Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'P. G. Edwards' ;School of Chemistry Cardiff University Cardiff, CF10 3AT ; 'Paul Newman' ;School of Chemistry Cardiff University Cardiff, CF10 3AT ; 'Li-ling Ooi.' '' 'Andreas Stasch' '' 'Huw A. Tallis' '' _publ_contact_author_name 'P. G. Edwards' _publ_contact_author_address ; School of Chemistry Cardiff University Main College Building Park Place Cardiff CF10 3AT UNITED KINGDOM ; _publ_contact_author_email EDWARDSPG@CARDIFF.AC.UK _publ_section_title ; 1-Trimethylsilylphosphirane as a ligand and as a stable masked reagent for phosphirane ; _publ_contact_author_fax '+44 (0)29 20874030' _publ_contact_author_phone '+44 (0)29 20874083' data_compound_3b _database_code_depnum_ccdc_archive 'CCDC 663023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H39 Cr O3 P3 Si3' _chemical_formula_weight 532.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.875(2) _cell_length_b 14.883(3) _cell_length_c 17.718(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.86(3) _cell_angle_gamma 90.00 _cell_volume 2847.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 11429 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6157 _reflns_number_gt 4805 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. One methyl group was modelled as disordered over two positions, C16 and C16A. ; _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^)+(0.0239P)^2^+1.4832P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6157 _refine_ls_number_parameters 273 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.010 _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 Cr1 Cr 0.61308(3) 0.30018(2) 0.234954(18) 0.02433(10) Uani 1 1 d . . . P1 P 0.70610(5) 0.39679(4) 0.15041(3) 0.02696(14) Uani 1 1 d . . . Si1 Si 0.75504(6) 0.34882(5) 0.03641(4) 0.03189(16) Uani 1 1 d . . . O1 O 0.86505(16) 0.21753(11) 0.27339(9) 0.0408(4) Uani 1 1 d . . . C1 C 0.7683(2) 0.25093(15) 0.25953(12) 0.0287(5) Uani 1 1 d . . . P2 P 0.64599(6) 0.40448(4) 0.33704(3) 0.02850(14) Uani 1 1 d . . . Si2 Si 0.78636(6) 0.38151(5) 0.44013(4) 0.03268(16) Uani 1 1 d . . . O2 O 0.51452(17) 0.17055(12) 0.34300(10) 0.0495(5) Uani 1 1 d . . . C2 C 0.5512(2) 0.22233(16) 0.30183(13) 0.0331(5) Uani 1 1 d . . . P3 P 0.41433(5) 0.36150(4) 0.19726(3) 0.02849(14) Uani 1 1 d . A . Si3 Si 0.23758(7) 0.30390(6) 0.23201(4) 0.0475(2) Uani 1 1 d D . . O3 O 0.55471(18) 0.15509(12) 0.11850(10) 0.0520(5) Uani 1 1 d . . . C3 C 0.5785(2) 0.21349(16) 0.16171(13) 0.0335(5) Uani 1 1 d . . . C4 C 0.6927(2) 0.51972(16) 