# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1469 data_mm9904 #COMPOUND 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H19 Mo2 O4 P' _chemical_formula_weight 570.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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 8.278(3) _cell_length_b 14.908(6) _cell_length_c 16.694(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.97(3) _cell_angle_gamma 90.00 _cell_volume 2057.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R ' _diffrn_measurement_method 'omega/2 theta ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5467 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3631 _reflns_number_gt 2960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku control software' _computing_cell_refinement 'Rigaku control software' _computing_data_reduction Texsan _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^)+(0.1163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3631 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 1.06075(6) 0.14903(4) 0.79629(3) 0.0177(2) Uani 1 1 d . . . Mo2 Mo 0.96775(7) 0.28177(4) 0.64727(3) 0.0199(2) Uani 1 1 d . . . P1 P 1.03861(19) 0.12941(12) 0.65133(10) 0.0188(4) Uani 1 1 d . . . C21 C 1.2259(8) 0.0942(5) 0.6943(4) 0.0253(16) Uani 1 1 d . . . H21A H 1.2355 0.0274 0.6956 0.030 Uiso 1 1 calc R . . C22 C 1.3822(8) 0.1388(6) 0.6726(5) 0.0340(19) Uani 1 1 d . . . H22A H 1.4302 0.1050 0.6294 0.051 Uiso 1 1 calc R . . H22B H 1.4578 0.1401 0.7197 0.051 Uiso 1 1 calc R . . H22C H 1.3598 0.2003 0.6545 0.051 Uiso 1 1 calc R . . C1 C 0.9307(8) 0.0295(5) 0.6157(4) 0.0218(14) Uani 1 1 d . . . C2 C 0.7608(8) 0.0322(5) 0.6044(4) 0.0256(15) Uani 1 1 d . . . H2A H 0.7037 0.0852 0.6171 0.031 Uiso 1 1 calc R . . C3 C 0.6777(11) -0.0410(6) 0.5750(5) 0.041(2) Uani 1 1 d . . . H3A H 0.5631 -0.0387 0.5680 0.049 Uiso 1 1 calc R . . C4 C 0.7576(12) -0.1173(6) 0.5556(5) 0.045(2) Uani 1 1 d . . . H4A H 0.6988 -0.1676 0.5348 0.054 Uiso 1 1 calc R . . C5 C 0.9234(12) -0.1216(6) 0.5663(5) 0.039(2) Uani 1 1 d . . . H5A H 0.9784 -0.1754 0.5541 0.047 Uiso 1 1 calc R . . C6 C 1.0106(9) -0.0476(5) 0.5947(4) 0.0283(16) Uani 1 1 d . . . H6A H 1.1254 -0.0501 0.5997 0.034 Uiso 1 1 calc R . . C7 C 0.7961(9) 0.2469(5) 0.5711(5) 0.0292(16) Uani 1 1 d . . . O7 O 0.6887(8) 0.2307(4) 0.5253(4) 0.0535(18) Uani 1 1 d . . . C8 C 0.7752(9) 0.2934(5) 0.7125(4) 0.0296(17) Uani 1 1 d . . . O8 O 0.6584(6) 0.3024(4) 0.7452(3) 0.0410(14) Uani 1 1 d . . . C9 C 1.0842(9) 0.2770(5) 0.8184(4) 0.0258(16) Uani 1 1 d . . . O9 O 1.1039(7) 0.3483(4) 0.8472(3) 0.0352(13) Uani 1 1 d . . . C10 C 1.2894(9) 0.1538(5) 0.8330(4) 0.0264(16) Uani 1 1 d . . . O10 O 1.4210(6) 0.1583(4) 0.8577(4) 0.0436(15) Uani 1 1 d . . . C11 C 1.2076(10) 0.3384(6) 0.5922(5) 0.038(2) Uani 1 1 d . . . H11A H 1.2877 0.3002 0.5719 0.046 Uiso 1 1 calc R . . C12 C 1.0718(11) 0.3727(6) 0.5483(5) 0.0366(19) Uani 1 1 d . . . H12A H 1.0437 0.3618 0.4933 0.044 Uiso 1 1 calc R . . C13 C 0.9838(11) 0.4269(5) 0.6012(5) 0.0360(18) Uani 1 1 d . . . H13A H 0.8863 0.4584 0.5877 0.043 Uiso 1 1 calc R . . C14 C 1.0653(10) 0.4257(5) 0.6759(5) 0.0355(18) Uani 1 1 d . . . H14A H 1.0333 0.4567 0.7222 0.043 Uiso 1 1 calc R . . C15 C 1.2041(10) 0.3707(5) 0.6720(5) 0.0322(18) Uani 1 1 d . . . H15A H 1.2806 0.3578 0.7148 0.039 Uiso 1 1 calc R . . C16 C 0.8268(9) 0.1422(6) 0.8693(5) 0.0318(18) Uani 1 1 d . . . H16A H 0.7601 0.1933 0.8754 0.038 Uiso 1 1 calc R . . C17 C 0.9606(9) 0.1184(6) 0.9194(4) 0.0291(16) Uani 1 1 d . . . H17A H 1.0023 0.1511 0.9647 0.035 Uiso 1 1 calc R . . C18 C 1.0235(9) 0.0360(5) 0.8902(4) 0.0321(18) Uani 1 1 d . . . H18A H 1.1137 0.0040 0.9131 0.039 Uiso 1 1 calc R . . C19 C 0.9281(10) 0.0104(6) 0.8212(5) 0.040(2) Uani 1 1 d . . . H19A H 0.9422 -0.0417 0.7896 0.048 Uiso 1 1 calc R . . C20 C 0.8081(9) 0.0768(6) 0.8080(4) 0.0343(19) Uani 1 1 d . . . H20A H 0.7280 0.0774 0.7652 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0106(3) 0.0242(4) 0.0185(3) -0.0005(2) 0.0008(2) -0.0003(2) Mo2 0.0195(3) 0.0195(4) 