7) Uani 1 1 d . . . O9 O 0.4106(2) 0.90096(16) 0.39337(14) 0.0413(5) Uani 1 1 d . . . O10 O 0.5741(3) 0.5745(3) 0.4272(3) 0.1289(19) Uani 1 1 d . . . C1 C -0.0085(3) 0.9780(2) 0.33178(15) 0.0224(5) Uani 1 1 d . . . C2 C -0.0819(3) 0.8841(2) 0.37819(15) 0.0228(5) Uani 1 1 d . . . C3 C -0.1795(3) 0.9015(2) 0.43574(16) 0.0287(5) Uani 1 1 d . . . H3 H -0.2290 0.8390 0.4672 0.034 Uiso 1 1 calc R . . C4 C -0.2051(3) 1.0082(3) 0.44764(17) 0.0333(6) Uani 1 1 d . . . H4 H -0.2730 1.0183 0.4864 0.040 Uiso 1 1 calc R . . C5 C -0.1320(3) 1.1005(2) 0.40308(17) 0.0323(6) Uani 1 1 d . . . H5 H -0.1490 1.1739 0.4117 0.039 Uiso 1 1 calc R . . C6 C -0.0343(3) 1.0855(2) 0.34607(16) 0.0275(5) Uani 1 1 d . . . H6 H 0.0160 1.1493 0.3161 0.033 Uiso 1 1 calc R . . C7 C 0.0857(3) 0.9681(2) 0.26497(15) 0.0229(5) Uani 1 1 d . . . C8 C 0.1239(3) 0.9035(2) 0.20759(16) 0.0259(5) Uani 1 1 d . . . H8 H 0.117(4) 0.831(3) 0.186(2) 0.042(9) Uiso 1 1 d . . . C9 C -0.0624(3) 0.7686(2) 0.36978(17) 0.0270(5) Uani 1 1 d . . . C10 C -0.1061(3) 0.6677(2) 0.4029(2) 0.0357(6) Uani 1 1 d . . . H10 H -0.163(3) 0.629(3) 0.447(2) 0.034(8) Uiso 1 1 d . . . C11 C 0.0509(3) 1.0937(2) 0.10848(15) 0.0234(5) Uani 1 1 d . . . C12 C 0.0929(3) 1.1921(2) 0.06053(17) 0.0296(5) Uani 1 1 d . . . H12 H 0.1961 1.2332 0.0657 0.036 Uiso 1 1 calc R . . C13 C -0.0159(3) 1.2302(2) 0.00508(18) 0.0347(6) Uani 1 1 d . . . H13 H 0.0133 1.2965 -0.0280 0.042 Uiso 1 1 calc R . . C14 C -0.1659(3) 1.1715(2) -0.00162(17) 0.0330(6) Uani 1 1 d . . . H14 H -0.2402 1.1985 -0.0381 0.040 Uiso 1 1 calc R . . C15 C -0.2084(3) 1.0733(2) 0.04472(17) 0.0308(5) Uani 1 1 d . . . H15 H -0.3117 1.0325 0.0392 0.037 Uiso 1 1 calc R . . C16 C -0.1012(3) 1.0339(2) 0.09909(16) 0.0281(5) Uani 1 1 d . . . H16 H -0.1313 0.9660 0.1301 0.034 Uiso 1 1 calc R . . C17 C -0.1086(3) 0.6106(2) 0.21534(18) 0.0307(6) Uani 1 1 d . . . C18 C -0.0782(3) 0.5266(2) 0.1637(2) 0.0381(6) Uani 1 1 d . . . H18 H 0.0056 0.4968 0.1831 0.046 Uiso 1 1 calc R . . C19 C -0.1695(4) 0.4857(3) 0.0836(2) 0.0459(7) Uani 1 1 d . . . H19 H -0.1490 0.4272 0.0491 0.055 Uiso 1 1 calc R . . C20 C -0.2903(3) 0.5303(3) 0.0545(2) 0.0474(8) Uani 1 1 d . . . H20 H -0.3518 0.5030 -0.0004 0.057 Uiso 1 1 calc R . . C21 C -0.3213(3) 0.6141(3) 0.1047(2) 0.0481(8) Uani 1 1 d . . . H21 H -0.4040 0.6447 0.0841 0.058 Uiso 1 1 calc R . . C22 C -0.2322(3) 0.6545(3) 0.1857(2) 0.0396(7) Uani 1 1 d . . . H22 H -0.2552 0.7114 0.2207 0.048 Uiso 1 1 calc R . . C23 C 0.4228(3) 1.3211(2) 0.20874(19) 0.0367(6) Uani 1 1 d . . . C24 C 0.4729(3) 1.1732(2) 0.07828(17) 0.0291(5) Uani 1 1 d . . . C25 C 0.5194(3) 1.0072(2) 0.21105(18) 0.0328(6) Uani 1 1 d . . . C26 C 0.4596(3) 1.1654(2) 0.34574(18) 0.0334(6) Uani 1 1 d . . . C27 C 0.6894(3) 1.2410(2) 0.23070(17) 0.0329(6) Uani 1 1 d . . . C28 C 0.2233(4) 0.6223(2) 0.4882(2) 0.0378(6) Uani 1 1 d . . . C29 C 0.1846(3) 0.4562(2) 0.3445(2) 0.0368(6) Uani 1 1 d . . . C30 C 0.3078(3) 0.6431(2) 0.2302(2) 0.0371(6) Uani 1 1 d . . . C31 C 0.3594(3) 0.8049(2) 0.38067(17) 0.0312(5) Uani 1 1 d . . . C32 C 0.4659(4) 0.5978(3) 0.4012(3) 0.0608(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 Mo1 0.02386(11) 0.02443(12) 0.01913(11) 0.00634(8) 0.00344(8) 0.00454(8) Mo2 0.02232(12) 0.02135(12) 0.03315(13) 0.00632(9) 0.00005(9) 0.00647(8) P1 0.0240(3) 0.0242(3) 0.0188(3) 0.0063(2) 0.0051(2) 