data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Miguel A. Ruiz' _publ_contact_author_address ; Departamento de Quimica Organica e Inorganica Universidad de Oviedo Oviedo E-33071 SPAIN ; _publ_contact_author_email MARA@FQ.UNIOVI.ES _publ_section_title ; Proton induced P-H and M-H bond activation at the phosphide bridged dimolybdenum complexes [Mo2Cp2(u-H)(u-PHR)(CO)4], (R = Cy, 2,4,6-C6H2Rī3; Rī = H, Me, tBu) ; _publ_requested_category FM loop_ _publ_author_name 'Miguel A. Ruiz' 'Celedonio M. Alvarez' 'M. Angeles Alvarez' 'Larry Falvello' 'M. Esther Garcia' ; D.Garcia-Vivo ; 'Patrick Herson' 'David Saez' 'Tatiana Soler' data_1b _database_code_depnum_ccdc_archive 'CCDC 248103' _audit_creation_date 2004-03-30T16:42:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C23 H23 Mo2 O4 P1' _chemical_formula_sum 'C23 H23 Mo2 O4 P1' _chemical_formula_weight 586.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.8525(4) _cell_length_b 8.54590(10) _cell_length_c 16.3577(2) _cell_angle_alpha 90 _cell_angle_beta 110.9950(10) _cell_angle_gamma 90 _cell_volume 4418.11(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6193 _cell_measurement_theta_min 2.796 _cell_measurement_theta_max 70.3 _cell_measurement_wavelength 1.54182 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.209 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details 'SADABS v. 2.03' _exptl_absorpt_correction_T_min 0.403695 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54182 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_number 18029 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.796 _diffrn_reflns_theta_max 70.42 _diffrn_reflns_theta_full 70.42 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 4050 _reflns_number_gt 3894 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER SMART v. 5.625' _computing_cell_refinement 'BRUKER SMART v. 5.625' _computing_data_reduction 'BRUKER SAINT v. 6.0' _computing_structure_solution 'DIRDIF (1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0276P)^2^+7.5812P] 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_number_reflns 4050 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.025 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.636 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.188016(5) 0.20995(2) 0.091899(11) 0.00793(7) Uani 1 1 d . . . Mo2 Mo 0.138889(5) 0.27170(2) 0.229610(11) 0.00964(7) Uani 1 1 d . . . P1 P 0.118221(17) 0.13713(6) 0.08992(4) 0.00931(13) Uani 1 1 d . . . O1 O 0.20081(5) 0.5688(2) 0.07644(11) 0.0188(4) Uani 1 1 d . . . O2 O 0.13537(6) 0.2908(2) -0.10252(11) 0.0190(4) Uani 1 1 d . . . O3 O 0.14497(5) 0.6328(2) 0.20771(12) 0.0203(4) Uani 1 1 d . . . O4 O 0.04265(5) 0.3479(2) 0.15499(13) 0.0233(4) Uani 1 1 d . . . C1 C 0.19598(7) 0.4360(3) 0.08336(14) 0.0133(5) Uani 1 1 d . . . C2 C 0.15382(8) 0.2587(3) -0.03058(16) 0.0129(5) Uani 1 1 d . . . C3 C 0.14261(7) 0.4992(3) 0.21473(15) 0.0145(5) Uani 1 1 d . . . C4 C 0.07823(8) 0.3222(3) 0.18010(16) 0.0160(5) Uani 1 1 d . . . C5 C 0.19114(8) 0.1223(3) 0.33865(15) 0.0210(6) Uani 1 1 d . . . C6 C 0.18463(9) 0.2663(4) 0.37483(17) 0.0227(6) Uani 1 1 d . . . C7 C 0.14235(9) 0.2687(3) 0.37229(16) 0.0194(5) Uani 1 1 d . . . C8 C 0.12302(8) 0.1257(3) 0.33317(16) 0.0169(5) Uani 1 1 d . . . C9 C 0.15335(8) 0.0361(3) 0.31299(15) 0.0173(5) Uani 1 1 d . . . C10 C 0.21647(7) -0.0278(3) 0.15944(16) 0.0152(5) Uani 1 1 d . . . C11 C 0.20866(8) -0.0406(3) 0.06852(17) 0.0173(5) Uani 1 1 d . . . C12 C 0.23547(7) 0.0686(3) 0.04801(16) 0.0165(5) Uani 1 1 d . . . C13 C 0.26001(7) 0.1445(3) 0.12567(16) 0.0160(5) Uani 1 1 d . . . C14 C 0.24854(7) 0.0867(3) 0.19478(16) 0.0154(5) Uani 1 1 d . . . C15 C 0.06881(7) 0.1571(3) -0.00398(14) 0.0109(4) Uani 1 1 d . . . C16 C 0.04520(7) 0.0231(3) -0.04378(15) 0.0123(5) Uani 1 1 d . . . C17 C 0.00670(7) 0.0421(3) -0.11233(16) 0.0148(5) Uani 1 1 d . . . C18 C -0.00965(7) 0.1886(3) -0.14438(16) 0.0157(5) Uani 1 1 d . . . C19 C 0.01466(8) 0.3184(3) -0.10620(16) 0.0157(5) Uani 1 1 d . . . C20 C 0.05316(7) 0.3061(3) -0.03774(16) 0.0122(5) Uani 1 1 d . . . C21 C 0.07643(8) 0.4584(3) -0.00389(17) 0.0165(5) Uani 1 1 d . . . C22 C 0.05921(8) -0.1424(3) -0.01696(17) 0.0170(5) Uani 1 1 d . . . C23 C -0.05179(8) 0.2054(4) -0.21728(19) 0.0234(6) Uani 1 1 d . . . H13 H 0.2795(11) 0.222(4) 0.132(2) 0.028(9) Uiso 1 1 d . . . H17 H -0.0091(9) -0.045(3) -0.1398(18) 0.016(7) Uiso 1 1 d . . . H11 H 0.1898(10) -0.107(4) 0.029(2) 0.025(8) Uiso 1 1 d . . . H14 H 0.2607(9) 0.124(3) 0.254(2) 0.023(8) Uiso 1 1 d . . . H2 H 0.1182(9) -0.013(3) 0.1010(18) 0.023(8) Uiso 1 1 d . . . H10 H 0.2042(9) -0.088(3) 0.1919(19) 0.019(7) Uiso 1 1 d . . . H19 H 0.0061(8) 0.415(3) -0.1275(17) 0.010(6) Uiso 1 1 d . . . H6 H 0.2036(11) 0.340(4) 0.397(2) 0.029(8) Uiso 1 1 d . . . H8 H 0.0958(10) 0.091(4) 0.323(2) 0.028(8) Uiso 1 1 d . . . H7 H 0.1304(10) 0.352(4) 0.393(2) 0.026(8) Uiso 1 1 d . . . H12 H 0.2377(9) 0.088(3) -0.0063(19) 0.018(7) Uiso 1 1 d . . . H9 H 0.1495(9) -0.064(4) 0.2900(19) 0.025(8) Uiso 1 1 d . . . H5 H 0.2167(9) 0.092(3) 0.3343(19) 0.022(7) Uiso 1 1 d . . . H21 H 0.0601(9) -0.166(3) 0.039(2) 0.017(7) Uiso 1 1 d . . . H24 H 0.0746(9) 0.521(4) -0.0528(19) 0.020(7) Uiso 1 1 d . . . H20 H 0.0861(10) -0.164(4) -0.0175(19) 0.020(7) Uiso 1 1 d . . . H25 H 0.0655(10) 0.513(4) 0.032(2) 0.036(9) Uiso 1 1 d . . . H23 H 0.1072(10) 0.450(4) 0.034(2) 0.029(8) Uiso 1 1 d . . . H22 H 0.0393(10) -0.215(3) -0.059(2) 0.020(8) Uiso 1 1 d . . . H1 H 0.1819(13) 0.317(5) 0.179(3) 0.064(12) Uiso 1 1 d . . . H27 H -0.0518(11) 0.163(4) -0.270(2) 0.038(9) Uiso 1 1 d . . . H28 H -0.0737(12) 0.154(5) -0.203(2) 0.045(10) Uiso 1 1 d . . . H26 H -0.0616(15) 0.308(6) -0.230(3) 0.072(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00538(11) 0.01089(12) 0.00570(11) 0.00081(6) -0.00022(8) 0.00125(6) Mo2 0.00724(11) 0.01284(13) 0.00816(11) -0.00116(6) 0.00194(8) -0.00089(6) P1 0.0067(3) 0.0097(3) 0.0092(3) 0.0003(2) 0.0000(2) 0.0004(2) O1 0.0221(9) 0.0139(10) 0.0179(9) 0.0023(7) 0.0043(7) -0.0027(7) O2 0.0182(9) 0.0258(11) 0.0079(9) 0.0028(6) -0.0014(8) 0.0042(7) O3 0.0201(9) 0.0151(11) 0.0260(10) -0.0019(7) 0.0084(8) -0.0014(7) O4 0.0113(9) 0.0231(10) 0.0352(11) -0.0007(8) 0.0076(8) 0.0027(7) C1 0.0062(10) 0.0251(16) 0.0068(11) -0.0015(9) 0.0001(9) 0.0012(9) C2 0.0123(12) 0.0124(12) 0.0140(13) -0.0015(9) 0.0048(10) 0.0001(9) C3 0.0098(11) 0.0210(16) 0.0124(11) -0.0030(9) 0.0036(10) 0.0005(9) C4 0.0173(13) 0.0141(12) 0.0173(12) -0.0019(9) 0.0068(10) -0.0023(9) C5 0.0130(12) 0.0409(17) 0.0071(11) 0.0102(10) 0.0010(10) 0.0054(11) C6 0.0198(14) 0.0343(16) 0.0078(12) 0.0018(10) -0.0026(11) -0.0134(12) C7 0.0276(15) 0.0234(15) 0.0096(12) -0.0031(10) 0.0095(11) -0.0029(11) C8 0.0158(12) 0.0240(14) 0.0120(12) 0.0025(9) 0.0061(10) -0.0063(10) C9 0.0234(13) 0.0168(14) 0.0093(11) 0.0037(9) 0.0030(10) 0.0025(10) C10 0.0137(11) 0.0141(13) 0.0176(12) 0.0074(9) 0.0053(10) 0.0065(9) C11 0.0150(12) 0.0146(13) 0.0186(13) -0.0016(10) 0.0016(10) 0.0068(10) C12 0.0166(12) 0.0221(14) 0.0133(12) 0.0031(9) 0.0083(10) 0.0105(10) C13 0.0075(11) 0.0197(14) 0.0196(13) 0.0046(10) 0.0034(10) 0.0060(9) C14 0.0086(11) 0.0230(14) 0.0113(12) 0.0022(9) -0.0005(10) 0.0073(9) C15 0.0075(10) 0.0147(12) 0.0099(11) 0.0001(9) 0.0025(9) 0.0012(9) C16 0.0110(11) 0.0151(12) 0.0111(11) 0.0002(9) 0.0042(9) -0.0017(9) C17 0.0120(12) 0.0161(13) 0.0153(12) -0.0028(9) 0.0037(10) -0.0042(9) C18 0.0068(11) 0.0246(14) 0.0130(12) -0.0003(9) 0.0003(10) 0.0006(9) C19 0.0131(12) 0.0157(13) 0.0172(13) 0.0020(10) 0.0040(10) 0.0051(10) C20 0.0102(11) 0.0126(12) 0.0138(12) 0.0000(9) 0.0044(10) 0.0014(9) C21 0.0145(12) 0.0116(13) 0.0197(13) 0.0021(10) 0.0015(11) 0.0010(9) C22 0.0163(13) 0.0130(13) 0.0185(13) -0.0009(10) 0.0022(11) -0.0018(10) C23 0.0101(13) 0.0341(18) 0.0192(15) -0.0016(11) -0.0030(12) -0.0007(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.962(3) . ? Mo1 C2 1.966(2) . ? Mo1 C12 2.320(2) . ? Mo1 C11 2.326(2) . ? Mo1 C10 2.348(2) . ? Mo1 C13 2.365(2) . ? Mo1 C14 2.381(2) . ? Mo1 P1 2.4323(5) . ? Mo1 Mo2 3.2868(2) . ? Mo1 H1 1.77(4) . ? Mo2 C4 1.966(2) . ? Mo2 C3 1.969(3) . ? Mo2 C7 2.295(2) . ? Mo2 C8 2.316(2) . ? Mo2 C6 2.325(3) . ? Mo2 C9 2.382(2) . ? Mo2 C5 2.383(2) . ? Mo2 P1 2.4264(6) . ? Mo2 H1 1.95(4) . ? P1 C15 1.829(2) . ? P1 H2 1.30(3) . ? O1 C1 1.158(3) . ? O2 C2 1.150(3) . ? O3 C3 1.153(3) . ? O4 C4 1.146(3) . ? C5 C9 1.404(4) . ? C5 C6 1.417(4) . ? C5 H5 0.93(3) . ? C6 C7 1.417(4) . ? C6 H6 0.88(3) . ? C7 C8 1.425(4) . ? C7 H7 0.94(3) . ? C8 C9 1.411(4) . ? C8 H8 0.93(3) . ? C9 H9 0.92(3) . ? C10 C11 1.418(4) . ? C10 C14 1.422(4) . ? C10 H10 0.94(3) . ? C11 C12 1.423(4) . ? C11 H11 0.93(3) . ? C12 C13 1.403(4) . ? C12 H12 0.93(3) . ? C13 C14 1.410(3) . ? C13 H13 0.91(3) . ? C14 H14 0.97(3) . ? C15 C20 1.413(3) . ? C15 C16 1.415(3) . ? C16 C17 1.391(3) . ? C16 C22 1.506(3) . ? C17 C18 1.393(4) . ? C17 H17 0.93(3) . ? C18 C19 1.389(4) . ? C18 C23 1.503(4) . ? C19 C20 1.385(4) . ? C19 H19 0.90(3) . ? C20 C21 1.519(3) . ? C21 H24 0.95(3) . ? C21 H25 0.92(4) . ? C21 H23 1.00(3) . ? C22 H21 0.93(3) . ? C22 H20 0.93(3) . ? C22 H22 0.99(3) . ? C23 H27 0.94(4) . ? C23 H28 0.96(4) . ? C23 H26 0.94(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 76.40(9) . . ? C1 Mo1 C12 111.26(9) . . ? C2 Mo1 C12 90.86(9) . . ? C1 Mo1 C11 146.87(9) . . ? C2 Mo1 C11 97.42(9) . . ? C12 Mo1 C11 35.67(9) . . ? C1 Mo1 C10 147.31(9) . . ? C2 Mo1 C10 130.93(9) . . ? C12 Mo1 C10 58.82(8) . . ? C11 Mo1 C10 35.33(9) . . ? C1 Mo1 C13 95.33(9) . . ? C2 Mo1 C13 117.99(9) . . ? C12 Mo1 C13 34.85(9) . . ? C11 Mo1 C13 58.38(9) . . ? C10 Mo1 C13 58.06(8) . . ? C1 Mo1 C14 112.35(9) . . ? C2 Mo1 C14 149.02(9) . . ? C12 Mo1 C14 58.17(8) . . ? C11 Mo1 C14 58.40(9) . . ? C10 Mo1 C14 34.98(9) . . ? C13 Mo1 C14 34.56(8) . . ? C1 Mo1 P1 114.11(6) . . ? C2 Mo1 P1 79.99(7) . . ? C12 Mo1 P1 129.77(7) . . ? C11 Mo1 P1 96.31(6) . . ? C10 Mo1 P1 91.01(6) . . ? C13 Mo1 P1 149.04(6) . . ? C14 Mo1 P1 118.82(6) . . ? C1 Mo1 Mo2 90.40(6) . . ? C2 Mo1 Mo2 113.99(7) . . ? C12 Mo1 Mo2 150.72(6) . . ? C11 Mo1 Mo2 121.07(6) . . ? C10 Mo1 Mo2 92.26(6) . . ? C13 Mo1 Mo2 127.59(6) . . ? C14 Mo1 Mo2 96.03(6) . . ? P1 Mo1 Mo2 47.356(13) . . ? C1 Mo1 H1 66.9(14) . . ? C2 Mo1 H1 121.1(13) . . ? C12 Mo1 H1 144.4(14) . . ? C11 Mo1 H1 137.5(14) . . ? C10 Mo1 H1 102.4(14) . . ? C13 Mo1 H1 110.0(14) . . ? C14 Mo1 H1 88.8(14) . . ? P1 Mo1 H1 75.5(14) . . ? Mo2 Mo1 H1 29.5(14) . . ? C4 Mo2 C3 80.57(10) . . ? C4 Mo2 C7 94.97(10) . . ? C3 Mo2 C7 98.89(9) . . ? C4 Mo2 C8 86.43(10) . . ? C3 Mo2 C8 131.60(9) . . ? C7 Mo2 C8 36.00(9) . . ? C4 Mo2 C6 129.79(10) . . ? C3 Mo2 C6 95.57(10) . . ? C7 Mo2 C6 35.72(10) . . ? C8 Mo2 C6 59.09(9) . . ? C4 Mo2 C9 113.03(9) . . ? C3 Mo2 C9 153.65(9) . . ? C7 Mo2 C9 58.88(9) . . ? C8 Mo2 C9 34.93(9) . . ? C6 Mo2 C9 58.22(9) . . ? C4 Mo2 C5 144.21(9) . . ? C3 Mo2 C5 123.94(10) . . ? C7 Mo2 C5 58.61(9) . . ? C8 Mo2 C5 57.90(8) . . ? C6 Mo2 C5 35.00(10) . . ? C9 Mo2 C5 34.26(9) . . ? C4 Mo2 P1 79.04(7) . . ? C3 Mo2 P1 111.17(7) . . ? C7 Mo2 P1 147.67(7) . . ? C8 Mo2 P1 111.67(6) . . ? C6 Mo2 P1 144.54(8) . . ? C9 Mo2 P1 93.98(6) . . ? C5 Mo2 P1 109.70(7) . . ? C4 Mo2 Mo1 117.59(7) . . ? C3 Mo2 Mo1 90.19(7) . . ? C7 Mo2 Mo1 147.28(7) . . ? C8 Mo2 Mo1 136.19(6) . . ? C6 Mo2 Mo1 112.44(7) . . ? C9 Mo2 Mo1 