0.0207(3) 0.0000(2) 0.0011(2) -0.0007(2) P1 0.0123(8) 0.0234(9) 0.0207(8) -0.0028(7) 0.0004(6) 0.0023(7) C21 0.013(3) 0.036(4) 0.027(4) -0.005(3) 0.002(3) 0.010(3) C22 0.012(3) 0.059(6) 0.031(4) 0.002(4) 0.003(3) 0.007(3) C1 0.020(3) 0.029(4) 0.016(3) -0.003(3) 0.000(3) -0.005(3) C2 0.025(4) 0.027(4) 0.025(3) 0.003(3) -0.002(3) 0.000(3) C3 0.038(5) 0.042(5) 0.041(5) 0.007(4) -0.009(4) -0.018(4) C4 0.071(6) 0.028(5) 0.035(5) 0.002(4) -0.010(4) -0.018(5) C5 0.066(6) 0.022(4) 0.029(4) -0.005(3) 0.007(4) -0.002(4) C6 0.035(4) 0.024(4) 0.026(4) -0.005(3) 0.003(3) 0.006(3) C7 0.036(4) 0.017(4) 0.034(4) 0.008(3) -0.003(3) 0.009(3) O7 0.054(4) 0.048(4) 0.055(4) 0.007(3) -0.033(3) 0.001(3) C8 0.025(4) 0.034(4) 0.029(4) -0.007(3) -0.004(3) 0.005(3) O8 0.028(3) 0.046(4) 0.051(4) 0.002(3) 0.018(3) 0.008(3) C9 0.023(4) 0.034(4) 0.020(3) 0.003(3) 0.001(3) -0.001(3) O9 0.046(3) 0.029(3) 0.030(3) -0.007(2) 0.004(2) -0.006(3) C10 0.029(4) 0.024(4) 0.026(4) 0.003(3) 0.001(3) 0.003(3) O10 0.017(3) 0.069(4) 0.043(3) 0.001(3) -0.011(2) 0.000(3) C11 0.039(5) 0.037(5) 0.041(5) -0.004(4) 0.018(4) -0.013(4) C12 0.055(5) 0.031(4) 0.025(4) 0.005(3) 0.008(4) -0.010(4) C13 0.049(5) 0.021(4) 0.038(4) 0.005(3) 0.003(4) -0.009(4) C14 0.050(5) 0.027(4) 0.031(4) 0.000(3) 0.011(4) -0.009(4) C15 0.038(4) 0.024(4) 0.035(4) 0.004(3) 0.004(3) -0.019(3) C16 0.018(4) 0.043(5) 0.035(4) 0.006(3) 0.017(3) 0.003(3) C17 0.027(4) 0.037(4) 0.024(4) 0.001(3) 0.008(3) -0.011(3) C18 0.028(4) 0.038(5) 0.031(4) 0.015(3) 0.008(3) 0.005(3) C19 0.042(5) 0.032(5) 0.049(5) -0.006(4) 0.028(4) -0.010(4) C20 0.021(4) 0.051(5) 0.031(4) 0.012(4) 0.002(3) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C9 1.951(8) . ? Mo1 C10 1.960(8) . ? Mo1 C17 2.301(7) . ? Mo1 C18 2.332(7) . ? Mo1 C16 2.343(7) . ? Mo1 C20 2.370(7) . ? Mo1 C21 2.382(7) . ? Mo1 C19 2.386(8) . ? Mo1 P1 2.435(2) . ? Mo1 Mo2 3.2403(12) . ? Mo2 C7 1.928(8) . ? Mo2 C8 1.984(8) . ? Mo2 C13 2.302(8) . ? Mo2 C14 2.333(8) . ? Mo2 C12 2.336(8) . ? Mo2 P1 2.346(2) . ? Mo2 C15 2.381(7) . ? Mo2 C11 2.385(8) . ? P1 C21 1.754(7) . ? P1 C1 1.821(7) . ? C21 C22 1.516(10) . ? C1 C6 1.381(10) . ? C1 C2 1.410(9) . ? C2 C3 1.368(11) . ? C3 C4 1.363(13) . ? C4 C5 1.376(14) . ? C5 C6 1.388(11) . ? C7 O7 1.167(9) . ? C8 O8 1.143(9) . ? C9 O9 1.174(9) . ? C10 O10 1.146(9) . ? C11 C12 1.406(12) . ? C11 C15 1.418(11) . ? C12 C13 1.425(12) . ? C13 C14 1.387(11) . ? C14 C15 1.416(12) . ? C16 C17 1.398(11) . ? C16 C20 1.416(12) . ? C17 C18 1.429(11) . ? C18 C19 1.415(12) . ? C19 C20 1.411(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Mo1 C10 79.6(3) . . ? C9 Mo1 C17 93.6(3) . . ? C10 Mo1 C17 96.6(3) . . ? C9 Mo1 C18 126.5(3) . . ? C10 Mo1 C18 88.6(3) . . ? C17 Mo1 C18 35.9(3) . . ? C9 Mo1 C16 91.2(3) . . ? C10 Mo1 C16 130.5(3) . . ? C17 Mo1 C16 35.0(3) . . ? C18 Mo1 C16 58.5(3) . . ? C9 Mo1 C20 120.6(3) . . ? C10 Mo1 C20 146.4(3) . . ? C17 Mo1 C20 58.4(3) . . ? C18 Mo1 C20 57.9(3) . . ? C16 Mo1 C20 35.0(3) . . ? C9 Mo1 C21 114.5(3) . . ? C10 Mo1 C21 69.8(3) . . ? C17 Mo1 C21 144.8(3) . . ? C18 Mo1 C21 109.5(3) . . ? C16 Mo1 C21 151.3(3) . . ? C20 Mo1 C21 116.4(3) . . ? C9 Mo1 C19 148.9(3) . . ? C10 Mo1 C19 115.0(3) . . ? C17 Mo1 C19 58.8(3) . . ? C18 Mo1 C19 34.9(3) . . ? C16 Mo1 C19 58.1(3) . . ? C20 Mo1 C19 34.5(3) . . ? C21 Mo1 C19 96.5(3) . . ? C9 Mo1 P1 107.9(2) . . ? C10 Mo1 P1 109.7(2) . . ? C17 Mo1 P1 148.38(19) . . ? C18 Mo1 P1 125.1(2) . . ? C16 Mo1 P1 119.3(2) . . ? C20 Mo1 P1 90.35(19) . . ? C21 Mo1 P1 42.69(16) . . ? C19 Mo1 P1 93.3(2) . . ? C9 Mo1 Mo2 64.2(2) . . ? C10 Mo1 Mo2 113.9(2) . . ? C17 Mo1 Mo2 136.4(2) . . ? C18 Mo1 Mo2 157.31(19) . . ? C16 Mo1 Mo2 104.8(2) . . ? C20 Mo1 Mo2 99.52(19) . . ? C21 Mo1 Mo2 77.46(18) . . ? C19 Mo1 Mo2 124.7(2) . . ? P1 Mo1 Mo2 46.19(5) . . ? C7 Mo2 C8 78.4(3) . . ? C7 Mo2 C13 95.0(3) . . ? C8 Mo2 C13 99.4(3) . . ? C7 Mo2 C14 128.2(3) . . ? C8 Mo2 C14 95.0(3) . . ? C13 Mo2 C14 34.8(3) . . ? C7 Mo2 C12 88.6(3) . . ? C8 Mo2 C12 132.3(3) . . ? C13 Mo2 C12 35.8(3) . . ? C14 Mo2 C12 58.3(3) . . ? C7 