# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1930 #M.J. Mays et al., Department of Chemistry, Lensfield Rd, Cambridge, CB2 1EW #Reaction of the anions [Cp2(CO)4Mo2((-PRR`)]- with chloroarsines #and chlorophosphines data_7 #DATA FOR COMPLEX 7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Mo2 O4 P2' _chemical_formula_weight 652.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 14.222(6) _cell_length_b 10.378(4) _cell_length_c 17.861(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.16(3) _cell_angle_gamma 90.00 _cell_volume 2556.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.978 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC7r' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.3 _diffrn_reflns_number 4674 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4484 _reflns_number_gt 3466 _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 w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+3.3160P] 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 4484 _refine_ls_number_parameters 312 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.89102(3) 0.40863(4) 0.31686(3) 0.02719(14) Uani 1 d . . . Mo2 Mo 0.93186(3) 0.33876(5) 0.14862(3) 0.03133(15) Uani 1 d . . . H100 H 0.881(5) 0.319(6) 0.232(4) 0.06(2) Uiso 1 d . . . P1 P 1.00829(11) 0.48573(15) 0.24946(9) 0.0358(4) Uani 1 d D . . H1 H 1.0933(7) 0.4411(4) 0.2837(3) 0.043 Uiso 1 calc RD . . P2 P 1.02065(13) 0.69222(16) 0.22921(10) 0.0451(4) Uani 1 d . . . O23 O 1.0774(3) 0.4313(5) 0.4489(3) 0.0565(13) Uani 1 d . . . O24 O 0.9401(3) 0.1233(4) 0.3645(2) 0.0486(11) Uani 1 d . . . O25 O 0.9200(4) 0.5843(5) 0.0466(3) 0.0633(14) Uani 1 d . . . O26 O 0.7098(3) 0.3766(4) 0.0778(2) 0.0466(11) Uani 1 d . . . C1 C 1.1229(5) 0.7016(6) 0.1820(3) 0.0449(15) Uani 1 d . . . C2 C 1.1735(5) 0.5976(7) 0.1630(5) 0.066(2) Uani 1 d . . . H2 H 1.1606 0.5133 0.1786 0.079 Uiso 1 calc R . . C3 C 1.2423(6) 0.6153(8) 0.1216(5) 0.074(3) Uani 1 d . . . H3 H 1.2744 0.5427 0.1070 0.088 Uiso 1 calc R . . C4 C 1.2649(6) 0.7347(9) 0.1016(4) 0.070(2) Uani 1 d . . . H4 H 1.3143 0.7460 0.0747 0.084 Uiso 1 calc R . . C5 C 1.2171(6) 0.8381(8) 0.1198(4) 0.066(2) Uani 1 d . . . H5 H 1.2330 0.9219 0.1053 0.079 Uiso 1 calc R . . C6 C 1.1454(5) 0.8237(7) 0.1591(4) 0.0552(18) Uani 1 d . . . H6 H 1.1114 0.8970 0.1705 0.066 Uiso 1 calc R . . C7 C 1.0800(4) 0.7422(6) 0.3289(4) 0.0431(15) Uani 1 d . . . C8 C 1.1752(5) 0.7118(6) 0.3661(4) 0.0497(16) Uani 1 d . . . H8 H 1.2140 0.6640 0.3396 0.060 Uiso 1 calc R . . C9 C 1.2137(5) 0.7504(7) 0.4412(4) 0.0560(18) Uani 1 d . . . H9 H 1.2784 0.7275 0.4666 0.067 Uiso 1 calc R . . C10 C 1.1583(6) 0.8225(7) 0.4798(4) 0.059(2) Uani 1 d . . . H10 H 1.1853 0.8522 0.5309 0.071 Uiso 1 calc R . . C11 C 1.0633(6) 0.8504(7) 0.4430(4) 0.061(2) Uani 1 d . . . H11 H 1.0237 0.8960 0.4698 0.073 Uiso 1 calc R . . C12 C 1.0256(5) 0.8126(6) 0.3678(4) 0.0519(17) Uani 1 d . . . H12 H 0.9610 0.8356 0.3425 0.062 Uiso 1 calc R . . C13 C 0.7842(5) 0.5848(6) 0.2884(4) 0.0515(17) Uani 1 d . . . H13 H 0.7929 0.6515 0.2543 0.062 Uiso 1 calc R . . C14 C 0.8258(4) 0.5811(6) 0.3683(4) 0.0418(14) Uani 1 d . . . H14 H 0.8674 0.6438 0.3981 0.050 Uiso 1 calc R . . C15 C 0.7933(4) 0.4654(6) 0.3956(3) 0.0372(13) Uani 1 d . . . H15 H 0.8097 0.4363 0.4476 0.045 Uiso 1 calc R . . C16 C 0.7326(4) 0.4005(7) 0.3328(4) 0.0476(16) Uani 1 d . . . H16 H 0.7006 0.3208 0.3350 0.057 Uiso 1 calc R . . C17 C 0.7280(4) 0.4740(8) 0.2675(4) 0.0552(19) Uani 1 d . . . H17 H 0.6925 0.4527 0.2167 0.066 Uiso 1 calc R . . C18 C 0.9848(6) 0.1222(6) 0.1776(5) 0.059(2) Uani 1 d . . . H18 H 0.9687 0.0724 0.2173 0.071 Uiso 1 calc R . . C19 C 0.9325(5) 0.1297(6) 0.1010(4) 0.0540(19) Uani 1 d . . . H19 H 0.8733 0.0857 0.0799 0.065 Uiso 1 calc R . . C20 C 0.9794(5) 0.2114(7) 0.0595(4) 0.0481(16) Uani 1 d . . . H20 H 0.9586 0.2321 0.0062 0.058 Uiso 1 calc R . . C21 C 1.0634(4) 0.2571(7) 0.1121(4) 0.0472(16) Uani 1 d . . . H21 H 1.1099 0.3146 0.1005 0.057 Uiso 1 calc R . . C22 C 1.0666(5) 0.2026(7) 0.1849(4) 0.0552(19) Uani 1 d . . . H22 H 1.1153 0.2175 0.2309 0.066 Uiso 1 calc R . . C23 C 1.0093(4) 0.4238(6) 0.3988(3) 0.0359(13) Uani 1 d . . . C24 C 0.9219(4) 0.2288(6) 0.3454(3) 0.0345(13) Uani 1 d . . . C25 C 0.9259(4) 0.4935(7) 0.0864(4) 0.0448(15) Uani 1 d . . . C26 C 0.7923(4) 0.3612(5) 0.1053(3) 0.0359(13) Uani 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 0.0261(2) 0.0271(3) 0.0295(3) -0.0001(2) 0.00898(19) 0.0018(2) Mo2 0.0313(3) 0.0354(3) 0.0305(3) 0.0002(2) 0.0139(2) -0.0072(2) P1 0.0331(8) 0.0356(8) 0.0410(8) -0.0013(7) 0.0134(7) -0.0091(7) P2 0.0471(10) 0.0358(9) 0.0565(10) -0.0010(8) 0.0206(8) -0.0035(7) O23 0.041(3) 0.080(4) 0.044(3) -0.014(2) 0.002(2) 0.009(2) O24 0.070(3) 0.034(2) 0.039(2) 0.0080(19) 0.008(2) 0.010(2) O25 0.066(3) 0.062(3) 0.059(3) 0.024(3) 0.010(3) -0.016(3) O26 0.037(2) 0.053(3) 0.047(3) 0.004(2) 0.005(2) -0.005(2) C1 0.051(4) 0.047(4) 0.041(3) -0.011(3) 0.020(3) -0.014(3) C2 0.074(5) 0.052(4) 0.088(6) -0.019(4) 0.052(5) -0.024(4) C3 0.068(5) 0.077(6) 0.093(6) -0.037(5) 0.053(5) -0.032(4) C4 0.071(5) 0.096(6) 0.049(4) -0.029(4) 0.027(4) -0.047(5) C5 0.068(5) 0.070(5) 0.062(5) 0.010(4) 0.019(4) -0.028(4) C6 0.050(4) 0.051(4) 0.062(4) -0.003(4) 0.009(3) -0.014(3) C7 0.045(4) 0.030(3) 0.061(4) -0.003(3) 0.025(3) -0.006(3) C8 0.056(4) 0.041(4) 0.059(4) -0.011(3) 0.027(4) -0.012(3) C9 0.048(4) 0.064(5) 0.060(4) 0.012(4) 0.021(3) -0.019(4) C10 0.096(6) 0.047(4) 0.040(4) -0.009(3) 0.027(4) -0.026(4) C11 0.092(6) 0.039(4) 0.059(5) -0.003(3) 0.035(4) 0.013(4) C12 0.054(4) 0.047(4) 0.060(4) -0.007(3) 0.022(4) 0.007(3) C13 0.051(4) 0.046(4) 0.062(4) 0.017(4) 0.022(3) 0.030(3) C14 0.037(3) 0.036(3) 0.052(4) -0.003(3) 0.012(3) 0.011(3) C15 0.036(3) 0.042(3) 0.038(3) -0.004(3) 0.017(3) 0.004(3) C16 0.023(3) 0.054(4) 0.068(4) -0.013(4) 0.016(3) 0.003(3) C17 0.030(3) 0.085(5) 0.046(4) -0.018(4) -0.001(3) 0.023(4) C18 0.082(5) 0.039(4) 0.072(5) 0.010(3) 0.048(5) 0.019(4) C19 0.044(4) 0.047(4) 0.079(5) -0.027(4) 0.031(4) -0.012(3) C20 0.046(4) 0.062(4) 0.042(3) -0.010(3) 0.023(3) -0.004(3) C21 0.037(3) 0.056(4) 0.055(4) -0.013(3) 0.025(3) -0.008(3) C22 0.056(4) 0.059(4) 0.047(4) -0.014(3) 0.006(3) 0.025(4) C23 0.035(3) 0.037(3) 0.036(3) -0.009(3) 0.010(3) 0.003(3) C24 0.041(3) 0.039(3) 0.024(3) 0.001(3) 0.009(2) 0.000(3) C25 0.035(3) 0.058(4) 0.043(3) 0.006(3) 0.012(3) -0.014(3) C26 0.044(4) 0.032(3) 0.036(3) 0.001(3) 