0.13409(15) 0.0397(6) Uani 1 1 d . . . H4A H 0.6941 0.5413 0.0813 0.048 Uiso 1 1 calc R . . H4B H 0.6352 0.5531 0.1632 0.048 Uiso 1 1 calc R . . C5 C 0.8137(2) 0.48998(16) 0.17660(15) 0.0410(6) Uani 1 1 d . . . H5A H 0.8291 0.5059 0.2312 0.049 Uiso 1 1 calc R . . H5B H 0.8880 0.4940 0.1494 0.049 Uiso 1 1 calc R . . C6 C 0.8655(2) 0.42732(18) -0.00246(14) 0.0439(7) Uani 1 1 d . . . H6A H 0.8734 0.4112 -0.0553 0.066 Uiso 1 1 calc R . . H6B H 0.9466 0.4230 0.0280 0.066 Uiso 1 1 calc R . . H6C H 0.8344 0.4890 -0.0005 0.066 Uiso 1 1 calc R . . C7 C 0.8265(3) 0.23521(18) 0.04887(14) 0.0472(7) Uani 1 1 d . . . H7A H 0.7624 0.1910 0.0567 0.071 Uiso 1 1 calc R . . H7B H 0.8898 0.2356 0.0931 0.071 Uiso 1 1 calc R . . H7C H 0.8647 0.2193 0.0033 0.071 Uiso 1 1 calc R . . C8 C 0.6049(2) 0.34448(19) -0.02658(14) 0.0437(6) Uani 1 1 d . . . H8A H 0.6199 0.3262 -0.0778 0.066 Uiso 1 1 calc R . . H8B H 0.5662 0.4040 -0.0288 0.066 Uiso 1 1 calc R . . H8C H 0.5498 0.3010 -0.0063 0.066 Uiso 1 1 calc R . . C9 C 0.6269(3) 0.52729(18) 0.33708(16) 0.0568(8) Uani 1 1 d . . . H9A H 0.6880 0.5623 0.3710 0.068 Uiso 1 1 calc R . . H9B H 0.6006 0.5564 0.2875 0.068 Uiso 1 1 calc R . . C10 C 0.5310(3) 0.4779(2) 0.37313(15) 0.0558(9) Uani 1 1 d . . . H10A H 0.4462 0.4771 0.3456 0.067 Uiso 1 1 calc R . . H10B H 0.5336 0.4830 0.4290 0.067 Uiso 1 1 calc R . . C11 C 0.7659(3) 0.26449(18) 0.47227(14) 0.0466(7) Uani 1 1 d . . . H11A H 0.7826 0.2227 0.4320 0.070 Uiso 1 1 calc R . . H11B H 0.6807 0.2562 0.4838 0.070 Uiso 1 1 calc R . . H11C H 0.8237 0.2527 0.5180 0.070 Uiso 1 1 calc R . . C12 C 0.7617(3) 0.46147(19) 0.51796(14) 0.0506(7) Uani 1 1 d . . . H12A H 0.8280 0.4541 0.5601 0.076 Uiso 1 1 calc R . . H12B H 0.6816 0.4492 0.5359 0.076 Uiso 1 1 calc R . . H12C H 0.7625 0.5232 0.4988 0.076 Uiso 1 1 calc R . . C13 C 0.9420(2) 0.3988(2) 0.40926(16) 0.0510(7) Uani 1 1 d . . . H13A H 0.9493 0.4609 0.3920 0.077 Uiso 1 1 calc R . . H13B H 0.9530 0.3575 0.3675 0.077 Uiso 1 1 calc R . . H13C H 1.0058 0.3870 0.4520 0.077 Uiso 1 1 calc R . . C14 C 0.3697(2) 0.47903(16) 0.17397(13) 0.0372(6) Uani 1 1 d . . . H14A H 0.2899 0.5002 0.1891 0.045 Uiso 1 1 calc R A . H14B H 0.4365 0.5246 0.1797 0.045 Uiso 1 1 calc R . . C15 C 0.3641(2) 0.41808(16) 0.10635(13) 0.0365(6) Uani 1 1 d . A . H15A H 0.4274 0.4271 0.0713 0.044 Uiso 1 1 calc R . . H15B H 0.2809 0.4027 0.0807 0.044 Uiso 1 1 calc R . . C17 C 0.2317(3) 0.1829(2) 0.2075(2) 0.0792(11) Uani 1 1 d D A . H17A H 0.3001 0.1515 0.2376 0.119 Uiso 1 1 calc R . . H17B H 0.2394 0.1755 0.1533 0.119 