# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 440/071 data_c2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Mo N2 O7 P' _chemical_formula_weight 653.44 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' 'N' 'N' 0.0061 0.0033 '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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 14.860(10) _cell_length_b 13.641(2) _cell_length_c 15.399(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.81(2) _cell_angle_gamma 90.00 _cell_volume 3031(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.934 _cell_measurement_theta_max 12.522 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 3937 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.95 _reflns_number_total 3794 _reflns_number_gt 2150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction MolEN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0570P)^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 -0.05(12) _refine_ls_number_reflns 3794 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 1.139 _refine_ls_shift/su_mean 0.120 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 Mo Mo 0.24733(4) 0.2511(3) 0.40375(3) 0.0490(2) Uani 1 d . . . P P 0.11406(10) 0.2538(5) 0.26475(9) 0.0378(4) Uani 1 d . . . O1 O 0.3923(3) 0.2529(15) 0.2823(3) 0.0737(15) Uani 1 d . . . N1 N 0.3214(11) 0.3300(10) -0.0897(10) 0.057(5) Uani 1 d . . . N2 N 0.3206(11) 0.1708(9) -0.0938(9) 0.049(4) Uani 1 d . . . O2 O 0.2547(13) 0.0207(15) 0.3999(11) 0.106(7) Uani 1 d . . . O3 O 0.4186(5) 0.261(2) 0.5688(4) 0.145(5) Uani 1 d . . . O4 O 0.1133(4) 0.258(2) 0.5363(4) 0.116(3) Uani 1 d . . . O5 O 0.2549(14) 0.4854(12) 0.4058(11) 0.106(8) Uani 1 d . . . O6 O 0.3140(13) 0.0808(9) -0.0674(11) 0.086(6) Uani 1 d . . . O7 O 0.3160(13) 0.4203(9) -0.0725(9) 0.078(5) Uani 1 d . . . C1 C 0.3392(4) 0.2478(17) 0.3247(4) 0.049(2) Uani 1 d . . . C2 C 0.2541(13) 0.1098(16) 0.4028(12) 0.067(6) Uani 1 d . . . C3 C 0.3560(6) 0.241(2) 0.5095(5) 0.077(4) Uani 1 d . . . C4 C 0.1596(5) 0.254(2) 0.4889(5) 0.076(3) Uani 1 d . . . C5 C 0.2477(13) 0.4052(17) 0.4031(9) 0.065(6) Uani 1 d . . . C6 C 0.1613(4) 0.2461(16) 0.1651(3) 0.0347(19) Uani 1 d . . . C7 C 0.1824(13) 0.1678(11) 0.1249(11) 0.044(4) Uani 1 d . . . H7 H 0.1620 0.1078 0.1418 0.052 Uiso 1 calc R . . C8 C 0.2314(11) 0.1659(12) 0.0605(11) 0.038(4) Uani 1 d . . . H8 H 0.2495 0.1068 0.0398 0.045 Uiso 1 calc R . . C9 C 0.2541(4) 0.2560(17) 0.0259(3) 0.0377(16) Uani 1 d . . . C10 C 0.2294(13) 0.3413(13) 0.0623(12) 0.048(5) Uani 1 d . . . H10 H 0.2415 0.4008 0.0379 0.058 Uiso 1 calc R . . C11 C 0.1870(11) 0.3426(11) 0.1338(11) 0.038(4) Uani 1 d . . . H11 H 0.1755 0.4009 0.1605 0.045 Uiso 1 calc R . . C12 C 0.2979(4) 0.2469(14) -0.0504(4) 0.0372(18) Uani 1 d . . . C13 C 0.3384(10) 0.2079(12) -0.1815(9) 0.061(4) Uani 1 d . . . C14 C 0.3747(10) 0.3091(12) -0.1605(11) 0.060(4) Uani 1 d . . . C15 C 0.2424(8) 0.2082(12) -0.2533(6) 0.131(8) Uani 1 d . . . H15A H 0.2034 0.2587 -0.2388 0.196 Uiso 1 calc R . . H15B H 0.2128 0.1457 -0.2530 0.196 Uiso 1 calc R . . H15C H 0.2528 0.2204 -0.3115 0.196 Uiso 1 calc R . . C16 C 0.389(2) 0.1314(11) -0.2162(15) 0.183(15) Uani 1 d . . . H16A H 0.3523 0.0731 -0.2278 0.275 Uiso 1 calc R . . H16B H 0.4460 0.1174 -0.1730 0.275 Uiso 1 calc R . . H16C H 0.4033 0.1535 -0.2708 0.275 Uiso 1 calc R . . C17 C 0.3617(15) 0.3842(14) -0.2275(8) 0.107(6) Uani 1 d . . . H17A H 0.3863 0.4450 -0.2006 0.160 Uiso 1 calc R . . H17B H 0.2967 0.3917 -0.2542 0.160 Uiso 1 calc R . . H17C H 0.3932 0.3662 -0.2727 0.160 Uiso 1 calc R . . C18 C 0.4805(6) 0.3110(9) -0.1163(6) 0.078(3) Uani 1 d . . . H18A H 0.4997 0.3772 -0.1006 0.117 Uiso 1 calc R . . H18B H 0.5140 0.2859 -0.1576 0.117 Uiso 1 calc R . . H18C H 0.4931 0.2711 -0.0634 0.117 Uiso 1 calc R . . C19 C 0.0342(13) 0.1460(13) 0.2440(12) 0.045(5) Uani 1 d . . . C20 C -0.0188(12) 0.1217(12) 0.1597(11) 0.049(4) Uani 1 d . . . H20 H -0.0098 0.1507 0.1079 0.058 Uiso 1 calc R . . C21 C -0.0870(15) 0.0502(15) 0.1583(14) 0.075(7) Uani 1 d . . . H21 H -0.1286 0.0381 0.1038 0.090 Uiso 1 calc R . . C22 C -0.0974(15) -0.0030(16) 0.2302(16) 0.090(8) Uani 1 d . . . H22 H -0.1367 -0.0569 0.2230 0.108 Uiso 1 calc R . . C23 C -0.0503(18) 0.0241(17) 0.310(2) 0.080(8) Uani 1 d . . . H23 H -0.0635 -0.0035 0.3607 0.097 Uiso 1 calc R . . C24 C 0.0192(13) 0.0941(13) 0.3186(12) 0.057(5) Uani 1 d . . . H24 H 0.0568 0.1070 0.3750 0.069 Uiso 1 calc R . . C25 C 0.0316(13) 0.3529(12) 0.2511(12) 0.040(4) Uani 1 d . . . C26 C -0.0221(15) 0.3783(13) 0.1681(14) 0.060(5) Uani 1 d . . . H26 H -0.0163 0.3395 0.1201 0.072 Uiso 1 calc R . . C27 C -0.0832(14) 0.4553(12) 0.1494(14) 0.062(5) Uani 1 d . . . H27 H -0.1108 0.4755 0.0915 0.074 Uiso 1 calc R . . C28 C -0.1000(12) 0.4995(13) 0.2240(12) 0.069(6) Uani 1 d . . . H28 H -0.1491 0.5433 0.2174 0.083 Uiso 1 calc R . . C29 C -0.0448(17) 0.4805(15) 0.3103(16) 0.073(7) Uani 1 d . . . H29 H -0.0504 0.5195 0.3582 0.088 Uiso 1 calc R . . C30 C 0.0185(12) 0.4025(13) 0.3238(13) 0.066(6) Uani 1 d . . . H30 H 0.0508 0.3850 0.3812 0.079 Uiso 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 Mo 0.0396(3) 0.0742(5) 0.0339(2) 0.0014(12) 0.01012(19) -0.0007(13) P 0.0348(8) 0.0451(11) 0.0359(7) -0.006(3) 0.0129(6) -0.011(3) O1 0.061(3) 0.095(4) 0.075(3) 0.005(13) 