101.90(6) . . ? C5 Mo2 Mo1 90.28(6) . . ? P1 Mo2 Mo1 47.507(13) . . ? C4 Mo2 H1 127.6(12) . . ? C3 Mo2 H1 70.1(12) . . ? C7 Mo2 H1 131.1(12) . . ? C8 Mo2 H1 145.0(12) . . ? C6 Mo2 H1 96.3(12) . . ? C9 Mo2 H1 112.3(12) . . ? C5 Mo2 H1 87.5(12) . . ? P1 Mo2 H1 72.8(12) . . ? Mo1 Mo2 H1 26.6(12) . . ? C15 P1 Mo2 127.95(7) . . ? C15 P1 Mo1 125.38(7) . . ? Mo2 P1 Mo1 85.137(18) . . ? C15 P1 H2 99.4(12) . . ? Mo2 P1 H2 110.7(12) . . ? Mo1 P1 H2 107.5(12) . . ? O1 C1 Mo1 178.4(2) . . ? O2 C2 Mo1 176.9(2) . . ? O3 C3 Mo2 178.7(2) . . ? O4 C4 Mo2 176.4(2) . . ? C9 C5 C6 108.6(2) . . ? C9 C5 Mo2 72.82(14) . . ? C6 C5 Mo2 70.27(15) . . ? C9 C5 H5 127.3(19) . . ? C6 C5 H5 124.0(19) . . ? Mo2 C5 H5 123.5(18) . . ? C5 C6 C7 107.9(2) . . ? C5 C6 Mo2 74.73(14) . . ? C7 C6 Mo2 70.97(14) . . ? C5 C6 H6 126(2) . . ? C7 C6 H6 126(2) . . ? Mo2 C6 H6 122(2) . . ? C6 C7 C8 107.3(2) . . ? C6 C7 Mo2 73.32(14) . . ? C8 C7 Mo2 72.83(14) . . ? C6 C7 H7 124.2(19) . . ? C8 C7 H7 128.5(19) . . ? Mo2 C7 H7 119.1(19) . . ? C9 C8 C7 108.3(2) . . ? C9 C8 Mo2 75.07(14) . . ? C7 C8 Mo2 71.17(14) . . ? C9 C8 H8 123(2) . . ? C7 C8 H8 128.4(19) . . ? Mo2 C8 H8 121.3(19) . . ? C5 C9 C8 107.9(2) . . ? C5 C9 Mo2 72.92(15) . . ? C8 C9 Mo2 70.00(14) . . ? C5 C9 H9 126.1(18) . . ? C8 C9 H9 126.0(18) . . ? Mo2 C9 H9 125.3(19) . . ? C11 C10 C14 107.9(2) . . ? C11 C10 Mo1 71.48(14) . . ? C14 C10 Mo1 73.75(14) . . ? C11 C10 H10 126.7(17) . . ? C14 C10 H10 125.3(17) . . ? Mo1 C10 H10 123.7(17) . . ? C10 C11 C12 107.6(2) . . ? C10 C11 Mo1 73.20(14) . . ? C12 C11 Mo1 71.92(14) . . ? C10 C11 H11 127.5(19) . . ? C12 C11 H11 124.9(19) . . ? Mo1 C11 H11 120.7(19) . . ? C13 C12 C11 108.1(2) . . ? C13 C12 Mo1 74.33(13) . . ? C11 C12 Mo1 72.40(13) . . ? C13 C12 H12 123.8(18) . . ? C11 C12 H12 128.1(18) . . ? Mo1 C12 H12 120.3(18) . . ? C12 C13 C14 108.7(2) . . ? C12 C13 Mo1 70.82(13) . . ? C14 C13 Mo1 73.33(13) . . ? C12 C13 H13 127(2) . . ? C14 C13 H13 124(2) . . ? Mo1 C13 H13 120(2) . . ? C13 C14 C10 107.8(2) . . ? C13 C14 Mo1 72.11(13) . . ? C10 C14 Mo1 71.27(13) . . ? C13 C14 H14 123.5(17) . . ? C10 C14 H14 128.8(17) . . ? Mo1 C14 H14 121.0(17) . . ? C20 C15 C16 118.6(2) . . ? C20 C15 P1 120.96(18) . . ? C16 C15 P1 120.44(17) . . ? C17 C16 C15 119.2(2) . . ? C17 C16 C22 116.8(2) . . ? C15 C16 C22 124.0(2) . . ? C16 C17 C18 122.7(2) . . ? C16 C17 H17 120.3(17) . . ? C18 C17 H17 117.0(17) . . ? C19 C18 C17 117.2(2) . . ? C19 C18 C23 121.4(2) . . ? C17 C18 C23 121.4(2) . . ? C20 C19 C18 122.5(2) . . ? C20 C19 H19 117.4(17) . . ? C18 C19 H19 120.1(17) . . ? C19 C20 C15 119.8(2) . . ? C19 C20 C21 116.4(2) . . ? C15 C20 C21 123.8(2) . . ? C20 C21 H24 107.8(18) . . ? C20 C21 H25 113(2) . . ? H24 C21 H25 110(3) . . ? C20 C21 H23 116.9(18) . . ? H24 C21 H23 107(2) . . ? H25 C21 H23 102(3) . . ? C16 C22 H21 112.6(18) . . ? C16 C22 H20 112.9(19) . . ? H21 C22 H20 106(2) . . ? C16 C22 H22 108.7(17) . . ? H21 C22 H22 109(2) . . ? H20 C22 H22 107(3) . . ? C18 C23 H27 112(2) . . ? C18 C23 H28 111(2) . . ? H27 C23 H28 107(3) . . ? C18 C23 H26 115(3) . . ? H27 C23 H26 106(4) . . ? H28 C23 H26 104(4) . . ? 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 C1 Mo1 Mo2 C4 83.61(10) . . . . ? C2 Mo1 Mo2 C4 8.35(11) . . . . ? C12 Mo1 Mo2 C4 -137.48(16) . . . . ? C11 Mo1 Mo2 C4 -107.33(11) . . . . ? C10 Mo1 Mo2 C4 -128.98(10) . . . . ? C13 Mo1 Mo2 C4 -179.35(11) . . . . ? C14 Mo1 Mo2 C4 -163.85(10) . . . . ? P1 Mo1 Mo2 C4 -39.69(8) . . . . ? C1 Mo1 Mo2 C3 4.16(9) . . . . ? C2 Mo1 Mo2 C3 -71.10(10) . . . . ? C12 Mo1 Mo2 C3 143.07(15) . . . . ? C11 Mo1 Mo2 C3 173.23(10) . . . . ? C10 Mo1 Mo2 C3 151.57(9) . . . . ? C13 Mo1 Mo2 C3 101.20(10) . . . . ? C14 Mo1 Mo2 C3 116.70(9) . . . . ? P1 Mo1 Mo2 C3 -119.14(7) . . . . ? C1 Mo1 Mo2 C7 -102.75(14) . . . . ? C2 Mo1 Mo2 C7 -178.01(14) . . . . ? C12 Mo1 Mo2 C7 36.16(18) . . . . ? C11 Mo1 Mo2 C7 66.32(14) . . . . ? C10 Mo1 Mo2 C7 44.66(14) . . . . ? C13 Mo1 Mo2 C7 -5.71(15) . . . . ? C14 Mo1 Mo2 C7 9.79(14) . . . . ? P1 Mo1 Mo2 C7 133.95(13) . . . . ? C1 Mo1 Mo2 C8 -160.09(11) . . . . ? C2 Mo1 Mo2 C8 124.65(12) . . . . ? C12 Mo1 Mo2 C8 -21.18(16) . . . . ? C11 Mo1 Mo2 C8 8.97(11) . . . . ? C10 Mo1 Mo2 C8 -12.68(11) . . . . ? C13 Mo1 Mo2 C8 -63.05(12) . . . . ? C14 Mo1 Mo2 C8 -47.55(11) . . . . ? P1 Mo1 Mo2 C8 76.61(9) . . . . ? C1 Mo1 Mo2 C6 -91.94(10) . . . . ? C2 Mo1 Mo2 C6 -167.21(11) . . . . ? C12 Mo1 Mo2 C6 46.96(15) . . . . ? C11 Mo1 Mo2 C6 77.12(11) . . . . ? C10 Mo1 Mo2 C6 55.47(10) . . . . ? C13 Mo1 Mo2 C6 5.10(11) . . . . ? C14 Mo1 Mo2 C6 20.59(10) . . . . ? P1 Mo1 Mo2 C6 144.76(8) . . . . ? C1 Mo1 Mo2 C9 -152.25(9) . . . . ? C2 Mo1 Mo2 C9 132.48(10) . . . . ? C12 Mo1 Mo2 C9 -13.35(15) . . . . ? C11 Mo1 Mo2 C9 16.81(10) . . . . ? C10 Mo1 Mo2 C9 -4.84(9) . . . . ? C13 Mo1 Mo2 C9 -55.21(10) . . . . ? C14 Mo1 Mo2 C9 -39.72(9) . . . . ? P1 Mo1 Mo2 C9 84.45(7) . . . . ? C1 Mo1 Mo2 C5 -119.78(9) . . . . ? C2 Mo1 Mo2 C5 164.96(10) . . . . ? C12 Mo1 Mo2 C5 19.13(15) . . . . ? C11 Mo1 Mo2 C5 49.28(10) . . . . ? C10 Mo1 Mo2 C5 27.63(9) . . . . ? C13 Mo1 Mo2 C5 -22.74(11) . . . . ? C14 Mo1 Mo2 C5 -7.24(9) . . . . ? P1 Mo1 Mo2 C5 116.92(7) . . . . ? C1 Mo1 Mo2 P1 123.30(7) . . . . ? C2 Mo1 Mo2 P1 48.03(8) . . . . ? C12 Mo1 Mo2 P1 -97.80(13) . . . . ? C11 Mo1 Mo2 P1 -67.64(8) . . . . ? C10 Mo1 Mo2 P1 -89.29(6) . . . . ? C13 Mo1 Mo2 P1 -139.66(8) . . . . ? C14 Mo1 Mo2 P1 -124.17(7) . . . . ? C4 Mo2 P1 C15 12.69(12) . . . . ? C3 Mo2 P1 C15 -62.60(12) . . . . ? C7 Mo2 P1 C15 94.58(17) . . . . ? C8 Mo2 P1 C15 94.34(12) . . . . ? C6 Mo2 P1 C15 161.08(15) . . . . ? C9 Mo2 P1 C15 125.39(11) . . . . ? C5 Mo2 P1 C15 156.62(11) . . . . ? Mo1 Mo2 P1 C15 -132.11(10) . . . . ? C4 Mo2 P1 Mo1 144.80(7) . . . . ? C3 Mo2 P1 Mo1 69.51(7) . . . . ? C7 Mo2 P1 Mo1 -133.32(14) . . . . ? C8 Mo2 P1 Mo1 -133.55(7) . . . . ? C6 Mo2 P1 Mo1 -66.81(12) . . . . ? C9 Mo2 P1 Mo1 -102.50(6) . . . . ? C5 Mo2 P1 Mo1 -71.27(7) . . . . ? C1 Mo1 P1 C15 67.85(12) . . . . ? C2 Mo1 P1 C15 -2.23(12) . . . . ? C12 Mo1 P1 C15 -84.93(12) . . . . ? C11 Mo1 P1 C15 -98.69(11) . . . . ? C10 Mo1 P1 C15 -133.70(11) . . . . ? C13 Mo1 P1 C15 -131.44(15) . . . . ? C14 Mo1 P1 C15 -155.94(12) . . . . ? Mo2 Mo1 P1 C15 134.15(10) . . . . ? C1 Mo1 P1 Mo2 -66.30(7) . . . . ? C2 Mo1 P1 Mo2 -136.39(7) . . . . ? C12 Mo1 P1 Mo2 140.92(8) . . . . ? C11 Mo1 P1 Mo2 127.16(6) . . . . ? C10 Mo1 P1 Mo2 92.14(6) . . . . ? C13 Mo1 P1 Mo2 94.41(12) . . . . ? C14 Mo1 P1 Mo2 69.90(7) . . . . ? C2 Mo1 C1 O1 -44(8) . . . . ? C12 Mo1 C1 O1 41(8) . . . . ? C11 Mo1 C1 O1 39(8) . . . . ? C10 Mo1 C1 O1 106(8) . . . . ? C13 Mo1 C1 O1 73(8) . . . . ? C14 Mo1 C1 O1 105(8) . . . . ? P1 Mo1 C1 O1 -116(8) . . . . ? Mo2 Mo1 C1 O1 -159(8) . . . . ? C1 Mo1 C2 O2 49(4) . . . . ? C12 Mo1 C2 O2 -63(4) . . . . ? C11 Mo1 C2 O2 -98(4) . . . . ? C10 Mo1 C2 O2 -110(4) . . . . ? C13 Mo1 C2 O2 -40(4) . . . . ? C14 Mo1 C2 O2 -62(4) . . . . ? P1 Mo1 C2 O2 167(4) . . . . ? Mo2 Mo1 C2 O2 133(4) . . . . ? C4 Mo2 C3 O3 103(8) . . . . ? C7 Mo2 C3 O3 9(8) . . . . ? C8 Mo2 C3 O3 26(8) . . . . ? C6 Mo2 C3 O3 -27(8) . . . . ? C9 Mo2 C3 O3 -21(9) . . . . ? C5 Mo2 C3 O3 -49(8) . . . . ? P1 Mo2 C3 O3 18E1(10) . . . . ? Mo1 Mo2 C3 O3 -139(8) . . . . ? C3 Mo2 C4 O4 -125(4) . . . . ? C7 Mo2 C4 O4 -27(4) . . . . ? C8 Mo2 C4 O4 8(4) . . . . ? C6 Mo2 C4 O4 -35(4) . . . . ? C9 Mo2 C4 O4 32(4) . . . . ? C5 Mo2 C4 O4 13(4) . . . . ? P1 Mo2 C4 O4 121(4) . . . . ? Mo1 Mo2 C4 O4 150(4) . . . . ? C4 Mo2 C5 C9 32.0(2) . . . . ? C3 Mo2 C5 C9 158.54(14) . . . . ? C7 Mo2 C5 C9 79.65(16) . . . . ? C8 Mo2 C5 C9 37.04(14) . . . . ? C6 Mo2 C5 C9 117.8(2) . . . . ? P1 Mo2 C5 C9 -66.75(15) . . . . ? Mo1 Mo2 C5 C9 -111.04(14) . . . . ? C4 Mo2 C5 C6 -85.8(2) . . . . ? C3 Mo2 C5 C6 40.78(18) . . . . ? C7 Mo2 C5 C6 -38.11(15) . . . . ? C8 Mo2 C5 C6 -80.72(16) . . . . ? C9 Mo2 C5 C6 -117.8(2) . . . . ? P1 Mo2 C5 C6 175.49(13) . . . . ? Mo1 Mo2 C5 C6 131.20(15) . . . . ? C9 C5 C6 C7 0.6(3) . . . . ? Mo2 C5 C6 C7 63.70(18) . . . . ? C9 C5 C6 Mo2 -63.14(17) . . . . ? C4 Mo2 C6 C5 130.63(16) . . . . ? C3 Mo2 C6 C5 -147.01(15) . . . . ? C7 Mo2 C6 C5 115.5(2) . . . . ? C8 Mo2 C6 C5 77.01(16) . . . . ? C9 Mo2 C6 C5 35.87(14) . . . . ? P1 Mo2 C6 C5 -7.3(2) . . . . ? Mo1 Mo2 C6 C5 -54.50(15) . . . . ? C4 Mo2 C6 C7 15.1(2) . . . . ? C3 Mo2 C6 C7 97.48(17) . . . . ? C8 Mo2 C6 C7 -38.50(15) . . . . ? C9 Mo2 C6 C7 -79.63(17) . . . . ? C5 Mo2 C6 C7 -115.5(2) . . . . ? P1 Mo2 C6 C7 -122.84(16) . . . . ? Mo1 Mo2 C6 C7 -170.00(14) . . . . ? C5 C6 C7 C8 -0.8(3) . . . . ? Mo2 C6 C7 C8 65.41(17) . . . . ? C5 C6 C7 Mo2 -66.18(18) . . . . ? C4 Mo2 C7 C6 -168.39(17) . . . . ? C3 Mo2 C7 C6 -87.18(17) . . . . ? C8 Mo2 C7 C6 114.7(2) . . . . ? C9 Mo2 C7 C6 77.64(18) . . . . ? C5 Mo2 C7 C6 37.33(17) . . . . ? P1 Mo2 C7 C6 114.30(17) . . . . ? Mo1 Mo2 C7 C6 17.3(2) . . . . ? C4 Mo2 C7 C8 76.94(16) . . . . ? C3 Mo2 C7 C8 158.15(15) . . . . ? C6 Mo2 C7 C8 -114.7(2) . . . . ? C9 Mo2 C7 C8 -37.03(15) . . . . ? C5 Mo2 C7 C8 -77.34(17) . . . . ? P1 Mo2 C7 C8 -0.4(2) . . . . ? Mo1 Mo2 C7 C8 -97.40(17) . . . . ? C6 C7 C8 C9 0.7(3) . . . . ? Mo2 C7 C8 C9 66.43(17) . . . . ? C6 C7 C8 Mo2 -65.74(18) . . . . ? C4 Mo2 C8 C9 140.71(16) . . . . ? C3 Mo2 C8 C9 -145.25(15) . . . . ? C7 Mo2 C8 C9 -115.8(2) . . . . ? C6 Mo2 C8 C9 -77.60(17) . . . . ? C5 Mo2 C8 C9 -36.32(15) . . . . ? P1 Mo2 C8 C9 63.99(15) . . . . ? Mo1 Mo2 C8 C9 13.47(19) . . . . ? C4 Mo2 C8 C7 -103.50(17) . . . . ? C3 Mo2 C8 C7 -29.5(2) . . . . ? C6 Mo2 C8 C7 38.19(16) . . . . ? C9 Mo2 C8 C7 115.8(2) . . . . ? C5 Mo2 C8 C7 79.47(17) . . . . ? P1 Mo2 C8 C7 179.78(14) . . . . ? Mo1 Mo2 C8 C7 129.26(14) . . . . ? C6 C5 C9 C8 -0.1(3) . . . . ? Mo2 C5 C9 C8 -61.64(17) . . . . ? C6 C5 C9 Mo2 61.51(17) . . . . ? C7 C8 C9 C5 -0.4(3) . . . . ? Mo2 C8 C9 C5 63.52(17) . . . . ? C7 C8 C9 Mo2 -63.88(17) . . . . ? C4 Mo2 C9 C5 -160.34(15) . . . . ? C3 Mo2 C9 C5 -43.1(3) . . . . ? C7 Mo2 C9 C5 -78.79(16) . . . . ? C8 Mo2 C9 C5 -117.0(2) . . . . ? C6 Mo2 C9 C5 -36.66(15) . . . . ? P1 Mo2 C9 C5 119.88(14) . . . . ? Mo1 Mo2 C9 C5 72.52(15) . . . . ? C4 Mo2 C9 C8 -43.38(17) . . . . ? C3 Mo2 C9 C8 73.8(2) . . . . ? C7 Mo2 C9 C8 38.18(15) . . . . ? C6 Mo2 C9 C8 80.31(16) . . . . ? C5 Mo2 C9 C8 117.0(2) . . . . ? P1 Mo2 C9 C8 -123.15(14) . . . . ? Mo1 Mo2 C9 C8 -170.51(13) . . . . ? C1 Mo1 C10 C11 -118.87(19) . . . . ? C2 Mo1 C10 C11 21.92(19) . . . . ? C12 Mo1 C10 C11 -37.98(15) . . . . ? C13 Mo1 C10 C11 -79.12(15) . . . . ? C14 Mo1 C10 C11 -115.8(2) . . . . ? P1 Mo1 C10 C11 99.51(14) . . . . ? Mo2 Mo1 C10 C11 146.87(14) . . . . ? C1 Mo1 C10 C14 -3.0(2) . . . . ? C2 Mo1 C10 C14 137.75(15) . . . . ? C12 Mo1 C10 C14 77.85(15) . . . . ? C11 Mo1 C10 C14 115.8(2) . . . . ? C13 Mo1 C10 C14 36.71(14) . . . . ? P1 Mo1 C10 C14 -144.66(13) . . . . ? Mo2 Mo1 C10 C14 -97.30(13) . . . . ? C14 C10 C11 C12 -1.1(3) . . . . ? Mo1 C10 C11 C12 64.18(16) . . . . ? C14 C10 C11 Mo1 -65.26(16) . . . . ? C1 Mo1 C11 C10 120.07(18) . . . . ? C2 Mo1 C11 C10 -163.48(15) . . . . ? C12 Mo1 C11 C10 115.5(2) . . . . ? C13 Mo1 C11 C10 78.12(15) . . . . ? C14 Mo1 C11 C10 37.29(13) . . . . ? P1 Mo1 C11 C10 -82.80(14) . . . . ? Mo2 Mo1 C11 C10 -39.61(16) . . . . ? C1 Mo1 C11 C12 4.6(2) . . . . ? C2 Mo1 C11 C12 81.06(15) . . . . ? C10 Mo1 C11 C12 -115.5(2) . . . . ? C13 Mo1 C11 C12 -37.34(14) . . . . ? C14 Mo1 C11 C12 -78.18(15) . . . . ? P1 Mo1 C11 C12 161.73(13) . . . . ? Mo2 Mo1 C11 C12 -155.08(12) . . . . ? C10 C11 C12 C13 1.3(3) . . . . ? Mo1 C11 C12 C13 66.32(16) . . . . ? C10 C11 C12 Mo1 -65.02(16) . . . . ? C1 Mo1 C12 C13 67.40(16) . . . . ? C2 Mo1 C12 C13 143.13(16) . . . . ? C11 Mo1 C12 C13 -115.3(2) . . . . ? C10 Mo1 C12 C13 -77.70(16) . . . . ? C14 Mo1 C12 C13 -36.42(14) . . . . ? P1 Mo1 C12 C13 -139.22(13) . . . . ? Mo2 Mo1 C12 C13 -67.7(2) . . . . ? C1 Mo1 C12 C11 -177.30(14) . . . . ? C2 Mo1 C12 C11 -101.57(15) . . . . ? C10 Mo1 C12 C11 37.60(14) . . . . ? C13 Mo1 C12 C11 115.3(2) . . . . ? C14 Mo1 C12 C11 78.88(15) . . . . ? P1 Mo1 C12 C11 -23.91(17) . . . . ? Mo2 Mo1 C12 C11 47.6(2) . . . . ? C11 C12 C13 C14 -1.0(3) . . . . ? Mo1 C12 C13 C14 64.02(17) . . . . ? C11 C12 C13 Mo1 -65.04(16) . . . . ? C1 Mo1 C13 C12 -120.22(15) . . . . ? C2 Mo1 C13 C12 -42.80(18) . . . . ? C11 Mo1 C13 C12 38.25(15) . . . . ? C10 Mo1 C13 C12 80.08(16) . . . . ? C14 Mo1 C13 C12 117.2(2) . . . . ? P1 Mo1 C13 C12 77.41(18) . . . . ? Mo2 Mo1 C13 C12 145.16(12) . . . . ? C1 Mo1 C13 C14 122.54(16) . . . . ? C2 Mo1 C13 C14 -160.04(15) . . . . ? C12 Mo1 C13 C14 -117.2(2) . . . . ? C11 Mo1 C13 C14 -78.99(16) . . . . ? C10 Mo1 C13 C14 -37.16(15) . . . . ? P1 Mo1 C13 C14 -39.8(2) . . . . ? Mo2 Mo1 C13 C14 27.92(18) . . . . ? C12 C13 C14 C10 0.3(3) . . . . ? Mo1 C13 C14 C10 62.76(16) . . . . ? C12 C13 C14 Mo1 -62.41(16) . . . . ? C11 C10 C14 C13 0.5(3) . . . . ? Mo1 C10 C14 C13 -63.31(16) . . . . ? C11 C10 C14 Mo1 63.77(16) . . . . ? C1 Mo1 C14 C13 -65.17(17) . . . . ? C2 Mo1 C14 C13 35.8(3) . . . . ? C12 Mo1 C14 C13 36.72(15) . . . . ? C11 Mo1 C14 C13 78.94(16) . . . . ? C10 Mo1 C14 C13 116.6(2) . . . . ? P1 Mo1 C14 C13 157.91(13) . . . . ? Mo2 Mo1 C14 C13 -158.09(14) . . . . ? C1 Mo1 C14 C10 178.23(14) . . . . ? C2 Mo1 C14 C10 -80.8(2) . . . . ? C12 Mo1 C14 C10 -79.88(15) . . . . ? C11 Mo1 C14 C10 -37.67(14) . . . . ? C13 Mo1 C14 C10 -116.6(2) . . . . ? P1 Mo1 C14 C10 41.31(15) . . . . ? Mo2 Mo1 C14 C10 85.30(13) . . . . ? Mo2 P1 C15 C20 50.1(2) . . . . ? Mo1 P1 C15 C20 -64.9(2) . . . . ? Mo2 P1 C15 C16 -129.24(15) . . . . ? Mo1 P1 C15 C16 115.80(16) . . . . ? C20 C15 C16 C17 -2.5(3) . . . . ? P1 C15 C16 C17 176.86(17) . . . . ? C20 C15 C16 C22 177.2(2) . . . . ? P1 C15 C16 C22 -3.5(3) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C22 C16 C17 C18 -179.1(2) . . . . ? C16 C17 C18 C19 1.4(4) . . . . ? C16 C17 C18 C23 -178.7(2) . . . . ? C17 C18 C19 C20 -1.5(4) . . . . ? C23 C18 C19 C20 178.6(2) . . . . ? C18 C19 C20 C15 -0.4(4) . . . . ? C18 C19 C20 C21 179.0(2) . . . . ? C16 C15 C20 C19 2.4(3) . . . . ? P1 C15 C20 C19 -176.90(18) . . . . ? C16 C15 C20 C21 -177.0(2) . . . . ? P1 C15 C20 C21 3.7(3) . . . . ? # ===END data_6b _database_code_depnum_ccdc_archive 'CCDC 248104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H21 F H1 Mo2 O4 P' _chemical_formula_weight 604.26 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' F F 0.0171 0.0103 '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' H H1- 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5683(9) _cell_length_b 10.8886(13) _cell_length_c 13.719(3) _cell_angle_alpha 94.019(15) _cell_angle_beta 103.809(10) _cell_angle_gamma 112.294(8) _cell_volume 1131.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.5 _cell_measurement_theta_max 15.9 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 30 _diffrn_standards_decay_% ? _diffrn_reflns_number 3972 _diffrn_reflns_av_R_equivalents 0.0064 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3958 _reflns_number_gt 3340 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CAD4/PC (Nonius, 1996)' _computing_cell_refinement 'CAD4/PC (Nonius, 1996)' _computing_data_reduction 'XCAD4B (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0285P)^2^+0.3818P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3958 _refine_ls_number_parameters 335 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.006 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 0.10218(4) 0.29743(3) 0.28432(2) 0.03159(10) Uani 1 1 d . . . Mo2 Mo 0.22547(4) 0.05913(3) 0.35142(2) 0.03454(10) Uani 1 1 d . A . H1 H1- 0.116(5) 0.170(4) 0.366(3) 0.019(11) Uiso 1 1 d . A . C1A C 0.2809(15) 0.4994(17) 0.4031(12) 0.032(2) Uani 0.67 1 d PD A 1 H1A H 0.4024 0.5269 0.4248 0.039 Uiso 0.67 1 calc PR A 1 C2A C 0.184(2) 0.528(2) 0.3162(15) 0.054(4) Uani 0.67 1 d PD A 1 H2A H 0.2305 0.5835 0.2727 0.065 Uiso 0.67 1 calc PR A 1 C3A C 0.003(2) 0.456(2) 0.3069(15) 0.076(7) Uani 0.67 1 d PD A 1 H3A H -0.0911 0.4531 0.2544 0.091 Uiso 0.67 1 calc PR A 1 C4A C -0.0090(16) 0.3919(17) 0.3903(13) 0.063(5) Uani 0.67 1 d PD A 1 H4A H -0.1127 0.3377 0.4035 0.076 Uiso 0.67 1 calc PR A 1 C5A C 0.1594(16) 0.4221(14) 0.4502(9) 0.038(3) Uani 0.67 1 d PD A 1 H5A H 0.1876 0.3951 0.5125 0.045 Uiso 0.67 1 calc PR A 1 C1B C 0.208(4) 0.523(4) 0.327(3) 0.054(10) Uani 0.33 1 d PDU A 2 H1B H 0.2915 0.5699 0.2950 0.065 Uiso 0.33 1 calc PR A 2 C2B C 0.024(4) 0.482(4) 0.292(3) 0.051(7) Uani 0.33 1 d PDU A 2 H2B H -0.0367 0.5025 0.2336 0.062 Uiso 0.33 1 calc PR A 2 C3B C -0.053(3) 0.405(4) 0.360(3) 0.060(7) Uani 0.33 1 d PDU A 2 H3B H -0.1719 0.3649 0.3550 0.072 Uiso 0.33 1 calc PR A 2 C4B C 0.084(3) 0.399(2) 0.4347(19) 0.046(7) Uani 0.33 1 d PDU A 2 H4B H 0.0704 0.3479 0.4863 0.056 Uiso 0.33 1 calc PR A 2 C5B C 0.240(3) 0.480(4) 0.421(2) 0.046(8) Uani 0.33 1 d PDU A 2 H5B H 0.3505 0.5020 0.4662 0.056 Uiso 0.33 1 calc PR A 2 C6 C -0.1293(5) 0.1465(4) 0.2214(3) 0.0484(10) Uani 1 1 d . A . O1 O -0.2668(4) 0.0637(3) 0.1838(3) 0.0713(10) Uani 1 1 d . . . C7 C 0.0843(5) 0.2897(4) 0.1385(3) 0.0438(9) Uani 1 1 d . A . O2 O 0.0691(4) 0.2863(3) 0.0523(2) 0.0669(9) Uani 1 1 d . . . C8 C 0.1253(8) -0.1585(4) 0.2627(4) 0.0687(15) Uani 1 1 d . . . H8 H 0.1866 -0.1777 0.2205 0.082 Uiso 1 1 calc R A . C9 C -0.0150(7) -0.1211(4) 0.2319(4) 0.0638(13) Uani 1 1 d . A . H9 H -0.0629 -0.1098 0.1666 0.077 Uiso 1 1 calc R . . C10 C -0.0706(6) -0.1036(4) 0.3192(4) 0.0593(12) Uani 1 1 d . . . H10 H -0.1623 -0.0783 0.3211 0.071 Uiso 1 1 calc R A . C11 C 0.0344(6) -0.1303(4) 0.4012(4) 0.0593(12) Uani 1 1 d . A . H11 H 0.0238 -0.1274 0.4671 0.071 Uiso 1 1 calc R . . C12 C 0.1595(7) -0.1625(4) 0.3682(4) 0.0639(13) Uani 1 1 d . A . H12 H 0.2479 -0.1826 0.4081 0.077 Uiso 1 1 calc R . . C13 C 0.3327(5) 0.1541(4) 0.4913(3) 0.0441(9) Uani 1 1 d . . . O3 O 0.3957(4) 0.2042(3) 0.5756(2) 0.0653(9) Uani 1 1 d . A . C14 C 0.4711(6) 0.0854(4) 0.3673(3) 0.0497(10) Uani 1 1 d . . . O4 O 0.6148(4) 0.1005(4) 0.3787(3) 0.0782(11) Uani 1 1 d . A . P1 P 0.35520(11) 0.25623(9) 0.27743(7) 0.0286(2) Uani 1 1 d . A . F1 F 0.5324(3) 0.3585(2) 0.36424(15) 0.0407(5) Uani 1 1 d . . . C15 C 0.4500(4) 0.2834(3) 0.1700(3) 0.0323(8) Uani 1 1 d . . . C16 C 0.4107(5) 0.1776(4) 0.0924(3) 0.0405(9) Uani 1 1 d . A . C17 C 0.4921(5) 0.2018(4) 0.0148(3) 0.0477(10) Uani 1 1 d . . . H17 H 0.4660 0.1301 -0.0362 0.057 Uiso 1 1 calc R A . C18 C 0.6092(5) 0.3277(4) 0.0110(3) 0.0453(10) Uani 1 1 d . A . C19 C 0.6380(5) 0.4336(4) 0.0843(3) 0.0422(9) Uani 1 1 d . . . H19 H 0.7108 0.5205 0.0801 0.051 Uiso 1 1 calc R A . C20 C 0.5627(4) 0.4153(3) 0.1638(3) 0.0341(8) Uani 1 1 d . A . C21 C 0.2807(6) 0.0356(4) 0.0858(3) 0.0659(15) Uani 1 1 d . . . H21A H 0.264(3) -0.0154(17) 0.026(2) 0.099 Uiso 1 1 calc R A . H21B H 0.176(3) 0.0363(6) 0.089(3) 0.099 Uiso 1 1 calc R . . H21C H 0.323(2) -0.0001(16) 0.139(2) 0.099 Uiso 1 1 calc R . . C22 C 0.7003(6) 0.3496(5) -0.0724(3) 0.0682(15) Uani 1 1 d . . . H22A H 0.799(4) 0.338(4) -0.0526(13) 0.102 Uiso 1 1 calc R A . H22B H 0.725(4) 0.433(3) -0.0845(19) 0.102 Uiso 1 1 calc R . . H22C H 0.630(3) 0.291(3) -0.1289(18) 0.102 Uiso 1 1 calc R . . C23 C 0.6053(5) 0.5405(4) 0.2376(3) 0.0471(10) Uani 1 1 d . . . H23A H 0.697(3) 0.5501(15) 0.2958(16) 0.071 Uiso 1 1 calc R A . H23B H 0.504(2) 0.5332(12) 0.2574(17) 0.071 Uiso 1 1 calc R . . H23C H 0.641(3) 0.6166(18) 0.2059(10) 0.071 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 0.02873(17) 0.02864(17) 0.03450(18) -0.00265(13) 0.00766(13) 0.01093(13) Mo2 0.04101(19) 0.02553(17) 0.0396(2) 0.00621(13) 0.02020(15) 0.01107(14) C1A 0.032(5) 0.027(4) 0.034(5) -0.005(3) 0.016(5) 0.006(5) C2A 0.094(11) 0.035(8) 0.049(7) 0.009(6) 0.016(7) 0.045(8) C3A 0.077(10) 0.10(2) 0.064(8) -0.019(9) -0.012(8) 0.071(13) C4A 0.024(8) 0.070(8) 0.079(11) -0.039(8) 0.009(7) 0.014(7) C5A 0.035(8) 0.029(7) 0.030(4) -0.015(4) 0.013(5) -0.005(6) C1B 0.050(12) 0.031(17) 0.08(2) -0.002(13) 0.043(16) -0.002(11) C2B 0.063(15) 0.017(7) 0.073(15) -0.013(10) 0.008(9) 0.027(9) C3B 0.018(8) 0.050(11) 0.12(3) -0.010(15) 0.033(12) 0.013(10) C4B 0.04(2) 0.019(9) 0.048(14) -0.018(10) 0.020(13) -0.018(15) C5B 0.017(10) 0.06(2) 0.058(17) -0.019(11) 0.018(8) 0.007(11) C6 0.045(2) 0.051(3) 0.044(2) -0.006(2) 0.0106(19) 0.017(2) O1 0.0402(18) 0.068(2) 0.071(2) -0.0155(18) 0.0013(16) -0.0005(16) C7 0.039(2) 0.041(2) 0.049(3) 0.0027(19) 0.0085(19) 0.0167(18) O2 0.074(2) 0.092(3) 0.0375(18) 0.0155(17) 0.0111(16) 0.039(2) C8 0.108(4) 0.026(2) 0.074(3) 0.004(2) 0.054(3) 0.015(3) C9 0.073(3) 0.032(2) 0.062(3) 0.004(2) 0.023(3) -0.006(2) C10 0.051(3) 0.033(2) 0.080(3) 0.008(2) 0.029(3) -0.002(2) C11 0.078(3) 0.032(2) 0.067(3) 0.013(2) 0.043(3) 0.007(2) C12 0.088(4) 0.027(2) 0.084(4) 0.018(2) 0.041(3) 0.020(2) C13 0.043(2) 0.039(2) 0.051(3) 0.0115(19) 0.024(2) 0.0107(18) O3 0.062(2) 0.070(2) 0.0423(18) 0.0000(16) 0.0143(16) 0.0066(17) C14 0.057(3) 0.050(3) 0.058(3) 0.021(2) 0.031(2) 0.028(2) O4 0.063(2) 0.095(3) 0.108(3) 0.044(2) 0.044(2) 0.048(2) P1 0.0279(4) 0.0250(4) 0.0299(5) 0.0011(4) 0.0097(4) 0.0077(4) F1 0.0345(11) 0.0371(12) 0.0370(12) 0.0005(9) 0.0057(9) 0.0041(9) C15 0.0283(18) 0.0333(19) 0.035(2) 0.0064(15) 0.0087(15) 0.0123(15) C16 0.043(2) 0.037(2) 0.037(2) 0.0033(17) 0.0149(17) 0.0109(18) C17 0.053(2) 0.052(3) 0.038(2) 0.0005(19) 0.0157(19) 0.020(2) C18 0.042(2) 0.062(3) 0.040(2) 0.020(2) 0.0170(18) 0.025(2) C19 0.037(2) 0.040(2) 0.049(2) 0.0183(19) 0.0149(18) 0.0115(18) C20 0.0310(18) 0.0339(19) 0.037(2) 0.0086(16) 0.0098(16) 0.0122(16) C21 0.077(3) 0.044(3) 0.054(3) -0.011(2) 0.032(3) -0.003(2) C22 0.075(3) 0.093(4) 0.053(3) 0.030(3) 0.039(3) 0.037(3) C23 0.051(2) 0.035(2) 0.057(3) 0.0124(19) 0.022(2) 0.0156(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 H1 1.86(4) . ? Mo1 C7 1.963(4) . ? Mo1 C6 1.972(4) . ? Mo1 C3A 2.23(2) . ? Mo1 C1B 2.25(4) . ? Mo1 C4A 2.297(17) . ? Mo1 C2A 2.31(2) . ? Mo1 C4B 2.34(3) . ? Mo1 C5B 2.34(4) . ? Mo1 C2B 2.35(4) . ? Mo1 C1A 2.364(17) . ? Mo1 P1 2.3959(9) . ? Mo1 C5A 2.407(14) . ? Mo1 C3B 2.42(4) . ? Mo1 Mo2 3.2629(6) . ? Mo2 H1 1.82(3) . ? Mo2 C13 1.938(4) . ? Mo2 C14 1.968(4) . ? Mo2 C12 2.302(4) . ? Mo2 C8 2.321(4) . ? Mo2 C11 2.360(4) . ? Mo2 C9 2.377(4) . ? Mo2 C10 2.391(4) . ? Mo2 P1 2.4303(10) . ? C1A C5A 1.394(11) . ? C1A C2A 1.407(13) . ? C1A H1A 0.9300 . ? C2A C3A 1.417(19) . ? C2A H2A 0.9300 . ? C3A C4A 1.387(16) . ? C3A H3A 0.9300 . ? C4A C5A 1.379(11) . ? C4A H4A 0.9300 . ? C5A H5A 0.9300 . ? C1B C5B 1.40(2) . ? C1B C2B 1.42(2) . ? C1B H1B 0.9300 . ? C2B C3B 1.41(3) . ? C2B H2B 0.9300 . ? C3B C4B 1.38(2) . ? C3B H3B 0.9300 . ? C4B C5B 1.364(16) . ? C4B H4B 0.9300 . ? C5B H5B 0.9300 . ? C6 O1 1.142(5) . ? C7 O2 1.155(5) . ? C8 C9 1.393(7) . ? C8 C12 1.415(7) . ? C8 H8 0.9300 . ? C9 C10 1.416(6) . ? C9 H9 0.9300 . ? C10 C11 1.386(6) . ? C10 H10 0.9300 . ? C11 C12 1.403(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 O3 1.148(5) . ? C14 O4 1.149(5) . ? P1 F1 1.623(2) . ? P1 C15 1.836(3) . ? C15 C16 1.392(5) . ? C15 C20 1.416(5) . ? C16 C17 1.395(5) . ? C16 C21 1.505(5) . ? C17 C18 1.372(6) . ? C17 H17 0.9300 . ? C18 C19 1.380(6) . ? C18 C22 1.516(5) . ? C19 C20 1.384(5) . ? C19 H19 0.9300 . ? C20 C23 1.506(5) . ? C21 H21A 0.9115 . ? C21 H21B 0.9115 . ? C21 H21C 0.9115 . ? C22 H22A 0.8877 . ? C22 H22B 0.8877 . ? C22 H22C 0.8877 . ? C23 H23A 0.9440 . ? C23 H23B 0.9440 . ? C23 H23C 0.9440 . ? 