Uiso 1 1 calc R . . H17C H 0.1527 0.1575 0.2186 0.119 Uiso 1 1 calc R . . C18 C 0.2452(3) 0.3202(3) 0.33590(17) 0.0783(11) Uani 1 1 d D A . H18A H 0.1726 0.2925 0.3543 0.117 Uiso 1 1 calc R . . H18B H 0.2462 0.3847 0.3474 0.117 Uiso 1 1 calc R . . H18C H 0.3207 0.2922 0.3611 0.117 Uiso 1 1 calc R . . C16A C 0.1023(6) 0.3472(8) 0.1691(6) 0.052(2) Uani 0.51(2) 1 d PDU A 2 H16A H 0.0258 0.3257 0.1872 0.078 Uiso 0.51(2) 1 calc PR A 2 H16B H 0.1060 0.3258 0.1171 0.078 Uiso 0.51(2) 1 calc PR A 2 H16C H 0.1034 0.4131 0.1697 0.078 Uiso 0.51(2) 1 calc PR A 2 C16 C 0.0999(6) 0.3775(7) 0.1967(7) 0.049(3) Uani 0.49(2) 1 d PDU A 1 H16D H 0.0240 0.3507 0.2114 0.073 Uiso 0.49(2) 1 calc PR A 1 H16E H 0.0932 0.3823 0.1412 0.073 Uiso 0.49(2) 1 calc PR A 1 H16F H 0.1114 0.4375 0.2193 0.073 Uiso 0.49(2) 1 calc PR A 1 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 Cr1 0.0283(2) 0.01909(19) 0.02580(19) 0.00085(14) 0.00419(14) 0.00095(15) P1 0.0292(3) 0.0207(3) 0.0312(3) 0.0015(2) 0.0046(2) -0.0018(2) Si1 0.0375(4) 0.0282(4) 0.0310(3) 0.0062(3) 0.0086(3) 0.0020(3) O1 0.0368(10) 0.0340(10) 0.0520(11) 0.0010(8) 0.0071(8) 0.0100(8) C1 0.0356(13) 0.0215(12) 0.0296(12) -0.0001(9) 0.0066(10) -0.0003(10) P2 0.0325(3) 0.0246(3) 0.0279(3) -0.0024(2) 0.0016(2) 0.0064(3) Si2 0.0323(4) 0.0324(4) 0.0321(4) -0.0028(3) -0.0010(3) 0.0068(3) O2 0.0527(12) 0.0411(11) 0.0582(12) 0.0236(9) 0.0211(9) 0.0052(9) C2 0.0343(13) 0.0275(13) 0.0382(13) 0.0013(11) 0.0071(10) 0.0058(10) P3 0.0286(3) 0.0286(3) 0.0280(3) 0.0043(2) 0.0022(2) 0.0002(3) Si3 0.0311(4) 0.0596(5) 0.0518(5) 0.0214(4) 0.0051(3) -0.0040(4) O3 0.0662(13) 0.0379(11) 0.0518(11) -0.0186(9) 0.0060(9) -0.0126(10) C3 0.0367(14) 0.0269(13) 0.0372(13) 0.0015(11) 0.0061(10) -0.0035(10) C4 0.0472(16) 0.0207(12) 0.0524(15) 0.0025(11) 0.0114(12) -0.0005(11) C5 0.0419(15) 0.0325(14) 0.0483(15) -0.0039(12) 0.0037(11) -0.0100(12) C6 0.0377(14) 0.0487(17) 0.0475(15) 0.0183(13) 0.0135(11) 0.0052(13) C7 0.0664(19) 0.0383(16) 0.0389(14) 0.0033(12) 0.0146(13) 0.0133(14) C8 0.0492(16) 0.0430(16) 0.0387(14) 0.0019(12) 0.0037(12) -0.0034(13) C9 0.090(2) 0.0319(16) 0.0435(16) -0.0060(13) -0.0100(15) 0.0176(16) C10 0.0532(18) 0.070(2) 0.0407(15) -0.0226(15) -0.0079(13) 0.0366(16) C11 0.0546(17) 0.0425(16) 0.0406(15) 0.0081(12) -0.0037(12) 0.0071(14) C12 0.0563(18) 0.0520(18) 0.0397(15) -0.0116(13) -0.0100(12) 0.0155(14) C13 0.0351(15) 0.0567(19) 0.0597(18) -0.0023(15) -0.0007(13) 0.0000(13) C14 0.0358(14) 0.0316(14) 0.0439(14) 0.0044(11) 0.0039(11) 0.0080(11) C15 0.0373(14) 0.0378(15) 