0.018(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C23 1.947(6) . ? Mo1 C24 1.956(6) . ? Mo1 C15 2.283(5) . ? Mo1 C14 2.308(6) . ? Mo1 C16 2.341(5) . ? Mo1 C13 2.352(6) . ? Mo1 C17 2.369(6) . ? Mo1 P1 2.4194(16) . ? Mo1 H100 1.76(6) . ? Mo2 C25 1.943(7) . ? Mo2 C26 1.960(6) . ? Mo2 C21 2.290(6) . ? Mo2 C20 2.294(6) . ? Mo2 C19 2.331(6) . ? Mo2 C22 2.341(6) . ? Mo2 C18 2.387(7) . ? Mo2 P1 2.4071(17) . ? Mo2 H100 1.82(6) . ? P1 P2 2.188(2) . ? P1 H1 1.2996 . ? P2 C7 1.848(7) . ? P2 C1 1.853(6) . ? O23 C23 1.149(7) . ? O24 C24 1.157(7) . ? O25 C25 1.171(7) . ? O26 C26 1.167(7) . ? C1 C2 1.385(9) . ? C1 C6 1.392(9) . ? C2 C3 1.375(9) . ? C2 H2 0.9500 . ? C3 C4 1.351(11) . ? C3 H3 0.9500 . ? C4 C5 1.352(11) . ? C4 H4 0.9500 . ? C5 C6 1.381(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.371(8) . ? C7 C8 1.391(9) . ? C8 C9 1.379(10) . ? C8 H8 0.9500 . ? C9 C10 1.387(10) . ? C9 H9 0.9500 . ? C10 C11 1.381(11) . ? C10 H10 0.9500 . ? C11 C12 1.375(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C17 1.398(10) . ? C13 C14 1.404(9) . ? C13 H13 0.9500 . ? C14 C15 1.415(8) . ? C14 H14 0.9500 . ? C15 C16 1.407(8) . ? C15 H15 0.9500 . ? C16 C17 1.382(10) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.391(11) . ? C18 C22 1.411(10) . ? C18 H18 0.9500 . ? C19 C20 1.398(9) . ? C19 H19 0.9500 . ? C20 C21 1.410(9) . ? C20 H20 0.9500 . ? C21 C22 1.408(9) . ? 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 C23 Mo1 C24 77.5(2) . . ? C23 Mo1 C15 93.5(2) . . ? C24 Mo1 C15 102.6(2) . . ? C23 Mo1 C14 89.8(2) . . ? C24 Mo1 C14 136.3(2) . . ? C15 Mo1 C14 35.9(2) . . ? C23 Mo1 C16 126.3(2) . . ? C24 Mo1 C16 95.5(2) . . ? C15 Mo1 C16 35.4(2) . . ? C14 Mo1 C16 59.1(2) . . ? C23 Mo1 C13 119.5(3) . . ? C24 Mo1 C13 152.9(2) . . ? C15 Mo1 C13 58.3(2) . . ? C14 Mo1 C13 35.1(2) . . ? C16 Mo1 C13 57.6(2) . . ? C23 Mo1 C17 147.5(2) . . ? C24 Mo1 C17 120.5(3) . . ? C15 Mo1 C17 57.8(2) . . ? C14 Mo1 C17 58.3(2) . . ? C16 Mo1 C17 34.1(2) . . ? C13 Mo1 C17 34.5(2) . . ? C23 Mo1 P1 76.89(17) . . ? C24 Mo1 P1 107.88(16) . . ? C15 Mo1 P1 144.97(16) . . ? C14 Mo1 P1 109.57(16) . . ? C16 Mo1 P1 150.90(18) . . ? C13 Mo1 P1 97.06(17) . . ? C17 Mo1 P1 116.81(19) . . ? C23 Mo1 H100 124(2) . . ? C24 Mo1 H100 72(2) . . ? C15 Mo1 H100 137(2) . . ? C14 Mo1 H100 143(2) . . ? C16 Mo1 H100 102(2) . . ? C13 Mo1 H100 108(2) . . ? C17 Mo1 H100 88(2) . . ? P1 Mo1 H100 70(2) . . ? C25 Mo2 C26 77.1(2) . . ? C25 Mo2 C21 93.9(2) . . ? C26 Mo2 C21 138.7(2) . . ? C25 Mo2 C20 93.4(3) . . ? C26 Mo2 C20 103.7(2) . . ? C21 Mo2 C20 35.8(2) . . ? C25 Mo2 C19 124.4(3) . . ? C26 Mo2 C19 93.4(2) . . ? C21 Mo2 C19 58.4(2) . . ? C20 Mo2 C19 35.2(2) . . ? C25 Mo2 C22 125.1(3) . . ? C26 Mo2 C22 149.6(3) . . ? C21 Mo2 C22 35.4(2) . . ? C20 Mo2 C22 58.9(2) . . ? C19 Mo2 C22 57.5(3) . . ? C25 Mo2 C18 150.4(2) . . ? C26 Mo2 C18 115.7(3) . . ? C21 Mo2 C18 58.4(2) . . ? C20 Mo2 C18 58.4(2) . . ? C19 Mo2 C18 34.3(3) . . ? C22 Mo2 C18 34.7(3) . . ? C25 Mo2 P1 81.52(19) . . ? C26 Mo2 P1 116.65(17) . . ? C21 Mo2 P1 101.34(17) . . ? C20 Mo2 P1 136.76(16) . . ? C19 Mo2 P1 145.2(2) . . ? C22 Mo2 P1 89.21(18) . . ? C18 Mo2 P1 111.9(2) . . ? C25 Mo2 H100 126(2) . . ? C26 Mo2 H100 77(2) . . ? C21 Mo2 H100 135(2) . . ? C20 Mo2 H100 138(2) . . ? C19 Mo2 H100 103(2) . . ? C22 Mo2 H100 100(2) . . ? C18 Mo2 H100 83(2) . . ? P1 Mo2 H100 70(2) . . ? P2 P1 Mo2 122.47(9) . . ? P2 P1 Mo1 119.96(8) . . ? Mo2 P1 Mo1 85.56(5) . . ? P2 P1 H1 108.9 . . ? Mo2 P1 H1 108.9 . . ? Mo1 P1 H1 108.9 . . ? C7 P2 C1 101.5(3) . . ? C7 P2 P1 98.7(2) . . ? C1 P2 P1 103.3(2) . . ? C2 C1 C6 117.8(6) . . ? C2 C1 P2 125.7(5) . . ? C6 C1 P2 116.3(5) . . ? C3 C2 C1 120.6(7) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 120.8(8) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.9(7) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.9(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 120.0(7) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 C7 C8 118.9(6) . . ? C12 C7 P2 117.2(5) . . ? C8 C7 P2 124.0(5) . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.1(7) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 119.0(7) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 120.5(6) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C7 C12 C11 120.9(7) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C17 C13 C14 108.7(6) . . ? C17 C13 Mo1 73.5(4) . . ? C14 C13 Mo1 70.8(3) . . ? C17 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? Mo1 C13 H13 121.8 . . ? C13 C14 C15 106.3(6) . . ? C13 C14 Mo1 74.2(3) . . ? C15 C14 Mo1 71.1(3) . . ? C13 C14 H14 126.8 . . ? C15 C14 H14 126.8 . . ? Mo1 C14 H14 119.9 . . ? C16 C15 C14 108.7(6) . . ? C16 C15 Mo1 74.6(3) . . ? C14 C15 Mo1 73.0(3) . . ? C16 C15 H15 125.7 . . ? C14 C15 H15 125.7 . . ? Mo1 C15 H15 118.6 . . ? C17 C16 C15 107.6(6) . . ? C17 C16 Mo1 74.1(3) . . ? C15 C16 Mo1 70.0(3) . . ? C17 C16 H16 126.2 . . ? C15 C16 H16 126.2 . . ? Mo1 C16 H16 121.4 . . ? C16 C17 C13 108.8(6) . . ? C16 C17 Mo1 71.8(3) . . ? C13 C17 Mo1 72.1(3) . . ? C16 C17 H17 125.6 . . ? C13 C17 H17 125.6 . . ? Mo1 C17 H17 122.1 . . ? C19 C18 C22 106.8(6) . . ? C19 C18 Mo2 70.7(4) . . ? C22 C18 Mo2 70.8(4) . . ? C19 C18 H18 126.6 . . ? C22 C18 H18 126.6 . . ? Mo2 C18 H18 123.5 . . ? C18 C19 C20 110.2(6) . . ? C18 C19 Mo2 75.1(4) . . ? C20 C19 Mo2 71.0(4) . . ? C18 C19 H19 124.9 . . ? C20 C19 H19 124.9 . . ? Mo2 C19 H19 120.7 . . ? C19 C20 C21 106.7(6) . . ? C19 C20 Mo2 73.9(3) . . ? C21 C20 Mo2 71.9(3) . . ? C19 C20 H20 126.6 . . ? C21 C20 H20 126.6 . . ? Mo2 C20 H20 119.5 . . ? C22 C21 C20 108.1(6) . . ? C22 C21 Mo2 74.3(3) . . ? C20 C21 Mo2 72.3(3) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Mo2 C21 H21 119.3 . . ? C21 C22 C18 108.3(6) . . ? C21 C22 Mo2 70.3(4) . . ? C18 C22 Mo2 74.4(4) . . ? C21 C22 H22 125.9 . . ? C18 C22 H22 125.9 . . ? Mo2 C22 H22 121.1 . . ? O23 C23 Mo1 177.7(5) . . ? O24 C24 Mo1 178.0(5) . . ? O25 C25 Mo2 177.4(6) . . ? O26 C26 Mo2 178.1(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 C25 Mo2 P1 P2 5.05(19) . . . . ? C26 Mo2 P1 P2 -65.90(19) . . . . ? C21 Mo2 P1 P2 97.3(2) . . . . ? C20 Mo2 P1 P2 90.9(3) . . . . ? C19 Mo2 P1 P2 146.8(3) . . . . ? C22 Mo2 P1 P2 130.8(2) . . . . ? C18 Mo2 P1 P2 157.67(19) . . . . ? C25 Mo2 P1 Mo1 128.02(18) . . . . ? C26 Mo2 P1 Mo1 57.08(18) . . . . ? C21 Mo2 P1 Mo1 -139.69(18) . . . . ? C20 Mo2 P1 Mo1 -146.1(3) . . . . ? C19 Mo2 P1 Mo1 -90.2(3) . . . . ? C22 