0.034(3) 0.017(12) N1 0.073(11) 0.052(10) 0.061(9) 0.003(7) 0.046(8) 0.023(7) N2 0.061(10) 0.048(9) 0.041(7) -0.007(6) 0.022(6) 0.017(7) O2 0.123(17) 0.105(15) 0.104(14) 0.008(9) 0.054(13) 0.004(10) O3 0.072(4) 0.281(15) 0.063(3) -0.049(12) -0.021(3) 0.037(13) O4 0.077(4) 0.222(10) 0.061(3) -0.040(12) 0.038(3) -0.016(16) O5 0.15(2) 0.063(11) 0.112(15) -0.033(8) 0.037(14) -0.028(10) O6 0.134(15) 0.039(8) 0.115(12) 0.003(7) 0.089(11) 0.016(8) O7 0.129(14) 0.040(8) 0.090(10) 0.005(6) 0.076(10) 0.019(8) C1 0.038(3) 0.059(6) 0.046(3) -0.023(9) 0.003(3) 0.009(10) C2 0.061(10) 0.065(12) 0.085(12) -0.006(8) 0.041(9) 0.015(8) C3 0.071(5) 0.113(13) 0.046(4) -0.009(9) 0.014(4) -0.028(11) C4 0.056(4) 0.130(9) 0.044(4) 0.045(10) 0.012(3) 0.001(14) C5 0.074(12) 0.082(14) 0.036(7) -0.032(8) 0.006(6) 0.016(9) C6 0.034(3) 0.039(5) 0.032(2) 0.008(7) 0.010(2) -0.015(8) C7 0.058(9) 0.024(7) 0.048(8) 0.009(6) 0.010(6) -0.010(6) C8 0.029(8) 0.045(11) 0.042(9) -0.018(7) 0.016(7) -0.001(7) C9 0.037(3) 0.043(4) 0.034(3) 0.015(8) 0.011(2) 0.014(10) C10 0.069(13) 0.035(11) 0.044(10) -0.017(8) 0.020(10) -0.006(9) C11 0.035(7) 0.052(9) 0.033(6) -0.006(5) 0.020(5) -0.014(6) C12 0.040(3) 0.034(5) 0.040(3) 0.023(7) 0.013(2) 0.004(8) C13 0.090(11) 0.051(7) 0.059(7) -0.006(5) 0.052(7) -0.014(7) C14 0.082(10) 0.045(7) 0.070(8) 0.000(6) 0.049(7) 0.008(7) C15 0.100(8) 0.25(2) 0.041(4) -0.001(7) 0.005(5) -0.076(11) C16 0.38(4) 0.039(8) 0.22(2) 0.043(11) 0.24(3) 0.093(14) C17 0.158(14) 0.140(15) 0.039(5) -0.001(7) 0.056(7) -0.025(12) C18 0.048(5) 0.122(9) 0.070(6) -0.012(6) 0.026(4) -0.007(5) C19 0.042(10) 0.047(9) 0.050(10) 0.012(7) 0.021(8) 0.005(8) C20 0.031(7) 0.065(11) 0.044(7) -0.011(7) -0.002(5) -0.009(7) C21 0.048(11) 0.091(15) 0.077(12) -0.033(10) -0.004(9) -0.015(10) C22 0.059(13) 0.082(14) 0.141(19) 0.041(12) 0.049(13) -0.021(10) C23 0.074(15) 0.071(18) 0.10(2) 0.009(16) 0.038(15) -0.026(13) C24 0.060(11) 0.061(11) 0.050(9) -0.002(7) 0.012(7) 0.006(8) C25 0.033(9) 0.044(9) 0.045(8) 0.009(6) 0.016(7) 0.000(7) C26 0.061(11) 0.050(10) 0.071(11) -0.012(8) 0.023(9) 0.001(9) C27 0.051(10) 0.056(10) 0.076(10) -0.025(8) 0.011(8) 0.005(8) C28 0.047(10) 0.062(11) 0.087(12) 0.030(9) -0.004(9) 0.012(8) C29 0.063(18) 0.090(16) 0.075(16) -0.018(13) 0.031(14) 0.021(14) C30 0.052(10) 0.084(13) 0.073(12) 0.005(9) 0.039(9) 0.040(9) _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 Mo C2 1.93(2) . ? Mo C3 2.006(8) . ? Mo C1 2.034(7) . ? Mo C4 2.059(8) . ? Mo C5 2.10(2) . ? Mo P 2.5458(19) . ? P C25 1.803(18) . ? P C6 1.836(6) . ? P C19 1.868(19) . ? O1 C1 1.141(8) . ? N1 O7 1.267(16) . ? N1 C12 1.37(2) . ? N1 C14 1.519(18) . ? N2 