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 H1 Mo1 C7 129.2(11) . . ? H1 Mo1 C6 78.9(11) . . ? C7 Mo1 C6 78.14(16) . . ? H1 Mo1 C3A 128.1(12) . . ? C7 Mo1 C3A 99.3(5) . . ? C6 Mo1 C3A 97.0(5) . . ? H1 Mo1 C1B 129.6(14) . . ? C7 Mo1 C1B 97.1(8) . . ? C6 Mo1 C1B 137.1(8) . . ? H1 Mo1 C4A 92.4(12) . . ? C7 Mo1 C4A 132.9(4) . . ? C6 Mo1 C4A 91.9(4) . . ? C2A Mo1 C1A 35.0(4) . . ? C3A Mo1 C1A 59.4(5) . . ? C4A Mo1 C1A 58.1(4) . . ? C1A Mo1 C5A 34.0(3) . . ? C3A Mo1 C2A 36.3(5) . . ? C4A Mo1 C2A 58.8(6) . . ? C2A Mo1 C5A 56.8(5) . . ? C3A Mo1 C4A 35.6(5) . . ? C3A Mo1 C5A 57.7(5) . . ? C4A Mo1 C5A 34.0(3) . . ? H1 Mo1 C2A 134.2(12) . . ? C7 Mo1 C2A 94.0(4) . . ? C6 Mo1 C2A 131.4(5) . . ? H1 Mo1 C4B 80.4(13) . . ? C7 Mo1 C4B 149.9(7) . . ? C6 Mo1 C4B 106.3(6) . . ? C1B Mo1 C2B 35.7(8) . . ? C1B Mo1 C3B 58.6(10) . . ? C1B Mo1 C4B 58.9(8) . . ? C1B Mo1 C5B 35.5(7) . . ? C2B Mo1 C3B 34.4(8) . . ? C4B Mo1 C2B 57.3(9) . . ? C5B Mo1 C2B 57.3(10) . . ? C4B Mo1 C3B 33.8(7) . . ? C5B Mo1 C3B 56.1(9) . . ? C4B Mo1 C5B 33.9(5) . . ? H1 Mo1 C5B 94.2(14) . . ? C7 Mo1 C5B 131.1(7) . . ? C6 Mo1 C5B 139.8(6) . . ? H1 Mo1 C2B 136.3(15) . . ? C7 Mo1 C2B 92.5(10) . . ? C6 Mo1 C2B 101.5(7) . . ? H1 Mo1 C1A 100.5(12) . . ? C7 Mo1 C1A 121.0(4) . . ? C6 Mo1 C1A 150.1(3) . . ? H1 Mo1 P1 72.0(11) . . ? C7 Mo1 P1 78.89(11) . . ? C6 Mo1 P1 116.43(12) . . ? C3A Mo1 P1 145.0(5) . . ? C1B Mo1 P1 104.0(8) . . ? C4A Mo1 P1 143.0(4) . . ? C2A Mo1 P1 108.7(5) . . ? C4B Mo1 P1 122.0(7) . . ? C5B Mo1 P1 98.2(6) . . ? C2B Mo1 P1 138.0(8) . . ? C1A Mo1 P1 91.1(3) . . ? H1 Mo1 C5A 79.1(12) . . ? C7 Mo1 C5A 150.9(3) . . ? C6 Mo1 C5A 119.2(3) . . ? P1 Mo1 C5A 109.0(3) . . ? H1 Mo1 C3B 103.2(14) . . ? C7 Mo1 C3B 119.9(9) . . ? C6 Mo1 C3B 86.7(8) . . ? P1 Mo1 C3B 154.0(8) . . ? H1 Mo1 Mo2 27.1(11) . . ? C7 Mo1 Mo2 105.61(11) . . ? C6 Mo1 Mo2 83.91(13) . . ? C3A Mo1 Mo2 154.6(5) . . ? C1B Mo1 Mo2 137.0(9) . . ? C4A Mo1 Mo2 119.1(4) . . ? C2A Mo1 Mo2 143.1(5) . . ? C4B Mo1 Mo2 104.5(7) . . ? C5B Mo1 Mo2 107.7(8) . . ? C2B Mo1 Mo2 161.8(9) . . ? C1A Mo1 Mo2 109.4(3) . . ? P1 Mo1 Mo2 47.91(2) . . ? C5A Mo1 Mo2 99.7(3) . . ? C3B Mo1 Mo2 130.3(8) . . ? H1 Mo2 C13 74.7(11) . . ? H1 Mo2 C14 134.8(11) . . ? C13 Mo2 C14 80.12(17) . . ? H1 Mo2 C12 133.0(11) . . ? C13 Mo2 C12 102.86(17) . . ? C14 Mo2 C12 88.70(18) . . ? H1 Mo2 C8 132.5(11) . . ? C13 Mo2 C8 138.06(18) . . ? C14 Mo2 C8 90.61(19) . . ? C12 Mo2 C8 35.63(16) . . ? H1 Mo2 C11 98.1(11) . . ? C13 Mo2 C11 91.73(16) . . ? C14 Mo2 C11 119.72(17) . . ? C12 Mo2 C11 35.00(15) . . ? C8 Mo2 C11 57.78(16) . . ? H1 Mo2 C9 98.3(11) . . ? C13 Mo2 C9 147.59(16) . . ? C14 Mo2 C9 121.87(18) . . ? C12 Mo2 C9 58.48(19) . . ? C8 Mo2 C9 34.47(17) . . ? C11 Mo2 C9 57.39(16) . . ? H1 Mo2 C10 79.9(11) . . ? C13 Mo2 C10 113.79(16) . . ? C14 Mo2 C10 145.19(17) . . ? C12 Mo2 C10 57.74(18) . . ? C8 Mo2 C10 57.22(17) . . ? C11 Mo2 C10 33.92(15) . . ? C9 Mo2 C10 34.56(15) . . ? H1 Mo2 P1 71.8(11) . . ? C13 Mo2 P1 94.79(11) . . ? C14 Mo2 P1 73.74(12) . . ? C12 Mo2 P1 152.61(12) . . ? C8 Mo2 P1 121.84(12) . . ? C11 Mo2 P1 165.97(13) . . ? C9 Mo2 P1 113.36(12) . . ? C10 Mo2 P1 132.40(13) . . ? H1 Mo2 Mo1 27.9(11) . . ? C13 Mo2 Mo1 91.27(12) . . ? C14 Mo2 Mo1 119.28(12) . . ? C12 Mo2 Mo1 150.69(14) . . ? C8 Mo2 Mo1 127.90(15) . . ? C11 Mo2 Mo1 120.53(12) . . ? C9 Mo2 Mo1 96.37(13) . . ? C10 Mo2 Mo1 93.12(12) . . ? P1 Mo2 Mo1 47.02(2) . . ? Mo2 H1 Mo1 125(2) . . ? C5A C1A C2A 106.6(10) . . ? C5A C1A Mo1 74.7(9) . . ? C2A C1A Mo1 70.4(12) . . ? C5A C1A H1A 126.7 . . ? C2A C1A H1A 126.7 . . ? Mo1 C1A H1A 120.0 . . ? C1A C2A C3A 107.8(12) . . ? C1A C2A Mo1 74.6(11) . . ? C3A C2A Mo1 68.8(12) . . ? C1A C2A H2A 126.1 . . ? C3A C2A H2A 126.1 . . ? Mo1 C2A H2A 122.3 . . ? C4A C3A C2A 107.5(11) . . ? C4A C3A Mo1 74.7(11) . . ? C2A C3A Mo1 74.9(12) . . ? C4A C3A H3A 126.3 . . ? C2A C3A H3A 126.3 . . ? Mo1 C3A H3A 116.1 . . ? C5A C4A C3A 108.3(11) . . ? C5A C4A Mo1 77.4(9) . . ? C3A C4A Mo1 69.6(12) . . ? C5A C4A H4A 125.8 . . ? C3A C4A H4A 125.8 . . ? Mo1 C4A H4A 119.0 . . ? C4A C5A C1A 109.5(9) . . ? C4A C5A Mo1 68.6(8) . . ? C1A C5A Mo1 71.3(10) . . ? C4A C5A H5A 125.3 . . ? C1A C5A H5A 125.3 . . ? Mo1 C5A H5A 126.4 . . ? C5B C1B C2B 106(2) . . ? C5B C1B Mo1 76(2) . . ? C2B C1B Mo1 76(2) . . ? C5B C1B H1B 127.1 . . ? C2B C1B H1B 127.1 . . ? Mo1 C1B H1B 113.7 . . ? C3B C2B C1B 108(2) . . ? C3B C2B Mo1 75(2) . . ? C1B C2B Mo1 68(2) . . ? C3B C2B H2B 126.0 . . ? C1B C2B H2B 126.0 . . ? Mo1 C2B H2B 122.4 . . ? C4B C3B C2B 107.1(17) . . ? C4B C3B Mo1 70.0(17) . . ? C2B C3B Mo1 70(2) . . ? C4B C3B H3B 126.4 . . ? C2B C3B H3B 126.5 . . ? Mo1 C3B H3B 124.7 . . ? C5B C4B C3B 109.0(16) . . ? C5B C4B Mo1 73.1(19) . . ? C3B C4B Mo1 76.3(19) . . ? C5B C4B H4B 125.5 . . ? C3B C4B H4B 125.5 . . ? Mo1 C4B H4B 117.1 . . ? C4B C5B C1B 109.3(17) . . ? C4B C5B Mo1 73.0(18) . . ? C1B C5B Mo1 69(2) . . ? C4B C5B H5B 125.4 . . ? C1B C5B H5B 125.3 . . ? Mo1 C5B H5B 124.5 . . ? O1 C6 Mo1 176.6(4) . . ? O2 C7 Mo1 177.7(3) . . ? C9 C8 C12 109.1(4) . . ? C9 C8 Mo2 75.0(2) . . ? C12 C8 Mo2 71.5(2) . . ? C9 C8 H8 125.5 . . ? C12 C8 H8 125.5 . . ? Mo2 C8 H8 119.8 . . ? C8 C9 C10 106.9(5) . . ? C8 C9 Mo2 70.5(3) . . ? C10 C9 Mo2 73.2(3) . . ? C8 C9 H9 126.5 . . ? C10 C9 H9 126.5 . . ? Mo2 C9 H9 121.5 . . ? C11 C10 C9 108.5(5) . . ? C11 C10 Mo2 71.8(2) . . ? C9 C10 Mo2 72.2(2) . . ? C11 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Mo2 C10 H10 121.9 . . ? C10 C11 C12 108.7(4) . . ? C10 C11 Mo2 74.3(2) . . ? C12 C11 Mo2 70.3(2) . . ? C10 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? Mo2 C11 H11 121.5 . . ? C11 C12 C8 106.8(5) . . ? C11 C12 Mo2 74.7(2) . . ? C8 C12 Mo2 72.9(2) . . ? C11 C12 H12 126.6 . . ? C8 C12 H12 126.6 . . ? Mo2 C12 H12 117.9 . . ? O3 C13 Mo2 176.5(4) . . ? O4 C14 Mo2 178.5(4) . . ? F1 P1 C15 96.01(13) . . ? F1 P1 Mo1 112.45(9) . . ? C15 P1 Mo1 123.07(11) . . ? F1 P1 Mo2 106.44(8) . . ? C15 P1 Mo2 133.64(12) . . ? Mo1 P1 Mo2 85.07(3) . . ? C16 C15 C20 118.7(3) . . ? C16 C15 P1 121.6(3) . . ? C20 C15 P1 119.7(3) . . ? C15 C16 C17 119.6(3) . . ? C15 C16 C21 123.5(3) . . ? C17 C16 C21 116.9(3) . . ? C18 C17 C16 122.2(4) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 117.7(4) . . ? C17 C18 C22 120.8(4) . . ? C19 C18 C22 121.5(4) . . ? C18 C19 C20 122.5(4) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C15 119.1(3) . . ? C19 C20 C23 116.5(3) . . ? C15 C20 C23 124.4(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.345 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.068 # ===END data_7c' _database_code_depnum_ccdc_archive 'CCDC 248105' _audit_creation_date 03-13-03 _audit_creation_method CRYSTALS_ver_12-03-99 # 1061225 Compound X # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file REFCIF.DAT # This is a character file which you may edit to reflect local conditions # # Items which need looking at are represented by a '?' # Items for which there are choices are prefixed with 'choose from' # _cell_length_a 20.6073(19) _cell_angle_alpha 90 _cell_length_b 9.5398(7) _cell_angle_beta 101.031(8) _cell_length_c 27.706(3) _cell_angle_gamma 90 _cell_volume 5346.1(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Mo ' -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C21.5 H23 B Cl O5 F4 Mo2 P ' _chemical_formula_moiety ' C21.5 H23 B Cl O5 F4 Mo2 P' _chemical_compound_source ; ? ; _chemical_formula_weight 706.53 _cell_measurement_reflns_used 70 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _cell_measurement_temperature 293 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2792.000 _exptl_absorpt_coefficient_mu 1.156 # Sheldrick geometric definitions 0.89 0.89 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; DIFABS (Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.89 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293 _diffrn_reflns_number 23625 _reflns_number_total 10840 _diffrn_reflns_av_R_equivalents 0.09 # Number of reflections with Friedels Law is 10840 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12294 _diffrn_reflns_theta_min 2.014 _diffrn_reflns_theta_max 27.510 _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 20.701 _diffrn_measured_fraction_theta_full 0.964 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min -26 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _refine_diff_density_min -0.97 _refine_diff_density_max 1.94 _refine_ls_number_reflns 6107 _refine_ls_number_parameters 576 #_refine_ls_R_factor_ref 0.0684 _refine_ls_wR_factor_ref 0.0809 _refine_ls_goodness_of_fit_ref 0.8787 #_reflns_number_all 10837 _refine_ls_R_factor_all 0.1215 _refine_ls_wR_factor_all 0.1639 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6107 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_gt 0.0809 _refine_ls_shift/su_max 0.000496 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 0.484 0.463 0.205 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens Mo1 Mo 0.18930(4) 1.36346(9) -0.14414(3) 0.0387 1.0000 Uani . Mo2 Mo 0.12625(4) 1.56872(9) -0.07433(3) 0.0359 1.0000 Uani . P12 P 0.20229(12) 1.6126(3) -0.13033(9) 0.0349 1.0000 Uani . O1 O 0.0359(4) 1.4144(9) -0.1599(3) 0.0678 1.0000 Uani . O11 O 0.3242(5) 1.3495(11) -0.0701(4) 0.0815 1.0000 Uani . O12 O 0.1577(5) 1.116(1) -0.0773(4) 0.0753 1.0000 Uani . O21 O 0.2632(4) 1.5645(12) -0.0005(3) 0.0767 1.0000 Uani . O22 O 0.0932(5) 1.3097(11) -0.0130(4) 0.0815 1.0000 Uani . C1 C 0.0871(6) 1.4386(12) -0.1364(4) 0.0527 1.0000 Uani . C11 C 0.2740(6) 1.3589(12) -0.0962(4) 0.0491 1.0000 Uani . C12 C 0.1662(6) 1.2062(11) -0.1008(4) 0.0476 1.0000 Uani . C21 C 0.2141(6) 1.5609(12) -0.0263(4) 0.0460 1.0000 Uani . C22 C 0.1049(6) 1.3979(13) -0.0355(4) 0.0517 1.0000 Uani . C101 C 0.2151(8) 1.409(2) -0.2206(4) 0.0798 1.0000 Uani . C102 C 0.243(1) 1.283(3) -0.2046(6) 0.0971 1.0000 Uani . C103 C 0.1961(12) 1.1913(17) -0.2009(6) 0.0893 1.0000 Uani . C104 C 0.1334(9) 1.2606(19) -0.2148(5) 0.0809 1.0000 Uani . C105 C 0.1481(7) 1.3969(16) -0.2265(4) 0.0689 1.0000 Uani . C121 C 0.2826(4) 1.703(1) -0.1126(3) 0.0368 1.0000 Uani . C122 C 0.3222(5) 1.6886(13) -0.1537(4) 0.0524 1.0000 Uani . C123 C 0.3874(6) 1.7718(15) -0.1406(5) 0.0647 1.0000 Uani . C124 C 0.3742(7) 1.9238(14) -0.1316(5) 0.0656 1.0000 Uani . C125 C 0.3351(7) 1.9386(12) -0.0893(5) 0.0598 1.0000 Uani . C126 C 0.2709(6) 1.8578(11) -0.1012(4) 0.0511 1.0000 Uani . C201 C 0.0406(6) 1.7107(14) -0.1131(5) 0.0623 1.0000 Uani . C202 C 0.0201(6) 1.6386(15) -0.0739(6) 0.0686 1.0000 Uani . C203 C 0.0619(7) 1.6876(16) -0.0295(5) 0.0670 1.0000 Uani . C204 C 0.1053(7) 1.7844(14) -0.0423(6) 0.0684 1.0000 Uani . C205 C 0.0915(6) 1.7977(13) -0.0942(5) 0.0600 1.0000 Uani . Mo3 Mo 0.31579(5) 1.09919(9) 