Mo2 P1 Mo1 -106.25(19) . . . . ? C18 Mo2 P1 Mo1 -79.36(18) . . . . ? C23 Mo1 P1 P2 -94.67(19) . . . . ? C24 Mo1 P1 P2 -166.73(19) . . . . ? C15 Mo1 P1 P2 -17.6(3) . . . . ? C14 Mo1 P1 P2 -9.7(2) . . . . ? C16 Mo1 P1 P2 51.5(3) . . . . ? C13 Mo1 P1 P2 24.1(2) . . . . ? C17 Mo1 P1 P2 53.8(2) . . . . ? C23 Mo1 P1 Mo2 140.10(18) . . . . ? C24 Mo1 P1 Mo2 68.05(18) . . . . ? C15 Mo1 P1 Mo2 -142.8(3) . . . . ? C14 Mo1 P1 Mo2 -134.91(17) . . . . ? C16 Mo1 P1 Mo2 -73.7(3) . . . . ? C13 Mo1 P1 Mo2 -101.13(19) . . . . ? C17 Mo1 P1 Mo2 -71.4(2) . . . . ? Mo2 P1 P2 C7 177.85(19) . . . . ? Mo1 P1 P2 C7 72.7(2) . . . . ? Mo2 P1 P2 C1 -78.1(2) . . . . ? Mo1 P1 P2 C1 176.8(2) . . . . ? C7 P2 C1 C2 104.3(7) . . . . ? P1 P2 C1 C2 2.3(7) . . . . ? C7 P2 C1 C6 -80.6(6) . . . . ? P1 P2 C1 C6 177.5(5) . . . . ? C6 C1 C2 C3 -1.1(11) . . . . ? P2 C1 C2 C3 174.0(6) . . . . ? C1 C2 C3 C4 2.8(13) . . . . ? C2 C3 C4 C5 -2.4(13) . . . . ? C3 C4 C5 C6 0.3(12) . . . . ? C4 C5 C6 C1 1.4(12) . . . . ? C2 C1 C6 C5 -0.9(10) . . . . ? P2 C1 C6 C5 -176.5(5) . . . . ? C1 P2 C7 C12 145.1(5) . . . . ? P1 P2 C7 C12 -109.3(5) . . . . ? C1 P2 C7 C8 -35.5(6) . . . . ? P1 P2 C7 C8 70.2(5) . . . . ? C12 C7 C8 C9 0.8(9) . . . . ? P2 C7 C8 C9 -178.6(5) . . . . ? C7 C8 C9 C10 -1.4(10) . . . . ? C8 C9 C10 C11 2.5(10) . . . . ? C9 C10 C11 C12 -3.1(10) . . . . ? C8 C7 C12 C11 -1.4(10) . . . . ? P2 C7 C12 C11 178.0(5) . . . . ? C10 C11 C12 C7 2.6(11) . . . . ? C23 Mo1 C13 C17 -152.6(4) . . . . ? C24 Mo1 C13 C17 -28.4(7) . . . . ? C15 Mo1 C13 C17 -78.1(4) . . . . ? C14 Mo1 C13 C17 -117.2(6) . . . . ? C16 Mo1 C13 C17 -36.1(4) . . . . ? P1 Mo1 C13 C17 128.5(4) . . . . ? C23 Mo1 C13 C14 -35.4(5) . . . . ? C24 Mo1 C13 C14 88.8(6) . . . . ? C15 Mo1 C13 C14 39.1(4) . . . . ? C16 Mo1 C13 C14 81.1(4) . . . . ? C17 Mo1 C13 C14 117.2(6) . . . . ? P1 Mo1 C13 C14 -114.3(4) . . . . ? C17 C13 C14 C15 -0.1(6) . . . . ? Mo1 C13 C14 C15 -64.3(4) . . . . ? C17 C13 C14 Mo1 64.1(4) . . . . ? C23 Mo1 C14 C13 149.8(4) . . . . ? C24 Mo1 C14 C13 -138.7(4) . . . . ? C15 Mo1 C14 C13 -114.0(6) . . . . ? C16 Mo1 C14 C13 -76.4(4) . . . . ? C17 Mo1 C14 C13 -36.3(4) . . . . ? P1 Mo1 C14 C13 73.8(4) . . . . ? C23 Mo1 C14 C15 -96.3(4) . . . . ? C24 Mo1 C14 C15 -24.7(5) . . . . ? C16 Mo1 C14 C15 37.5(4) . . . . ? C13 Mo1 C14 C15 114.0(6) . . . . ? C17 Mo1 C14 C15 77.7(4) . . . . ? P1 Mo1 C14 C15 -172.3(3) . . . . ? C13 C14 C15 C16 -0.2(6) . . . . ? Mo1 C14 C15 C16 -66.6(4) . . . . ? C13 C14 C15 Mo1 66.4(4) . . . . ? C23 Mo1 C15 C16 -159.7(4) . . . . ? C24 Mo1 C15 C16 -81.7(4) . . . . ? C14 Mo1 C15 C16 115.6(6) . . . . ? C13 Mo1 C15 C16 77.4(4) . . . . ? C17 Mo1 C15 C16 36.6(4) . . . . ? P1 Mo1 C15 C16 128.4(4) . . . . ? C23 Mo1 C15 C14 84.8(4) . . . . ? C24 Mo1 C15 C14 162.8(4) . . . . ? C16 Mo1 C15 C14 -115.6(6) . . . . ? C13 Mo1 C15 C14 -38.1(4) . . . . ? C17 Mo1 C15 C14 -79.0(4) . . . . ? P1 Mo1 C15 C14 12.8(5) . . . . ? C14 C15 C16 C17 0.5(6) . . . . ? Mo1 C15 C16 C17 -65.1(4) . . . . ? C14 C15 C16 Mo1 65.6(4) . . . . ? C23 Mo1 C16 C17 141.4(4) . . . . ? C24 Mo1 C16 C17 -140.0(4) . . . . ? C15 Mo1 C16 C17 115.9(6) . . . . ? C14 Mo1 C16 C17 77.9(4) . . . . ? C13 Mo1 C16 C17 36.5(4) . . . . ? P1 Mo1 C16 C17 3.7(6) . . . . ? C23 Mo1 C16 C15 25.5(5) . . . . ? C24 Mo1 C16 C15 104.0(4) . . . . ? C14 Mo1 C16 C15 -38.1(4) . . . . ? C13 Mo1 C16 C15 -79.5(4) . . . . ? C17 Mo1 C16 C15 -115.9(6) . . . . ? P1 Mo1 C16 C15 -112.2(4) . . . . ? C15 C16 C17 C13 -0.6(6) . . . . ? Mo1 C16 C17 C13 -63.0(4) . . . . ? C15 C16 C17 Mo1 62.4(4) . . . . ? C14 C13 C17 C16 0.4(7) . . . . ? Mo1 C13 C17 C16 62.9(4) . . . . ? C14 C13 C17 Mo1 -62.4(4) . . . . ? C23 Mo1 C17 C16 -69.3(7) . . . . ? C24 Mo1 C17 C16 47.9(5) . . . . ? C15 Mo1 C17 C16 -38.0(4) . . . . ? C14 Mo1 C17 C16 -80.6(4) . . . . ? C13 Mo1 C17 C16 -117.5(6) . . . . ? P1 Mo1 C17 C16 -178.0(3) . . . . ? C23 Mo1 C17 C13 48.2(7) . . . . ? C24 Mo1 C17 C13 165.4(4) . . . . ? C15 Mo1 C17 C13 79.5(4) . . . . ? C14 Mo1 C17 C13 36.9(4) . . . . ? C16 Mo1 C17 C13 117.5(6) . . . . ? P1 Mo1 C17 C13 -60.5(4) . . . . ? C25 Mo2 C18 C19 -56.2(7) . . . . ? C26 Mo2 C18 C19 54.1(4) . . . . ? C21 Mo2 C18 C19 -79.0(4) . . . . ? C20 Mo2 C18 C19 -36.6(4) . . . . ? C22 Mo2 C18 C19 -116.4(6) . . . . ? P1 Mo2 C18 C19 -169.0(3) . . . . ? C25 Mo2 C18 C22 60.2(8) . . . . ? C26 Mo2 C18 C22 170.5(4) . . . . ? C21 Mo2 C18 C22 37.5(4) . . . . ? C20 Mo2 C18 C22 79.8(4) . . . . ? C19 Mo2 C18 C22 116.4(6) . . . . ? P1 Mo2 C18 C22 -52.6(4) . . . . ? C22 C18 C19 C20 0.7(7) . . . . ? Mo2 C18 C19 C20 62.8(5) . . . . ? C22 C18 C19 Mo2 -62.0(4) . . . . ? C25 Mo2 C19 C18 150.2(4) . . . . ? C26 Mo2 C19 C18 -133.0(4) . . . . ? C21 Mo2 C19 C18 79.2(4) . . . . ? C20 Mo2 C19 C18 118.0(6) . . . . ? C22 Mo2 C19 C18 37.2(4) . . . . ? P1 Mo2 C19 C18 18.0(5) . . . . ? C25 Mo2 C19 C20 32.2(5) . . . . ? C26 Mo2 C19 C20 109.0(4) . . . . ? C21 Mo2 C19 C20 -38.8(4) . . . . ? C22 Mo2 C19 C20 -80.8(4) . . . . ? C18 Mo2 C19 C20 -118.0(6) . . . . ? P1 Mo2 C19 C20 -100.0(5) . . . . ? C18 C19 C20 C21 -0.4(7) . . . . ? Mo2 C19 C20 C21 64.9(4) . . . . ? C18 C19 C20 Mo2 -65.3(5) . . . . ? C25 Mo2 C20 C19 -153.8(4) . . . . ? C26 Mo2 C20 C19 -76.3(5) . . . . ? C21 Mo2 C20 C19 114.2(6) . . . . ? C22 Mo2 C20 C19 76.5(5) . . . . ? C18 Mo2 C20 C19 35.7(4) . . . . ? P1 Mo2 C20 C19 124.9(4) . . . . ? C25 Mo2 C20 C21 92.0(4) . . . . ? C26 Mo2 C20 C21 169.5(4) . . . . ? C19 Mo2 C20 C21 -114.2(6) . . . . ? C22 Mo2 C20 C21 -37.7(4) . . . . ? C18 Mo2 C20 C21 -78.5(5) . . . . ? P1 Mo2 C20 C21 10.7(5) . . . . ? C19 C20 C21 C22 0.0(7) . . . . ? Mo2 C20 C21 C22 66.2(4) . . . . ? C19 C20 C21 Mo2 -66.2(4) . . . . ? C25 Mo2 C21 C22 154.3(4) . . . . ? C26 Mo2 C21 C22 -130.8(5) . . . . ? C20 Mo2 C21 C22 -115.3(6) . . . . ? C19 Mo2 C21 C22 -77.2(5) . . . . ? C18 Mo2 C21 C22 -36.8(4) . . . . ? P1 Mo2 C21 C22 72.1(4) . . . . ? C25 Mo2 C21 C20 -90.4(4) . . . . ? C26 Mo2 C21 C20 -15.5(6) . . . . ? C19 Mo2 C21 C20 38.1(4) . . . . ? C22 Mo2 C21 C20 115.3(6) . . . . ? C18 Mo2 C21 C20 78.6(5) . . . . ? P1 Mo2 C21 C20 -172.5(4) . . . . ? C20 C21 C22 C18 0.5(7) . . . . ? Mo2 C21 C22 C18 65.3(4) . . . . ? C20 C21 C22 Mo2 -64.9(4) . . . . ? C19 C18 C22 C21 -0.7(7) . . . . ? Mo2 C18 C22 C21 -62.6(4) . . . . ? C19 C18 C22 Mo2 61.9(4) . . . . ? C25 Mo2 C22 C21 -32.0(5) . . . . ? C26 Mo2 C22 C21 99.4(6) . . . . ? C20 Mo2 C22 C21 38.1(4) . . . . ? C19 Mo2 C22 C21 79.7(4) . . . . ? C18 Mo2 C22 C21 116.4(6) . . . . ? P1 