0.0342(13) 0.0090(11) 0.0039(10) 0.0056(11) C17 0.077(2) 0.072(3) 0.090(3) 0.009(2) 0.0142(19) -0.039(2) C18 0.064(2) 0.115(3) 0.063(2) 0.017(2) 0.0357(17) 0.012(2) C16A 0.046(3) 0.055(3) 0.054(3) 0.0001(18) 0.0042(17) 0.0000(17) C16 0.044(3) 0.051(3) 0.051(3) 0.0020(18) 0.0043(17) 0.0010(17) _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 Cr1 C3 1.837(2) . ? Cr1 C2 1.841(2) . ? Cr1 C1 1.844(2) . ? Cr1 P3 2.3677(8) . ? Cr1 P2 2.3779(8) . ? Cr1 P1 2.3868(8) . ? P1 C5 1.838(2) . ? P1 C4 1.855(2) . ? P1 Si1 2.2648(10) . ? Si1 C7 1.863(3) . ? Si1 C8 1.865(3) . ? Si1 C6 1.865(3) . ? O1 C1 1.163(3) . ? P2 C10 1.833(3) . ? P2 C9 1.840(3) . ? P2 Si2 2.2621(11) . ? Si2 C11 1.854(3) . ? Si2 C13 1.858(3) . ? Si2 C12 1.865(3) . ? O2 C2 1.164(3) . ? P3 C15 1.842(2) . ? P3 C14 1.849(2) . ? P3 Si3 2.2564(10) . ? Si3 C18 1.849(3) . ? Si3 C16A 1.852(6) . ? Si3 C17 1.852(4) . ? Si3 C16 1.900(7) . ? O3 C3 1.167(3) . ? C4 C5 1.503(3) . ? C9 C10 1.482(4) . ? C14 C15 1.498(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Cr1 C2 87.30(10) . . ? C3 Cr1 C1 89.54(10) . . ? C2 Cr1 C1 89.56(10) . . ? C3 Cr1 P3 88.20(8) . . ? C2 Cr1 P3 91.87(8) . . ? C1 Cr1 P3 177.26(7) . . ? C3 Cr1 P2 174.55(8) . . ? C2 Cr1 P2 87.40(8) . . ? C1 Cr1 P2 91.69(7) . . ? P3 Cr1 P2 90.70(3) . . ? C3 Cr1 P1 92.64(8) . . ? C2 Cr1 P1 176.29(8) . . ? C1 Cr1 P1 86.73(7) . . ? P3 Cr1 P1 91.83(3) . . ? P2 Cr1 P1 92.73(3) . . ? C5 P1 C4 48.02(11) . . ? C5 P1 Si1 104.63(9) . . ? C4 P1 Si1 101.21(9) . . ? C5 P1 Cr1 126.94(9) . . ? C4 P1 Cr1 131.33(9) . . ? Si1 P1 Cr1 122.16(3) . . ? C7 Si1 C8 111.23(13) . . ? C7 Si1 C6 109.54(12) . . ? C8 Si1 C6 110.91(12) . . ? C7 Si1 P1 108.63(8) . . ? C8 Si1 P1 105.21(9) . . ? C6 Si1 P1 111.24(10) . . ? O1 C1 Cr1 177.7(2) . . ? C10 P2 C9 47.60(14) . . ? C10 P2 Si2 103.37(9) . . ? C9 P2 Si2 102.43(9) . . ? C10 P2 Cr1 127.42(9) . . ? C9 P2 Cr1 129.95(9) . . ? Si2 P2 Cr1 122.77(3) . . ? C11 Si2 C13 111.55(13) . . ? C11 Si2 C12 109.83(13) . . ? C13 Si2 C12 110.25(14) . . ? C11 Si2 P2 107.21(9) . . ? C13 Si2 P2 106.98(9) . . ? C12 Si2 P2 110.95(9) . . ? O2 C2 Cr1 177.5(2) . . ? C15 P3 C14 47.90(10) . . ? C15 P3 Si3 103.84(9) . . ? C14 P3 Si3 102.19(9) . . ? C15 P3 Cr1 126.03(9) . . ? C14 P3 Cr1 129.34(9) . . ? Si3 P3 Cr1 123.74(4) . . ? C18 Si3 C16A 119.4(4) . . ? C18 Si3 C17 110.94(17) . . ? C16A Si3 C17 101.2(4) . . ? C18 Si3 C16 101.1(4) . . ? C16A Si3 C16 20.4(2) . . ? C17 Si3 C16 118.7(4) . . ? C18 Si3 P3 106.47(12) . . ? C16A Si3 P3 110.2(2) . . ? C17 Si3 P3 108.18(12) . . ? C16 Si3 P3 