0.10789(3) 0.0442 1.0000 Uani . Mo4 Mo 0.35938(4) 0.9414(1) 0.21054(3) 0.0389 1.0000 Uani . C2 C 0.2700(6) 1.0305(12) 0.1739(4) 0.0540 1.0000 Uani . O2 O 0.2141(4) 1.0430(11) 0.1783(4) 0.0767 1.0000 Uani . P34 P 0.35768(13) 0.8653(3) 0.12607(9) 0.0399 1.0000 Uani . O31 O 0.4574(6) 1.1661(15) 0.0917(5) 0.1078 1.0000 Uani . O32 O 0.3401(9) 1.3767(12) 0.1687(5) 0.1222 1.0000 Uani . O41 O 0.5048(4) 1.0251(13) 0.2013(4) 0.0813 1.0000 Uani . O42 O 0.3741(6) 1.2337(14) 0.2643(4) 0.1063 1.0000 Uani . C31 C 0.4065(6) 1.1384(15) 0.1000(5) 0.0641 1.0000 Uani . C32 C 0.3300(9) 1.2762(15) 0.1479(6) 0.0799 1.0000 Uani . C41 C 0.4523(6) 0.9951(13) 0.2036(4) 0.0539 1.0000 Uani . C42 C 0.3689(7) 1.1293(16) 0.2451(5) 0.0656 1.0000 Uani . C301 C 0.2576(9) 1.003(2) 0.0355(6) 0.0866 1.0000 Uani . C302 C 0.285(1) 1.120(3) 0.0247(5) 0.1066 1.0000 Uani . C303 C 0.2556(14) 1.230(2) 0.0474(9) 0.1256 1.0000 Uani . C304 C 0.2098(7) 1.170(2) 0.0742(6) 0.0814 1.0000 Uani . C305 C 0.2127(7) 1.0290(16) 0.0657(5) 0.0734 1.0000 Uani . C341 C 0.4310(6) 0.7931(13) 0.1053(4) 0.0531 1.0000 Uani . C342 C 0.4194(9) 0.7859(17) 0.0493(4) 0.0801 1.0000 Uani . C343 C 0.480(1) 0.727(3) 0.0346(6) 0.1127 1.0000 Uani . C344 C 0.500(1) 0.587(3) 0.0575(8) 0.1259 1.0000 Uani . C345 C 0.5067(11) 0.587(2) 0.1109(7) 0.1184 1.0000 Uani . C346 C 0.4480(9) 0.6493(18) 0.1279(5) 0.0899 1.0000 Uani . C401 C 0.344(1) 0.7055(14) 0.2250(6) 0.0792 1.0000 Uani . C402 C 0.3976(8) 0.7505(17) 0.2588(6) 0.0768 1.0000 Uani . C403 C 0.3713(9) 0.8500(18) 0.2876(5) 0.0834 1.0000 Uani . C404 C 0.3059(8) 0.8675(18) 0.2710(5) 0.0748 1.0000 Uani . C405 C 0.2869(8) 0.7745(17) 0.2312(6) 0.0748 1.0000 Uani . B1 B 0.1708(9) 0.5975(18) 0.1042(6) 0.067(4) 1.0000 Uiso . F11 F 0.1783(7) 0.7063(16) 0.0746(5) 0.151(5) 1.0000 Uiso . F12 F 0.2247(15) 0.519(3) 0.1076(11) 0.275(12) 1.0000 Uiso . F13 F 0.1708(12) 0.646(3) 0.1465(9) 0.223(8) 1.0000 Uiso . F14 F 0.1187(16) 0.533(3) 0.0878(12) 0.276(12) 1.0000 Uiso . B2 B 0.5944(14) 0.663(3) 0.253(1) 0.111(7) 1.0000 Uiso . F21 F 0.6103(14) 0.760(3) 0.221(1) 0.26(1) 1.0000 Uiso . F22 F 0.6437(11) 0.614(2) 0.2864(8) 0.201(7) 1.0000 Uiso . F23 F 0.5433(14) 0.565(3) 0.237(1) 0.25(1) 1.0000 Uiso . F24 F 0.5587(9) 0.757(2) 0.2741(7) 0.182(6) 1.0000 Uiso . C500 C 0.4442(11) 0.392(2) 0.3709(8) 0.116(6) 1.0000 Uiso . Cl1 Cl 0.4911(3) 0.4519(6) 0.3304(2) 0.1154(16) 1.0000 Uiso . Cl2 Cl 0.4680(4) 0.4530(8) 0.4312(3) 0.146(2) 1.0000 Uiso . H121 H 0.1953 1.6846 -0.1571 0.089(7) 1.0000 Uiso . H341 H 0.3353 0.7786 0.1107 0.089(7) 1.0000 Uiso . H1011 H 0.2397 1.4959 -0.2267 0.089(7) 1.0000 Uiso . H1021 H 0.2914 1.2624 -0.1967 0.089(7) 1.0000 Uiso . H1031 H 0.2026 1.0912 -0.1904 0.089(7) 1.0000 Uiso . H1041 H 0.0886 1.2192 -0.2158 0.089(7) 1.0000 Uiso . H1051 H 0.1152 1.4728 -0.2375 0.089(7) 1.0000 Uiso . H1211 H 0.3088 1.6594 -0.0822 0.089(7) 1.0000 Uiso . H1221 H 0.2956 1.7257 -0.1851 0.089(7) 1.0000 Uiso . H1222 H 0.3325 1.5873 -0.1580 0.089(7) 1.0000 Uiso . H1231 H 0.4118 1.7647 -0.1684 0.089(7) 1.0000 Uiso . H1232 H 0.4149 1.7311 -0.1102 0.089(7) 1.0000 Uiso . H1241 H 0.4173 1.9748 -0.1225 0.089(7) 1.0000 Uiso . H1242 H 0.3479 1.9659 -0.1623 0.089(7) 1.0000 Uiso . H1251 H 0.3251 2.0399 -0.0847 0.089(7) 1.0000 Uiso . H1252 H 0.3623 1.9012 -0.0582 0.089(7) 1.0000 Uiso . H1261 H 0.2421 1.9013 -0.1304 0.089(7) 1.0000 Uiso . H1262 H 0.2483 1.8627 -0.0723 0.089(7) 1.0000 Uiso . H2011 H 0.0211 1.6992 -0.1488 0.089(7) 1.0000 Uiso . H2021 H -0.0163 1.5680 -0.0766 0.089(7) 1.0000 Uiso . H2031 H 0.0598 1.6571 0.0047 0.089(7) 1.0000 Uiso . H2041 H 0.1405 1.8360 -0.0191 0.089(7) 1.0000 Uiso . H2051 H 0.1154 1.8604 -0.1137 0.089(7) 1.0000 Uiso . H3011 H 0.2679 0.9088 0.0236 0.089(7) 1.0000 Uiso . H3021 H 0.3195 1.1303 0.0043 0.089(7) 1.0000 Uiso . H3031 H 0.2655 1.3325 0.0450 0.089(7) 1.0000 Uiso . H3041 H 0.1821 1.2201 0.0948 0.089(7) 1.0000 Uiso . H3051 H 0.1862 0.9558 0.0792 0.089(7) 1.0000 Uiso . H3411 H 0.4695 0.8570 0.1164 0.089(7) 1.0000 Uiso . H3421 H 0.4106 0.8820 0.0352 0.089(7) 1.0000 Uiso . H3422 H 0.3809 0.7237 0.0368 0.089(7) 1.0000 Uiso . H3431 H 0.5178 0.7947 0.0452 0.089(7) 1.0000 Uiso . H3432 H 0.4721 0.7169 -0.0019 0.089(7) 1.0000 Uiso . H3441 H 0.5442 0.5602 0.0495 0.089(7) 1.0000 Uiso . H3442 H 0.4664 0.5161 0.0432 0.089(7) 1.0000 Uiso . H3451 H 0.5467 0.6424 0.1255 0.089(7) 1.0000 Uiso . H3452 H 0.5120 0.4880 0.1228 0.089(7) 1.0000 Uiso . H3461 H 0.4583 0.6588 0.1645 0.089(7) 1.0000 Uiso . H3462 H 0.4091 0.5859 0.1182 0.089(7) 1.0000 Uiso . H4011 H 0.3456 0.6326 0.1993 0.089(7) 1.0000 Uiso . H4021 H 0.4447 0.7200 0.2622 0.089(7) 1.0000 Uiso . H4031 H 0.3977 0.9005 0.3165 0.089(7) 1.0000 Uiso . H4041 H 0.2763 0.9340 0.2843 0.089(7) 1.0000 Uiso . H4051 H 0.2415 0.7611 0.2113 0.089(7) 1.0000 Uiso . H5001 H 0.4465 0.2878 0.3716 0.089(7) 1.0000 Uiso . H5002 H 0.3974 0.4224 0.3586 0.089(7) 1.0000 Uiso . 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 0.0432(5) 0.0350(5) 0.0381(4) -0.0035(4) 0.0087(3) -0.0040(4) Mo2 0.0336(4) 0.0369(5) 0.0382(4) -0.0007(4) 0.0094(3) -0.0028(4) P12 0.0340(12) 0.0351(13) 0.0352(12) 0.004(1) 0.0054(9) -0.004(1) O1 0.039(4) 0.069(6) 0.088(6) -0.031(5) -0.006(4) -0.014(4) O11 0.048(5) 0.078(6) 0.109(8) 0.005(6) -0.010(5) 0.004(5) O12 0.088(7) 0.048(5) 0.093(7) 0.020(5) 0.026(5) -0.008(5) O21 0.047(5) 0.123(8) 0.053(5) 0.025(5) -0.007(4) -0.003(5) O22 0.090(7) 0.070(6) 0.092(7) 0.021(6) 0.038(6) -0.018(5) C1 0.051(6) 0.049(6) 0.061(7) -0.015(5) 0.018(5) -0.018(5) C11 0.049(7) 0.042(6) 0.059(6) 0.003(5) 0.016(5) 0.005(5) C12 0.055(6) 0.034(6) 0.055(6) -0.000(5) 0.015(5) -0.009(5) C21 0.050(6) 0.049(6) 0.045(5) 0.010(5) 0.026(5) 0.002(5) C22 0.057(7) 0.051(7) 0.051(6) -0.000(5) 0.020(5) -0.012(5) C101 0.091(11) 0.115(13) 0.037(6) -0.030(7) 0.022(6) -0.05(1) C102 0.091(12) 0.147(19) 0.055(8) -0.02(1) 0.017(8) 0.043(13) C103 0.146(18) 0.062(9) 0.07(1) -0.017(7) 0.055(11) 0.004(11) C104 0.099(12) 0.092(11) 0.058(8) -0.041(8) 0.031(8) -0.05(1) C105 0.076(9) 0.09(1) 0.039(6) -0.012(6) -0.001(6) 0.014(8) C121 0.030(5) 0.043(5) 0.037(5) 0.003(4) 0.005(4) -0.009(4) C122 0.044(6) 0.067(7) 0.051(6) -0.007(5) 0.023(5) -0.016(5) C123 0.055(7) 0.070(8) 0.075(8) -0.010(7) 0.029(6) -0.016(6) C124 0.073(8) 0.064(8) 0.065(7) -0.003(6) 0.024(6) -0.027(7) C125 0.072(8) 0.037(6) 0.074(8) -0.014(6) 0.020(6) -0.015(6) C126 0.054(7) 0.037(6) 0.064(7) -0.010(5) 0.018(5) -0.005(5) C201 0.060(8) 0.060(8) 0.066(8) -0.003(6) 0.007(6) 0.017(6) C202 0.045(7) 0.061(8) 0.106(11) -0.007(8) 0.030(7) -0.000(6) C203 0.067(8) 0.076(9) 0.061(7) -0.002(7) 0.020(6) 0.017(7) C204 0.060(8) 0.049(7) 0.10(1) -0.040(7) 0.015(7) 0.003(6) C205 0.040(6) 0.049(7) 0.09(1) -0.003(7) 0.021(6) 0.005(5) Mo3 0.0469(5) 0.0379(5) 0.0456(5) 0.0032(4) 0.0029(4) 0.0022(4) Mo4 0.0360(4) 0.0453(5) 0.0359(4) -0.0034(4) 0.0081(3) -0.0019(4) C2 0.060(8) 0.043(6) 0.063(7) -0.011(5) 0.023(6) 0.001(5) O2 0.047(5) 0.097(7) 0.090(6) -0.005(6) 0.023(5) 0.009(5) P34 0.0402(13) 0.0408(14) 0.0373(12) -0.0058(11) 0.004(1) 0.0013(11) O31 0.067(7) 0.13(1) 0.13(1) 0.019(8) 0.026(7) -0.033(7) O32 0.189(14) 0.049(6) 0.13(1) -0.024(7) 0.03(1) -0.016(8) O41 0.035(5) 0.128(9) 0.081(6) -0.011(6) 0.011(4) -0.016(5) O42 0.12(1) 0.106(9) 0.096(8) -0.059(7) 0.032(7) -0.022(8) C31 0.049(7) 0.072(9) 0.067(7) 0.018(7) 0.000(6) -0.014(6) C32 0.101(11) 0.048(8) 0.09(1) -0.012(7) 0.025(9) -0.014(7) C41 0.050(7) 0.065(7) 0.046(6) -0.014(5) 0.009(5) -0.012(6) C42 0.063(8) 0.079(9) 0.054(7) -0.024(7) 0.010(6) -0.008(7) C301 0.091(12) 0.104(13) 0.054(8) -0.017(9) -0.011(8) 0.02(1) C302 0.096(13) 0.17(2) 0.042(8) 0.025(11) -0.012(8) 0.008(15) C303 0.17(2) 0.067(11) 0.113(15) 0.042(11) -0.050(15) -0.007(13) C304 0.051(8) 0.102(13) 0.09(1) 0.010(9) -0.004(7) 0.024(8) C305 0.066(9) 0.08(1) 0.062(8) 0.012(7) -0.025(7) -0.008(7) C341 0.060(7) 0.062(7) 0.039(5) -0.015(5) 0.012(5) 0.013(6) C342 0.112(12) 0.09(1) 0.040(6) -0.015(7) 0.019(7) 0.023(9) C343 0.102(13) 0.18(2) 0.060(9) -0.015(11) 0.021(9) 0.029(14) C344 0.093(13) 0.18(2) 0.107(14) -0.056(15) 0.014(11) 0.055(14) C345 0.141(17) 0.119(15) 0.091(12) -0.024(11) 0.011(11) 0.086(14) C346 0.118(13) 0.089(11) 0.070(9) 0.020(8) 0.038(9) 0.07(1) C401 0.125(14) 0.042(7) 0.076(9) 0.011(6) 0.03(1) 0.002(8) C402 0.066(9) 0.073(9) 0.096(11) 0.026(8) 0.024(8) 0.025(7) C403 0.113(13) 0.08(1) 0.052(7) 0.005(7) 0.009(8) 0.00(1) C404 0.08(1) 0.098(11) 0.059(8) 0.030(8) 0.035(7) 0.013(8) C405 0.08(1) 0.08(1) 0.076(9) 0.019(8) 0.023(8) -0.006(8) _refine_ls_extinction_coef 107.784 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 . Mo2 . 3.1983(12) yes Mo1 . P12 . 2.414(3) yes Mo1 . C1 . 2.273(12) yes Mo1 . C11 . 1.981(12) yes Mo1 . C12 . 2.035(11) yes Mo1 . C101 . 2.321(12) yes Mo1 . C102 . 2.309(15) yes Mo1 . C103 . 2.297(14) yes Mo1 . C104 . 2.293(12) yes Mo1 . C105 . 2.300(12) yes Mo2 . P12 . 2.443(3) yes Mo2 . C1 . 2.149(11) yes Mo2 . C21 . 2.032(12) yes Mo2 . C22 . 2.046(12) yes Mo2 . C201 . 2.319(12) yes Mo2 . C202 . 2.289(12) yes Mo2 . C203 . 2.284(13) yes Mo2 . C204 . 2.314(11) yes Mo2 . C205 . 2.331(12) yes P12 . C121 . 1.848(9) yes P12 . H121 . 1.001 no O1 . C1 . 1.152(13) yes O11 . C11 . 1.147(14) yes O12 . C12 . 1.110(13) yes O21 . C21 . 1.122(13) yes O22 . C22 . 1.101(13) yes C101 . C102 . 1.37(3) yes C101 . C105 . 1.36(2) yes C101 . H1011 . 0.999 no C102 . C103 . 1.32(3) yes C102 . H1021 . 1.000 no C103 . C104 . 1.44(3) yes C103 . H1031 . 1.000 no C104 . C105 . 1.39(2) yes C104 . H1041 . 0.999 no C105 . H1051 . 0.999 no C121 . C122 . 1.532(14) yes C121 . C126 . 1.537(15) yes C121 . H1211 . 1.001 no C122 . C123 . 1.542(16) yes C122 . H1221 . 1.000 no C122 . H1222 . 1.001 no C123 . C124 . 1.51(2) yes C123 . H1231 . 0.998 no C123 . H1232 . 0.999 no C124 . C125 . 1.551(18) yes C124 . H1241 . 1.001 no C124 . H1242 . 1.002 no C125 . C126 . 1.511(16) yes C125 . H1251 . 1.001 no C125 . H1252 . 1.001 no C126 . H1261 . 0.998 no C126 . H1262 . 1.000 no C201 . C202 . 1.42(2) yes C201 . C205 . 1.361(18) yes C201 . H2011 . 1.000 no C202 . C203 . 1.44(2) yes C202 . H2021 . 0.999 no C203 . C204 . 1.38(2) yes C203 . H2031 . 1.000 no C204 . C205 . 1.42(2) yes C204 . H2041 . 1.002 no C205 . H2051 . 0.998 no Mo3 . Mo4 . 3.1913(12) yes Mo3 . C2 . 2.307(12) yes Mo3 . P34 . 2.411(3) yes Mo3 . C31 . 1.960(13) yes Mo3 . C32 . 2.011(15) yes Mo3 . C301 . 2.318(15) yes Mo3 . C302 . 2.279(14) yes Mo3 . C303 . 2.262(16) yes Mo3 . C304 . 2.305(13) yes Mo3 . C305 . 2.319(12) yes Mo4 . C2 . 2.105(13) yes Mo4 . P34 . 2.444(3) yes Mo4 . C41 . 2.026(12) yes Mo4 . C42 . 2.023(14) yes Mo4 . C401 . 2.318(13) yes Mo4 . C402 . 2.307(14) yes Mo4 . C403 . 2.276(14) yes Mo4 . C404 . 2.285(12) yes Mo4 . C405 . 2.327(14) yes C2 . O2 . 1.187(14) yes P34 . C341 . 1.851(11) yes P34 . H341 . 1.001 no O31 . C31 . 1.146(16) yes O32 . C32 . 1.117(17) yes O41 . C41 . 1.132(13) yes O42 . C42 . 1.125(16) yes C301 . C302 . 1.31(3) yes C301 . C305 . 1.38(2) yes C301 . H3011 . 0.999 no C302 . C303 . 1.41(3) yes C302 . H3021 . 1.000 no C303 . C304 . 1.43(3) yes C303 . H3031 . 1.001 no C304 . C305 . 1.37(2) yes C304 . H3041 . 1.003 no C305 . H3051 . 1.001 no C341 . C342 . 1.525(16) yes C341 . C346 . 1.521(19) yes C341 . H3411 . 1.001 no C342 . C343 . 1.50(2) yes C342 . H3421 . 1.000 no C342 . H3422 . 0.999 no C343 . C344 . 1.50(3) yes C343 . H3431 . 