Mo2 P1 86.1(2) . . ? C8 Mo2 P1 106.0(2) . . ? C13 Mo2 P1 154.3(2) . . ? C14 Mo2 P1 143.2(2) . . ? C12 Mo2 P1 118.8(2) . . ? C7 Mo2 C15 146.6(3) . . ? C8 Mo2 C15 122.2(3) . . ? C13 Mo2 C15 58.3(3) . . ? C14 Mo2 C15 34.9(3) . . ? C12 Mo2 C15 58.0(3) . . ? P1 Mo2 C15 109.4(2) . . ? C7 Mo2 C11 116.2(3) . . ? C8 Mo2 C11 152.8(3) . . ? C13 Mo2 C11 58.4(3) . . ? C14 Mo2 C11 57.8(3) . . ? C12 Mo2 C11 34.6(3) . . ? P1 Mo2 C11 98.1(2) . . ? C15 Mo2 C11 34.6(3) . . ? C7 Mo2 Mo1 118.6(2) . . ? C8 Mo2 Mo1 78.3(2) . . ? C13 Mo2 Mo1 144.6(2) . . ? C14 Mo2 Mo1 109.8(2) . . ? C12 Mo2 Mo1 144.7(2) . . ? P1 Mo2 Mo1 48.50(5) . . ? C15 Mo2 Mo1 92.7(2) . . ? C11 Mo2 Mo1 110.0(2) . . ? C21 P1 C1 107.3(4) . . ? C21 P1 Mo2 121.0(3) . . ? C1 P1 Mo2 131.7(2) . . ? C21 P1 Mo1 67.1(2) . . ? C1 P1 Mo1 115.7(2) . . ? Mo2 P1 Mo1 85.31(6) . . ? C22 C21 P1 121.2(6) . . ? C22 C21 Mo1 123.3(5) . . ? P1 C21 Mo1 70.3(2) . . ? C6 C1 C2 118.6(7) . . ? C6 C1 P1 122.0(5) . . ? C2 C1 P1 119.3(5) . . ? C3 C2 C1 120.3(7) . . ? C4 C3 C2 120.7(8) . . ? C3 C4 C5 120.1(8) . . ? C4 C5 C6 120.3(8) . . ? C1 C6 C5 120.0(7) . . ? O7 C7 Mo2 176.1(7) . . ? O8 C8 Mo2 175.1(7) . . ? O9 C9 Mo1 166.6(6) . . ? O10 C10 Mo1 176.8(7) . . ? C12 C11 C15 108.1(8) . . ? C12 C11 Mo2 70.8(4) . . ? C15 C11 Mo2 72.5(4) . . ? C11 C12 C13 107.7(7) . . ? C11 C12 Mo2 74.6(4) . . ? C13 C12 Mo2 70.8(4) . . ? C14 C13 C12 108.0(8) . . ? C14 C13 Mo2 73.8(5) . . ? C12 C13 Mo2 73.4(4) . . ? C13 C14 C15 108.9(7) . . ? C13 C14 Mo2 71.4(5) . . ? C15 C14 Mo2 74.4(4) . . ? C14 C15 C11 107.2(7) . . ? C14 C15 Mo2 70.7(4) . . ? C11 C15 Mo2 72.8(4) . . ? C17 C16 C20 108.1(7) . . ? C17 C16 Mo1 70.8(4) . . ? C20 C16 Mo1 73.6(4) . . ? C16 C17 C18 107.8(7) . . ? C16 C17 Mo1 74.1(4) . . ? C18 C17 Mo1 73.2(4) . . ? C19 C18 C17 108.2(7) . . ? C19 C18 Mo1 74.7(4) . . ? C17 C18 Mo1 70.8(4) . . ? C20 C19 C18 107.3(7) . . ? C20 C19 Mo1 72.1(5) . . ? C18 C19 Mo1 70.5(4) . . ? C19 C20 C16 108.7(7) . . ? C19 C20 Mo1 73.4(4) . . ? C16 C20 Mo1 71.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.753 _refine_diff_density_min -2.112 _refine_diff_density_rms 0.202 #*************************************************************************** #END OF DATA FOR COMPOUND 2 #*************************************************************************** data_mm9914 # compound 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H19 Mo2 O4 P' _chemical_formula_weight 570.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.615(3) _cell_length_b 14.568(4) _cell_length_c 15.191(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2127.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.279 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8313 _exptl_absorpt_correction_T_max 0.8616 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 4861 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4861 _reflns_number_gt 4648 _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. ; _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^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 4861 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 Mo2 Mo 0.62333(3) 0.113979(17) 0.650742(16) 0.02777(8) Uani 1 1 d . . . Mo1 Mo 0.91746(3) 0.065420(17) 0.740723(16) 0.02826(8) Uani 1 1 d . . . P1 P 0.79805(8) 0.01078(5) 0.61084(5) 0.02566(15) Uani 1 1 d . . . O7 O 0.4209(3) -0.0439(2) 0.6027(2) 0.0602(8) Uani 1 1 d . . . C7 C 0.4996(3) 0.0135(3) 0.6206(2) 0.0418(8) Uani 1 1 d . . . O8 O 0.5140(3) 0.0444(2) 0.83193(17) 0.0549(7) Uani 1 1 d . . . C8 C 0.5591(3) 0.0709(2) 0.7665(2) 0.0363(7) Uani 1 1 d . . . O10 O 1.1413(3) 0.20489(19) 0.68055(19) 0.0531(7) Uani 1 1 d . . . C10 C 1.0571(4) 0.1532(2) 0.7027(2) 0.0376(7) Uani 1 1 d . . . O9 O 0.7963(3) 0.24719(18) 0.81430(17) 0.0528(7) Uani 1 1 d . . . C9 C 0.8288(4) 0.1797(2) 0.7797(2) 0.0391(7) Uani 1 1 d . . . C11 C 0.6675(4) 0.2173(3) 0.5336(2) 0.0441(8) Uani 1 1 d . . . H11 H 0.7292 0.2022 0.4870 0.053 Uiso 1 1 calc R . . C15 C 0.7034(4) 0.2638(2) 0.6110(3) 0.0426(8) Uani 1 1 d . . . H15 H 0.7933 