0.0059(2) P2 0.0229(3) 0.0214(3) 0.0322(3) 0.0070(2) 0.0020(3) 0.0059(2) O1 0.0852(19) 0.0378(13) 0.0751(18) 0.0092(12) 0.0273(15) 0.0268(13) O2 0.0439(11) 0.0605(14) 0.0258(10) 0.0137(9) 0.0105(9) 0.0178(10) O3 0.0706(16) 0.0397(12) 0.0571(14) 0.0121(11) 0.0220(12) 0.0264(11) O4 0.0751(17) 0.0543(14) 0.0257(11) 0.0033(9) 0.0090(11) 0.0036(12) O5 0.0280(10) 0.0565(14) 0.0561(14) 0.0250(11) -0.0033(9) -0.0032(9) O6 0.106(2) 0.0442(13) 0.0373(13) 0.0114(10) 0.0148(13) 0.0254(14) O7 0.0628(15) 0.0247(11) 0.090(2) 0.0046(11) -0.0018(14) 0.0048(10) O8 0.0838(19) 0.0533(15) 0.0513(15) 0.0150(12) 0.0337(14) 0.0285(13) O9 0.0498(12) 0.0275(10) 0.0396(11) 0.0043(8) 0.0032(9) -0.0007(9) O10 0.0284(13) 0.123(3) 0.237(5) 0.111(3) 0.007(2) 0.0262(16) C1 0.0234(11) 0.0265(12) 0.0169(10) 0.0041(9) -0.0008(9) 0.0074(9) C2 0.0224(11) 0.0274(12) 0.0186(11) 0.0048(9) 0.0001(9) 0.0081(9) C3 0.0270(12) 0.0371(14) 0.0233(12) 0.0076(10) 0.0067(10) 0.0088(11) C4 0.0345(14) 0.0465(16) 0.0229(12) 0.0004(11) 0.0059(11) 0.0169(12) C5 0.0423(15) 0.0351(14) 0.0240(12) -0.0003(10) 0.0029(11) 0.0189(12) C6 0.0368(13) 0.0275(12) 0.0181(11) 0.0028(9) 0.0012(10) 0.0094(10) C7 0.0242(11) 0.0237(11) 0.0194(11) 0.0073(9) 0.0005(9) 0.0049(9) C8 0.0299(12) 0.0250(12) 0.0248(12) 0.0070(10) 0.0062(10) 0.0090(10) C9 0.0228(11) 0.0308(13) 0.0281(12) 0.0081(10) 0.0038(9) 0.0079(10) C10 0.0307(13) 0.0353(14) 0.0438(16) 0.0185(12) 0.0136(12) 0.0086(11) C11 0.0286(12) 0.0276(12) 0.0151(10) 0.0019(9) 0.0028(9) 0.0096(10) C12 0.0285(12) 0.0351(14) 0.0253(12) 0.0090(10) 0.0050(10) 0.0075(11) C13 0.0371(14) 0.0400(15) 0.0295(13) 0.0129(11) 0.0056(11) 0.0139(12) C14 0.0345(13) 0.0456(16) 0.0228(12) 0.0045(11) 0.0027(10) 0.0181(12) C15 0.0255(12) 0.0410(15) 0.0252(12) 0.0001(11) 0.0015(10) 0.0087(11) C16 0.0311(13) 0.0296(13) 0.0232(12) 0.0031(10) 0.0054(10) 0.0061(10) C17 0.0252(12) 0.0233(12) 0.0387(14) 0.0066(11) -0.0028(11) 0.0014(10) C18 0.0389(15) 0.0254(13) 0.0453(16) 0.0032(12) -0.0067(13) 0.0068(11) C19 0.0519(18) 0.0315(15) 0.0456(17) -0.0034(13) -0.0046(14) 0.0017(13) C20 0.0379(16) 0.0469(18) 0.0441(17) 0.0045(14) -0.0101(14) -0.0041(14) C21 0.0281(14) 0.0549(19) 0.0539(19) 0.0124(16) -0.0111(13) 0.0066(13) C22 0.0276(13) 0.0383(15) 0.0504(18) 0.0052(13) -0.0019(12) 0.0082(12) C23 0.0434(16) 0.0326(14) 0.0373(15) 0.0053(12) 0.0140(12) 0.0110(12) C24 0.0252(12) 0.0353(14) 0.0278(13) 0.0073(11) 0.0066(10) 0.0081(10) C25 0.0365(14) 0.0327(14) 0.0306(13) 0.0095(11) 0.0101(11) 0.0084(11) C26 0.0374(14) 0.0324(14) 0.0250(13) 0.0045(11) 0.0034(11) 0.0002(11) C27 0.0336(14) 0.0344(14) 0.0273(13) 0.0123(11) 0.0006(11) 0.0040(11) C28 0.0484(17) 0.0281(14) 0.0369(16) 0.0053(12) 0.0004(13) 0.0130(12) C29 0.0323(14) 0.0310(15) 0.0455(16) 0.0073(12) 0.0017(12) 0.0078(11) C30 0.0380(15) 0.0296(14) 0.0490(18) 0.0067(12) 0.0130(13) 0.0146(12) C31 0.0312(13) 0.0321(14) 0.0285(13) 0.0070(10) 0.0005(10) 0.0068(11) C32 0.0293(15) 0.053(2) 0.100(3) 0.040(2) 0.0051(17) 0.0119(14) _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 Mo1 C27 2.017(3) . ? Mo1 C24 2.041(3) . ? Mo1 C23 2.044(3) . ? Mo1 C25 2.065(3) . ? Mo1 C26 2.067(3) . ? Mo1 P1 2.5180(6) . ? Mo2 C32 1.997(3) . ? Mo2 C29 2.050(3) . ? Mo2 C28 2.055(3) . ? Mo2 C31 2.057(3) . ? Mo2 C30 2.066(3) . ? Mo2 P2 2.4885(7) . ? P1 C8 1.795(3) . ? P1 C7 1.808(2) . ? P1 C11 