1.004 no C343 . H3432 . 0.997 no C344 . C345 . 1.46(3) yes C344 . H3441 . 1.001 no C344 . H3442 . 1.000 no C345 . C346 . 1.50(2) yes C345 . H3451 . 0.998 no C345 . H3452 . 0.999 no C346 . H3461 . 1.000 no C346 . H3462 . 1.000 no C401 . C402 . 1.37(2) yes C401 . C405 . 1.39(2) yes C401 . H4011 . 0.999 no C402 . C403 . 1.41(2) yes C402 . H4021 . 1.002 no C403 . C404 . 1.35(2) yes C403 . H4031 . 1.000 no C404 . C405 . 1.41(2) yes C404 . H4041 . 1.000 no C405 . H4051 . 1.000 no B1 . F11 . 1.35(2) yes B1 . F12 . 1.33(3) yes B1 . F13 . 1.26(3) yes B1 . F14 . 1.25(3) yes B2 . F21 . 1.35(3) yes B2 . F22 . 1.33(3) yes B2 . F23 . 1.41(3) yes B2 . F24 . 1.37(3) yes C500 . Cl1 . 1.71(2) yes C500 . Cl2 . 1.75(2) yes C500 . H5001 . 0.999 no C500 . H5002 . 1.002 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Mo2 . Mo1 . P12 . 49.20(6) yes Mo2 . Mo1 . C1 . 42.2(3) yes P12 . Mo1 . C1 . 75.6(3) yes Mo2 . Mo1 . C11 . 90.9(3) yes P12 . Mo1 . C11 . 81.9(3) yes C1 . Mo1 . C11 . 131.0(4) yes Mo2 . Mo1 . C12 . 85.8(3) yes P12 . Mo1 . C12 . 131.6(3) yes C1 . Mo1 . C12 . 81.5(4) yes C11 . Mo1 . C12 . 82.1(5) yes Mo2 . Mo1 . C101 . 128.8(5) yes P12 . Mo1 . C101 . 85.5(4) yes C1 . Mo1 . C101 . 113.8(6) yes C11 . Mo1 . C101 . 106.9(5) yes C12 . Mo1 . C101 . 143.0(5) yes Mo2 . Mo1 . C102 . 161.7(7) yes P12 . Mo1 . C102 . 112.9(7) yes C1 . Mo1 . C102 . 139.0(5) yes C11 . Mo1 . C102 . 89.8(5) yes C12 . Mo1 . C102 . 112.4(7) yes Mo2 . Mo1 . C103 . 159.6(6) yes P12 . Mo1 . C103 . 142.5(4) yes C1 . Mo1 . C103 . 118.0(7) yes C11 . Mo1 . C103 . 106.4(7) yes C12 . Mo1 . C103 . 85.9(5) yes Mo2 . Mo1 . C104 . 125.6(5) yes P12 . Mo1 . C104 . 125.4(5) yes C1 . Mo1 . C104 . 83.8(6) yes C11 . Mo1 . C104 . 142.9(6) yes C12 . Mo1 . C104 . 93.0(5) yes Mo2 . Mo1 . C105 . 113.5(3) yes P12 . Mo1 . C105 . 91.7(4) yes C1 . Mo1 . C105 . 82.9(5) yes C11 . Mo1 . C105 . 141.2(5) yes C12 . Mo1 . C105 . 127.2(5) yes C101 . Mo1 . C102 . 34.5(6) yes C101 . Mo1 . C103 . 57.0(6) yes C102 . Mo1 . C103 . 33.3(7) yes C101 . Mo1 . C104 . 57.8(5) yes C102 . Mo1 . C104 . 58.0(6) yes C103 . Mo1 . C104 . 36.5(7) yes C101 . Mo1 . C105 . 34.3(5) yes C102 . Mo1 . C105 . 57.6(6) yes C103 . Mo1 . C105 . 58.6(6) yes C104 . Mo1 . C105 . 35.2(6) yes Mo1 . Mo2 . P12 . 48.42(6) yes Mo1 . Mo2 . C1 . 45.2(3) yes P12 . Mo2 . C1 . 77.2(3) yes Mo1 . Mo2 . C21 . 87.7(3) yes P12 . Mo2 . C21 . 79.8(3) yes C1 . Mo2 . C21 . 130.8(5) yes Mo1 . Mo2 . C22 . 89.0(3) yes P12 . Mo2 . C22 . 134.3(3) yes C1 . Mo2 . C22 . 82.8(5) yes C21 . Mo2 . C22 . 83.1(4) yes Mo1 . Mo2 . C201 . 116.0(3) yes P12 . Mo2 . C201 . 97.5(4) yes C1 . Mo2 . C201 . 80.3(5) yes C21 . Mo2 . C201 . 145.9(5) yes C22 . Mo2 . C201 . 119.2(5) yes Mo1 . Mo2 . C202 . 132.9(4) yes P12 . Mo2 . C202 . 133.1(4) yes C1 . Mo2 . C202 . 87.7(5) yes C21 . Mo2 . C202 . 137.7(5) yes C22 . Mo2 . C202 . 85.9(5) yes Mo1 . Mo2 . C203 . 168.0(4) yes P12 . Mo2 . C203 . 140.4(4) yes C1 . Mo2 . C203 . 123.6(5) yes C21 . Mo2 . C203 . 101.5(5) yes C22 . Mo2 . C203 . 84.5(5) yes Mo1 . Mo2 . C204 . 154.7(4) yes P12 . Mo2 . C204 . 106.3(4) yes C1 . Mo2 . C204 . 138.7(5) yes C21 . Mo2 . C204 . 89.4(5) yes C22 . Mo2 . C204 . 115.6(5) yes Mo1 . Mo2 . C205 . 125.0(3) yes P12 . Mo2 . C205 . 84.0(3) yes C1 . Mo2 . C205 . 107.5(5) yes C21 . Mo2 . C205 . 112.6(5) yes C22 . Mo2 . C205 . 141.5(5) yes C201 . Mo2 . C202 . 35.8(5) yes C201 . Mo2 . C203 . 59.5(5) yes C202 . Mo2 . C203 . 36.6(5) yes C201 . Mo2 . C204 . 58.4(5) yes C202 . Mo2 . C204 . 59.3(5) yes C203 . Mo2 . C204 . 34.9(5) yes C201 . Mo2 . C205 . 34.0(5) yes C202 . Mo2 . C205 . 58.5(5) yes C203 . Mo2 . C205 . 58.6(5) yes C204 . Mo2 . C205 . 35.5(5) yes Mo1 . P12 . Mo2 . 82.38(8) yes Mo1 . P12 . C121 . 124.7(3) yes Mo2 . P12 . C121 . 124.2(3) yes Mo1 . P12 . H121 . 124.192 no Mo2 . P12 . H121 . 124.750 no C121 . P12 . H121 . 82.537 no Mo1 . C1 . Mo2 . 92.6(4) yes Mo1 . C1 . O1 . 130.5(9) yes Mo2 . C1 . O1 . 136.9(9) yes Mo1 . C11 . O11 . 175.7(10) yes Mo1 . C12 . O12 . 175.2(11) yes Mo2 . C21 . O21 . 175.9(10) yes Mo2 . C22 . O22 . 176.9(11) yes Mo1 . C101 . C102 . 72.2(9) yes Mo1 . C101 . C105 . 72.0(7) yes C102 . C101 . C105 . 108.3(15) yes Mo1 . C101 . H1011 . 121.519 no C102 . C101 . H1011 . 125.822 no C105 . C101 . H1011 . 125.914 no Mo1 . C102 . C101 . 73.2(8) yes Mo1 . C102 . C103 . 72.8(9) yes C101 . C102 . C103 . 109.8(16) yes Mo1 . C102 . H1021 . 120.264 no C101 . C102 . H1021 . 125.413 no C103 . C102 . H1021 . 124.806 no Mo1 . C103 . C102 . 73.9(9) yes Mo1 . C103 . C104 . 71.6(7) yes C102 . C103 . C104 . 108.0(15) yes Mo1 . C103 . H1031 . 120.411 no C102 . C103 . H1031 . 126.350 no C104 . C103 . H1031 . 125.610 no Mo1 . C104 . C103 . 71.9(8) yes Mo1 . C104 . C105 . 72.7(7) yes C103 . C104 . C105 . 105.6(13) yes Mo1 . C104 . H1041 . 120.233 no C103 . C104 . H1041 . 127.149 no C105 . C104 . H1041 . 127.298 no Mo1 . C105 . C101 . 73.7(7) yes Mo1 . C105 . C104 . 72.1(8) yes C101 . C105 . C104 . 108.4(15) yes Mo1 . C105 . H1051 . 120.174 no C101 . C105 . H1051 . 125.894 no C104 . C105 . H1051 . 125.746 no P12 . C121 . C122 . 109.7(7) yes P12 . C121 . C126 . 109.6(7) yes C122 . C121 . C126 . 111.6(8) yes P12 . C121 . H1211 . 109.860 no C122 . C121 . H1211 . 107.977 no C126 . C121 . H1211 . 108.029 no C121 . C122 . C123 . 110.0(9) yes C121 . C122 . H1221 . 109.425 no C123 . C122 . H1221 . 109.364 no C121 . C122 . H1222 . 109.415 no C123 . C122 . H1222 . 109.226 no H1221 . C122 . H1222 . 109.353 no C122 . C123 . C124 . 111.0(11) yes C122 . C123 . H1231 . 109.125 no C124 . C123 . H1231 . 109.132 no C122 . C123 . H1232 . 108.997 no C124 . C123 . H1232 . 108.936 no H1231 . C123 . H1232 . 109.663 no C123 . C124 . C125 . 110.5(10) yes C123 . C124 . H1241 . 109.247 no C125 . C124 . H1241 . 109.313 no C123 . C124 . H1242 . 109.253 no C125 . C124 . H1242 . 109.216 no H1241 . C124 . H1242 . 109.251 no C124 . C125 . C126 . 110.4(10) yes C124 . C125 . H1251 . 109.360 no C126 . C125 . H1251 . 109.180 no C124 . C125 . H1252 . 109.241 no C126 . C125 . H1252 . 109.269 no H1251 . C125 . H1252 . 109.345 no C121 . C126 . C125 . 111.6(9) yes C121 . C126 . H1261 . 108.928 no C125 . C126 . H1261 . 108.872 no C121 . C126 . H1262 . 108.915 no C125 . C126 . H1262 . 108.865 no H1261 . C126 . H1262 . 109.606 no Mo2 . C201 . C202 . 71.0(7) yes Mo2 . C201 . C205 . 73.5(7) yes C202 . C201 . C205 . 108.8(12) yes Mo2 . C201 . H2011 . 121.418 no C202 . C201 . H2011 . 125.634 no C205 . C201 . H2011 . 125.612 no Mo2 . C202 . C201 . 73.3(7) yes Mo2 . C202 . C203 . 71.5(7) yes C201 . C202 . C203 . 106.3(11) yes Mo2 . C202 . H2021 . 120.495 no C201 . C202 . H2021 . 126.866 no C203 . C202 . H2021 . 126.855 no Mo2 . C203 . C202 . 71.9(7) yes Mo2 . C203 . C204 . 73.8(7) yes C202 . C203 . C204 . 108.0(12) yes Mo2 . C203 . H2031 . 120.343 no C202 . C203 . H2031 . 126.125 no C204 . C203 . H2031 . 125.829 no Mo2 . C204 . C203 . 71.4(7) yes Mo2 . C204 . C205 . 72.9(7) yes C203 . C204 . C205 . 107.9(11) yes Mo2 . C204 . H2041 . 121.189 no C203 . C204 . H2041 . 126.180 no C205 . C204 . H2041 . 125.943 no Mo2 . C205 . C201 . 72.5(7) yes Mo2 . C205 . C204 . 71.6(7) yes C201 . C205 . C204 . 109.0(12) yes Mo2 . C205 . H2051 . 121.905 no C201 . C205 . H2051 . 125.432 no C204 . C205 . H2051 . 125.523 no Mo4 . Mo3 . C2 . 41.2(3) yes Mo4 . Mo3 . P34 . 49.36(6) yes C2 . Mo3 . P34 . 75.9(3) yes Mo4 . Mo3 . C31 . 94.5(4) yes C2 . Mo3 . C31 . 133.3(5) yes P34 . Mo3 . C31 . 83.6(4) yes Mo4 . Mo3 . C32 . 85.3(5) yes C2 . Mo3 . C32 . 80.7(5) yes P34 . Mo3 . C32 . 130.8(5) yes C31 . Mo3 . C32 . 82.0(7) yes Mo4 . Mo3 . C301 . 126.6(6) yes C2 . Mo3 . C301 . 110.6(7) yes P34 . Mo3 . C301 . 85.5(5) yes C31 . Mo3 . C301 . 109.0(7) yes C32 . Mo3 . C301 . 143.6(7) yes Mo4 . Mo3 . C302 . 156.8(8) yes C2 . Mo3 . C302 . 138.4(6) yes P34 . Mo3 . C302 . 108.2(8) yes C31 . Mo3 . C302 . 87.7(7) yes C32 . Mo3 . C302 . 117.8(9) yes Mo4 . Mo3 . C303 . 160.4(9) yes C2 . Mo3 . C303 . 119.7(10) yes P34 . Mo3 . C303 . 142.3(7) yes C31 . Mo3 . C303 . 102.2(9) yes C32 . Mo3 . C303 . 86.8(8) yes Mo4 . Mo3 . C304 . 125.6(5) yes C2 . Mo3 . C304 . 84.5(6) yes P34 . Mo3 . C304 . 129.0(5) yes C31 . Mo3 . C304 . 138.5(6) yes C32 . Mo3 . C304 . 90.2(7) yes Mo4 . Mo3 . C305 . 112.8(4) yes C2 . Mo3 . C305 . 81.0(5) yes P34 . Mo3 . C305 . 95.5(4) yes C31 . Mo3 . C305 . 143.2(6) yes C32 . Mo3 . C305 . 122.8(7) yes C301 . Mo3 . C302 . 33.0(7) yes C301 . Mo3 . C303 . 57.1(7) yes C302 . Mo3 . C303 . 36.3(8) yes C301 . Mo3 . C304 . 58.1(6) yes C302 . Mo3 . C304 . 60.2(7) yes C303 . Mo3 . C304 . 36.4(8) yes C301 . Mo3 . C305 . 34.7(6) yes C302 . Mo3 . C305 . 57.5(7) yes C303 . Mo3 . C305 . 57.8(7) yes C304 . Mo3 . C305 . 34.4(6) yes Mo3 . Mo4 . C2 . 46.2(3) yes Mo3 . Mo4 . P34 . 48.45(7) yes C2 . Mo4 . P34 . 78.9(3) yes Mo3 . Mo4 . C41 . 84.6(3) yes C2 . Mo4 . C41 . 127.4(5) yes P34 . Mo4 . C41 . 79.9(3) yes Mo3 . Mo4 . C42 . 89.3(4) yes C2 . Mo4 . C42 . 82.3(5) yes P34 . Mo4 . C42 . 134.3(4) yes C41 . Mo4 . C42 . 79.3(5) yes Mo3 . Mo4 . C401 . 126.0(4) yes C2 . Mo4 . C401 . 109.9(6) yes P34 . Mo4 . C401 . 84.2(4) yes C41 . Mo4 . C401 . 115.1(6) yes C42 . Mo4 . C401 . 141.5(6) yes Mo3 . Mo4 . C402 . 153.6(4) yes C2 . Mo4 . C402 . 140.2(5) yes P34 . Mo4 . C402 . 105.2(4) yes C41 . Mo4 . C402 . 91.7(5) yes C42 . Mo4 . C402 . 115.7(6) yes Mo3 . Mo4 . C403 . 168.1(5) yes C2 . Mo4 . C403 . 122.4(6) yes P34 . Mo4 . C403 . 139.8(4) yes C41 . Mo4 . C403 . 104.5(6) yes C42 . Mo4 . C403 . 85.0(6) yes Mo3 . Mo4 . C404 . 134.9(4) yes C2 . Mo4 . C404 . 88.8(5) yes P34 . Mo4 . C404 . 133.6(5) yes C41 . Mo4 . C404 . 138.1(5) yes C42 . Mo4 . C404 . 86.7(6) yes Mo3 . Mo4 . C405 . 117.2(4) yes C2 . Mo4 . C405 . 81.5(5) yes P34 . Mo4 . C405 . 98.1(4) yes C41 . Mo4 . C405 . 149.1(5) yes C42 . Mo4 . C405 . 119.9(6) yes C401 . Mo4 . C402 . 34.5(6) yes C401 . Mo4 . C403 . 57.3(6) yes C402 . Mo4 . C403 . 35.9(6) yes C401 . Mo4 . C404 . 58.2(6) yes C402 . Mo4 . C404 . 59.4(5) yes C403 . Mo4 . C404 . 34.4(6) yes C401 . Mo4 . C405 . 34.8(6) yes C402 . Mo4 . C405 . 58.7(6) yes C403 . Mo4 . C405 . 57.8(6) yes C404 . Mo4 . C405 . 35.6(6) yes Mo3 . C2 . Mo4 . 92.6(5) yes Mo3 . C2 . O2 . 127.2(10) yes Mo4 . C2 . O2 . 140.2(10) yes Mo3 . P34 . Mo4 . 82.19(9) yes Mo3 . P34 . C341 . 124.1(4) yes Mo4 . P34 . C341 . 123.1(4) yes Mo3 . P34 . H341 . 123.981 no Mo4 . P34 . H341 . 124.990 no C341 . P34 . H341 . 84.028 no Mo3 . C31 . O31 . 174.4(12) yes Mo3 . C32 . O32 . 176.3(15) yes Mo4 . C41 . O41 . 177.9(10) yes Mo4 . C42 . O42 . 179.9(13) yes Mo3 . C301 . C302 . 71.9(10) yes Mo3 . C301 . C305 . 72.7(8) yes C302 . C301 . C305 . 110.7(17) yes Mo3 . C301 . H3011 . 122.285 no C302 . C301 . H3011 . 124.548 no C305 . C301 . H3011 . 124.800 no Mo3 . C302 . C301 . 75.1(10) yes Mo3 . C302 . C303 . 71.2(9) yes C301 . C302 . C303 . 107.2(19) yes Mo3 . C302 . H3021 . 119.132 no C301 . C302 . H3021 . 126.568 no C303 . C302 . H3021 . 126.187 no Mo3 . C303 . C302 . 72.5(9) yes Mo3 . C303 . C304 . 73.4(9) yes C302 . C303 . C304 . 108.0(17) yes Mo3 . C303 . H3031 . 119.918 no C302 . C303 . H3031 . 125.869 no C304 . C303 . H3031 . 126.136 no Mo3 . C304 . C303 . 70.1(9) yes Mo3 . C304 . C305 . 73.3(8) yes C303 . C304 . C305 . 104.6(16) yes Mo3 . C304 . H3041 . 120.640 no C303 . C304 . H3041 . 127.441 no C305 . C304 . H3041 . 127.922 no Mo3 . C305 . C301 . 