0.2861 0.6257 0.051 Uiso 1 1 calc R . . C14 C 0.5818(4) 0.2716(2) 0.6637(3) 0.0484(9) Uani 1 1 d . . . H14 H 0.5761 0.2991 0.7203 0.058 Uiso 1 1 calc R . . C13 C 0.4713(4) 0.2311(3) 0.6167(3) 0.0540(11) Uani 1 1 d . . . H13 H 0.3773 0.2275 0.6357 0.065 Uiso 1 1 calc R . . C12 C 0.5243(4) 0.1968(3) 0.5364(3) 0.0512(10) Uani 1 1 d . . . H12 H 0.4727 0.1655 0.4923 0.061 Uiso 1 1 calc R . . C20 C 0.8621(5) -0.0697(3) 0.8219(3) 0.0565(10) Uani 1 1 d . . . H20 H 0.7793 -0.1039 0.8125 0.068 Uiso 1 1 calc R . . C19 C 0.9853(7) -0.0843(3) 0.7798(3) 0.0699(14) Uani 1 1 d . . . H19 H 1.0019 -0.1294 0.7358 0.084 Uiso 1 1 calc R . . C18 C 1.0835(5) -0.0215(6) 0.8124(5) 0.111(3) Uani 1 1 d . . . H18 H 1.1785 -0.0159 0.7961 0.133 Uiso 1 1 calc R . . C17 C 1.0068(8) 0.0331(4) 0.8767(4) 0.090(2) Uani 1 1 d . . . H17 H 1.0428 0.0824 0.9108 0.108 Uiso 1 1 calc R . . C16 C 0.8751(6) 0.0005(3) 0.8789(3) 0.0685(14) Uani 1 1 d . . . H16 H 0.8027 0.0237 0.9152 0.082 Uiso 1 1 calc R . . C22 C 1.0899(3) 0.0096(3) 0.5563(2) 0.0461(8) Uani 1 1 d . . . H22A H 1.0892 0.0032 0.4920 0.069 Uiso 1 1 calc R . . H22B H 1.0929 -0.0515 0.5834 0.069 Uiso 1 1 calc R . . H22C H 1.1719 0.0448 0.5743 0.069 Uiso 1 1 calc R . . C21 C 0.9597(3) 0.0591(2) 0.58566(19) 0.0327(6) Uani 1 1 d . . . H21 H 0.9503 0.1207 0.5572 0.039 Uiso 1 1 calc R . . C1 C 0.7866(3) -0.1121(2) 0.59171(19) 0.0313(6) Uani 1 1 d . . . C2 C 0.6943(4) -0.1620(2) 0.6416(2) 0.0406(7) Uani 1 1 d . . . H2 H 0.6447 -0.1330 0.6880 0.049 Uiso 1 1 calc R . . C3 C 0.6733(5) -0.2550(3) 0.6243(3) 0.0554(10) Uani 1 1 d . . . H3 H 0.6105 -0.2894 0.6596 0.066 Uiso 1 1 calc R . . C4 C 0.7416(5) -0.2963(3) 0.5577(3) 0.0599(12) Uani 1 1 d . . . H4 H 0.7258 -0.3594 0.5456 0.072 Uiso 1 1 calc R . . C5 C 0.8349(5) -0.2468(3) 0.5066(3) 0.0561(11) Uani 1 1 d . . . H5 H 0.8842 -0.2765 0.4605 0.067 Uiso 1 1 calc R . . C6 C 0.8565(4) -0.1543(2) 0.5227(2) 0.0417(8) Uani 1 1 d . . . H6 H 0.9186 -0.1201 0.4868 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo2 0.02334(12) 0.02959(13) 0.03039(13) 0.00205(9) 0.00364(9) 0.00232(10) Mo1 0.02945(13) 0.02719(13) 0.02814(12) 0.00039(9) -0.00322(10) -0.00228(10) P1 0.0233(3) 0.0275(4) 0.0262(3) -0.0017(3) 0.0017(3) -0.0002(3) O7 0.0356(13) 0.0624(18) 0.083(2) -0.0141(15) -0.0081(14) -0.0105(13) C7 0.0262(15) 0.051(2) 0.0480(19) -0.0049(16) 0.0005(14) 0.0007(15) O8 0.0656(17) 0.0553(16) 0.0436(14) 0.0048(12) 0.0236(14) -0.0020(14) C8 0.0348(16) 0.0351(16) 0.0391(16) -0.0018(13) 0.0118(14) 0.0002(14) O10 0.0434(14) 0.0500(15) 0.0658(16) -0.0055(13) 0.0067(13) -0.0174(13) C10 0.0340(16) 0.0347(16) 0.0439(16) -0.0081(13) -0.0021(14) -0.0021(14) O9 0.0709(18) 0.0403(14) 0.0474(15) -0.0111(12) 0.0074(14) 0.0022(14) C9 0.0431(18) 0.0382(18) 0.0360(16) -0.0005(13) 0.0031(15) -0.0007(15) C11 0.0428(18) 0.051(2) 0.0386(17) 0.0166(16) 0.0041(15) 0.0104(17) C15 0.0400(18) 0.0344(18) 0.054(2) 0.0137(15) 0.0060(17) 0.0050(15) C14 0.056(2) 0.0346(17) 0.054(2) 0.0064(15) 0.0153(19) 0.0125(17) C13 0.0328(18) 0.053(2) 0.076(3) 0.023(2) 0.0106(19) 0.0177(17) C12 0.0370(18) 0.064(2) 0.053(2) 0.023(2) -0.0101(17) 0.0061(18) C20 0.066(3) 0.048(2) 0.056(2) 0.0254(19) -0.015(2) -0.007(2) C19 0.112(4) 0.045(2) 0.053(2) 0.0151(19) 0.005(3) 0.030(3) C18 0.040(2) 0.148(6) 0.145(6) 0.109(6) -0.014(3) 0.008(3) C17 0.138(6) 0.061(3) 0.072(3) 0.022(3) -0.074(4) -0.034(3) C16 0.113(4) 0.060(3) 0.0329(18) 0.0164(18) 0.006(2) 0.018(3) C22 0.0321(17) 0.057(2) 0.049(2) -0.0071(16) 0.0046(16) 0.0055(16) C21 0.0254(13) 0.0441(18) 0.0285(13) -0.0017(13) 0.0031(11) -0.0052(13) C1 0.0352(15) 0.0306(15) 0.0281(13) -0.0027(11) -0.0072(12) 0.0010(14) C2 0.0419(17) 0.0346(17) 0.0452(18) -0.0017(14) -0.0068(15) -0.0069(14) C3 0.061(2) 0.0350(19) 0.070(3) 0.0006(18) -0.024(2) -0.0163(18) C4 0.069(3) 0.0286(17) 0.082(3) -0.0103(19) -0.038(3) 0.0026(19) C5 0.067(3) 0.044(2) 0.058(2) -0.0241(17) -0.022(2) 0.018(2) C6 0.050(2) 0.0354(18) 0.0397(16) -0.0069(14) -0.0027(16) 0.0089(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo2 