110.8(2) . . ? O3 C3 Cr1 176.0(2) . . ? C5 C4 P1 65.40(13) . . ? C4 C5 P1 66.59(13) . . ? C10 C9 P2 65.96(15) . . ? C9 C10 P2 66.44(15) . . ? C15 C14 P3 65.80(13) . . ? C14 C15 P3 66.29(12) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.414 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.058 # Attachment 'B715327A cmpd_4a.cif' data_compound_4a _database_code_depnum_ccdc_archive 'CCDC 663024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pge0703 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H15 Mo O3 P3' _chemical_formula_weight 360.06 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5870(4) _cell_length_b 8.2520(3) _cell_length_c 13.8730(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.499(1) _cell_angle_gamma 90.00 _cell_volume 1439.59(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 31095 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7239 _exptl_absorpt_correction_T_max 0.7905 _exptl_absorpt_process_details 'Sortav (Blessing,1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20472 _diffrn_reflns_av_R_equivalents 0.1391 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3278 _reflns_number_gt 2806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997' _computing_structure_solution ' Dirdiff-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-99 for Windows (Farrugia, 1995)' _computing_publication_material 'WinGX publication routines (Farrugia, 1995)' _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^)+(0.0268P)^2^+2.4740P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3278 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.24787(2) -0.01649(4) -0.13656(2) 0.01854(11) Uani 1 1 d . . . P1 P 0.13029(8) -0.25712(12) -0.16269(8) 0.0271(2) Uani 1 1 d . . . H1A H 0.0612 -0.2404 -0.1311 0.032 Uiso 1 1 calc R . . P2 P 0.19826(8) 0.08759(12) -0.30182(8) 0.0228(2) Uani 1 1 d . . . H2A H 0.1749 0.2032 -0.2985 0.027 Uiso 1 1 calc R . . P3 P 0.39870(8) -0.17637(12) -0.19800(8) 0.0256(2) Uani 1 1 d . . . H3A H 0.3947 -0.1905 -0.2697 0.031 Uiso 1 1 calc R . . C1 C 0.3446(3) 0.1702(4) -0.1156(3) 0.0231(8) Uani 1 1 d . . . C2 C 0.1300(3) 0.1058(4) -0.0791(3) 0.0249(8) Uani 1 1 d . . . C3 C 0.2878(3) -0.0950(5) -0.0060(3) 0.0266(8) Uani 1 1 d . . . C4 C 0.1150(4) -0.4059(5) -0.2590(4) 0.0419(11) Uani 1 1 d . . . H4A H 0.0416 -0.4402 -0.2780 0.050 Uiso 1 1 calc R . . H4B H 0.1624 -0.3953 -0.3137 0.050 Uiso 1 1 calc R . . C5 C 0.1621(4) -0.4725(5) -0.1679(4) 0.0427(12) Uani 1 1 d . . . H5A H 0.2383 -0.5023 -0.1670 0.051 Uiso 1 1 calc R . . H5B