C12 1.320(19) . ? N2 O6 1.305(17) . ? N2 C13 1.525(17) . ? O2 C2 1.22(3) . ? O3 C3 1.169(13) . ? O4 C4 1.117(9) . ? O5 C5 1.10(3) . ? C6 C7 1.31(2) . ? C6 C11 1.48(2) . ? C7 C8 1.36(2) . ? C8 C9 1.41(2) . ? C9 C10 1.38(2) . ? C9 C12 1.479(9) . ? C10 C11 1.39(2) . ? C13 C16 1.46(2) . ? C13 C14 1.490(13) . ? C13 C15 1.582(17) . ? C14 C17 1.43(2) . ? C14 C18 1.557(17) . ? C19 C20 1.39(2) . ? C19 C24 1.41(2) . ? C20 C21 1.40(3) . ? C21 C22 1.36(3) . ? C22 C23 1.31(3) . ? C23 C24 1.39(3) . ? C25 C30 1.36(2) . ? C25 C26 1.38(3) . ? C26 C27 1.37(3) . ? C27 C28 1.37(2) . ? C28 C29 1.41(3) . ? C29 C30 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo C3 84.6(10) . . ? C2 Mo C1 85.9(8) . . ? C3 Mo C1 87.7(3) . . ? C2 Mo C4 93.9(9) . . ? C3 Mo C4 89.6(3) . . ? C1 Mo C4 177.3(2) . . ? C2 Mo C5 176.6(4) . . ? C3 Mo C5 93.9(10) . . ? C1 Mo C5 91.0(8) . . ? C4 Mo C5 89.2(9) . . ? C2 Mo P 92.2(6) . . ? C3 Mo P 176.0(7) . . ? C1 Mo P 89.75(17) . . ? C4 Mo P 92.95(19) . . ? C5 Mo P 89.1(5) . . ? C25 P C6 109.3(8) . . ? C25 P C19 100.6(3) . . ? C6 P C19 99.5(8) . . ? C25 P Mo 118.6(6) . . ? C6 P Mo 109.03(19) . . ? C19 P Mo 117.9(6) . . ? O7 N1 C12 132.6(13) . . ? O7 N1 C14 113.8(13) . . ? C12 N1 C14 113.2(12) . . ? C12 N2 O6 122.4(14) . . ? C12 N2 C13 107.9(12) . . ? O6 N2 C13 129.1(13) . . ? O1 C1 Mo 175(2) . . ? O2 C2 Mo 177.3(18) . . ? O3 C3 Mo 163(3) . . ? O4 C4 Mo 178(2) . . ? O5 C5 Mo 174.6(18) . . ? C7 C6 C11 117.4(6) . . ? C7 C6 P 128.6(14) . . ? C11 C6 P 113.6(12) . . ? C6 C7 C8 126.1(14) . . ? C7 C8 C9 118.4(13) . . ? C10 C9 C8 118.1(5) . . ? C10 C9 C12 127.2(17) . . ? C8 C9 C12 114.6(17) . . ? C9 C10 C11 123.1(15) . . ? C10 C11 C6 116.5(13) . . ? N2 C12 N1 107.7(5) . . ? N2 C12 C9 133.0(16) . . ? N1 C12 C9 119.2(16) . . ? C16 C13 C14 123.2(19) . . ? C16 C13 N2 107.6(13) . . ? C14 C13 N2 104.2(15) . . ? C16 C13 C15 101.9(15) . . ? C14 C13 C15 111.7(11) . . ? N2 C13 C15 107.5(11) . . ? C17 C14 C13 121.7(16) . . ? C17 C14 N1 112.2(14) . . ? C13 C14 N1 96.1(14) . . ? C17 C14 C18 104.6(13) . . ? C13 C14 C18 112.7(12) . . ? N1 C14 C18 109.1(12) . . ? C20 C19 C24 118.4(17) . . ? C20 C19 P 122.9(14) . . ? C24 C19 P 118.2(14) . . ? C19 C20 C21 115.3(18) . . ? C22 C21 C20 125.3(19) . . ? C23 C22 C21 118(2) . . ? C22 C23 C24 120(2) . . ? C19 C24 C23 122(2) . . ? C30 C25 C26 118.2(17) . . ? C30 C25 P 120.2(14) . . ? C26 C25 P 121.5(15) . . ? C27 C26 C25 126.4(19) . . ? C26 C27 C28 113.9(19) . . ? C27 C28 C29 121.9(18) . . ? C30 C29 C28 120(2) . . ? C25 C30 C29 119(2) . . ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 0.344 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.092