1.830(2) . ? P2 C10 1.781(3) . ? P2 C9 1.808(3) . ? P2 C17 1.834(3) . ? O1 C23 1.139(4) . ? O2 C24 1.136(3) . ? O3 C25 1.135(3) . ? O4 C26 1.127(3) . ? O5 C27 1.138(3) . ? O6 C28 1.129(4) . ? O7 C29 1.131(3) . ? O8 C30 1.132(4) . ? O9 C31 1.138(3) . ? O10 C32 1.130(4) . ? C1 C6 1.399(3) . ? C1 C2 1.416(3) . ? C1 C7 1.456(3) . ? C2 C3 1.398(3) . ? C2 C9 1.457(3) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.311(4) . ? C8 H8 0.91(3) . ? C9 C10 1.311(4) . ? C10 H10 0.96(3) . ? C11 C16 1.397(3) . ? C11 C12 1.399(3) . ? C12 C13 1.397(4) . ? C12 H12 0.9500 . ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.386(4) . ? C17 C22 1.403(4) . ? C18 C19 1.393(4) . ? C18 H18 0.9500 . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 C21 1.375(5) . ? C20 H20 0.9500 . ? C21 C22 1.396(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Mo1 C24 87.93(10) . . ? C27 Mo1 C23 89.35(12) . . ? C24 Mo1 C23 87.55(11) . . ? C27 Mo1 C25 88.48(11) . . ? C24 Mo1 C25 91.03(11) . . ? C23 Mo1 C25 177.44(11) . . ? C27 Mo1 C26 91.44(11) . . ? C24 Mo1 C26 175.97(11) . . ? C23 Mo1 C26 88.46(11) . . ? C25 Mo1 C26 92.94(11) . . ? C27 Mo1 P1 175.80(8) . . ? C24 Mo1 P1 92.47(7) . . ? C23 Mo1 P1 94.85(9) . . ? C25 Mo1 P1 87.33(8) . . ? C26 Mo1 P1 88.46(8) . . ? C32 Mo2 C29 85.43(13) . . ? C32 Mo2 C28 89.11(15) . . ? C29 Mo2 C28 89.06(12) . . ? C32 Mo2 C31 92.01(13) . . ? C29 Mo2 C31 177.04(11) . . ? C28 Mo2 C31 89.40(11) . . ? C32 Mo2 C30 92.59(15) . . ? C29 Mo2 C30 91.93(12) . . ? C28 Mo2 C30 178.10(11) . . ? C31 Mo2 C30 89.68(11) . . ? C32 Mo2 P2 174.30(11) . . ? C29 Mo2 P2 91.88(8) . . ? C28 Mo2 P2 85.82(9) . . ? C31 Mo2 P2 90.53(8) . . ? C30 Mo2 P2 92.52(8) . . ? C8 P1 C7 42.66(11) . . ? C8 P1 C11 107.91(11) . . ? C7 P1 C11 103.94(11) . . ? C8 P1 Mo1 125.37(8) . . ? C7 P1 Mo1 128.73(8) . . ? C11 P1 Mo1 122.60(8) . . ? C10 P2 C9 42.85(12) . . ? C10 P2 C17 108.58(13) . . ? C9 P2 C17 107.27(12) . . ? C10 P2 Mo2 122.09(10) . . ? C9 P2 Mo2 127.14(8) . . ? C17 P2 Mo2 122.91(9) . . ? C6 C1 C2 118.9(2) . . ? C6 C1 C7 117.2(2) . . ? C2 C1 C7 123.7(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 C9 117.1(2) . . ? C1 C2 C9 124.0(2) . . ? C4 C3 C2 121.1(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 121.1(2) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C1 148.8(2) . . ? C8 C7 P1 68.13(15) . . ? C1 C7 P1 141.37(19) . . ? C7 C8 P1 69.22(15) . . ? C7 C8 H8 148(2) . . ? P1 C8 H8 143(2) . . ? C10 C9 C2 139.6(2) . . ? C10 C9 P2 67.50(17) . . ? C2 C9 P2 152.85(19) . . ? C9 C10 P2 69.65(16) . . ? C9 C10 H10 141.9(18) . . ? P2 C10 H10 148.4(18) . . ? C16 C11 C12 118.8(2) . . ? C16 C11 P1 121.68(18) . . ? C12 C11 P1 119.35(18) . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 119.9(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.1(2) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.3(2) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C18 C17 C22 119.1(3) . . ? C18 C17 P2 119.7(2) . . ? C22 C17 P2 121.1(2) . . ? C17 C18 C19 120.6(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 119.7(3) . . ? C21 C22 H22 120.1 . . ? C17 C22 H22 120.1 . . ? O1 C23 Mo1 177.3(3) . . ? O2 C24 Mo1 177.1(2) . . ? O3 C25 Mo1 178.0(2) . . ? O4 C26 Mo1 178.0(3) . . ? O5 C27 Mo1 178.6(3) . . ? O6 C28 Mo2 179.0(3) . . ? O7 C29 Mo2 175.2(3) . . ? O8 C30 Mo2 179.5(3) . . ? O9 C31 Mo2 179.0(2) . . ? O10 C32 Mo2 176.