Mo2 C22 C21 -111.0(4) . . . . ? C25 Mo2 C22 C18 -148.4(4) . . . . ? C26 Mo2 C22 C18 -17.0(7) . . . . ? C21 Mo2 C22 C18 -116.4(6) . . . . ? C20 Mo2 C22 C18 -78.3(4) . . . . ? C19 Mo2 C22 C18 -36.7(4) . . . . ? P1 Mo2 C22 C18 132.5(4) . . . . ? C24 Mo1 C23 O23 -68(13) . . . . ? C15 Mo1 C23 O23 34(13) . . . . ? C14 Mo1 C23 O23 70(13) . . . . ? C16 Mo1 C23 O23 19(13) . . . . ? C13 Mo1 C23 O23 89(13) . . . . ? C17 Mo1 C23 O23 60(13) . . . . ? P1 Mo1 C23 O23 180(100) . . . . ? C23 Mo1 C24 O24 56(14) . . . . ? C15 Mo1 C24 O24 -35(14) . . . . ? C14 Mo1 C24 O24 -21(14) . . . . ? C16 Mo1 C24 O24 -70(14) . . . . ? C13 Mo1 C24 O24 -77(14) . . . . ? C17 Mo1 C24 O24 -95(14) . . . . ? P1 Mo1 C24 O24 127(14) . . . . ? C26 Mo2 C25 O25 -51(12) . . . . ? C21 Mo2 C25 O25 89(12) . . . . ? C20 Mo2 C25 O25 53(12) . . . . ? C19 Mo2 C25 O25 35(12) . . . . ? C22 Mo2 C25 O25 107(12) . . . . ? C18 Mo2 C25 O25 69(12) . . . . ? P1 Mo2 C25 O25 -171(12) . . . . ? C25 Mo2 C26 O26 23(15) . . . . ? C21 Mo2 C26 O26 -58(15) . . . . ? C20 Mo2 C26 O26 -67(15) . . . . ? C19 Mo2 C26 O26 -101(15) . . . . ? C22 Mo2 C26 O26 -118(15) . . . . ? C18 Mo2 C26 O26 -128(15) . . . . ? P1 Mo2 C26 O26 97(15) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.487 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.110 data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'COMPLEX 9' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Mo2 O6 P2' _chemical_formula_weight 664.27 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' '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)/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 9.7396(5) _cell_length_b 17.1917(7) _cell_length_c 15.3458(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.401(3) _cell_angle_gamma 90.00 _cell_volume 2548.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6787 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7464 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4492 _reflns_number_gt 3527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SIR-92' _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^)+(0.0300P)^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 4492 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.30274(3) 0.052285(15) 0.701868(19) 0.02095(10) Uani 1 1 d . . . Mo2 Mo 0.01359(3) 0.204314(15) 0.765899(19) 0.02246(10) Uani 1 1 d . . . P1 P 0.26899(9) 0.18311(5) 0.77140(6) 0.0230(2) Uani 1 1 d . . . H100 H 0.337(3) 0.2323(18) 0.730(2) 0.040(10) Uiso 1 1 d . . . P2 P 0.08595(9) 0.06491(5) 0.76960(6) 0.0208(2) Uani 1 1 d . . . O1 O 0.5809(3) 0.06969(17) 0.8259(2) 0.0577(8) Uani 1 1 d . . . O2 O 0.3591(3) -0.10576(14) 0.79831(17) 0.0457(7) Uani 1 1 d . . . O8 O 0.1102(3) 0.30918(16) 0.61945(18) 0.0526(8) Uani 1 1 d . . . O9 O -0.1662(3) 0.14115(16) 0.5985(2) 0.0608(9) Uani 1 1 d . . . O10 O 0.0871(2) 0.04249(11) 0.87339(14) 0.0254(5) Uani 1 1 d . . . O11 O -0.0226(2) 0.00076(12) 0.72173(15) 0.0281(6) Uani 1 1 d . . . C1 C 0.4769(4) 0.0650(2) 0.7795(3) 0.0358(9) Uani 1 1 d . . . C2 C 0.3301(3) -0.0459(2) 0.7657(2) 0.0292(8) Uani 1 1 d . . . C3 C 0.2274(4) -0.0094(2) 0.5707(2) 0.0344(9) Uani 1 1 d . . . H3A H 0.1786 -0.0573 0.5710 0.041 Uiso 1 1 calc R . . C4 C 0.1679(4) 0.0657(2) 0.5641(2) 0.0386(10) Uani 1 1 d . . . H4A H 0.0719 0.0776 0.5590 0.046 Uiso 1 1 calc R . . C5 C 0.2775(4) 0.1198(2) 0.5664(2) 0.0405(10) Uani 1 1 d . . . H5A H 0.2679 0.1747 0.5633 0.049 Uiso 1 1 calc R . . C6 C 0.4018(4) 0.0790(2) 0.5740(2) 0.0367(9) Uani 1 1 d . . . H6A H 0.4915 0.1013 0.5768 0.044 Uiso 1 1 calc R . . C7 C 0.3720(4) -0.0005(2) 0.5768(2) 0.0341(9) Uani 1 1 d . . . H7A H 0.4380 -0.0415 0.5820 0.041 Uiso 1 1 calc R . . C8 C 0.0734(4) 0.2699(2) 0.6730(2) 0.0339(9) Uani 1 1 d . . . C9 C -0.0965(4) 0.1628(2) 0.6605(3) 0.0402(10) Uani 1 1 d . . . C10 C -0.0204(4) 0.2040(2) 0.9139(2) 0.0390(10) Uani 1 1 d . . . H10A H 0.0244 0.1662 0.9529 0.047 Uiso 1 1 calc R . . C11 C 0.0312(4) 0.27791(19) 0.8970(2) 0.0349(9) Uani 1 1 d . . . H11A H 0.1170 0.2992 0.9229 0.042 Uiso 1 1 calc R . . C12 C -0.0654(4) 0.31471(19) 0.8357(2) 0.0323(9) Uani 1 1 d . . . H12A H -0.0571 0.3655 0.8126 0.039 Uiso 1 1 calc R . . C13 C -0.1766(4) 0.2640(2) 0.8140(2) 0.0372(9) Uani 1 1 d . . . H13A H -0.2564 0.2741 0.7731 0.045 Uiso 1 1 calc R . . C14 C -0.1502(4) 0.1958(2) 0.8628(3) 0.0389(10) Uani 1 1 d . . . H14A H -0.2093 0.1518 0.8617 0.047 Uiso 1 1 calc R . . C15 C 0.3725(3) 0.20433(18) 0.8765(2) 0.0256(8) Uani 1 1 d . . . C16 C 0.3490(4) 0.16559(19) 0.9532(2) 0.0328(9) Uani 1 1 d . . . H16A H 0.2739 0.1302 0.9516 0.039 Uiso 1 1 calc R . . C17 C 0.4331(4) 0.1780(2) 1.0311(2) 0.0383(9) Uani 1 1 d . . . H17A H 0.4158 0.1510 1.0826 0.046 Uiso 1 1 calc R . . C18 C 0.5431(4) 0.2297(2) 1.0348(2) 0.0369(10) Uani 1 1 d . . . H18A H 0.6024 0.2374 1.0882 0.044 Uiso 1 1 calc R . . C19 C 0.5653(4) 0.2700(2) 0.9595(3) 0.0332(9) Uani 1 1 d . . . H19A H 0.6391 0.3064 0.9615 0.040 Uiso 1 1 calc R . . C20 C 0.4803(3) 0.25727(18) 0.8818(2) 0.0287(8) Uani 1 1 d . . . H20A H 0.4961 0.2855 0.8308 0.034 Uiso 1 1 calc R . . C21 C 0.1137(4) -0.03637(19) 0.9061(2) 0.0367(9) Uani 1 1 d . . . H21A H 0.1305 -0.0709 0.8570 0.044 Uiso 1 1 calc R . . H21B H 0.0316 -0.0561 0.9312 0.044 Uiso 1 1 calc R . . C22 C 0.2366(4) -0.0375(2) 0.9750(3) 0.0506(11) Uani 1 1 d . . . H22A H 0.2561 -0.0911 0.9943 0.076 Uiso 1 1 calc R . . H22B H 0.2175 -0.0058 1.0251 0.076 Uiso 1 1 calc R . . H22C H 0.3169 -0.0162 0.9507 0.076 Uiso 1 1 calc R . . C23 C -0.1603(3) -0.0042(2) 0.7469(3) 0.0380(10) Uani 1 1 d . . . H23A H -0.2014 0.0484 0.7471 0.046 Uiso 1 1 calc R . . H23B H -0.1553 -0.0259 0.8070 0.046 Uiso 1 1 calc R . . C24 C -0.2497(4) -0.0552(2) 0.6840(3) 0.0460(11) Uani 1 1 d . . . H24A H -0.3433 -0.0573 0.7009 0.069 Uiso 1 1 calc R . . H24B H -0.2106 -0.1078 0.6853 0.069 Uiso 1 1 calc R . . H24C H -0.2539 -0.0339 0.6244 0.069 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 0.02004(17) 0.02166(17) 0.02114(18) -0.00129(12) 0.00265(13) 0.00028(12) Mo2 0.02474(17) 0.01933(17) 0.02225(17) -0.00178(13) -0.00101(13) 0.00425(13) P1 0.0244(5) 0.0216(4) 0.0224(5) -0.0004(4) 0.0009(4) -0.0017(4) P2 0.0193(4) 0.0186(4) 0.0239(5) -0.0020(4) 0.0004(4) -0.0003(4) O1 0.0280(16) 0.077(2) 0.065(2) -0.0318(17) -0.0086(15) 0.0048(15) O2 0.0623(19) 0.0283(14) 0.0443(18) 0.0060(13) -0.0018(14) 0.0115(14) O8 0.073(2) 0.0513(17) 0.0362(17) 0.0188(14) 0.0166(15) 0.0197(16) O9 