H 0.1175 -0.5472 -0.1312 0.051 Uiso 1 1 calc R . . C6 C 0.1383(3) -0.0107(5) -0.4096(3) 0.0282(9) Uani 1 1 d . . . H6A H 0.1256 -0.1289 -0.4061 0.034 Uiso 1 1 calc R . . H6B H 0.0820 0.0500 -0.4464 0.034 Uiso 1 1 calc R . . C7 C 0.2509(3) 0.0442(6) -0.4197(3) 0.0336(10) Uani 1 1 d . . . H7A H 0.2625 0.1377 -0.4627 0.040 Uiso 1 1 calc R . . H7B H 0.3061 -0.0411 -0.4224 0.040 Uiso 1 1 calc R . . C8 C 0.5341(3) -0.1799(5) -0.1462(4) 0.0378(11) Uani 1 1 d . . . H8A H 0.5925 -0.1797 -0.1918 0.045 Uiso 1 1 calc R . . H8B H 0.5489 -0.1144 -0.0873 0.045 Uiso 1 1 calc R . . C9 C 0.4749(4) -0.3359(6) -0.1346(5) 0.0478(13) Uani 1 1 d . . . H9A H 0.4538 -0.3643 -0.0688 0.057 Uiso 1 1 calc R . . H9B H 0.4974 -0.4296 -0.1733 0.057 Uiso 1 1 calc R . . O1 O 0.4023(2) 0.2774(4) -0.1026(2) 0.0374(7) Uani 1 1 d . . . O2 O 0.0629(2) 0.1742(4) -0.0438(3) 0.0397(8) Uani 1 1 d . . . O3 O 0.3105(3) -0.1363(4) 0.0717(2) 0.0488(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01716(17) 0.01936(18) 0.01912(18) -0.00103(12) 0.00101(12) -0.00018(11) P1 0.0224(5) 0.0265(5) 0.0326(6) -0.0029(4) 0.0047(4) -0.0041(4) P2 0.0222(5) 0.0227(5) 0.0232(5) 0.0013(4) -0.0012(4) 0.0001(4) P3 0.0195(5) 0.0305(5) 0.0265(6) -0.0061(4) -0.0017(4) 0.0021(4) C1 0.0215(18) 0.0255(19) 0.022(2) -0.0039(15) 0.0023(15) 0.0008(14) C2 0.026(2) 0.0246(19) 0.024(2) -0.0021(16) 0.0032(16) -0.0025(15) C3 0.0236(19) 0.027(2) 0.029(2) 0.0014(17) -0.0016(16) -0.0032(15) C4 0.057(3) 0.034(2) 0.035(3) -0.006(2) 0.001(2) -0.010(2) C5 0.056(3) 0.025(2) 0.046(3) 0.002(2) -0.015(2) -0.004(2) C6 0.029(2) 0.032(2) 0.024(2) 0.0005(16) -0.0042(16) -0.0030(16) C7 0.031(2) 0.051(3) 0.020(2) 0.0031(19) 0.0045(17) -0.0030(19) C8 0.024(2) 0.041(2) 0.049(3) -0.008(2) -0.0059(19) 0.0024(18) C9 0.037(3) 0.036(3) 0.070(4) 0.004(2) -0.002(2) 0.012(2) O1 0.0365(17) 0.0359(16) 0.0402(19) -0.0042(14) 0.0068(14) -0.0144(13) O2 0.0340(17) 0.0384(17) 0.048(2) -0.0127(15) 0.0141(15) 0.0053(13) O3 0.059(2) 0.055(2) 0.031(2) 0.0146(16) -0.0151(16) -0.0121(17) _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 C3 1.968(4) . ? Mo1 C1 1.978(4) . ? Mo1 C2 1.989(4) . ? Mo1 P3 2.4925(10) . ? Mo1 P1 2.4936(10) . ? Mo1 P2 2.5017(11) . ? P1 C4 1.819(5) . ? P1 C5 1.824(4) . ? P2 C7 1.827(4) . ? P2 C6 1.835(4) . ? P3 C8 1.821(4) . ? P3 C9 1.831(5) . ? C1 O1 1.154(4) . ? C2 O2 1.144(5) . ? C3 O3 1.155(5) . ? C4 C5 1.478(7) . ? C6 C7 1.501(6) . ? C8 C9 1.500(6) . ? 