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C24 Mo1 P1 C8 108.63(13) . . . . ? C23 Mo1 P1 C8 -163.62(13) . . . . ? C25 Mo1 P1 C8 17.71(13) . . . . ? C26 Mo1 P1 C8 -75.30(13) . . . . ? C24 Mo1 P1 C7 162.70(13) . . . . ? C23 Mo1 P1 C7 -109.55(13) . . . . ? C25 Mo1 P1 C7 71.78(13) . . . . ? C26 Mo1 P1 C7 -21.23(13) . . . . ? C24 Mo1 P1 C11 -45.73(12) . . . . ? C23 Mo1 P1 C11 42.02(12) . . . . ? C25 Mo1 P1 C11 -136.65(12) . . . . ? C26 Mo1 P1 C11 130.34(12) . . . . ? C29 Mo2 P2 C10 89.88(14) . . . . ? C28 Mo2 P2 C10 0.96(14) . . . . ? C31 Mo2 P2 C10 -88.40(14) . . . . ? C30 Mo2 P2 C10 -178.10(14) . . . . ? C29 Mo2 P2 C9 142.25(13) . . . . ? C28 Mo2 P2 C9 53.33(13) . . . . ? C31 Mo2 P2 C9 -36.03(13) . . . . ? C30 Mo2 P2 C9 -125.73(13) . . . . ? C29 Mo2 P2 C17 -58.74(13) . . . . ? C28 Mo2 P2 C17 -147.66(13) . . . . ? C31 Mo2 P2 C17 122.98(12) . . . . ? C30 Mo2 P2 C17 33.28(13) . . . . ? C6 C1 C2 C3 1.0(3) . . . . ? C7 C1 C2 C3 -174.8(2) . . . . ? C6 C1 C2 C9 -179.1(2) . . . . ? C7 C1 C2 C9 5.1(4) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C9 C2 C3 C4 -179.8(2) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C2 C1 C6 C5 -1.3(4) . . . . ? C7 C1 C6 C5 174.8(2) . . . . ? C6 C1 C7 C8 -154.7(4) . . . . ? C2 C1 C7 C8 21.2(6) . . . . ? C6 C1 C7 P1 1.2(4) . . . . ? C2 C1 C7 P1 177.1(2) . . . . ? C11 P1 C7 C8 101.44(16) . . . . ? Mo1 P1 C7 C8 -102.97(15) . . . . ? C8 P1 C7 C1 -166.8(4) . . . . ? C11 P1 C7 C1 -65.4(3) . . . . ? Mo1 P1 C7 C1 90.2(3) . . . . ? C1 C7 C8 P1 164.1(4) . . . . ? C11 P1 C8 C7 -91.31(16) . . . . ? Mo1 P1 C8 C7 111.22(14) . . . . ? C3 C2 C9 C10 -2.9(5) . . . . ? C1 C2 C9 C10 177.2(3) . . . . ? C3 C2 C9 P2 174.9(3) . . . . ? C1 C2 C9 P2 -5.0(6) . . . . ? C17 P2 C9 C10 98.96(19) . . . . ? Mo2 P2 C9 C10 -99.40(17) . . . . ? C10 P2 C9 C2 -178.5(5) . . . . ? C17 P2 C9 C2 -79.5(4) . . . . ? Mo2 P2 C9 C2 82.1(4) . . . . ? C2 C9 C10 P2 178.9(4) . . . . ? C17 P2 C10 C9 -95.62(18) . . . . ? Mo2 P2 C10 C9 111.84(15) . . . . ? C8 P1 C11 C16 24.5(2) . . . . ? C7 P1 C11 C16 -19.8(2) . . . . ? Mo1 P1 C11 C16 -177.27(16) . . . . ? C8 P1 C11 C12 -160.0(2) . . . . ? C7 P1 C11 C12 155.7(2) . . . . ? Mo1 P1 C11 C12 -1.8(2) . . . . ? C16 C11 C12 C13 0.7(4) . . . . ? P1 C11 C12 C13 -174.9(2) . . . . ? C11 C12 C13 C14 0.9(4) . . . . ? C12 C13 C14 C15 -1.6(4) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C14 C15 C16 C11 0.7(4) . . . . ? C12 C11 C16 C15 -1.5(4) . . . . ? P1 C11 C16 C15 174.04(19) . . . . ? C10 P2 C17 C18 -134.4(2) . . . . ? C9 P2 C17 C18 -179.5(2) . . . . ? Mo2 P2 C17 C18 17.9(3) . . . . ? C10 P2 C17 C22 45.0(3) . . . . ? C9 P2 C17 C22 -0.1(3) . . . . ? Mo2 P2 C17 C22 -162.70(19) . . . . ? C22 C17 C18 C19 -0.4(4) . . . . ? P2 C17 C18 C19 179.1(2) . . . . ? C17 C18 C19 C20 1.1(5) . . . . ? C18 C19 C20 C21 -0.7(5) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C20 C21 C22 C17 1.1(5) . . . . ? C18 C17 C22 C21 -0.7(4) . . . . ? P2 C17 C22 C21 179.