0.0611(19) 0.0589(18) 0.052(2) -0.0252(15) -0.0330(16) 0.0228(15) O10 0.0321(13) 0.0187(11) 0.0255(13) 0.0017(10) 0.0044(11) 0.0013(10) O11 0.0190(12) 0.0283(13) 0.0373(15) -0.0100(11) 0.0042(11) -0.0029(10) C1 0.026(2) 0.035(2) 0.047(3) -0.0142(18) 0.0098(19) 0.0034(17) C2 0.0261(19) 0.037(2) 0.024(2) -0.0066(17) 0.0006(16) 0.0004(17) C3 0.052(3) 0.032(2) 0.019(2) -0.0059(16) 0.0044(18) -0.0072(19) C4 0.039(2) 0.056(3) 0.020(2) -0.0029(18) 0.0022(18) 0.012(2) C5 0.071(3) 0.031(2) 0.020(2) 0.0010(16) 0.007(2) 0.007(2) C6 0.039(2) 0.047(2) 0.027(2) -0.0017(18) 0.0147(18) -0.012(2) C7 0.039(2) 0.038(2) 0.026(2) -0.0037(17) 0.0099(18) 0.0047(18) C8 0.044(2) 0.031(2) 0.027(2) 0.0018(17) 0.0053(18) 0.0168(18) C9 0.043(2) 0.037(2) 0.037(3) -0.0106(19) -0.009(2) 0.0213(19) C10 0.061(3) 0.033(2) 0.025(2) 0.0007(17) 0.014(2) 0.012(2) C11 0.036(2) 0.035(2) 0.033(2) -0.0174(17) 0.0048(18) -0.0062(18) C12 0.044(2) 0.0211(18) 0.035(2) -0.0028(16) 0.0167(19) 0.0059(18) C13 0.025(2) 0.047(2) 0.040(2) -0.0062(19) 0.0067(18) 0.0086(18) C14 0.043(2) 0.031(2) 0.047(3) -0.0057(19) 0.023(2) -0.0095(19) C15 0.0233(18) 0.0231(17) 0.029(2) -0.0027(15) -0.0007(16) 0.0042(15) C16 0.029(2) 0.031(2) 0.035(2) 0.0025(17) -0.0048(18) -0.0059(17) C17 0.042(2) 0.040(2) 0.029(2) 0.0009(18) -0.0078(18) 0.0009(19) C18 0.034(2) 0.038(2) 0.034(2) -0.0152(18) -0.0157(18) 0.0069(18) C19 0.0244(19) 0.032(2) 0.043(3) -0.0135(18) -0.0005(18) -0.0021(16) C20 0.0251(19) 0.0248(18) 0.036(2) -0.0054(16) 0.0049(17) -0.0010(16) C21 0.048(2) 0.0258(19) 0.038(2) 0.0083(17) 0.013(2) 0.0027(18) C22 0.067(3) 0.042(2) 0.041(3) 0.008(2) 0.000(2) 0.017(2) C23 0.0227(19) 0.038(2) 0.054(3) -0.0146(19) 0.0084(19) -0.0036(17) C24 0.026(2) 0.054(3) 0.058(3) -0.021(2) 0.002(2) -0.0102(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 C2 1.953(4) . ? Mo1 C1 1.955(4) . ? Mo1 C7 2.301(3) . ? Mo1 C3 2.310(3) . ? Mo1 C6 2.341(3) . ? Mo1 C4 2.353(4) . ? Mo1 C5 2.366(3) . ? Mo1 P2 2.4801(9) . ? Mo1 P1 2.5290(9) . ? Mo2 C9 1.956(4) . ? Mo2 C8 1.964(4) . ? Mo2 C13 2.320(3) . ? Mo2 C14 2.321(3) . ? Mo2 C10 2.337(3) . ? Mo2 C12 2.357(3) . ? Mo2 C11 2.365(3) . ? Mo2 P2 2.4967(8) . ? Mo2 P1 2.5047(9) . ? P1 C15 1.825(3) . ? P1 H100 1.29(3) . ? P2 O11 1.635(2) . ? P2 O10 1.637(2) . ? O1 C1 1.164(4) . ? O2 C2 1.163(4) . ? O8 C8 1.156(4) . ? O9 C9 1.157(4) . ? O10 C21 1.457(4) . ? O11 C23 1.446(4) . ? C3 C7 1.408(5) . ? C3 C4 1.414(5) . ? C3 H3A 0.9500 . ? C4 C5 1.413(5) . ? C4 H4A 0.9500 . ? C5 C6 1.390(5) . ? C5 H5A 0.9500 . ? C6 C7 1.400(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C10 C11 1.402(5) . ? C10 C14 1.406(5) . ? C10 H10A 0.9500 . ? C11 C12 1.394(5) . ? C11 H11A 0.9500 . ? C12 C13 1.397(5) . ? C12 H12A 0.9500 . ? C13 C14 1.397(5) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.384(4) . ? C15 C16 1.397(5) . ? C16 C17 1.374(5) . ? C16 H16A 0.9500 . ? C17 C18 1.388(5) . ? C17 H17A 0.9500 . ? C18 C19 1.388(5) . ? C18 H18A 0.9500 . ? C19 C20 1.379(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.491(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.498(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 74.88(15) . . ? C2 Mo1 C7 92.37(13) . . ? C1 Mo1 C7 103.18(14) . . ? C2 Mo1 C3 92.72(13) . . ? C1 Mo1 C3 137.36(14) . . ? C7 Mo1 C3 35.55(12) . . ? C2 Mo1 C6 123.08(14) . . ? C1 Mo1 C6 94.03(14) . . ? C7 Mo1 C6 35.09(12) . . ? C3 Mo1 C6 58.58(13) . . ? C2 Mo1 C4 124.05(14) . . ? C1 Mo1 C4 151.28(15) . . ? C7 Mo1 C4 58.59(13) . . ? C3 Mo1 C4 35.29(12) . . ? C6 Mo1 C4 58.00(13) . . ? C2 Mo1 C5 148.94(13) . . ? C1 Mo1 C5 117.70(15) . . ? C7 Mo1 C5 57.93(12) . . ? C3 Mo1 C5 58.26(13) . . ? C6 Mo1 C5 34.36(12) . . ? C4 Mo1 C5 34.84(12) . . ? C2 Mo1 P2 86.21(10) . . ? C1 Mo1 P2 116.94(11) . . ? C7 Mo1 P2 137.80(9) . . ? C3 Mo1 P2 102.32(10) . . ? C6 Mo1 P2 143.05(10) . . ? C4 Mo1 P2 87.77(9) . . ? C5 Mo1 P2 109.13(10) . . ? C2 Mo1 P1 125.03(10) . . ? C1 Mo1 P1 78.07(10) . . ? C7 Mo1 P1 140.42(9) . . ? C3 Mo1 P1 137.07(9) . . ? C6 Mo1 P1 105.61(10) . . ? C4 Mo1 P1 101.78(9) . . ? C5 Mo1 P1 86.01(9) . . ? P2 Mo1 P1 65.26(3) . . ? C9 Mo2 C8 77.94(16) . . ? C9 Mo2 C13 92.82(14) . . ? C8 Mo2 C13 107.51(14) . . ? C9 Mo2 C14 99.09(15) . . ? C8 Mo2 C14 142.54(13) . . ? C13 Mo2 C14 35.04(12) . . ? C9 Mo2 C10 132.19(16) . . ? C8 Mo2 C10 143.06(14) . . ? C13 Mo2 C10 58.19(13) . . ? C14 Mo2 C10 35.14(13) . . ? C9 Mo2 C12 119.54(13) . . ? C8 Mo2 C12 90.72(13) . . ? C13 Mo2 C12 34.75(12) . . ? C14 Mo2 C12 57.86(12) . . ? C10 Mo2 C12 57.63(12) . . ? C9 Mo2 C11 150.53(14) . . ? C8 Mo2 C11 108.37(14) . . ? C13 Mo2 C11 57.72(13) . . ? C14 Mo2 C11 57.93(13) . . ? C10 Mo2 C11 34.70(12) . . ? C12 Mo2 C11 34.35(12) . . ? C9 Mo2 P2 77.99(10) . . ? C8 Mo2 P2 117.27(10) . . ? C13 Mo2 P2 130.69(10) . . ? C14 Mo2 P2 98.06(9) . . ? C10 Mo2 P2 92.91(9) . . ? C12 Mo2 P2 150.51(9) . . ? C11 Mo2 P2 120.33(9) . . ? C9 Mo2 P1 114.27(11) . . ? C8 Mo2 P1 73.86(10) . . ? C13 Mo2 P1 152.12(10) . . ? C14 Mo2 P1 136.94(11) . . ? C10 Mo2 P1 103.37(10) . . ? C12 Mo2 P1 118.87(9) . . ? C11 Mo2 P1 94.95(9) . . ? P2 Mo2 P1 65.38(3) . . ? C15 P1 Mo2 115.71(11) . . ? C15 P1 Mo1 117.62(10) . . ? Mo2 P1 Mo1 107.32(3) . . ? C15 P1 H100 92.4(15) . . ? Mo2 P1 H100 117.4(14) . . ? Mo1 P1 H100 105.9(13) . . ? O11 P2 O10 101.62(11) . . ? O11 P2 Mo1 106.77(8) . . ? O10 P2 Mo1 119.18(9) . . ? O11 P2 Mo2 118.24(9) . . ? O10 P2 Mo2 102.39(8) . . ? Mo1 P2 Mo2 109.12(3) . . ? C21 O10 P2 122.2(2) . . ? C23 O11 P2 119.22(19) . . ? O1 C1 Mo1 177.6(3) . . ? O2 C2 Mo1 172.2(3) . . ? C7 C3 C4 107.6(3) . . ? C7 C3 Mo1 71.9(2) . . ? C4 C3 Mo1 74.0(2) . . ? C7 C3 H3A 126.2 . . ? C4 C3 H3A 126.2 . . ? Mo1 C3 H3A 119.8 . . ? C5 C4 C3 107.3(3) . . ? C5 C4 Mo1 73.1(2) . . ? C3 C4 Mo1 70.7(2) . . ? C5 C4 H4A 126.4 . . ? C3 C4 H4A 126.4 . . ? Mo1 C4 H4A 121.6 . . ? C6 C5 C4 108.6(3) . . ? C6 C5 Mo1 71.9(2) . . ? C4 C5 Mo1 72.1(2) . . ? C6 C5 H5A 125.7 . . ? C4 C5 H5A 125.7 . . ? Mo1 C5 H5A 122.0 . . ? C5 C6 C7 108.2(3) . . ? C5 C6 Mo1 73.8(2) . . ? C7 C6 Mo1 70.89(19) . . ? C5 C6 H6A 125.9 . . ? C7 C6 H6A 125.9 . . ? Mo1 C6 H6A 121.2 . . ? C6 C7 C3 108.3(3) . . ? C6 C7 Mo1 74.0(2) . . ? C3 C7 Mo1 72.57(19) . . ? C6 C7 H7A 125.9 . . ? C3 C7 H7A 125.9 . . ? Mo1 C7 H7A 119.4 . . ? O8 C8 Mo2 178.7(4) . . ? O9 C9 Mo2 176.7(3) . . ? C11 C10 C14 107.8(3) . . ? C11 C10 Mo2 73.7(2) . . ? C14 C10 Mo2 71.8(2) . . ? C11 C10 H10A 126.1 . . ? C14 C10 H10A 126.1 . . ? Mo2 C10 H10A 120.2 . . ? C12 