C7 1.941(4) . ? Mo2 C8 1.967(3) . ? Mo2 C13 2.306(4) . ? Mo2 C12 2.319(3) . ? Mo2 P1 2.3345(9) . ? Mo2 C14 2.339(4) . ? Mo2 C11 2.369(3) . ? Mo2 C15 2.391(4) . ? Mo2 Mo1 3.2198(9) . ? Mo1 C10 1.942(3) . ? Mo1 C9 1.961(4) . ? Mo1 C17 2.287(4) . ? Mo1 C18 2.310(4) . ? Mo1 C16 2.338(4) . ? Mo1 C19 2.353(4) . ? Mo1 C20 2.383(4) . ? Mo1 C21 2.392(3) . ? Mo1 P1 2.4176(9) . ? P1 C21 1.749(3) . ? P1 C1 1.817(3) . ? O7 C7 1.160(5) . ? O8 C8 1.151(4) . ? O10 C10 1.156(4) . ? O9 C9 1.158(4) . ? C11 C15 1.399(6) . ? C11 C12 1.410(6) . ? C15 C14 1.422(5) . ? C14 C13 1.410(6) . ? C13 C12 1.413(6) . ? C20 C16 1.346(7) . ? C20 C19 1.363(7) . ? C19 C18 1.405(9) . ? C18 C17 1.461(9) . ? C17 C16 1.353(8) . ? C22 C21 1.512(5) . ? C1 C2 1.375(5) . ? C1 C6 1.389(5) . ? C2 C3 1.395(5) . ? C3 C4 1.349(6) . ? C4 C5 1.388(7) . ? C5 C6 1.385(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 C7 Mo2 C8 77.14(15) . . ? C7 Mo2 C13 96.69(16) . . ? C8 Mo2 C13 103.75(15) . . ? C7 Mo2 C12 87.93(16) . . ? C8 Mo2 C12 134.97(14) . . ? C13 Mo2 C12 35.59(15) . . ? C7 Mo2 P1 83.93(11) . . ? C8 Mo2 P1 104.62(10) . . ? C13 Mo2 P1 151.01(11) . . ? C12 Mo2 P1 115.85(11) . . ? C7 Mo2 C14 130.97(15) . . ? C8 Mo2 C14 100.64(14) . . ? C13 Mo2 C14 35.34(16) . . ? C12 Mo2 C14 58.84(16) . . ? P1 Mo2 C14 140.98(10) . . ? C7 Mo2 C11 114.33(16) . . ? C8 Mo2 C11 158.55(14) . . ? C13 Mo2 C11 58.33(13) . . ? C12 Mo2 C11 34.98(14) . . ? P1 Mo2 C11 94.89(10) . . ? C14 Mo2 C11 58.00(14) . . ? C7 Mo2 C15 145.69(15) . . ? C8 Mo2 C15 128.19(13) . . ? C13 Mo2 C15 58.16(14) . . ? C12 Mo2 C15 57.90(15) . . ? P1 Mo2 C15 106.87(9) . . ? C14 Mo2 C15 34.97(13) . . ? C11 Mo2 C15 34.19(14) . . ? C7 Mo2 Mo1 118.21(11) . . ? C8 Mo2 Mo1 79.98(10) . . ? C13 Mo2 Mo1 144.57(12) . . ? C12 Mo2 Mo1 142.47(10) . . ? P1 Mo2 Mo1 48.45(2) . . ? C14 Mo2 Mo1 109.25(11) . . ? C11 Mo2 Mo1 107.53(10) . . ? C15 Mo2 Mo1 91.42(9) . . ? C10 Mo1 C9 80.31(15) . . ? C10 Mo1 C17 98.33(19) . . ? C9 Mo1 C17 93.7(2) . . ? C10 Mo1 C18 91.35(18) . . ? C9 Mo1 C18 128.6(3) . . ? C17 Mo1 C18 37.0(2) . . ? C10 Mo1 C16 130.84(18) . . ? C9 Mo1 C16 89.79(16) . . ? C17 Mo1 C16 34.0(2) . . ? C18 Mo1 C16 58.4(2) . . ? C10 Mo1 C19 119.60(19) . . ? C9 Mo1 C19 146.21(16) . . ? C17 Mo1 C19 58.48(19) . . ? C18 Mo1 C19 35.1(2) . . ? C16 Mo1 C19 56.43(17) . . ? C10 Mo1 C20 148.46(15) . . ? C9 Mo1 C20 116.58(16) . . ? C17 Mo1 C20 56.37(16) . . ? C18 Mo1 C20 57.15(18) . . ? C16 Mo1 C20 33.11(16) . . ? C19 Mo1 C20 33.45(18) . . ? C10 Mo1 C21 67.33(12) . . ? C9 Mo1 C21 113.80(13) . . ? C17 Mo1 C21 144.9(2) . . ? C18 Mo1 C21 109.0(2) . . ? C16 Mo1 C21 153.93(15) . . ? C19 Mo1 C21 99.53(15) . . ? C20 Mo1 C21 121.07(14) . . ? C10 Mo1 P1 107.59(10) . . ? C9 Mo1 P1 108.63(10) . . ? C17 Mo1 P1 148.00(14) . . ? C18 Mo1 P1 122.1(3) . . ? C16 Mo1 P1 121.13(15) . . ? C19 Mo1 P1 91.83(14) . . ? C20 Mo1 P1 92.55(10) . . ? C21 Mo1 P1 42.64(8) . . ? C10 Mo1 Mo2 109.65(10) . . ? C9 Mo1 Mo2 63.90(10) . . ? C17 Mo1 Mo2 139.4(2) . . ? C18 Mo1 Mo2 158.02(18) . . ? C16 Mo1 Mo2 108.48(15) . . ? C19 Mo1 Mo2 123.65(16) . . ? C20 Mo1 Mo2 101.83(11) . . ? C21 Mo1 Mo2 74.91(8) . . ? P1 Mo1 Mo2 46.27(2) . . ? C21 P1 C1 114.56(16) . . ? C21 P1 Mo2 115.92(12) . . ? C1 P1 Mo2 129.23(11) . . ? C21 P1 Mo1 67.90(10) . . ? C1 P1 Mo1 118.92(10) . . ? Mo2 P1 Mo1 85.28(3) . . ? O7 C7 Mo2 177.0(3) . . ? O8 C8 Mo2 175.9(3) . . ? O10 C10 Mo1 179.2(3) . . ? O9 C9 Mo1 167.2(3) . . ? C15 C11 C12 108.6(4) . . ? C15 C11 Mo2 73.8(2) . . ? C12 C11 Mo2 70.6(2) . . ? C11 C15 C14 108.0(4) . . ? C11 C15 Mo2 72.0(2) . . ? C14 C15 Mo2 70.5(2) . . ? C13 C14 C15 107.5(4) . . ? C13 C14 Mo2 71.1(2) . . ? C15 C14 Mo2 74.5(2) . . ? C14 C13 C12 108.3(3) . . ? C14 C13 Mo2 73.6(2) . . ? C12 C13 Mo2 72.7(2) . . ? C11 C12 C13 107.6(4) . . ? C11 C12 Mo2 74.4(2) . . ? C13 C12 Mo2 71.7(2) . . ? C16 C20 C19 109.9(5) . . ? C16 C20 Mo1 71.6(2) . . ? C19 C20 Mo1 72.1(2) . . ? C20 C19 C18 108.4(5) . . ? C20 C19 Mo1 74.5(3) . . ? C18 C19 Mo1 70.8(3) . . ? C19 C18 C17 104.6(4) . . ? C19 C18 Mo1 74.1(3) . . ? C17 C18 