72.6(9) yes Mo3 . C305 . C304 . 72.3(8) yes C301 . C305 . C304 . 109.4(15) yes Mo3 . C305 . H3051 . 121.711 no C301 . C305 . H3051 . 125.341 no C304 . C305 . H3051 . 125.216 no P34 . C341 . C342 . 110.8(9) yes P34 . C341 . C346 . 110.2(9) yes C342 . C341 . C346 . 111.0(11) yes P34 . C341 . H3411 . 108.828 no C342 . C341 . H3411 . 107.547 no C346 . C341 . H3411 . 108.413 no C341 . C342 . C343 . 108.4(12) yes C341 . C342 . H3421 . 109.810 no C343 . C342 . H3421 . 109.669 no C341 . C342 . H3422 . 109.831 no C343 . C342 . H3422 . 109.516 no H3421 . C342 . H3422 . 109.595 no C342 . C343 . C344 . 113.3(17) yes C342 . C343 . H3431 . 108.251 no C344 . C343 . H3431 . 108.429 no C342 . C343 . H3432 . 108.619 no C344 . C343 . H3432 . 108.829 no H3431 . C343 . H3432 . 109.387 no C343 . C344 . C345 . 113.0(16) yes C343 . C344 . H3441 . 108.674 no C345 . C344 . H3441 . 108.452 no C343 . C344 . H3442 . 108.588 no C345 . C344 . H3442 . 108.684 no H3441 . C344 . H3442 . 109.358 no C344 . C345 . C346 . 113.5(15) yes C344 . C345 . H3451 . 108.497 no C346 . C345 . H3451 . 108.396 no C344 . C345 . H3452 . 108.458 no C346 . C345 . H3452 . 108.282 no H3451 . C345 . H3452 . 109.687 no C341 . C346 . C345 . 111.3(14) yes C341 . C346 . H3461 . 108.947 no C345 . C346 . H3461 . 109.032 no C341 . C346 . H3462 . 108.935 no C345 . C346 . H3462 . 109.133 no H3461 . C346 . H3462 . 109.504 no Mo4 . C401 . C402 . 72.3(8) yes Mo4 . C401 . C405 . 73.0(8) yes C402 . C401 . C405 . 110.9(14) yes Mo4 . C401 . H4011 . 121.885 no C402 . C401 . H4011 . 124.843 no C405 . C401 . H4011 . 124.247 no Mo4 . C402 . C401 . 73.2(8) yes Mo4 . C402 . C403 . 70.8(8) yes C401 . C402 . C403 . 104.6(13) yes Mo4 . C402 . H4021 . 120.078 no C401 . C402 . H4021 . 127.709 no C403 . C402 . H4021 . 127.724 no Mo4 . C403 . C402 . 73.3(8) yes Mo4 . C403 . C404 . 73.2(8) yes C402 . C403 . C404 . 110.8(15) yes Mo4 . C403 . H4031 . 120.694 no C402 . C403 . H4031 . 124.556 no C404 . C403 . H4031 . 124.618 no Mo4 . C404 . C403 . 72.4(8) yes Mo4 . C404 . C405 . 73.8(7) yes C403 . C404 . C405 . 107.4(14) yes Mo4 . C404 . H4041 . 119.326 no C403 . C404 . H4041 . 126.441 no C405 . C404 . H4041 . 126.190 no Mo4 . C405 . C401 . 72.3(8) yes Mo4 . C405 . C404 . 70.6(8) yes C401 . C405 . C404 . 106.3(14) yes Mo4 . C405 . H4051 . 121.988 no C401 . C405 . H4051 . 126.801 no C404 . C405 . H4051 . 126.910 no F11 . B1 . F12 . 106.6(19) yes F11 . B1 . F13 . 107.4(18) yes F12 . B1 . F13 . 106.9(22) yes F11 . B1 . F14 . 110.5(20) yes F12 . B1 . F14 . 113.5(24) yes F13 . B1 . F14 . 111.6(22) yes F21 . B2 . F22 . 116.6(27) yes F21 . B2 . F23 . 121.3(27) yes F22 . B2 . F23 . 113.7(26) yes F21 . B2 . F24 . 92.5(23) yes F22 . B2 . F24 . 109.3(23) yes F23 . B2 . F24 . 97.8(23) yes Cl1 . C500 . Cl2 . 115.3(13) yes Cl1 . C500 . H5001 . 108.103 no Cl2 . C500 . H5001 . 108.059 no Cl1 . C500 . H5002 . 107.975 no Cl2 . C500 . H5002 . 107.946 no H5001 . C500 . H5002 . 109.380 no # ===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2004-03-11 at 12:32:58 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\archivos de programa\wingx\files\archive.dat # CIF files read : dg4 struct data_8 _database_code_depnum_ccdc_archive 'CCDC 248106' _audit_creation_date 2004-03-11T12:32:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H16 Cl1 Mo2 O4 P1' _chemical_formula_sum 'C20 H16 Cl Mo2 O4 P' _chemical_formula_weight 578.63 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.63500(10) _cell_length_b 9.89690(10) _cell_length_c 13.70360(10) _cell_angle_alpha 104.2950(10) _cell_angle_beta 102.8910(10) _cell_angle_gamma 106.6910(10) _cell_volume 1031.057(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5234 _cell_measurement_theta_min 3.509 _cell_measurement_theta_max 70.5 _cell_measurement_wavelength 1.54183 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.093 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details 'SADABS v. 2.03' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54183 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_unetI/netI 0.056 _diffrn_reflns_number 6603 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.509 _diffrn_reflns_theta_max 70.55 _diffrn_reflns_theta_full 70.55 _diffrn_measured_fraction_theta_full 0.861 _diffrn_measured_fraction_theta_max 0.861 _reflns_number_total 3407 _reflns_number_gt 3240 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER SMART v. 5.625' _computing_cell_refinement 'BRUKER SMART v. 5.625' _computing_data_reduction 'BRUKER SAINT v. 6.0' _computing_structure_solution 'DIRDIF (1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0385P)^2^+0.2486P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0034(2) _refine_ls_number_reflns 3407 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.542 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.65814(3) 0.52494(3) 0.778287(18) 0.03012(13) Uani 1 1 d . . . Mo2 Mo 0.85624(3) 0.31346(3) 0.691959(19) 0.03416(13) Uani 1 1 d . . . P1 P 0.95958(9) 0.56135(9) 0.81523(6) 0.03027(19) Uani 1 1 d . . . Cl1 Cl 0.68056(13) 0.40203(11) 0.91961(7) 0.0531(2) Uani 1 1 d . . . O4 O 1.1114(4) 0.4418(4) 0.5824(3) 0.0761(9) Uani 1 1 d . . . O2 O 0.6797(3) 0.5668(4) 0.5619(2) 0.0581(7) Uani 1 1 d . . . O3 O 0.6031(4) 0.2302(4) 0.4663(2) 0.0816(10) Uani 1 1 d . . . O1 O 0.3617(4) 0.2203(4) 0.6326(3) 0.0751(9) Uani 1 1 d . . . C31 C 1.0983(4) 0.7323(3) 0.8062(3) 0.0357(7) Uani 1 1 d . . . C3 C 0.6932(5) 0.2654(4) 0.5513(3) 0.0537(9) Uani 1 1 d . . . C1 C 0.4749(5) 0.3261(4) 0.6854(3) 0.0467(8) Uani 1 1 d . . . C36 C 1.0894(5) 0.7570(4) 0.7097(3) 0.0454(8) Uani 1 1 d . . . C32 C 1.2152(5) 0.8423(4) 0.8993(3) 0.0519(9) Uani 1 1 d . . . C22 C 0.7404(6) 0.7652(5) 0.8990(4) 0.0592(11) Uani 1 1 d . . . C34 C 1.3089(5) 0.9988(5) 0.7991(5) 0.0685(13) Uani 1 1 d . . . C14 C 0.7681(10) 0.0600(5) 0.6722(6) 0.100(2) Uani 1 1 d . . . C11 C 0.9391(7) 0.2250(6) 0.8305(4) 0.0638(12) Uani 1 1 d . . . C25 C 0.5056(7) 0.6722(6) 0.7512(4) 0.0643(12) Uani 1 1 d . . . C21 C 0.6815(6) 0.7647(5) 0.7940(4) 0.0618(11) Uani 1 1 d . . . C13 C 0.9343(10) 0.1088(7) 0.6672(5) 0.0862(18) Uani 1 1 d . . . C2 C 0.6778(4) 0.5440(4) 0.6388(3) 0.0406(7) Uani 1 1 d . . . C15 C 0.7730(7) 0.1316(6) 0.7741(6) 0.0812(18) Uani 1 1 d . . . C4 C 1.0133(5) 0.3993(4) 0.6235(3) 0.0469(8) Uani 1 1 d . . . C33 C 1.3186(6) 0.9750(5) 0.8937(5) 0.0674(14) Uani 1 1 d . . . C35 C 1.1957(6) 0.8910(5) 0.7078(5) 0.0628(12) Uani 1 1 d . . . C24 C 0.4589(6) 0.6174(5) 0.8301(4) 0.0601(11) Uani 1 1 d . . . C12 C 1.0374(8) 0.2075(7) 0.7641(5) 0.0700(14) Uani 1 1 d . . . C23 C 0.6000(6) 0.6763(5) 0.9190(4) 0.0597(11) Uani 1 1 d . . . H2 H 1.027(5) 0.576(4) 0.908(3) 0.046(10) Uiso 1 1 d . . . H32 H 1.229(6) 0.823(5) 0.969(4) 0.068(13) Uiso 1 1 d . . . H34 H 1.386(7) 1.098(7) 0.800(4) 0.090(17) Uiso 1 1 d . . . H36 H 1.011(5) 0.689(4) 0.652(3) 0.039(10) Uiso 1 1 d . . . H33 H 1.378(7) 1.030(6) 0.946(4) 0.063(15) Uiso 1 1 d . . . H15 H 0.691(7) 0.126(6) 0.799(4) 0.074(16) Uiso 1 1 d . . . H11 H 0.966(6) 0.282(5) 0.892(4) 0.053(12) Uiso 1 1 d . . . H14 H 0.695(11) -0.010(10) 0.622(6) 0.14(3) Uiso 1 1 d . . . H35 H 1.185(6) 0.908(6) 0.648(4) 0.068(15) Uiso 1 1 d . . . H23 H 0.624(10) 0.664(9) 0.984(6) 0.13(3) Uiso 1 1 d . . . H22 H 0.842(8) 0.816(7) 0.948(4) 0.085(18) Uiso 1 1 d . . . H12 H 1.139(8) 0.242(6) 0.781(4) 0.079(18) Uiso 1 1 d . . . H21 H 0.759(6) 0.823(6) 0.759(4) 0.076(14) Uiso 1 1 d . . . H25 H 0.431(6) 0.658(5) 0.693(3) 0.052(12) Uiso 1 1 d . . . H24 H 0.345(7) 0.542(6) 0.816(4) 0.081(15) Uiso 1 1 d . . . H13 H 0.958(8) 0.070(7) 0.605(5) 0.092(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03009(18) 0.03436(18) 0.03685(18) 0.02171(13) 0.01723(12) 0.01385(11) Mo2 0.03576(19) 0.03073(18) 0.03953(18) 0.01465(13) 0.01446(13) 0.01268(11) P1 0.0288(4) 0.0332(4) 0.0310(4) 0.0149(3) 0.0102(3) 0.0102(3) Cl1 0.0649(6) 0.0675(6) 0.0588(5) 0.0470(5) 0.0370(5) 0.0339(4) O4 0.075(2) 0.099(2) 0.078(2) 0.0411(19) 0.0538(18) 0.0322(18) O2 0.0515(15) 0.090(2) 0.0479(14) 0.0439(14) 0.0200(12) 0.0267(13) O3 0.077(2) 0.093(3) 0.0448(16) 0.0048(16) -0.0032(15) 0.0207(18) O1 0.0497(16) 0.0608(18) 0.091(2) 0.0187(17) 0.0202(16) -0.0074(13) C31 0.0285(15) 0.0313(15) 0.0478(17) 0.0139(14) 0.0142(13) 0.0092(11) C3 0.053(2) 0.051(2) 0.050(2) 0.0112(17) 0.0145(18) 0.0144(16) C1 0.0418(19) 0.050(2) 0.055(2) 0.0273(17) 0.0214(17) 0.0126(15) C36 0.0415(19) 0.0441(19) 0.059(2) 0.0279(18) 0.0237(18) 0.0125(15) C32 0.047(2) 0.0391(19) 0.060(2) 0.0077(18) 0.0137(18) 0.0123(15) C22 0.065(3) 0.045(2) 0.069(3) 0.010(2) 0.027(2) 0.0254(19) C34 0.046(2) 0.038(2) 0.126(4) 0.034(3) 0.035(3) 0.0106(16) C14 0.124(6) 0.024(2) 0.120(5) 0.029(3) -0.004(4) 0.010(2) C11 0.098(4) 0.057(3) 0.065(3) 0.038(2) 0.036(3) 0.046(3) C25 0.075(3) 0.078(3) 0.078(3) 0.045(3) 0.035(3) 0.057(3) C21 0.084(3) 0.045(2) 0.091(3) 0.042(2) 0.049(3) 0.039(2) C13 0.136(6) 0.064(3) 0.094(4) 0.034(3) 0.057(4) 0.065(4) C2 0.0333(17) 0.053(2) 0.0407(16) 0.0255(15) 0.0130(14) 0.0141(13) C15 0.082(3) 0.062(3) 0.147(6) 0.074(4) 0.065(4) 0.038(3) C4 0.047(2) 0.054(2) 0.0437(17) 0.0157(16) 0.0199(17) 0.0203(15) C33 0.048(2) 0.0322(19) 0.095(4) -0.002(2) 0.011(2) 0.0039(16) C35 0.057(3) 0.060(3) 0.102(4) 0.052(3) 0.045(3) 0.026(2) C24 0.052(2) 0.067(3) 0.086(3) 0.035(2) 0.041(2) 0.036(2) C12 0.069(3) 0.075(3) 0.101(4) 0.054(3) 0.036(3) 0.049(3) C23 0.084(3) 0.060(2) 0.063(2) 0.027(2) 0.045(3) 0.044(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.006(3) . ? Mo1 C1 2.018(4) . ? Mo1 C25 2.269(4) . ? Mo1 C21 2.274(4) . ? Mo1 C24 2.331(4) . ? Mo1 C22 2.336(4) . ? Mo1 C23 2.378(4) . ? Mo1 P1 2.4381(8) . ? Mo1 Cl1 2.5296(8) . ? Mo2 C4 1.934(4) . ? Mo2 C3 1.969(4) . ? Mo2 C13 2.285(5) . ? Mo2 C12 2.300(5) . ? Mo2 C14 2.328(4) . ? Mo2 C11 2.336(4) . ? Mo2 C15 2.375(5) . ? Mo2 P1 2.3857(8) . ? P1 C31 1.822(3) . ? P1 H2 1.22(4) . ? O4 C4 1.156(5) . ? O2 C2 1.134(4) . ? O3 C3 1.150(5) . ? O1 C1 1.140(5) . ? C31 C32 1.392(5) . ? C31 C36 1.393(5) . ? C36 C35 1.389(5) . ? C36 H36 0.88(4) . ? C32 C33 1.391(6) . ? C32 H32 1.01(5) . ? C22 C23 1.405(7) . ? C22 C21 1.414(7) . ? C22 H22 0.89(6) . ? C34 C33 1.362(8) . ? C34 C35 1.362(8) . ? C34 H34 1.01(6) . ? C14 C15 1.385(10) . ? C14 C13 1.400(10) . ? C14 H14 0.82(9) . ? C11 C15 1.379(8) . ? C11 C12 1.390(7) . ? C11 H11 0.82(5) . ? C25 C24 1.409(7) . ? C25 C21 1.424(8) . ? C25 H25 0.86(4) . ? C21 H21 1.04(5) . ? C13 C12 1.357(9) . ? C13 H13 0.94(6) . ? C15 H15 0.84(6) . ? C33 H33 0.74(5) . ? C35 H35 0.87(5) . ? C24 C23 1.374(7) . ? C24 H24 0.99(6) . ? C12 H12 0.80(6) . ? C23 H23 0.91(7) . ? 