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.099 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.103 #===END data_s3249a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H16 Mn O2 P' _chemical_formula_sum 'C21 H16 Mn O2 P' _chemical_formula_weight 386.25 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' 'Mn' 'Mn' 0.3368 0.7283 '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 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 9.2488(1) _cell_length_b 10.0296(1) _cell_length_c 10.8435(2) _cell_angle_alpha 110.0434(9) _cell_angle_beta 95.2573(10) _cell_angle_gamma 105.1996(8) _cell_volume 893.42(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17071 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16043 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4040 _reflns_number_gt 3303 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000, SortAV' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.2933P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4040 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Mn1 Mn 0.33152(3) 0.27856(3) 0.22024(2) 0.02536(8) Uani 1 1 d . . . P1 P 0.54654(5) 0.23479(5) 0.18006(4) 0.02446(10) Uani 1 1 d . . . O1 O 0.38027(18) 0.28820(17) 0.49394(13) 0.0512(4) Uani 1 1 d . . . O2 O 0.15097(14) -0.03824(14) 0.10940(13) 0.0412(3) Uani 1 1 d . . . C1 C 0.71354(18) 0.36717(18) 0.17083(16) 0.0263(3) Uani 1 1 d . . . C2 C 0.6422(2) 0.2654(2) 0.05257(18) 0.0336(4) Uani 1 1 d . . . H2 H 0.646(2) 0.236(2) -0.037(2) 0.046(6) Uiso 1 1 d . . . C3 C 0.83998(18) 0.50341(18) 0.24245(16) 0.0265(3) Uani 1 1 d . . . C4 C 0.9286(2) 0.5750(2) 0.17238(19) 0.0339(4) Uani 1 1 d . . . H4 H 0.9056 0.5350 0.0772 0.041 Uiso 1 1 calc R . . C5 C 1.0494(2) 0.7036(2) 0.2407(2) 0.0464(5) Uani 1 1 d . . . H5 H 1.1096 0.7519 0.1926 0.056 Uiso 1 1 calc R . . C6 C 1.0828(2) 0.7620(2) 0.3782(3) 0.0540(6) Uani 1 1 d . . . H6 H 1.1663 0.8507 0.4250 0.065 Uiso 1 1 calc R . . C7 C 0.9958(2) 0.6926(2) 0.4486(2) 0.0517(5) Uani 1 1 d . . . H7 H 1.0194 0.7336 0.5438 0.062 Uiso 1 1 calc R . . C8 C 0.8745(2) 0.5638(2) 0.38133(18) 0.0371(4) Uani 1 1 d . . . H8 H 0.8146 0.5165 0.4302 0.044 Uiso 1 1 calc R . . C9 C 0.61061(18) 0.09650(17) 0.22552(15) 0.0255(3) Uani 1 1 d . . . C10 C 0.7462(2) 0.0699(2) 0.19699(17) 0.0333(4) Uani 1 1 d . . . H10 H 0.8057 0.1222 0.1512 0.040 Uiso 1 1 calc R . . C11 C 0.7955(2) -0.0322(2) 0.23450(19) 0.0390(4) Uani 1 1 d . . . H11 H 0.8888 -0.0489 0.2147 0.047 Uiso 1 1 calc R . . C12 C 0.7100(2) -0.1101(2) 0.30058(18) 0.0370(4) Uani 1 1 d . . . H12 H 0.7444 -0.1798 0.3264 0.044 Uiso 1 1 calc R . . C13 C 0.5745(2) -0.08569(19) 0.32870(17) 0.0333(4) Uani 1 1 d . . . H13 H 0.5149 -0.1394 0.3734 0.040 Uiso 1 1 calc R . . C14 C 0.52485(19) 0.01704(19) 0.29191(16) 0.0293(4) Uani 1 1 d . . . H14 H 0.4316 0.0334 0.3121 0.035 Uiso 1 1 calc R . . C15 C 0.3637(2) 0.28323(19) 0.38524(18) 0.0326(4) Uani 1 1 d . . . C16 C 0.22593(18) 0.0868(2) 0.15387(17) 0.0290(4) Uani 1 1 d . . . C17 C 0.1710(2) 0.3176(2) 0.0943(2) 0.0477(6) Uani 1 1 d . . . H17 H 0.100(3) 0.242(3) 0.029(2) 0.057(7) Uiso 1 1 d . . . C18 C 0.3199(2) 0.3781(2) 0.0758(2) 0.0407(5) Uani 1 1 d . . . H18 H 0.358(2) 0.349(2) 0.000(2) 0.037(5) Uiso 1 1 d . . . C19 C 0.4036(2) 0.4905(2) 0.2008(2) 0.0362(4) Uani 1 1 d . . . H19 H 0.509(2) 0.549(2) 0.221(2) 0.045(6) Uiso 1 1 d . . . C20 C 0.3071(2) 0.4978(2) 0.2930(2) 0.0420(5) Uani 1 1 d . . . H20 H 0.332(2) 0.563(2) 0.385(2) 0.044(6) Uiso 1 1 d . . . C21 C 0.1638(2) 0.3906(2) 0.2283(3) 0.0474(5) Uani 1 1 d . . . H21 H 0.081(2) 0.365(2) 0.268(2) 0.047(6) Uiso 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 Mn1 0.02275(14) 0.02410(15) 0.03059(15) 0.01304(11) 0.00075(10) 