Mo1 70.6(3) . . ? C16 C17 C18 107.3(5) . . ? C16 C17 Mo1 75.1(3) . . ? C18 C17 Mo1 72.4(3) . . ? C20 C16 C17 109.7(5) . . ? C20 C16 Mo1 75.3(2) . . ? C17 C16 Mo1 70.9(3) . . ? C22 C21 P1 127.4(3) . . ? C22 C21 Mo1 116.7(2) . . ? P1 C21 Mo1 69.46(10) . . ? C2 C1 C6 119.7(3) . . ? C2 C1 P1 118.1(2) . . ? C6 C1 P1 121.8(3) . . ? C1 C2 C3 120.2(4) . . ? C4 C3 C2 120.3(4) . . ? C3 C4 C5 120.2(4) . . ? C6 C5 C4 120.2(4) . . ? C5 C6 C1 119.4(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.557 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.167 #************************************************************************* # END OF DATA FOR COMPOUND 3 #************************************************************************** data_mm9917 # COMPOUND 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 Mo2 O4 P' _chemical_formula_weight 646.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3040(10) _cell_length_b 9.9780(10) _cell_length_c 16.0240(10) _cell_angle_alpha 94.190(10) _cell_angle_beta 102.920(10) _cell_angle_gamma 106.260(10) _cell_volume 1229.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8963 _exptl_absorpt_correction_T_max 0.9672 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 8409 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5582 _reflns_number_gt 3928 _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. ; _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^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5582 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.174 _refine_ls_shift/su_mean 0.005 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 -0.25043(4) 0.42448(3) 0.727383(17) 0.02289(10) Uani 1 1 d . . . Mo2 Mo -0.13024(4) 0.18064(3) 0.630800(17) 0.02470(10) Uani 1 1 d . . . P1 P 0.04826(12) 0.43160(9) 0.77692(5) 0.0209(2) Uani 1 1 d . . . O1 O -0.2034(4) 0.4861(3) 0.92544(16) 0.0426(7) Uani 1 1 d . . . C1 C -0.2140(5) 0.4641(4) 0.8521(2) 0.0283(9) Uani 1 1 d . . . O2 O -0.5130(4) 0.1741(3) 0.77685(19) 0.0572(9) Uani 1 1 d . . . C2 C -0.4112(5) 0.2634(4) 0.7571(2) 0.0320(9) Uani 1 1 d . . . O3 O -0.2027(4) 0.2210(3) 0.43809(16) 0.0507(8) Uani 1 1 d . . . C3 C -0.1720(5) 0.2065(4) 0.5104(2) 0.0328(9) Uani 1 1 d . . . O4 O -0.5132(4) 0.1704(3) 0.57507(18) 0.0594(9) Uani 1 1 d . . . C4 C -0.3656(6) 0.1991(4) 0.6062(2) 0.0367(10) Uani 1 1 d . . . C5 C -0.3976(7) 0.5863(5) 0.7092(3) 0.0550(13) Uani 1 1 d . . . H5A H -0.4654 0.5971 0.7483 0.066 Uiso 1 1 calc R . . C6 C -0.4548(6) 0.4946(5) 0.6308(3) 0.0549(13) Uani 1 1 d . . . H6A H -0.5686 0.4318 0.6073 0.066 Uiso 1 1 calc R . . C7 C -0.3151(6) 0.5116(5) 0.5933(2) 0.0427(11) Uani 1 1 d . . . H7 H -0.3182 0.4618 0.5399 0.051 Uiso 1 1 calc R . . C8 C -0.1699(6) 0.6138(4) 0.6473(2) 0.0396(10) Uani 1 1 d . . . H8 H -0.0580 0.6460 0.6370 0.048 Uiso 1 1 calc R . . C9 C -0.2207(7) 0.6598(4) 0.7194(3) 0.0496(12) Uani 1 1 d . . . H9 H -0.1482 0.7287 0.7670 0.060 Uiso 1 1 calc R . . C10 C -0.0046(6) 0.0439(4) 0.7248(2) 0.0388(11) Uani 1 1 d . . . H10 H 0.0859 0.0861 0.7755 0.047 Uiso 1 1 calc R . . C11 C -0.1807(6) 0.0048(4) 0.7198(2) 0.0384(10) Uani 1 1 d . . . H11 H -0.2315 0.0163 0.7663 0.046 Uiso 1 1 calc R . . C12 C -0.2720(6) -0.0554(4) 0.6332(2) 0.0444(11) Uani 1 1 d . . . H12 H -0.3944 -0.0917 0.6116 0.053 Uiso 1 1 calc R . . C13 C -0.1495(6) -0.0516(4) 0.5855(2) 0.0434(12) Uani 1 1 d . . . H13 H -0.1747 -0.0850 0.5255 0.052 Uiso 1 1 calc R . . C14 C 0.0178(6) 0.0101(4) 0.6411(2) 0.0377(10) Uani 1 1 d . . . H14 H 0.1250 0.0261 0.6257 0.045 Uiso 1 1 calc R . . C15 C 0.0714(5) 0.3804(4) 0.6062(2) 0.0303(9) Uani 1 1 d . . . H15A H -0.0047 0.4350 0.5902 0.036 Uiso 1 1 calc R . . H15B H 0.1138 0.3397 0.5635 0.036 Uiso 1 1 calc R . . C16 C 0.1213(5) 0.3596(3) 0.69305(19) 0.0242(8) Uani 1 1 d . . . H16 H 0.2297 0.3324 0.7109 0.029 Uiso 1 1 calc R . . C17 C 0.1838(5) 0.6162(3) 0.8141(2) 0.0229(8) Uani 1 1 d . . . C18 C 0.2606(5) 0.6982(4) 0.7593(2) 0.0273(9) Uani 1 1 d . . . H18 H 0.2553 0.6556 0.7033 0.033 Uiso 1 1 calc R . . C19 C 0.3446(5) 