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 83.21(14) . . ? C2 Mo1 C25 78.35(16) . . ? C1 Mo1 C25 97.8(2) . . ? C2 Mo1 C21 75.65(16) . . ? C1 Mo1 C21 132.28(17) . . ? C25 Mo1 C21 36.54(19) . . ? C2 Mo1 C24 112.54(16) . . ? C1 Mo1 C24 91.75(17) . . ? C25 Mo1 C24 35.65(17) . . ? C21 Mo1 C24 59.59(16) . . ? C2 Mo1 C22 108.20(16) . . ? C1 Mo1 C22 150.17(16) . . ? C25 Mo1 C22 59.6(2) . . ? C21 Mo1 C22 35.68(17) . . ? C24 Mo1 C22 58.45(17) . . ? C2 Mo1 C23 132.24(15) . . ? C1 Mo1 C23 118.17(17) . . ? C25 Mo1 C23 57.83(17) . . ? C21 Mo1 C23 58.16(16) . . ? C24 Mo1 C23 33.92(17) . . ? C22 Mo1 C23 34.66(16) . . ? C2 Mo1 P1 82.70(10) . . ? C1 Mo1 P1 121.36(11) . . ? C25 Mo1 P1 133.81(15) . . ? C21 Mo1 P1 97.98(13) . . ? C24 Mo1 P1 145.65(13) . . ? C22 Mo1 P1 87.92(12) . . ? C23 Mo1 P1 113.16(13) . . ? C2 Mo1 Cl1 152.61(11) . . ? C1 Mo1 Cl1 84.64(11) . . ? C25 Mo1 Cl1 127.72(13) . . ? C21 Mo1 Cl1 129.48(13) . . ? C24 Mo1 Cl1 92.27(12) . . ? C22 Mo1 Cl1 94.39(13) . . ? C23 Mo1 Cl1 75.02(11) . . ? P1 Mo1 Cl1 82.84(3) . . ? C4 Mo2 C3 80.84(16) . . ? C4 Mo2 C13 90.2(2) . . ? C3 Mo2 C13 101.3(2) . . ? C4 Mo2 C12 91.17(18) . . ? C3 Mo2 C12 135.3(2) . . ? C13 Mo2 C12 34.4(2) . . ? C4 Mo2 C14 121.4(3) . . ? C3 Mo2 C14 89.6(2) . . ? C13 Mo2 C14 35.3(3) . . ? C12 Mo2 C14 57.5(2) . . ? C4 Mo2 C11 122.27(17) . . ? C3 Mo2 C11 145.64(19) . . ? C13 Mo2 C11 57.8(2) . . ? C12 Mo2 C11 34.87(18) . . ? C14 Mo2 C11 57.2(2) . . ? C4 Mo2 C15 146.39(17) . . ? C3 Mo2 C15 112.7(2) . . ? C13 Mo2 C15 57.7(2) . . ? C12 Mo2 C15 57.1(2) . . ? C14 Mo2 C15 34.2(2) . . ? C11 Mo2 C15 34.0(2) . . ? C4 Mo2 P1 84.71(11) . . ? C3 Mo2 P1 119.13(12) . . ? C13 Mo2 P1 137.7(2) . . ? C12 Mo2 P1 103.59(17) . . ? C14 Mo2 P1 145.2(2) . . ? C11 Mo2 P1 90.14(13) . . ? C15 Mo2 P1 111.47(18) . . ? C31 P1 Mo2 128.01(11) . . ? C31 P1 Mo1 116.94(10) . . ? Mo2 P1 Mo1 84.11(2) . . ? C31 P1 H2 100.2(19) . . ? Mo2 P1 H2 115.6(18) . . ? Mo1 P1 H2 111.9(18) . . ? C32 C31 C36 119.2(3) . . ? C32 C31 P1 118.7(3) . . ? C36 C31 P1 122.1(3) . . ? O3 C3 Mo2 175.2(4) . . ? O1 C1 Mo1 174.0(4) . . ? C35 C36 C31 119.7(4) . . ? C35 C36 H36 122(2) . . ? C31 C36 H36 118(2) . . ? C33 C32 C31 119.2(4) . . ? C33 C32 H32 121(3) . . ? C31 C32 H32 120(3) . . ? C23 C22 C21 106.8(5) . . ? C23 C22 Mo1 74.3(3) . . ? C21 C22 Mo1 69.8(2) . . ? C23 C22 H22 124(4) . . ? C21 C22 H22 129(4) . . ? Mo1 C22 H22 125(4) . . ? C33 C34 C35 119.7(4) . . ? C33 C34 H34 118(3) . . ? C35 C34 H34 122(3) . . ? C15 C14 C13 107.8(6) . . ? C15 C14 Mo2 74.7(3) . . ? C13 C14 Mo2 70.7(3) . . ? C15 C14 H14 133(6) . . ? C13 C14 H14 118(6) . . ? Mo2 C14 H14 128(6) . . ? C15 C11 C12 107.7(5) . . ? C15 C11 Mo2 74.5(3) . . ? C12 C11 Mo2 71.1(3) . . ? C15 C11 H11 122(3) . . ? C12 C11 H11 130(3) . . ? Mo2 C11 H11 118(3) . . ? C24 C25 C21 107.7(5) . . ? C24 C25 Mo1 74.6(2) . . ? C21 C25 Mo1 71.9(2) . . ? C24 C25 H25 122(3) . . ? C21 C25 H25 130(3) . . ? Mo1 C25 H25 126(3) . . ? C22 C21 C25 107.5(4) . . ? C22 C21 Mo1 74.6(2) . . ? C25 C21 Mo1 71.5(2) . . ? C22 C21 H21 123(3) . . ? C25 C21 H21 129(3) . . ? Mo1 C21 H21 119(3) . . ? C12 C13 C14 107.7(6) . . ? C12 C13 Mo2 73.4(3) . . ? C14 C13 Mo2 74.0(3) . . ? C12 C13 H13 132(4) . . ? C14 C13 H13 120(4) . . ? Mo2 C13 H13 120(4) . . ? O2 C2 Mo1 171.8(3) . . ? C11 C15 C14 107.8(6) . . ? C11 C15 Mo2 71.4(3) . . ? C14 C15 Mo2 71.0(3) . . ? C11 C15 H15 124(4) . . ? C14 C15 H15 128(4) . . ? Mo2 C15 H15 120(4) . . ? O4 C4 Mo2 174.9(4) . . ? C34 C33 C32 121.4(5) . . ? C34 C33 H33 124(4) . . ? C32 C33 H33 114(4) . . ? C34 C35 C36 120.9(5) . . ? C34 C35 H35 120(4) . . ? C36 C35 H35 119(4) . . ? C23 C24 C25 107.8(4) . . ? C23 C24 Mo1 74.9(2) . . ? C25 C24 Mo1 69.8(2) . . ? C23 C24 H24 130(3) . . ? C25 C24 H24 122(3) . . ? Mo1 C24 H24 116(3) . . ? C13 C12 C11 108.9(6) . . ? C13 C12 Mo2 72.2(3) . . ? C11 C12 Mo2 74.0(3) . . ? C13 C12 H12 125(4) . . ? C11 C12 H12 126(4) . . ? Mo2 C12 H12 125(4) . . ? C24 C23 C22 110.2(4) . . ? C24 C23 Mo1 71.2(2) . . ? C22 C23 Mo1 71.1(2) . . ? C24 C23 H23 135(5) . . ? C22 C23 H23 115(5) . . ? Mo1 C23 H23 119(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 C4 Mo2 P1 C31 8.72(17) . . . . ? C3 Mo2 P1 C31 -67.71(19) . . . . ? C13 Mo2 P1 C31 93.2(3) . . . . ? C12 Mo2 P1 C31 98.64(19) . . . . ? C14 Mo2 P1 C31 150.3(4) . . . . ? C11 Mo2 P1 C31 131.13(19) . . . . ? C15 Mo2 P1 C31 158.3(2) . . . . ? C4 Mo2 P1 Mo1 128.56(11) . . . . ? C3 Mo2 P1 Mo1 52.13(14) . . . . ? C13 Mo2 P1 Mo1 -147.0(3) . . . . ? C12 Mo2 P1 Mo1 -141.52(14) . . . . ? C14 Mo2 P1 Mo1 -89.8(4) . . . . ? C11 Mo2 P1 Mo1 -109.03(13) . . . . ? C15 Mo2 P1 Mo1 -81.86(15) . . . . ? C2 Mo1 P1 C31 57.82(16) . . . . ? C1 Mo1 P1 C31 135.26(17) . . . . ? C25 Mo1 P1 C31 -8.3(2) . . . . ? C21 Mo1 P1 C31 -16.50(17) . . . . ? C24 Mo1 P1 C31 -62.0(2) . . . . ? C22 Mo1 P1 C31 -50.82(18) . . . . ? C23 Mo1 P1 C31 -75.21(17) . . . . ? Cl1 Mo1 P1 C31 -145.51(12) . . . . ? C2 Mo1 P1 Mo2 -72.12(11) . . . . ? C1 Mo1 P1 Mo2 5.31(12) . . . . ? C25 Mo1 P1 Mo2 -138.24(19) . . . . ? C21 Mo1 P1 Mo2 -146.44(13) . . . . ? C24 Mo1 P1 Mo2 168.1(2) . . . . ? C22 Mo1 P1 Mo2 179.23(12) . . . . ? C23 Mo1 P1 Mo2 154.85(12) . . . . ? Cl1 Mo1 P1 Mo2 84.55(3) . . . . ? Mo2 P1 C31 C32 -145.5(2) . . . . ? Mo1 P1 C31 C32 109.9(3) . . . . ? Mo2 P1 C31 C36 35.4(3) . . . . ? Mo1 P1 C31 C36 -69.2(3) . . . . ? C4 Mo2 C3 O3 69(4) . . . . ? C13 Mo2 C3 O3 -19(5) . . . . ? C12 Mo2 C3 O3 -13(5) . . . . ? C14 Mo2 C3 O3 -53(4) . . . . ? C11 Mo2 C3 O3 -67(5) . . . . ? C15 Mo2 C3 O3 -79(4) . . . . ? P1 Mo2 C3 O3 148(4) . . . . ? C2 Mo1 C1 O1 -89(3) . . . . ? C25 Mo1 C1 O1 -11(3) . . . . ? C21 Mo1 C1 O1 -25(3) . . . . ? C24 Mo1 C1 O1 24(3) . . . . ? C22 Mo1 C1 O1 26(3) . . . . ? C23 Mo1 C1 O1 46(3) . . . . ? P1 Mo1 C1 O1 -166(3) . . . . ? Cl1 Mo1 C1 O1 116(3) . . . . ? C32 C31 C36 C35 -0.6(5) . . . . ? P1 C31 C36 C35 178.5(3) . . . . ? C36 C31 C32 C33 0.9(5) . . . . ? P1 C31 C32 C33 -178.3(3) . . . . ? C2 Mo1 C22 C23 140.2(3) . . . . ? C1 Mo1 C22 C23 31.4(5) . . . . ? C25 Mo1 C22 C23 76.3(3) . . . . ? C21 Mo1 C22 C23 115.1(4) . . . . ? C24 Mo1 C22 C23 34.5(3) . . . . ? P1 Mo1 C22 C23 -138.1(3) . . . . ? Cl1 Mo1 C22 C23 -55.5(3) . . . . ? C2 Mo1 C22 C21 25.2(3) . . . . ? C1 Mo1 C22 C21 -83.7(4) . . . . ? C25 Mo1 C22 C21 -38.8(3) . . . . ? C24 Mo1 C22 C21 -80.6(3) . . . . ? C23 Mo1 C22 C21 -115.1(4) . . . . ? P1 Mo1 C22 C21 106.8(3) . . . . ? Cl1 Mo1 C22 C21 -170.6(3) . . . . ? C4 Mo2 C14 C15 146.8(4) . . . . ? C3 Mo2 C14 C15 -134.2(4) . . . . ? C13 Mo2 C14 C15 115.5(6) . . . . ? C12 Mo2 C14 C15 78.0(4) . . . . ? C11 Mo2 C14 C15 36.3(3) . . . . ? P1 Mo2 C14 C15 13.3(7) . . . . ? C4 Mo2 C14 C13 31.3(5) . . . . ? C3 Mo2 C14 C13 110.3(4) . . . . ? C12 Mo2 C14 C13 -37.6(4) . . . . ? C11 Mo2 C14 C13 -79.2(4) . . . . ? C15 Mo2 C14 C13 -115.5(6) . . . . ? P1 Mo2 C14 C13 -102.2(5) . . . . ? C4 Mo2 C11 C15 -145.6(3) . . . . ? C3 Mo2 C11 C15 -19.4(5) . . . . ? C13 Mo2 C11 C15 -78.7(4) . . . . ? C12 Mo2 C11 C15 -115.4(5) . . . . ? C14 Mo2 C11 C15 -36.5(4) . . . . ? P1 Mo2 C11 C15 130.6(3) . . . . ? C4 Mo2 C11 C12 -30.2(4) . . . . ? C3 Mo2 C11 C12 95.9(4) . . . . ? C13 Mo2 C11 C12 36.7(4) . . . . ? C14 Mo2 C11 C12 78.9(4) . . . . ? C15 Mo2 C11 C12 115.4(5) . . . . ? P1 Mo2 C11 C12 -114.0(4) . . . . ? C2 Mo1 C25 C24 163.5(3) . . . . ? C1 Mo1 C25 C24 82.1(3) . . . . ? C21 Mo1 C25 C24 -115.0(5) . . . . ? C22 Mo1 C25 C24 -77.1(3) . . . . ? C23 Mo1 C25 C24 -36.4(3) . . . . ? P1 Mo1 C25 C24 -128.7(3) . . . . ? Cl1 Mo1 C25 C24 -7.1(4) . . . . ? C2 Mo1 C25 C21 -81.6(3) . . . . ? C1 Mo1 C25 C21 -162.9(3) . . . . ? C24 Mo1 C25 C21 115.0(5) . . . . ? C22 Mo1 C25 C21 37.8(3) . . . . ? C23 Mo1 C25 C21 78.6(3) . . . . ? P1 Mo1 C25 C21 -13.7(4) . . . . ? Cl1 Mo1 C25 C21 107.8(3) . . . . ? C23 C22 C21 C25 -1.2(5) . . . . ? Mo1 C22 C21 C25 64.4(3) . . . . ? C23 C22 C21 Mo1 -65.6(3) . . . . ? C24 C25 C21 C22 0.1(5) . . . . ? Mo1 C25 C21 C22 -66.5(3) . . . . ? C24 C25 C21 Mo1 66.5(3) . . . . ? C2 Mo1 C21 C22 -155.4(3) . . . . ? C1 Mo1 C21 C22 138.1(3) . . . . ? C25 Mo1 C21 C22 114.9(4) . . . . ? C24 Mo1 C21 C22 77.1(3) . . . . ? C23 Mo1 C21 C22 37.3(3) . . . . ? P1 Mo1 C21 C22 -75.0(3) . . . . ? Cl1 Mo1 C21 C22 12.2(3) . . . . ? C2 Mo1 C21 C25 89.7(3) . . . . ? C1 Mo1 C21 C25 23.1(4) . . . . ? C24 Mo1 C21 C25 -37.8(3) . . . . ? C22 Mo1 C21 C25 -114.9(4) . . . . ? C23 Mo1 C21 C25 -77.6(3) . . . . ? P1 Mo1 C21 C25 170.0(3) . . . . ? Cl1 Mo1 C21 C25 -102.7(3) . . . . ? C15 C14 C13 C12 0.1(6) . . . . ? Mo2 C14 C13 C12 66.2(4) . . . . ? C15 C14 C13 Mo2 -66.1(4) . . . . ? C4 Mo2 C13 C12 91.7(4) . . . . ? C3 Mo2 C13 C12 172.4(4) . . . . ? C14 Mo2 C13 C12 -114.6(6) . . . . ? C11 Mo2 C13 C12 -37.2(3) . . . . ? C15 Mo2 C13 C12 -77.7(4) . . . . ? P1 Mo2 C13 C12 9.4(5) . . . . ? C4 Mo2 C13 C14 -153.7(4) . . . . ? C3 Mo2 C13 C14 -73.0(4) . . . . ? C12 Mo2 C13 C14 114.6(6) . . . . ? C11 Mo2 C13 C14 77.4(4) . . . . ? C15 Mo2 C13 C14 36.9(4) . . . . ? P1 Mo2 C13 C14 123.9(4) . . . . ? C1 Mo1 C2 O2 107(2) . . . . ? C25 Mo1 C2 O2 7(2) . . . . ? C21 Mo1 C2 O2 -30(2) . . . . ? C24 Mo1 C2 O2 18(2) . . . . ? C22 Mo1 C2 O2 -45(2) . . . . ? C23 Mo1 C2 O2 -15(2) . . . . ? P1 Mo1 C2 O2 -130(2) . . . . ? Cl1 Mo1 C2 O2 171(2) . . . . ? C12 C11 C15 C14 -1.8(5) . . . . ? Mo2 C11 C15 C14 62.1(4) . . . . ? C12 C11 C15 Mo2 -63.9(3) . . . . ? C13 C14 C15 C11 1.0(6) . . . . ? Mo2 C14 C15 C11 -62.3(3) . . . . ? C13 C14 C15 Mo2 63.4(3) . . . . ? C4 Mo2 C15 C11 59.7(5) . . . . ? C3 Mo2 C15 C11 168.3(3) . . . . ? C13 Mo2 C15 C11 79.1(4) . . . . ? C12 Mo2 C15 C11 38.0(3) . . . . ? C14 Mo2 C15 C11 117.2(5) . . . . ? P1 Mo2 C15 C11 -54.7(3) . . . . ? C4 Mo2 C15 C14 -57.5(6) . . . . ? C3 Mo2 C15 C14 51.1(5) . . . . ? C13 Mo2 C15 C14 -38.1(4) . . . . ? C12 Mo2 C15 C14 -79.2(4) . . . . ? C11 Mo2 C15 C14 -117.2(5) . . . . ? P1 Mo2 C15 C14 -171.9(4) . . . . ? C3 Mo2 C4 O4 -107(4) . . . . ? C13 Mo2 C4 O4 -6(4) . . . . ? C12 Mo2 C4 O4 28(4) . . . . ? C14 Mo2 C4 O4 -23(4) . . . . ? C11 Mo2 C4 O4 45(4) . . . . ? C15 Mo2 C4 O4 10(4) . . . . ? P1 Mo2 C4 O4 132(4) . . . . ? C35 C34 C33 C32 0.1(7) . . . . ? C31 C32 C33 C34 -0.7(6) . . . . ? C33 C34 C35 C36 0.2(7) . . . . ? C31 C36 C35 C34 0.1(6) . . . . ? C21 C25 C24 C23 1.1(5) . . . . ? Mo1 C25 C24 C23 65.8(3) . . . . ? C21 C25 C24 Mo1 -64.8(3) . . . . ? C2 Mo1 C24 C23 -133.4(3) . . . . ? C1 Mo1 C24 C23 143.2(3) . . . . ? C25 Mo1 C24 C23 -115.8(4) . . . . ? C21 Mo1 C24 C23 -77.1(3) . . . . ? C22 Mo1 C24 C23 -35.2(3) . . . . ? P1 Mo1 C24 C23 -22.1(4) . . . . ? Cl1 Mo1 C24 C23 58.5(3) . . . . ? C2 Mo1 C24 C25 -17.6(4) . . . . ? C1 Mo1 C24 C25 -100.9(3) . . . . ? C21 Mo1 C24 C25 38.7(3) . . . . ? C22 Mo1 C24 C25 80.6(3) . . . . ? C23 Mo1 C24 C25 115.8(4) . . . . ? P1 Mo1 C24 C25 93.7(4) . . . . ? Cl1 Mo1 C24 C25 174.4(3) . . . . ? C14 C13 C12 C11 -1.2(6) . . . . ? Mo2 C13 C12 C11 65.4(3) . . . . ? C14 C13 C12 Mo2 -66.6(4) . . . . ? C15 C11 C12 C13 1.9(5) . . . . ? Mo2 C11 C12 C13 -64.2(3) . . . . ? C15 C11 C12 Mo2 66.1(3) . . . . ? C4 Mo2 C12 C13 -88.7(4) . . . . ? C3 Mo2 C12 C13 -10.6(5) . . . . ? C14 Mo2 C12 C13 38.6(4) . . . . ? C11 Mo2 C12 C13 116.5(5) . . . . ? C15 Mo2 C12 C13 79.5(4) . . . . ? P1 Mo2 C12 C13 -173.5(4) . . . . ? C4 Mo2 C12 C11 154.8(4) . . . . ? C3 Mo2 C12 C11 -127.1(3) . . . . ? C13 Mo2 C12 C11 -116.5(5) . . . . ? C14 Mo2 C12 C11 -77.9(4) . . . . ? C15 Mo2 C12 C11 -37.0(4) . . . . ? P1 Mo2 C12 C11 70.0(4) . . . . ? C25 C24 C23 C22 -1.9(5) . . . . ? Mo1 C24 C23 C22 60.6(3) . . . . ? C25 C24 C23 Mo1 -62.5(3) . . . . ? C21 C22 C23 C24 1.9(5) . . . . ? Mo1 C22 C23 C24 -60.7(3) . . . . ? C21 C22 C23 Mo1 62.6(3) . . . . ? C2 Mo1 C23 C24 65.0(3) . . . . ? C1 Mo1 C23 C24 -42.8(3) . . . . ? C25 Mo1 C23 C24 38.3(3) . . . . ? C21 Mo1 C23 C24 81.7(3) . . . . ? C22 Mo1 C23 C24 120.1(4) . . . . ? P1 Mo1 C23 C24 166.6(2) . . . . ? Cl1 Mo1 C23 C24 -118.1(3) . . . . ? C2 Mo1 C23 C22 -55.1(4) . . . . ? C1 Mo1 C23 C22 -162.9(3) . . . . ? C25 Mo1 C23 C22 -81.8(3) . . . . ? C21 Mo1 C23 C22 -38.4(3) . . . . ? C24 Mo1 C23 C22 -120.1(4) . . . . ? P1 Mo1 C23 C22 46.5(3) . . . . ? Cl1 Mo1 C23 C22 121.7(3) . . . . ?