0.00759(10) P1 0.0241(2) 0.0231(2) 0.0260(2) 0.01021(17) 0.00306(16) 0.00647(17) O1 0.0729(10) 0.0607(10) 0.0306(7) 0.0179(7) 0.0098(7) 0.0376(8) O2 0.0364(7) 0.0303(7) 0.0525(8) 0.0194(6) 0.0034(6) 0.0005(6) C1 0.0264(8) 0.0281(9) 0.0311(9) 0.0157(7) 0.0099(7) 0.0117(7) C2 0.0399(10) 0.0361(10) 0.0286(9) 0.0148(8) 0.0101(8) 0.0137(8) C3 0.0241(8) 0.0260(9) 0.0362(9) 0.0163(7) 0.0087(7) 0.0120(7) C4 0.0316(9) 0.0381(10) 0.0472(10) 0.0288(9) 0.0113(8) 0.0172(8) C5 0.0329(10) 0.0403(11) 0.0821(16) 0.0421(12) 0.0153(10) 0.0110(9) C6 0.0373(11) 0.0312(11) 0.0824(17) 0.0196(11) -0.0029(11) 0.0006(9) C7 0.0510(13) 0.0410(12) 0.0466(12) 0.0061(10) -0.0028(10) 0.0064(10) C8 0.0372(10) 0.0351(10) 0.0378(10) 0.0139(8) 0.0089(8) 0.0092(8) C9 0.0280(8) 0.0201(8) 0.0247(8) 0.0055(7) 0.0014(6) 0.0069(7) C10 0.0321(9) 0.0304(10) 0.0375(10) 0.0125(8) 0.0086(8) 0.0103(8) C11 0.0351(10) 0.0369(11) 0.0491(11) 0.0146(9) 0.0108(8) 0.0194(9) C12 0.0434(11) 0.0307(10) 0.0408(10) 0.0137(8) 0.0046(8) 0.0190(8) C13 0.0400(10) 0.0273(9) 0.0359(9) 0.0149(8) 0.0069(8) 0.0124(8) C14 0.0301(9) 0.0267(9) 0.0324(9) 0.0112(7) 0.0060(7) 0.0112(7) C15 0.0341(9) 0.0306(10) 0.0365(10) 0.0111(8) 0.0061(8) 0.0181(8) C16 0.0250(8) 0.0336(10) 0.0332(9) 0.0182(8) 0.0047(7) 0.0101(7) C17 0.0363(11) 0.0379(12) 0.0666(15) 0.0303(11) -0.0194(10) 0.0042(9) C18 0.0507(12) 0.0374(11) 0.0420(11) 0.0252(9) 0.0019(9) 0.0158(9) C19 0.0329(10) 0.0251(9) 0.0533(12) 0.0208(9) 0.0014(9) 0.0079(8) C20 0.0485(12) 0.0329(11) 0.0528(13) 0.0174(10) 0.0090(10) 0.0248(9) C21 0.0324(11) 0.0508(13) 0.0782(16) 0.0398(12) 0.0118(11) 0.0233(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 Mn1 C16 1.7633(18) . ? Mn1 C15 1.7691(18) . ? Mn1 C17 2.1265(18) . ? Mn1 C21 2.1329(19) . ? Mn1 C18 2.1354(18) . ? Mn1 C19 2.1440(17) . ? Mn1 C20 2.1474(19) . ? Mn1 P1 2.1961(5) . ? P1 C2 1.7781(18) . ? P1 C1 1.7896(16) . ? P1 C9 1.8341(16) . ? O1 C15 1.157(2) . ? O2 C16 1.163(2) . ? C1 C2 1.310(2) . ? C1 C3 1.451(2) . ? C2 H2 0.92(2) . ? C3 C8 1.386(2) . ? C3 C4 1.394(2) . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.372(3) . ? C5 H5 0.9500 . ? C6 C7 1.378(3) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.389(2) . ? C9 C14 1.396(2) . ? C10 C11 1.385(2) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 C14 1.389(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C17 C21 1.402(3) . ? C17 C18 1.415(3) . ? C17 H17 0.89(2) . ? C18 C19 1.418(3) . ? C18 H18 0.912(19) . ? C19 C20 1.396(3) . ? C19 H19 0.96(2) . ? C20 C21 1.404(3) . ? C20 H20 0.95(2) . ? C21 H21 0.94(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Mn1 C15 92.49(8) . . ? C16 Mn1 C17 89.89(8) . . ? C15 Mn1 C17 138.48(9) . . ? C16 Mn1 C21 104.85(8) . . ? C15 Mn1 C21 101.61(9) . . ? C17 Mn1 C21 38.44(9) . . ? C16 Mn1 C18 112.16(8) . . ? C15 Mn1 C18 153.86(8) . . ? C17 Mn1 C18 38.77(8) . . ? C21 Mn1 C18 64.78(9) . . ? C16 Mn1 C19 150.70(7) . . ? C15 Mn1 C19 115.91(8) . . ? C17 Mn1 C19 64.43(8) . . ? C21 Mn1 C19 64.25(8) . . ? C18 Mn1 C19 38.69(7) . . ? C16 Mn1 C20 142.64(8) . . ? C15 Mn1 C20 91.01(8) . . ? C17 Mn1 C20 64.03(9) . . ? C21 Mn1 C20 38.29(8) . . ? C18 Mn1 C20 64.27(8) . . ? C19 Mn1 C20 37.96(8) . . ? C16 Mn1 P1 92.92(5) . . ? C15 Mn1 P1 93.49(6) . . ? C17 Mn1 P1 127.79(7) . . ? C21 Mn1 P1 155.97(6) . . ? C18 Mn1 P1 93.76(6) . . ? C19 Mn1 P1 92.40(5) . . ? C20 