0.8402(4) 0.7840(2) 0.0326(9) Uani 1 1 d . . . H19 H 0.3957 0.8948 0.7451 0.039 Uiso 1 1 calc R . . C20 C 0.3548(5) 0.9037(4) 0.8660(2) 0.0352(10) Uani 1 1 d . . . H20 H 0.4125 1.0017 0.8835 0.042 Uiso 1 1 calc R . . C21 C 0.2805(5) 0.8233(4) 0.9213(2) 0.0313(9) Uani 1 1 d . . . H21 H 0.2885 0.8661 0.9776 0.038 Uiso 1 1 calc R . . C22 C 0.1945(5) 0.6810(4) 0.8963(2) 0.0293(9) Uani 1 1 d . . . H22 H 0.1423 0.6271 0.9351 0.035 Uiso 1 1 calc R . . C23 C 0.1272(5) 0.3457(3) 0.86776(19) 0.0217(8) Uani 1 1 d . . . C24 C 0.3057(5) 0.3715(4) 0.8970(2) 0.0297(9) Uani 1 1 d . . . H24 H 0.3827 0.4361 0.8722 0.036 Uiso 1 1 calc R . . C25 C 0.3709(6) 0.3018(4) 0.9629(2) 0.0364(10) Uani 1 1 d . . . H25 H 0.4923 0.3165 0.9814 0.044 Uiso 1 1 calc R . . C26 C 0.2597(6) 0.2120(4) 1.0010(2) 0.0419(11) Uani 1 1 d . . . H26 H 0.3045 0.1668 1.0469 0.050 Uiso 1 1 calc R . . C27 C 0.0842(6) 0.1880(4) 0.9726(2) 0.0361(10) Uani 1 1 d . . . H27 H 0.0079 0.1247 0.9985 0.043 Uiso 1 1 calc R . . C28 C 0.0164(5) 0.2550(4) 0.9063(2) 0.0275(9) Uani 1 1 d . . . H28 H -0.1053 0.2387 0.8877 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01959(19) 0.02372(19) 0.02790(18) 0.00946(13) 0.00730(13) 0.00816(14) Mo2 0.0256(2) 0.02425(19) 0.02198(17) 0.00203(13) 0.00442(13) 0.00570(15) P1 0.0196(5) 0.0209(5) 0.0218(4) 0.0050(4) 0.0045(4) 0.0057(4) O1 0.053(2) 0.0469(19) 0.0321(15) 0.0012(12) 0.0144(13) 0.0207(16) C1 0.023(2) 0.025(2) 0.039(2) 0.0051(16) 0.0107(17) 0.0077(17) O2 0.063(2) 0.0377(19) 0.071(2) 0.0094(15) 0.0397(18) -0.0017(17) C2 0.037(3) 0.028(2) 0.032(2) 0.0022(16) 0.0114(18) 0.010(2) O3 0.068(2) 0.056(2) 0.0245(15) 0.0077(13) 0.0074(14) 0.0154(17) C3 0.035(3) 0.031(2) 0.029(2) -0.0009(16) 0.0062(17) 0.0087(19) O4 0.0272(19) 0.082(2) 0.0530(18) -0.0181(16) -0.0021(15) 0.0089(17) C4 0.037(3) 0.043(3) 0.029(2) -0.0048(17) 0.0094(19) 0.013(2) C5 0.056(3) 0.061(3) 0.082(3) 0.046(3) 0.038(3) 0.046(3) C6 0.027(3) 0.080(4) 0.066(3) 0.050(3) 0.008(2) 0.023(3) C7 0.036(3) 0.058(3) 0.041(2) 0.031(2) 0.008(2) 0.020(2) C8 0.027(2) 0.041(3) 0.060(3) 0.033(2) 0.013(2) 0.017(2) C9 0.060(4) 0.032(3) 0.073(3) 0.026(2) 0.027(3) 0.026(2) C10 0.053(3) 0.025(2) 0.036(2) 0.0006(17) 0.001(2) 0.015(2) C11 0.055(3) 0.024(2) 0.035(2) 0.0089(16) 0.011(2) 0.011(2) C12 0.049(3) 0.020(2) 0.049(3) 0.0049(18) -0.001(2) -0.002(2) C13 0.069(4) 0.026(2) 0.028(2) -0.0019(17) -0.001(2) 0.014(2) C14 0.050(3) 0.025(2) 0.044(2) 0.0006(17) 0.014(2) 0.019(2) C15 0.026(2) 0.038(2) 0.0233(19) 0.0035(15) 0.0062(16) 0.0046(18) C16 0.0140(19) 0.026(2) 0.0296(19) 0.0013(15) 0.0056(15) 0.0029(16) C17 0.022(2) 0.022(2) 0.0245(18) 0.0045(14) 0.0035(15) 0.0080(16) C18 0.024(2) 0.027(2) 0.0299(19) 0.0036(15) 0.0071(16) 0.0075(17) C19 0.030(2) 0.028(2) 0.037(2) 0.0113(17) 0.0082(17) 0.0040(19) C20 0.031(2) 0.026(2) 0.041(2) 0.0047(17) 0.0033(18) 0.0001(18) C21 0.031(2) 0.030(2) 0.0286(19) -0.0011(16) 0.0008(17) 0.0088(19) C22 0.032(2) 0.029(2) 0.0271(19) 0.0089(15) 0.0056(16) 0.0093(18) C23 0.024(2) 0.0204(19) 0.0209(17) 0.0005(14) 0.0032(15) 0.0100(16) C24 0.027(2) 0.031(2) 0.031(2) 0.0027(16) 0.0047(16) 0.0108(18) C25 0.039(3) 0.036(2) 0.035(2) 0.0017(18) 0.0003(19) 0.021(2) C26 0.061(3) 0.037(3) 0.034(2) 0.0063(18) 0.001(2) 0.032(2) C27 0.057(3) 0.027(2) 0.033(2) 0.0140(17) 0.018(2) 0.020(2) C28 0.032(2) 0.025(2) 0.0297(19) 0.0060(15) 0.0084(16) 0.0140(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.946(4) . ? Mo1 C2 1.946(4) . ? Mo1 C5 2.281(4) . ? Mo1 C9 2.307(4) . ? Mo1 C6 2.326(4) . ? Mo1 C7 2.382(3) . ? Mo1 C8 2.386(4) . ? Mo1 P1 2.4083(10) . ? Mo1 Mo2 3.2881(5) . ? Mo2 C3 1.933(4) . ? Mo2 C4 1.969(4) . ? Mo2 C16 2.295(3) . ? Mo2 C12 2.327(4) . ? Mo2 C13 2.328(4) . ? Mo2 C11 2.347(4) . ? Mo2 C14 2.357(4) . ? Mo2 C10 2.369(4) . ? P1 C16 1.777(3) . ? P1 C23 1.832(3) . ? P1 C17 1.842(4) . ? O1 C1 1.159(4) . ? O2 C2 1.160(4) . ? O3 C3 1.158(4) . ? O4 C4 1.158(5) . ? C5 C6 1.402(6) . ? C5 C9 1.412(6) . ? C6 C7 1.396(6) . ? C7 C8 1.399(6) . ? C8 C9 1.405(6) . ? C10 C11 1.385(6) . ? C10 C14 