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 C3 Mo1 C1 89.42(16) . . ? C3 Mo1 C2 87.89(16) . . ? C1 Mo1 C2 90.64(15) . . ? C3 Mo1 P3 88.43(12) . . ? C1 Mo1 P3 89.38(11) . . ? C2 Mo1 P3 176.32(12) . . ? C3 Mo1 P1 89.87(11) . . ? C1 Mo1 P1 178.38(11) . . ? C2 Mo1 P1 90.79(11) . . ? P3 Mo1 P1 89.13(3) . . ? C3 Mo1 P2 179.10(11) . . ? C1 Mo1 P2 89.72(12) . . ? C2 Mo1 P2 91.86(12) . . ? P3 Mo1 P2 91.82(4) . . ? P1 Mo1 P2 90.99(4) . . ? C4 P1 C5 47.9(2) . . ? C4 P1 Mo1 133.43(17) . . ? C5 P1 Mo1 130.67(17) . . ? C7 P2 C6 48.41(18) . . ? C7 P2 Mo1 131.85(15) . . ? C6 P2 Mo1 132.28(14) . . ? C8 P3 C9 48.5(2) . . ? C8 P3 Mo1 125.96(16) . . ? C9 P3 Mo1 127.4(2) . . ? O1 C1 Mo1 178.9(4) . . ? O2 C2 Mo1 178.2(4) . . ? O3 C3 Mo1 177.8(4) . . ? C5 C4 P1 66.2(3) . . ? C4 C5 P1 65.9(2) . . ? C7 C6 P2 65.5(2) . . ? C6 C7 P2 66.1(2) . . ? C9 C8 P3 66.1(2) . . ? C8 C9 P3 65.4(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 C3 Mo1 P1 C4 -130.3(3) . . . . ? C1 Mo1 P1 C4 -66(4) . . . . ? C2 Mo1 P1 C4 141.8(3) . . . . ? P3 Mo1 P1 C4 -41.9(2) . . . . ? P2 Mo1 P1 C4 49.9(2) . . . . ? C3 Mo1 P1 C5 -64.2(3) . . . . ? C1 Mo1 P1 C5 0(4) . . . . ? C2 Mo1 P1 C5 -152.1(3) . . . . ? P3 Mo1 P1 C5 24.2(2) . . . . ? P2 Mo1 P1 C5 116.1(2) . . . . ? C3 Mo1 P2 C7 110(8) . . . . ? C1 Mo1 P2 C7 93.3(2) . . . . ? C2 Mo1 P2 C7 -176.1(2) . . . . ? P3 Mo1 P2 C7 3.9(2) . . . . ? P1 Mo1 P2 C7 -85.3(2) . . . . ? C3 Mo1 P2 C6 177(100) . . . . ? C1 Mo1 P2 C6 160.3(2) . . . . ? C2 Mo1 P2 C6 -109.0(2) . . . . ? P3 Mo1 P2 C6 70.95(19) . . . . ? P1 Mo1 P2 C6 -18.22(19) . . . . ? C3 Mo1 P3 C8 -47.2(2) . . . . ? C1 Mo1 P3 C8 42.2(2) . . . . ? C2 Mo1 P3 C8 -48.3(17) . . . . ? P1 Mo1 P3 C8 -137.1(2) . . . . ? P2 Mo1 P3 C8 131.9(2) . . . . ? C3 Mo1 P3 C9 14.4(2) . . . . ? C1 Mo1 P3 C9 103.8(2) . . . . ? C2 Mo1 P3 C9 13.3(17) . . . . ? P1 Mo1 P3 C9 -75.5(2) . . . . ? P2 Mo1 P3 C9 -166.5(2) . . . . ? C3 Mo1 C1 O1 43(20) . . . . ? C2 Mo1 C1 O1 131(20) . . . . ? P3 Mo1 C1 O1 -45(20) . . . . ? P1 Mo1 C1 O1 -21(23) . . . . ? P2 Mo1 C1 O1 -137(20) . . . . ? C3 Mo1 C2 O2 -5(11) . . . . ? C1 Mo1 C2 O2 -94(11) . . . . ? P3 Mo1 C2 O2 -4(13) . . . . ? P1 Mo1 C2 O2 85(11) . . . . ? P2 Mo1 C2 O2 176(100) . . . . ? C1 Mo1 C3 O3 52(10) . . . . ? C2 Mo1 C3 O3 -39(10) . . . . ? P3 Mo1 C3 O3 141(10) . . . . ? P1 Mo1 C3 O3 -130(10) . . . . ? P2 Mo1 C3 O3 35(16) . . . . ? Mo1 P1 C4 C5 110.7(3) . . . . ? Mo1 P1 C5 C4 -116.4(3) . . . . ? Mo1 P2 C6 C7 -113.5(2) . . . . ? Mo1 P2 C7 C6 114.4(2) . . . . ? Mo1 P3 C8 C9 111.1(3) . . . . ? Mo1 P3 C9 C8 -108.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.594 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.143