C11 C10 108.0(3) . . ? C12 C11 Mo2 72.5(2) . . ? C10 C11 Mo2 71.6(2) . . ? C12 C11 H11A 126.0 . . ? C10 C11 H11A 126.0 . . ? Mo2 C11 H11A 121.6 . . ? C11 C12 C13 108.3(3) . . ? C11 C12 Mo2 73.14(19) . . ? C13 C12 Mo2 71.19(19) . . ? C11 C12 H12A 125.9 . . ? C13 C12 H12A 125.9 . . ? Mo2 C12 H12A 121.5 . . ? C12 C13 C14 108.2(3) . . ? C12 C13 Mo2 74.06(19) . . ? C14 C13 Mo2 72.5(2) . . ? C12 C13 H13A 125.9 . . ? C14 C13 H13A 125.9 . . ? Mo2 C13 H13A 119.3 . . ? C13 C14 C10 107.8(3) . . ? C13 C14 Mo2 72.4(2) . . ? C10 C14 Mo2 73.0(2) . . ? C13 C14 H14A 126.1 . . ? C10 C14 H14A 126.1 . . ? Mo2 C14 H14A 120.2 . . ? C20 C15 C16 118.0(3) . . ? C20 C15 P1 120.8(3) . . ? C16 C15 P1 121.2(2) . . ? C17 C16 C15 121.0(3) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C16 C17 C18 120.3(4) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C19 119.2(3) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C15 121.5(3) . . ? C19 C20 H20A 119.3 . . ? C15 C20 H20A 119.3 . . ? O10 C21 C22 110.3(3) . . ? O10 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? O10 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O11 C23 C24 110.2(3) . . ? O11 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? O11 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? 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 C9 Mo2 P1 C15 -169.09(16) . . . . ? C8 Mo2 P1 C15 122.57(16) . . . . ? C13 Mo2 P1 C15 25.5(2) . . . . ? C14 Mo2 P1 C15 -31.68(18) . . . . ? C10 Mo2 P1 C15 -19.29(15) . . . . ? C12 Mo2 P1 C15 40.88(15) . . . . ? C11 Mo2 P1 C15 14.85(15) . . . . ? P2 Mo2 P1 C15 -106.33(12) . . . . ? C9 Mo2 P1 Mo1 -35.54(13) . . . . ? C8 Mo2 P1 Mo1 -103.88(11) . . . . ? C13 Mo2 P1 Mo1 159.1(2) . . . . ? C14 Mo2 P1 Mo1 101.88(13) . . . . ? C10 Mo2 P1 Mo1 114.27(9) . . . . ? C12 Mo2 P1 Mo1 174.43(10) . . . . ? C11 Mo2 P1 Mo1 148.41(9) . . . . ? P2 Mo2 P1 Mo1 27.22(3) . . . . ? C2 Mo1 P1 C15 39.41(18) . . . . ? C1 Mo1 P1 C15 -22.31(17) . . . . ? C7 Mo1 P1 C15 -118.63(19) . . . . ? C3 Mo1 P1 C15 -173.57(18) . . . . ? C6 Mo1 P1 C15 -113.20(16) . . . . ? C4 Mo1 P1 C15 -172.95(16) . . . . ? C5 Mo1 P1 C15 -141.72(16) . . . . ? P2 Mo1 P1 C15 105.08(13) . . . . ? C2 Mo1 P1 Mo2 -93.12(12) . . . . ? C1 Mo1 P1 Mo2 -154.84(12) . . . . ? C7 Mo1 P1 Mo2 108.83(15) . . . . ? C3 Mo1 P1 Mo2 53.90(14) . . . . ? C6 Mo1 P1 Mo2 114.26(10) . . . . ? C4 Mo1 P1 Mo2 54.51(10) . . . . ? C5 Mo1 P1 Mo2 85.75(10) . . . . ? P2 Mo1 P1 Mo2 -27.45(3) . . . . ? C2 Mo1 P2 O11 -71.68(13) . . . . ? C1 Mo1 P2 O11 -142.60(15) . . . . ? C7 Mo1 P2 O11 17.67(17) . . . . ? C3 Mo1 P2 O11 20.28(13) . . . . ? C6 Mo1 P2 O11 73.60(18) . . . . ? C4 Mo1 P2 O11 52.66(13) . . . . ? C5 Mo1 P2 O11 80.66(13) . . . . ? P1 Mo1 P2 O11 156.71(10) . . . . ? C2 Mo1 P2 O10 42.48(13) . . . . ? C1 Mo1 P2 O10 -28.44(15) . . . . ? C7 Mo1 P2 O10 131.83(16) . . . . ? C3 Mo1 P2 O10 134.44(13) . . . . ? C6 Mo1 P2 O10 -172.24(17) . . . . ? C4 Mo1 P2 O10 166.82(13) . . . . ? C5 Mo1 P2 O10 -165.18(13) . . . . ? P1 Mo1 P2 O10 -89.13(9) . . . . ? C2 Mo1 P2 Mo2 159.46(10) . . . . ? C1 Mo1 P2 Mo2 88.54(12) . . . . ? C7 Mo1 P2 Mo2 -111.19(14) . . . . ? C3 Mo1 P2 Mo2 -108.58(9) . . . . ? C6 Mo1 P2 Mo2 -55.26(16) . . . . ? C4 Mo1 P2 Mo2 -76.20(10) . . . . ? C5 Mo1 P2 Mo2 -48.20(10) . . . . ? P1 Mo1 P2 Mo2 27.85(3) . . . . ? C9 Mo2 P2 O11 -26.27(15) . . . . ? C8 Mo2 P2 O11 -95.79(16) . . . . ? C13 Mo2 P2 O11 57.03(17) . . . . ? C14 Mo2 P2 O11 71.37(14) . . . . ? C10 Mo2 P2 O11 106.31(14) . . . . ? C12 Mo2 P2 O11 104.1(2) . . . . ? C11 Mo2 P2 O11 128.79(14) . . . . ? P1 Mo2 P2 O11 -150.31(10) . . . . ? C9 Mo2 P2 O10 -136.89(15) . . . . ? C8 Mo2 P2 O10 153.60(15) . . . . ? C13 Mo2 P2 O10 -53.59(16) . . . . ? C14 Mo2 P2 O10 -39.25(13) . . . . ? C10 Mo2 P2 O10 -4.31(13) . . . . ? C12 Mo2 P2 O10 -6.5(2) . . . . ? C11 Mo2 P2 O10 18.17(14) . . . . ? P1 Mo2 P2 O10 99.07(9) . . . . ? C9 Mo2 P2 Mo1 95.92(12) . . . . ? C8 Mo2 P2 Mo1 26.40(13) . . . . ? C13 Mo2 P2 Mo1 179.22(13) . . . . ? C14 Mo2 P2 Mo1 -166.44(10) . . . . ? C10 Mo2 P2 Mo1 -131.50(10) . . . . ? C12 Mo2 P2 Mo1 -133.70(18) . . . . ? C11 Mo2 P2 Mo1 -109.02(11) . . . . ? P1 Mo2 P2 Mo1 -28.12(3) . . . . ? O11 P2 O10 C21 52.5(3) . . . . ? Mo1 P2 O10 C21 -64.3(3) . . . . ? Mo2 P2 O10 C21 175.2(2) . . . . ? O10 P2 O11 C23 55.7(3) . . . . ? Mo1 P2 O11 C23 -178.7(2) . . . . ? Mo2 P2 O11 C23 -55.4(3) . . . . ? C2 Mo1 C1 O1 21(8) . . . . ? C7 Mo1 C1 O1 -67(8) . . . . ? C3 Mo1 C1 O1 -56(8) . . . . ? C6 Mo1 C1 O1 -102(8) . . . . ? C4 Mo1 C1 O1 -114(8) . . . . ? C5 Mo1 C1 O1 -128(8) . . . . ? P2 Mo1 C1 O1 99(8) . . . . ? P1 Mo1 C1 O1 153(8) . . . . ? C1 Mo1 C2 O2 -68(2) . . . . ? C7 Mo1 C2 O2 35(2) . . . . ? C3 Mo1 C2 O2 70(2) . . . . ? C6 Mo1 C2 O2 17(2) . . . . ? C4 Mo1 C2 O2 88(2) . . . . ? C5 Mo1 C2 O2 51(2) . . . . ? P2 Mo1 C2 O2 172(2) . . . . ? P1 Mo1 C2 O2 -132(2) . . . . ? C2 Mo1 C3 C7 -90.3(2) . . . . ? C1 Mo1 C3 C7 -19.8(3) . . . . ? C6 Mo1 C3 C7 37.4(2) . . . . ? C4 Mo1 C3 C7 115.2(3) . . . . ? C5 Mo1 C3 C7 78.0(2) . . . . ? P2 Mo1 C3 C7 -176.99(19) . . . . ? P1 Mo1 C3 C7 116.2(2) . . . . ? C2 Mo1 C3 C4 154.5(2) . . . . ? C1 Mo1 C3 C4 -135.0(3) . . . . ? C7 Mo1 C3 C4 -115.2(3) . . . . ? C6 Mo1 C3 C4 -77.8(2) . . . . ? C5 Mo1 C3 C4 -37.2(2) . . . . ? P2 Mo1 C3 C4 67.8(2) . . . . ? P1 Mo1 C3 C4 1.0(3) . . . . ? C7 C3 C4 C5 -0.1(4) . . . . ? Mo1 C3 C4 C5 64.4(2) . . . . ? C7 C3 C4 Mo1 -64.5(2) . . . . ? C2 Mo1 C4 C5 -147.0(2) . . . . ? C1 Mo1 C4 C5 -21.7(4) . . . . ? C7 Mo1 C4 C5 -77.8(2) . . . . ? C3 Mo1 C4 C5 -115.8(3) . . . . ? C6 Mo1 C4 C5 -36.3(2) . . . . ? P2 Mo1 C4 C5 129.0(2) . . . . ? P1 Mo1 C4 C5 64.9(2) . . . . ? C2 Mo1 C4 C3 -31.2(3) . . . . ? C1 Mo1 C4 C3 94.1(3) . . . . ? C7 Mo1 C4 C3 38.1(2) . . . . ? C6 Mo1 C4 C3 79.6(2) . . . . ? C5 Mo1 C4 C3 115.8(3) . . . . ? P2 Mo1 C4 C3 -115.1(2) . . . . ? P1 Mo1 C4 C3 -179.3(2) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? Mo1 C4 C5 C6 63.0(3) . . . . ? C3 C4 C5 Mo1 -62.8(2) . . . . ? C2 Mo1 C5 C6 -56.3(4) . . . . ? C1 Mo1 C5 C6 51.2(3) . . . . ? C7 Mo1 C5 C6 -37.4(2) . . . . ? C3 Mo1 C5 C6 -79.6(2) . . . . ? C4 Mo1 C5 C6 -117.2(3) . . . . ? P2 Mo1 C5 C6 -172.47(19) . . . . ? P1 Mo1 C5 C6 125.5(2) . . . . ? C2 Mo1 C5 C4 60.9(4) . . . . ? C1 Mo1 C5 C4 168.4(2) . . . . ? C7 Mo1 C5 C4 79.8(2) . . . . ? C3 Mo1 C5 C4 37.7(2) . . . . ? C6 Mo1 C5 C4 117.2(3) . . . . ? P2 Mo1 C5 C4 -55.2(2) . . . . ? P1 Mo1 C5 C4 -117.3(2) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? Mo1 