1.425(5) . ? C11 C12 1.418(5) . ? C12 C13 1.398(6) . ? C13 C14 1.411(6) . ? C15 C16 1.409(4) . ? C17 C18 1.382(5) . ? C17 C22 1.398(4) . ? C18 C19 1.375(5) . ? C19 C20 1.390(5) . ? C20 C21 1.371(5) . ? C21 C22 1.381(5) . ? C23 C28 1.384(5) . ? C23 C24 1.393(5) . ? C24 C25 1.398(5) . ? C25 C26 1.378(6) . ? C26 C27 1.371(6) . ? C27 C28 1.393(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 74.97(15) . . ? C1 Mo1 C5 89.70(16) . . ? C2 Mo1 C5 104.31(17) . . ? C1 Mo1 C9 88.97(15) . . ? C2 Mo1 C9 138.01(17) . . ? C5 Mo1 C9 35.86(16) . . ? C1 Mo1 C6 121.95(17) . . ? C2 Mo1 C6 97.45(16) . . ? C5 Mo1 C6 35.41(15) . . ? C9 Mo1 C6 58.60(17) . . ? C1 Mo1 C7 145.15(15) . . ? C2 Mo1 C7 122.44(16) . . ? C5 Mo1 C7 58.05(15) . . ? C9 Mo1 C7 57.48(15) . . ? C6 Mo1 C7 34.48(14) . . ? C1 Mo1 C8 119.71(15) . . ? C2 Mo1 C8 154.88(15) . . ? C5 Mo1 C8 58.61(16) . . ? C9 Mo1 C8 34.79(14) . . ? C6 Mo1 C8 57.74(15) . . ? C7 Mo1 C8 34.12(13) . . ? C1 Mo1 P1 79.06(11) . . ? C2 Mo1 P1 113.12(11) . . ? C5 Mo1 P1 136.12(14) . . ? C9 Mo1 P1 101.05(13) . . ? C6 Mo1 P1 147.26(12) . . ? C7 Mo1 P1 113.86(11) . . ? C8 Mo1 P1 90.60(10) . . ? C1 Mo1 Mo2 124.20(10) . . ? C2 Mo1 Mo2 83.58(11) . . ? C5 Mo1 Mo2 145.90(13) . . ? C9 Mo1 Mo2 135.38(12) . . ? C6 Mo1 Mo2 111.38(13) . . ? C7 Mo1 Mo2 89.45(11) . . ? C8 Mo1 Mo2 101.09(10) . . ? P1 Mo1 Mo2 63.17(2) . . ? C3 Mo2 C4 77.82(16) . . ? C3 Mo2 C16 102.42(14) . . ? C4 Mo2 C16 125.41(14) . . ? C3 Mo2 C12 106.22(15) . . ? C4 Mo2 C12 84.13(17) . . ? C16 Mo2 C12 142.72(13) . . ? C3 Mo2 C13 87.36(14) . . ? C4 Mo2 C13 108.81(17) . . ? C16 Mo2 C13 125.78(15) . . ? C12 Mo2 C13 34.95(15) . . ? C3 Mo2 C11 141.38(14) . . ? C4 Mo2 C11 96.06(17) . . ? C16 Mo2 C11 111.59(13) . . ? C12 Mo2 C11 35.32(12) . . ? C13 Mo2 C11 58.20(14) . . ? C3 Mo2 C14 104.45(14) . . ? C4 Mo2 C14 141.80(16) . . ? C16 Mo2 C14 91.85(14) . . ? C12 Mo2 C14 58.31(16) . . ? C13 Mo2 C14 35.05(14) . . ? C11 Mo2 C14 57.99(15) . . ? C3 Mo2 C10 139.51(15) . . ? C4 Mo2 C10 129.91(17) . . ? C16 Mo2 C10 84.86(14) . . ? C12 Mo2 C10 57.86(15) . . ? C13 Mo2 C10 57.99(12) . . ? C11 Mo2 C10 34.16(14) . . ? C14 Mo2 C10 35.08(12) . . ? C3 Mo2 Mo1 105.53(11) . . ? C4 Mo2 Mo1 53.94(11) . . ? C16 Mo2 Mo1 74.62(9) . . ? C12 Mo2 Mo1 118.70(12) . . ? C13 Mo2 Mo1 153.63(13) . . ? C11 Mo2 Mo1 100.77(10) . . ? C14 Mo2 Mo1 149.10(9) . . ? C10 Mo2 Mo1 114.74(9) . . ? C16 P1 C23 101.94(15) . . ? C16 P1 C17 108.84(16) . . ? C23 P1 C17 101.20(15) . . ? C16 P1 Mo1 111.37(11) . . ? C23 P1 Mo1 123.30(12) . . ? C17 P1 Mo1 109.14(11) . . ? O1 C1 Mo1 175.7(3) . . ? O2 C2 Mo1 175.0(3) . . ? O3 C3 Mo2 177.8(4) . . ? O4 C4 Mo2 158.2(3) . . ? C6 C5 C9 107.4(4) . . ? C6 C5 Mo1 74.1(2) . . ? C9 C5 Mo1 73.1(2) . . ? C7 C6 C5 108.0(4) . . ? C7 C6 Mo1 75.0(2) . . ? C5 C6 Mo1 70.5(2) . . ? C6 C7 C8 109.0(4) . . ? C6 C7 Mo1 70.6(2) . . ? C8 C7 Mo1 73.1(2) . . ? C7 C8 C9 107.1(4) . . ? C7 C8 Mo1 72.8(2) . . ? C9 C8 Mo1 69.5(2) . . ? C8 C9 C5 108.4(4) . . ? C8 C9 Mo1 75.7(2) . . ? C5 C9 Mo1 71.0(2) . . ? C11 C10 C14 108.5(4) . . ? C11 C10 Mo2 72.0(2) . . ? C14 C10 Mo2 72.0(2) . . ? C10 C11 C12 108.3(4) . . ? C10 C11 Mo2 73.8(2) . . ? C12 C11 Mo2 71.6(2) . . ? C13 C12 C11 107.7(4) . . ? C13 C12 Mo2 72.5(2) . . ? C11 C12 Mo2 73.1(2) . . ? C12 C13 C14 108.7(3) . . ? C12 C13 Mo2 72.5(2) . . ? C14 C13 Mo2 73.6(2) . . ? C13 C14 C10 106.9(4) . . ? C13 C14 Mo2 71.3(2) . . ? C10 C14 Mo2 72.9(2) . . ? C15 C16 P1 123.0(3) . . ? C15 C16 Mo2 74.03(19) . . ? P1 C16 Mo2 97.32(16) . . ? C18 C17 C22 118.3(3) . . ? C18 C17 P1 121.6(2) . . ? C22 C17 P1 119.7(3) . . ? C19 C18 C17 121.4(3) . . ? C18 C19 C20 119.9(4) . . ? C21 C20 C19 119.3(4) . . ? C20 C21 C22 120.9(3) . . ? C21 C22 C17 120.2(3) . . ? C28 C23 C24 119.7(3) . . ? C28 C23 P1 122.4(3) . . ? C24 C23 P1 117.8(3) . . ? C23 C24 C25 119.7(4) . . ? C26 C25 C24 120.2(4) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C28 120.9(4) . . ? C23 C28 C27 119.7(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.675 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.113