Mn1 P1 123.98(6) . . ? C2 P1 C1 43.08(8) . . ? C2 P1 C9 107.55(8) . . ? C1 P1 C9 106.94(7) . . ? C2 P1 Mn1 125.97(6) . . ? C1 P1 Mn1 125.48(5) . . ? C9 P1 Mn1 122.51(5) . . ? C2 C1 C3 144.93(16) . . ? C2 C1 P1 67.99(11) . . ? C3 C1 P1 146.94(12) . . ? C1 C2 P1 68.93(10) . . ? C1 C2 H2 142.6(13) . . ? P1 C2 H2 148.5(13) . . ? C8 C3 C4 119.14(16) . . ? C8 C3 C1 120.47(15) . . ? C4 C3 C1 120.39(15) . . ? C5 C4 C3 120.21(18) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 120.13(18) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.22(19) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 120.2(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 120.08(18) . . ? C7 C8 H8 120.0 . . ? C3 C8 H8 120.0 . . ? C10 C9 C14 118.37(15) . . ? C10 C9 P1 121.13(13) . . ? C14 C9 P1 120.49(12) . . ? C11 C10 C9 120.75(16) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.45(17) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 119.48(16) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.31(16) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 120.62(16) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O1 C15 Mn1 177.53(15) . . ? O2 C16 Mn1 177.26(15) . . ? C21 C17 C18 108.52(19) . . ? C21 C17 Mn1 71.03(11) . . ? C18 C17 Mn1 70.95(10) . . ? C21 C17 H17 129.0(15) . . ? C18 C17 H17 122.4(15) . . ? Mn1 C17 H17 120.9(15) . . ? C17 C18 C19 107.0(2) . . ? C17 C18 Mn1 70.27(11) . . ? C19 C18 Mn1 70.98(10) . . ? C17 C18 H18 127.5(12) . . ? C19 C18 H18 125.4(12) . . ? Mn1 C18 H18 122.3(12) . . ? C20 C19 C18 108.15(18) . . ? C20 C19 Mn1 71.15(11) . . ? C18 C19 Mn1 70.33(10) . . ? C20 C19 H19 125.0(12) . . ? C18 C19 H19 126.8(12) . . ? Mn1 C19 H19 122.1(12) . . ? C19 C20 C21 108.7(2) . . ? C19 C20 Mn1 70.89(11) . . ? C21 C20 Mn1 70.30(11) . . ? C19 C20 H20 126.9(12) . . ? C21 C20 H20 124.5(12) . . ? Mn1 C20 H20 124.7(12) . . ? C17 C21 C20 107.69(19) . . ? C17 C21 Mn1 70.53(11) . . ? C20 C21 Mn1 71.41(11) . . ? C17 C21 H21 125.4(13) . . ? C20 C21 H21 126.6(13) . . ? Mn1 C21 H21 119.0(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 C16 Mn1 P1 C2 107.05(9) . . . . ? C15 Mn1 P1 C2 -160.28(10) . . . . ? C17 Mn1 P1 C2 14.92(11) . . . . ? C21 Mn1 P1 C2 -31.06(19) . . . . ? C18 Mn1 P1 C2 -5.40(10) . . . . ? C19 Mn1 P1 C2 -44.13(9) . . . . ? C20 Mn1 P1 C2 -66.70(11) . . . . ? C16 Mn1 P1 C1 160.82(8) . . . . ? C15 Mn1 P1 C1 -106.50(9) . . . . ? C17 Mn1 P1 C1 68.70(10) . . . . ? C21 Mn1 P1 C1 22.71(18) . . . . ? C18 Mn1 P1 C1 48.37(9) . . . . ? C19 Mn1 P1 C1 9.65(9) . . . . ? C20 Mn1 P1 C1 -12.92(10) . . . . ? C16 Mn1 P1 C9 -47.71(8) . . . . ? C15 Mn1 P1 C9 44.96(9) . . . . ? C17 Mn1 P1 C9 -139.84(10) . . . . ? C21 Mn1 P1 C9 174.18(18) . . . . ? C18 Mn1 P1 C9 -160.16(8) . . . . ? C19 Mn1 P1 C9 161.11(8) . . . . ? C20 Mn1 P1 C9 138.54(9) . . . . ? C9 P1 C1 C2 97.81(11) . . . . ? Mn1 P1 C1 C2 -107.09(10) . . . . ? C2 P1 C1 C3 175.8(3) . . . . ? C9 P1 C1 C3 -86.4(2) . . . . ? Mn1 P1 C1 C3 68.7(2) . . . . ? C3 C1 C2 P1 -176.0(3) . . . . ? C9 P1 C2 C1 -96.27(11) . . . . ? Mn1 P1 C2 C1 105.89(10) . . . . ? C2 C1 C3 C8 -174.2(2) . . . . ? P1 C1 C3 C8 12.6(3) . . . . ? C2 C1 C3 C4 5.6(3) . . . . ? P1 C1 C3 C4 -167.59(17) . . . . ? C8 C3 C4 C5 0.4(2) . . . . ? C1 C3 C4 C5 -179.42(15) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C5 C6 C7 C8 0.0(3) . . . . ? C6 C7 C8 C3 