C5 C6 C7 63.0(2) . . . . ? C4 C5 C6 Mo1 -63.2(3) . . . . ? C2 Mo1 C6 C5 149.2(2) . . . . ? C1 Mo1 C6 C5 -136.3(2) . . . . ? C7 Mo1 C6 C5 116.4(3) . . . . ? C3 Mo1 C6 C5 78.5(2) . . . . ? C4 Mo1 C6 C5 36.8(2) . . . . ? P2 Mo1 C6 C5 11.9(3) . . . . ? P1 Mo1 C6 C5 -57.5(2) . . . . ? C2 Mo1 C6 C7 32.7(3) . . . . ? C1 Mo1 C6 C7 107.3(2) . . . . ? C3 Mo1 C6 C7 -37.9(2) . . . . ? C4 Mo1 C6 C7 -79.7(2) . . . . ? C5 Mo1 C6 C7 -116.4(3) . . . . ? P2 Mo1 C6 C7 -104.6(2) . . . . ? P1 Mo1 C6 C7 -174.0(2) . . . . ? C5 C6 C7 C3 0.2(4) . . . . ? Mo1 C6 C7 C3 65.0(2) . . . . ? C5 C6 C7 Mo1 -64.8(3) . . . . ? C4 C3 C7 C6 0.0(4) . . . . ? Mo1 C3 C7 C6 -65.9(2) . . . . ? C4 C3 C7 Mo1 65.9(2) . . . . ? C2 Mo1 C7 C6 -153.0(2) . . . . ? C1 Mo1 C7 C6 -78.0(2) . . . . ? C3 Mo1 C7 C6 115.6(3) . . . . ? C4 Mo1 C7 C6 77.8(2) . . . . ? C5 Mo1 C7 C6 36.6(2) . . . . ? P2 Mo1 C7 C6 120.0(2) . . . . ? P1 Mo1 C7 C6 9.1(3) . . . . ? C2 Mo1 C7 C3 91.4(2) . . . . ? C1 Mo1 C7 C3 166.4(2) . . . . ? C6 Mo1 C7 C3 -115.6(3) . . . . ? C4 Mo1 C7 C3 -37.8(2) . . . . ? C5 Mo1 C7 C3 -79.0(2) . . . . ? P2 Mo1 C7 C3 4.4(3) . . . . ? P1 Mo1 C7 C3 -106.5(2) . . . . ? C9 Mo2 C8 O8 -179(100) . . . . ? C13 Mo2 C8 O8 92(14) . . . . ? C14 Mo2 C8 O8 92(14) . . . . ? C10 Mo2 C8 O8 32(14) . . . . ? C12 Mo2 C8 O8 61(14) . . . . ? C11 Mo2 C8 O8 31(14) . . . . ? P2 Mo2 C8 O8 -110(14) . . . . ? P1 Mo2 C8 O8 -59(14) . . . . ? C8 Mo2 C9 O9 -84(7) . . . . ? C13 Mo2 C9 O9 23(7) . . . . ? C14 Mo2 C9 O9 58(7) . . . . ? C10 Mo2 C9 O9 72(7) . . . . ? C12 Mo2 C9 O9 0(7) . . . . ? C11 Mo2 C9 O9 22(7) . . . . ? P2 Mo2 C9 O9 154(7) . . . . ? P1 Mo2 C9 O9 -150(7) . . . . ? C9 Mo2 C10 C11 -139.0(2) . . . . ? C8 Mo2 C10 C11 -1.6(4) . . . . ? C13 Mo2 C10 C11 -78.0(2) . . . . ? C14 Mo2 C10 C11 -115.5(3) . . . . ? C12 Mo2 C10 C11 -36.7(2) . . . . ? P2 Mo2 C10 C11 144.6(2) . . . . ? P1 Mo2 C10 C11 79.2(2) . . . . ? C9 Mo2 C10 C14 -23.5(3) . . . . ? C8 Mo2 C10 C14 113.9(3) . . . . ? C13 Mo2 C10 C14 37.6(2) . . . . ? C12 Mo2 C10 C14 78.8(2) . . . . ? C11 Mo2 C10 C14 115.5(3) . . . . ? P2 Mo2 C10 C14 -99.9(2) . . . . ? P1 Mo2 C10 C14 -165.26(19) . . . . ? C14 C10 C11 C12 -0.4(4) . . . . ? Mo2 C10 C11 C12 63.8(2) . . . . ? C14 C10 C11 Mo2 -64.2(2) . . . . ? C9 Mo2 C11 C12 -35.6(4) . . . . ? C8 Mo2 C11 C12 62.5(2) . . . . ? C13 Mo2 C11 C12 -37.0(2) . . . . ? C14 Mo2 C11 C12 -78.7(2) . . . . ? C10 Mo2 C11 C12 -116.5(3) . . . . ? P2 Mo2 C11 C12 -158.63(17) . . . . ? P1 Mo2 C11 C12 137.08(19) . . . . ? C9 Mo2 C11 C10 80.9(4) . . . . ? C8 Mo2 C11 C10 179.0(2) . . . . ? C13 Mo2 C11 C10 79.5(2) . . . . ? C14 Mo2 C11 C10 37.8(2) . . . . ? C12 Mo2 C11 C10 116.5(3) . . . . ? P2 Mo2 C11 C10 -42.1(2) . . . . ? P1 Mo2 C11 C10 -106.4(2) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? Mo2 C11 C12 C13 63.0(2) . . . . ? C10 C11 C12 Mo2 -63.2(2) . . . . ? C9 Mo2 C12 C11 160.8(2) . . . . ? C8 Mo2 C12 C11 -122.7(2) . . . . ? C13 Mo2 C12 C11 116.7(3) . . . . ? C14 Mo2 C12 C11 78.9(2) . . . . ? C10 Mo2 C12 C11 37.1(2) . . . . ? P2 Mo2 C12 C11 39.7(3) . . . . ? P1 Mo2 C12 C11 -50.8(2) . . . . ? C9 Mo2 C12 C13 44.1(3) . . . . ? C8 Mo2 C12 C13 120.6(2) . . . . ? C14 Mo2 C12 C13 -37.7(2) . . . . ? C10 Mo2 C12 C13 -79.6(2) . . . . ? C11 Mo2 C12 C13 -116.7(3) . . . . ? P2 Mo2 C12 C13 -77.0(3) . . . . ? P1 Mo2 C12 C13 -167.46(19) . . . . ? C11 C12 C13 C14 0.8(4) . . . . ? Mo2 C12 C13 C14 65.0(2) . . . . ? C11 C12 C13 Mo2 -64.2(2) . . . . ? C9 Mo2 C13 C12 -142.7(2) . . . . ? C8 Mo2 C13 C12 -64.4(2) . . . . ? C14 Mo2 C13 C12 115.5(3) . . . . ? C10 Mo2 C13 C12 77.8(2) . . . . ? C11 Mo2 C13 C12 36.6(2) . . . . ? P2 Mo2 C13 C12 140.76(18) . . . . ? P1 Mo2 C13 C12 24.0(3) . . . . ? C9 Mo2 C13 C14 101.9(2) . . . . ? C8 Mo2 C13 C14 -179.9(2) . . . . ? C10 Mo2 C13 C14 -37.7(2) . . . . ? C12 Mo2 C13 C14 -115.5(3) . . . . ? C11 Mo2 C13 C14 -78.9(2) . . . . ? P2 Mo2 C13 C14 25.3(3) . . . . ? P1 Mo2 C13 C14 -91.5(3) . . . . ? C12 C13 C14 C10 -1.0(4) . . . . ? Mo2 C13 C14 C10 65.0(2) . . . . ? C12 C13 C14 Mo2 -66.0(2) . . . . ? C11 C10 C14 C13 0.9(4) . . . . ? Mo2 C10 C14 C13 -64.6(2) . . . . ? C11 C10 C14 Mo2 65.5(2) . . . . ? C9 Mo2 C14 C13 -81.9(2) . . . . ? C8 Mo2 C14 C13 0.1(4) . . . . ? C10 Mo2 C14 C13 115.5(3) . . . . ? C12 Mo2 C14 C13 37.4(2) . . . . ? C11 Mo2 C14 C13 78.2(2) . . . . ? P2 Mo2 C14 C13 -160.9(2) . . . . ? P1 Mo2 C14 C13 136.8(2) . . . . ? C9 Mo2 C14 C10 162.6(2) . . . . ? C8 Mo2 C14 C10 -115.4(3) . . . . ? C13 Mo2 C14 C10 -115.5(3) . . . . ? C12 Mo2 C14 C10 -78.1(2) . . . . ? C11 Mo2 C14 C10 -37.3(2) . . . . ? P2 Mo2 C14 C10 83.6(2) . . . . ? P1 Mo2 C14 C10 21.3(3) . . . . ? Mo2 P1 C15 C20 -123.5(2) . . . . ? Mo1 P1 C15 C20 107.9(2) . . . . ? Mo2 P1 C15 C16 59.0(3) . . . . ? Mo1 P1 C15 C16 -69.6(3) . . . . ? C20 C15 C16 C17 -1.9(5) . . . . ? P1 C15 C16 C17 175.6(3) . . . . ? C15 C16 C17 C18 0.2(5) . . . . ? C16 C17 C18 C19 1.4(5) . . . . ? C17 C18 C19 C20 -1.3(5) . . . . ? C18 C19 C20 C15 -0.4(5) . . . . ? C16 C15 C20 C19 2.0(5) . . . . ? P1 C15 C20 C19 -175.5(2) . . . . ? P2 O10 C21 C22 121.2(3) . . . . ? P2 O11 C23 C24 169.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.372 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.083 data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 As Mo2 O4 P' _chemical_formula_weight 572.07 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' 'As' 'As' 0.0499 2.0058 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.945(4) _cell_length_b 21.547(6) _cell_length_c 8.022(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1891.8(15) _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 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 3.162 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5849 _exptl_absorpt_correction_T_max 0.9395 _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 3954 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.1909 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3002 _reflns_number_gt 1717 _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^)+(0.0716P)^2^+14.8665P] 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 0.04(6) _refine_ls_number_reflns 3002 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1658 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2039 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.0001(3) 0.78134(9) 0.7644(2) 0.0223(5) Uani 1 1 d . . . Mo2 Mo -0.0007(2) 0.96929(9) 0.8586(2) 0.0216(5) Uani 1 1 d . . . As1 As 0.1354(2) 0.87094(11) 0.8815(3) 0.0211(6) Uani 1 1 d . . . P1 P -0.0401(6) 0.8864(3) 0.6457(8) 0.0257(16) Uani 1 1 d . . . H10A H -0.159(12) 0.8899(4) 0.593(5) 0.031 Uiso 1 1 calc R . . H10B H 0.034(8) 0.8958(10) 0.511(14) 0.031 Uiso 1 1 calc R . . O1 O -0.2804(19) 0.8025(9) 0.811(2) 0.048(5) Uiso 1 1 d . . . C1 C -0.173(3) 0.7941(13) 0.792(3) 0.041(7) Uiso 1 1 d . . . O2 O -0.0428(17) 0.7710(8) 1.152(2) 0.048(5) Uiso 1 1 d . . . C2 C -0.020(3) 0.7763(10) 1.003(3) 0.031(6) Uiso 1 1 d . . . O3 O 0.0085(19) 1.0483(7) 0.5324(18) 0.034(4) Uiso 1 1 d . . . C3 C 0.006(3) 1.0197(11) 0.643(3) 0.037(6) Uiso 1 1 d . . . O4 O 0.2587(16) 1.0278(8) 0.887(2) 0.047(5) Uiso 1 1 d . . . C4 C 0.165(2) 1.0039(10) 0.878(3) 0.025(6) Uiso 1 1 d . . . C5 C 0.288(2) 0.8737(13) 0.756(3) 0.042(7) Uiso 1 1 d . . . H5A H 0.3316 0.8344 0.7705 0.063 Uiso 1 1 calc R . . H5B H 0.3386 0.9079 0.7980 0.063 Uiso 1 1 calc R . . H5C H 0.2701 0.8803 0.6381 0.063 Uiso 1 1 calc R . . C6 C 0.204(2) 0.8606(11) 1.107(3) 0.030(6) Uiso 1 1 d . . . H6A H 0.2689 0.8911 1.1247 0.044 Uiso 1 1 calc R . . H6B H 0.2370 0.8187 1.1188 0.044 Uiso 1 1 calc R . . H6C H 0.1391 0.8670 1.1899 0.044 Uiso 1 1 calc R . . C7 C 0.090(3) 0.6825(14) 0.755(4) 0.054(9) Uiso 1 1 d . . . H7 H 0.1033 0.6587 0.8532 0.065 Uiso 1 1 calc R . . C8 C 0.174(3) 0.7220(14) 0.683(4) 0.056(9) Uiso 1 1 d . . . H8 H 0.2535 0.7307 0.7238 0.067 Uiso 1 1 calc R . . C9 C 0.124(3) 0.7461(14) 0.545(4) 0.052(8) Uiso 1 1 d . . . H9 H 0.1623 0.7751 0.4718 0.063 Uiso 1 1 calc R . . C10 C 0.005(4) 0.7207(12) 0.525(3) 0.053(7) Uiso 1 1 d . . . H10 H -0.0492 0.7282 0.4348 0.064 Uiso 1 1 calc R . . C11 C -0.019(3) 0.6829(11) 0.662(3) 0.036(7) Uiso 1 1 d . . . H11 H -0.0928 0.6618 0.6871 0.044 Uiso 1 1 calc R . . C12 C -0.195(2) 0.9478(12) 0.964(3) 0.036(7) Uiso 1 1 d . . . H12 H -0.2482 0.9199 0.9081 0.043 Uiso 1 1 calc R . . C13 C -0.112(2) 0.9323(12) 1.091(3) 0.041(7) Uiso 1 1 d . . . H13 H -0.1014 0.8923 1.1388 0.050 Uiso 1 1 calc R . . C14 C -0.048(2) 0.9858(11) 1.136(3) 0.035(6) Uiso 1 1 d . . . H14 H 0.0160 0.9881 1.2156 0.042 Uiso 1 1 calc R . . C15 C -0.096(2) 1.0375(13) 1.037(3) 0.038(7) Uiso 1 1 d . . . H15 H -0.0714 1.0798 1.0412 0.046 Uiso 1 1 calc R . . C16 C -0.186(3) 1.0106(14) 0.936(4) 0.047(9) Uiso 1 1 d . . . H16 H -0.2346 1.0328 0.8580 0.056 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 0.0217(10) 0.0213(10) 0.0240(11) 0.0000(8) -0.0017(15) 0.0000(12) Mo2 0.0209(10) 0.0219(10) 0.0219(10) -0.0013(9) 0.0019(15) 0.0033(12) As1 0.0185(11) 0.0220(12) 0.0228(13) -0.0007(11) -0.0011(14) 0.0012(11) P1 0.032(4) 0.023(4) 0.022(3) -0.003(3) -0.005(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.93(3) . ? Mo1 C2 1.93(2) . ? Mo1 C11 2.28(2) . ? Mo1 C10 2.32(3) . ? Mo1 C7 2.35(3) . ? Mo1 C9 2.35(3) . ? Mo1 C8 2.39(3) . ? Mo1 P1 2.495(6) . ? Mo1 As1 2.609(3) . ? Mo2 C4 1.96(2) . ? Mo2 C3 2.04(2) . ? Mo2 C16 2.30(3) . ? Mo2 C15 2.30(3) . ? Mo2 C14 2.31(3) . ? Mo2 C12 2.34(3) . ? Mo2 C13 2.37(3) . ? Mo2 P1 2.508(6) . ? Mo2 As1 2.597(3) . ? As1 C5 1.95(2) . ? As1 C6 1.97(2) . ? O1 C1 1.19(3) . ? O2 C2 1.22(3) . ? O3 C3 1.08(2) . ? O4 C4 1.15(3) . ? C7 C8 1.38(4) . ? C7 C11 1.40(4) . ? C8 C9 1.34(4) . ? C9 C10 1.43(5) . ? C10 C11 1.39(3) . ? C12 C16 1.37(3) . ? C12 C13 1.41(4) . ? C13 C14 1.40(3) . ? C14 C15 1.46(3) . ? C15 C16 1.41(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 77.5(12) . . ? C1 Mo1 C11 94.9(11) . . ? C2 Mo1 C11 107.1(9) . . ? C1 Mo1 C10 101.4(13) . . ? C2 Mo1 C10 142.2(9) . . ? C11 Mo1 C10 35.1(9) . . ? C1 Mo1 C7 123.0(11) . . ? C2 Mo1 C7 91.6(11) . . ? C11 Mo1 C7 35.2(9) . . ? C10 Mo1 C7 56.9(11) . . ? C1 Mo1 C9 134.5(11) . . ? C2 Mo1 C9 142.2(11) . . ? C11 Mo1 C9 58.9(11) . . ? C10 Mo1 C9 35.5(12) . . ? C7 Mo1 C9 56.0(11) . . ? C1 Mo1 C8 153.2(11) . . ? C2 Mo1 C8 109.4(11) . . ? C11 Mo1 C8 58.3(10) . . ? C10 Mo1 C8 56.8(12) . . ? C7 Mo1 C8 34.0(9) . . ? C9 Mo1 C8 32.7(10) . . ? C1 Mo1 P1 75.1(8) . . ? C2 Mo1 P1 114.2(7) . . ? C11 Mo1 P1 133.6(6) . . ? C10 Mo1 P1 101.5(7) . . ? C7 Mo1 P1 152.3(8) . . ? C9 Mo1 P1 96.2(8) . . ? C8 Mo1 P1 121.4(8) . . ? C1 Mo1 As1 114.4(8) . . ? C2 Mo1 As1 75.4(7) . . ? C11 Mo1 As1 150.2(7) . . ? C10 Mo1 As1 134.5(9) . . ? C7 Mo1 As1 116.4(8) . . ? C9 Mo1 As1 100.3(8) . . ? C8 Mo1 As1 92.4(8) . . ? P1 Mo1 As1 64.26(16) . . ? C4 Mo2 C3 80.3(11) . . ? C4 Mo2 C16 130.1(9) . . ? C3 Mo2 C16 93.2(11) . . ? C4 Mo2 C15 97.1(10) . . ? C3 Mo2 C15 101.8(10) . . ? C16 Mo2 C15 35.6(9) . . ? C4 Mo2 C14 94.0(10) . . ? C3 Mo2 C14 137.8(9) . . ? C16 Mo2 C14 58.9(10) . . ? C15 Mo2 C14 37.0(8) . . ? C4 Mo2 C12 152.3(10) . . ? C3 Mo2 C12 116.5(11) . . ? C16 Mo2 C12 34.5(8) . . ? C15 Mo2 C12 59.3(9) . . ? C14 Mo2 C12 58.5(9) . . ? C4 Mo2 C13 122.6(10) . . ? C3 Mo2 C13 149.9(11) . . ? C16 Mo2 C13 57.6(10) . . ? C15 Mo2 C13 59.4(10) . . ? C14 Mo2 C13 34.7(8) . . ? C12 Mo2 C13 34.8(9) . . ? C4 Mo2 P1 118.9(7) . . ? C3 Mo2 P1 79.0(7) . . ? C16 Mo2 P1 107.9(7) . . ? C15 Mo2 P1 143.2(7) . . ? C14 Mo2 P1 136.6(6) . . ? C12 Mo2 P1 87.1(7) . . ? C13 Mo2 P1 102.1(6) . . ? C4 Mo2 As1 77.1(6) . . ? C3 Mo2 As1 118.2(8) . . ? C16 Mo2 As1 143.4(7) . . ? C15 Mo2 As1 137.4(7) . . ? C14 Mo2 As1 100.7(6) . . ? C12 Mo2 As1 109.6(6) . . ? C13 Mo2 As1 88.0(7) . . ? P1 Mo2 As1 64.27(16) . . ? C5 As1 C6 98.7(10) . . ? C5 As1 Mo2 115.5(8) . . ? C6 As1 Mo2 112.0(7) . . ? C5 As1 Mo1 108.9(8) . . ? C6 As1 Mo1 117.6(7) . . ? Mo2 As1 Mo1 104.61(11) . . ? Mo1 P1 Mo2 110.8(2) . . ? O1 C1 Mo1 179(3) . . ? O2 C2 Mo1 174(2) . . ? O3 C3 Mo2 177(2) . . ? O4 C4 Mo2 176(2) . . ? C8 C7 C11 110(3) . . ? C8 C7 Mo1 74.5(18) . . ? C11 C7 Mo1 69.9(16) . . ? C9 C8 C7 108(3) . . ? C9 C8 Mo1 72.4(19) . . ? C7 C8 Mo1 71.5(18) . . ? C8 C9 C10 108(3) . . ? C8 C9 Mo1 74.9(19) . . ? C10 C9 Mo1 71.0(17) . . ? C11 C10 C9 108(3) . . ? C11 C10 Mo1 70.9(15) . . ? C9 C10 Mo1 73.5(17) . . ? C10 C11 C7 105(3) . . ? C10 C11 Mo1 73.9(15) . . ? C7 C11 Mo1 74.8(16) . . ? C16 C12 C13 108(3) . . ? C16 C12 Mo2 71.3(17) . . ? C13 C12 Mo2 73.8(15) . . ? C14 C13 C12 108(2) . . ? C14 C13 Mo2 70.3(15) . . ? C12 C13 Mo2 71.5(15) . . ? C13 C14 C15 108(2) . . ? C13 C14 Mo2 75.0(16) . . ? C15 C14 Mo2 71.3(15) . . ? C16 C15 C14 104(2) . . ? C16 C15 Mo2 72.2(16) . . ? C14 C15 Mo2 71.7(15) . . ? C12 C16 C15 111(3) . . ? C12 C16 Mo2 74.2(17) . . ? C15 C16 Mo2 72.3(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.940 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.237