0.2(3) . . . . ? C4 C3 C8 C7 -0.4(3) . . . . ? C1 C3 C8 C7 179.38(17) . . . . ? C2 P1 C9 C10 20.28(16) . . . . ? C1 P1 C9 C10 -24.94(15) . . . . ? Mn1 P1 C9 C10 179.06(11) . . . . ? C2 P1 C9 C14 -160.77(14) . . . . ? C1 P1 C9 C14 154.01(13) . . . . ? Mn1 P1 C9 C14 -1.99(16) . . . . ? C14 C9 C10 C11 -0.5(3) . . . . ? P1 C9 C10 C11 178.46(14) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C12 C13 C14 C9 0.3(3) . . . . ? C10 C9 C14 C13 0.2(2) . . . . ? P1 C9 C14 C13 -178.78(13) . . . . ? C16 Mn1 C17 C21 114.49(13) . . . . ? C15 Mn1 C17 C21 20.87(19) . . . . ? C18 Mn1 C17 C21 -118.29(19) . . . . ? C19 Mn1 C17 C21 -80.11(13) . . . . ? C20 Mn1 C17 C21 -37.76(12) . . . . ? P1 Mn1 C17 C21 -151.90(11) . . . . ? C16 Mn1 C17 C18 -127.22(14) . . . . ? C15 Mn1 C17 C18 139.16(14) . . . . ? C21 Mn1 C17 C18 118.29(19) . . . . ? C19 Mn1 C17 C18 38.18(12) . . . . ? C20 Mn1 C17 C18 80.53(14) . . . . ? P1 Mn1 C17 C18 -33.61(16) . . . . ? C21 C17 C18 C19 -0.4(2) . . . . ? Mn1 C17 C18 C19 -61.87(12) . . . . ? C21 C17 C18 Mn1 61.42(13) . . . . ? C16 Mn1 C18 C17 59.31(15) . . . . ? C15 Mn1 C18 C17 -100.2(2) . . . . ? C21 Mn1 C18 C17 -37.24(13) . . . . ? C19 Mn1 C18 C17 -116.86(19) . . . . ? C20 Mn1 C18 C17 -79.84(15) . . . . ? P1 Mn1 C18 C17 154.00(13) . . . . ? C16 Mn1 C18 C19 176.17(11) . . . . ? C15 Mn1 C18 C19 16.7(2) . . . . ? C17 Mn1 C18 C19 116.86(19) . . . . ? C21 Mn1 C18 C19 79.62(13) . . . . ? C20 Mn1 C18 C19 37.02(12) . . . . ? P1 Mn1 C18 C19 -89.14(11) . . . . ? C17 C18 C19 C20 0.0(2) . . . . ? Mn1 C18 C19 C20 -61.43(13) . . . . ? C17 C18 C19 Mn1 61.41(12) . . . . ? C16 Mn1 C19 C20 110.87(17) . . . . ? C15 Mn1 C19 C20 -53.78(14) . . . . ? C17 Mn1 C19 C20 79.87(14) . . . . ? C21 Mn1 C19 C20 37.03(13) . . . . ? C18 Mn1 C19 C20 118.14(17) . . . . ? P1 Mn1 C19 C20 -148.84(11) . . . . ? C16 Mn1 C19 C18 -7.3(2) . . . . ? C15 Mn1 C19 C18 -171.92(12) . . . . ? C17 Mn1 C19 C18 -38.27(13) . . . . ? C21 Mn1 C19 C18 -81.11(14) . . . . ? C20 Mn1 C19 C18 -118.14(17) . . . . ? P1 Mn1 C19 C18 93.03(12) . . . . ? C18 C19 C20 C21 0.5(2) . . . . ? Mn1 C19 C20 C21 -60.42(13) . . . . ? C18 C19 C20 Mn1 60.91(12) . . . . ? C16 Mn1 C20 C19 -131.10(13) . . . . ? C15 Mn1 C20 C19 133.47(12) . . . . ? C17 Mn1 C20 C19 -81.01(13) . . . . ? C21 Mn1 C20 C19 -118.92(18) . . . . ? C18 Mn1 C20 C19 -37.73(12) . . . . ? P1 Mn1 C20 C19 38.57(14) . . . . ? C16 Mn1 C20 C21 -12.2(2) . . . . ? C15 Mn1 C20 C21 -107.61(14) . . . . ? C17 Mn1 C20 C21 37.91(13) . . . . ? C18 Mn1 C20 C21 81.20(14) . . . . ? C19 Mn1 C20 C21 118.92(18) . . . . ? P1 Mn1 C20 C21 157.49(11) . . . . ? C18 C17 C21 C20 0.7(2) . . . . ? Mn1 C17 C21 C20 62.12(13) . . . . ? C18 C17 C21 Mn1 -61.38(13) . . . . ? C19 C20 C21 C17 -0.8(2) . . . . ? Mn1 C20 C21 C17 -61.55(13) . . . . ? C19 C20 C21 Mn1 60.79(13) . . . . ? C16 Mn1 C21 C17 -70.29(13) . . . . ? C15 Mn1 C21 C17 -166.05(13) . . . . ? C18 Mn1 C21 C17 37.56(12) . . . . ? C19 Mn1 C21 C17 80.61(13) . . . . ? C20 Mn1 C21 C17 117.32(18) . . . . ? P1 Mn1 C21 C17 66.1(2) . . . . ? C16 Mn1 C21 C20 172.39(13) . . . . ? C15 Mn1 C21 C20 76.63(14) . . . . ? C17 Mn1 C21 C20 -117.32(18) . . . . ? C18 Mn1 C21 C20 -79.76(14) . . . . ? C19 Mn1 C21 C20 -36.71(12) . . . . ? P1 Mn1 C21 C20 -51.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.428 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.050 #===END