# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chun Yuan Liu' _publ_contact_author_email cyliu06@mail.tongji.edu.cn _publ_author_name 'Chun Yuan Liu' #====end data_Mo2C45H32N4Cl2F10O8 _database_code_depnum_ccdc_archive 'CCDC 825961' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-Mo2(DAniF)2(OOCC6F5)2(CH2Cl2) _chemical_melting_point ? _chemical_formula_moiety 'Mo2 C45 H32 N4 Cl2 F10 O8' _chemical_formula_sum 'C45 H32 Cl2 F10 Mo2 N4 O8' _chemical_formula_weight 1209.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 22.421(3) _cell_length_b 12.2647(15) _cell_length_c 17.654(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.3860(10) _cell_angle_gamma 90.00 _cell_volume 4657.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6641 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'non-area detector' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12408 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4579 _reflns_number_gt 3984 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0425P)^2^+5.8926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4579 _refine_ls_number_parameters 325 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.742144(9) 0.716047(16) 0.550610(11) 0.03041(8) Uani 1 1 d . . . N1 N 0.64367(10) 0.70784(16) 0.49785(12) 0.0351(4) Uani 1 1 d . . . N2 N 0.83862(10) 0.71324(16) 0.61156(12) 0.0354(5) Uani 1 1 d . . . O3 O 0.48628(11) 0.4971(2) 0.64680(15) 0.0706(7) Uani 1 1 d . . . O4 O 0.92639(11) 0.5844(2) 0.92734(12) 0.0686(7) Uani 1 1 d . . . O1 O 0.73669(8) 0.87333(14) 0.59883(10) 0.0368(4) Uani 1 1 d . . . O2 O 0.75277(8) 0.94491(13) 0.48980(10) 0.0372(4) Uani 1 1 d . . . F1 F 0.67607(9) 1.12808(15) 0.46599(10) 0.0643(5) Uani 1 1 d . . . F2 F 0.66818(11) 1.32721(16) 0.52350(13) 0.0797(6) Uani 1 1 d . . . F3 F 0.72879(12) 1.37493(15) 0.67542(14) 0.0840(7) Uani 1 1 d . . . F4 F 0.79646(12) 1.21963(17) 0.77140(12) 0.0819(7) Uani 1 1 d . . . F5 F 0.80379(9) 1.01810(15) 0.71525(10) 0.0613(5) Uani 1 1 d . . . C10 C 0.62241(12) 0.7436(2) 0.42422(15) 0.0379(5) Uani 1 1 d . . . H1A H 0.5803 0.7383 0.3978 0.045 Uiso 1 1 calc R . . C7 C 0.74392(11) 0.9537(2) 0.55737(14) 0.0361(5) Uani 1 1 d . . . C11 C 0.60092(12) 0.6589(2) 0.53443(14) 0.0363(5) Uani 1 1 d . . . C12 C 0.62105(13) 0.5697(2) 0.58396(16) 0.0443(6) Uani 1 1 d . . . H12A H 0.6615 0.5444 0.5926 0.053 Uiso 1 1 calc R . . C13 C 0.58194(14) 0.5187(3) 0.62029(18) 0.0529(7) Uani 1 1 d . . . H13A H 0.5962 0.4596 0.6534 0.063 Uiso 1 1 calc R . . C14 C 0.52158(14) 0.5546(2) 0.60795(17) 0.0495(7) Uani 1 1 d . . . C15 C 0.50057(13) 0.6435(3) 0.55941(17) 0.0489(7) Uani 1 1 d . . . H15A H 0.4600 0.6683 0.5508 0.059 Uiso 1 1 calc R . . C16 C 0.54098(12) 0.6954(2) 0.52363(16) 0.0422(6) Uani 1 1 d . . . H16A H 0.5271 0.7559 0.4918 0.051 Uiso 1 1 calc R . . C17 C 0.42598(18) 0.5356(4) 0.6407(3) 0.0841(12) Uani 1 1 d . . . H17A H 0.4067 0.4894 0.6709 0.126 Uiso 1 1 calc R . . H17B H 0.4018 0.5348 0.5863 0.126 Uiso 1 1 calc R . . H17C H 0.4283 0.6087 0.6607 0.126 Uiso 1 1 calc R . . C21 C 0.86204(12) 0.6790(2) 0.69180(14) 0.0364(5) Uani 1 1 d . . . C22 C 0.84359(13) 0.5799(2) 0.71448(16) 0.0437(6) Uani 1 1 d . . . H22A H 0.8167 0.5360 0.6770 0.052 Uiso 1 1 calc R . . C23 C 0.86446(14) 0.5445(2) 0.79241(17) 0.0500(7) Uani 1 1 d . . . H23A H 0.8518 0.4771 0.8066 0.060 Uiso 1 1 calc R . . C24 C 0.90376(13) 0.6092(2) 0.84842(16) 0.0474(7) Uani 1 1 d . . . C25 C 0.92146(16) 0.7098(3) 0.82674(18) 0.0568(8) Uani 1 1 d . . . H25A H 0.9475 0.7544 0.8646 0.068 Uiso 1 1 calc R . . C26 C 0.90062(15) 0.7448(3) 0.74897(17) 0.0507(7) Uani 1 1 d . . . H26A H 0.9126 0.8128 0.7351 0.061 Uiso 1 1 calc R . . C27 C 0.92117(17) 0.4741(3) 0.9497(2) 0.0726(11) Uani 1 1 d . . . H27A H 0.9384 0.4669 1.0058 0.109 Uiso 1 1 calc R . . H27B H 0.9434 0.4278 0.9233 0.109 Uiso 1 1 calc R . . H27C H 0.8781 0.4533 0.9351 0.109 Uiso 1 1 calc R . . C1 C 0.74074(12) 1.0659(2) 0.58861(15) 0.0379(5) Uani 1 1 d . . . C2 C 0.70706(14) 1.1480(2) 0.54167(16) 0.0451(6) Uani 1 1 d . . . C3 C 0.70249(15) 1.2508(2) 0.57013(19) 0.0527(7) Uani 1 1 d . . . C4 C 0.73277(16) 1.2749(2) 0.6474(2) 0.0551(8) Uani 1 1 d . . . C5 C 0.76671(16) 1.1962(3) 0.69578(18) 0.0530(7) Uani 1 1 d . . . C6 C 0.77011(13) 1.0929(2) 0.66641(16) 0.0436(6) Uani 1 1 d . . . Cl3 Cl 0.5342(6) 0.8763(9) 0.8262(7) 0.1672(16) Uiso 0.25 1 d PD A 1 C2S C 0.5000 0.9502(11) 0.7500 0.105(4) Uiso 0.50 2 d SPD . 1 Cl4 Cl 0.5585(5) 0.8516(9) 0.8140(7) 0.1672(16) Uiso 0.25 1 d PD A 1 Cl1 Cl 0.5626(4) 0.7973(8) 0.7555(6) 0.1672(16) Uiso 0.25 1 d PD . 2 C1S C 0.4915(8) 0.8238(16) 0.7836(11) 0.105(4) Uiso 0.25 1 d PD . 2 Cl2 Cl 0.5384(5) 0.9244(9) 0.8385(6) 0.1672(16) Uiso 0.25 1 d PD B 2 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 0.03400(13) 0.03074(12) 0.02580(12) 0.00172(8) 0.00732(8) 0.00199(8) N1 0.0357(11) 0.0363(11) 0.0326(11) 0.0029(8) 0.0086(9) 0.0003(9) N2 0.0366(11) 0.0382(11) 0.0288(10) 0.0037(8) 0.0048(8) 0.0011(9) O3 0.0688(15) 0.0790(16) 0.0744(16) 0.0233(13) 0.0371(13) -0.0052(13) O4 0.0788(16) 0.0752(15) 0.0406(11) 0.0240(11) -0.0015(10) -0.0027(13) O1 0.0455(10) 0.0342(9) 0.0318(9) -0.0004(7) 0.0127(7) 0.0024(8) O2 0.0461(10) 0.0326(9) 0.0339(9) 0.0009(7) 0.0131(8) 0.0023(8) F1 0.0822(13) 0.0555(10) 0.0455(9) 0.0032(8) 0.0020(9) 0.0161(9) F2 0.1002(16) 0.0465(10) 0.0883(15) 0.0122(10) 0.0197(12) 0.0274(11) F3 0.1160(18) 0.0414(10) 0.0958(16) -0.0244(10) 0.0319(14) 0.0050(11) F4 0.1095(18) 0.0726(14) 0.0525(12) -0.0265(10) 0.0049(11) -0.0035(12) F5 0.0749(12) 0.0543(10) 0.0445(9) 0.0017(8) 0.0002(8) 0.0080(9) C10 0.0349(13) 0.0406(13) 0.0357(13) 0.0011(11) 0.0060(10) 0.0014(11) C7 0.0360(13) 0.0371(13) 0.0352(13) -0.0002(10) 0.0098(10) 0.0043(10) C11 0.0387(13) 0.0378(13) 0.0315(12) -0.0013(10) 0.0083(10) -0.0016(10) C12 0.0425(14) 0.0443(15) 0.0454(15) 0.0094(12) 0.0112(12) 0.0040(12) C13 0.0571(18) 0.0521(17) 0.0490(16) 0.0146(14) 0.0143(14) 0.0005(14) C14 0.0550(17) 0.0540(17) 0.0431(15) 0.0031(13) 0.0194(13) -0.0085(14) C15 0.0394(14) 0.0592(18) 0.0498(16) 0.0011(14) 0.0157(12) 0.0002(13) C16 0.0413(14) 0.0452(14) 0.0387(14) 0.0060(11) 0.0089(11) 0.0012(11) C17 0.076(3) 0.087(3) 0.108(3) 0.018(2) 0.056(2) -0.004(2) C21 0.0363(13) 0.0395(13) 0.0312(12) 0.0043(10) 0.0059(10) 0.0037(10) C22 0.0462(15) 0.0419(14) 0.0379(13) 0.0025(11) 0.0034(11) -0.0037(12) C23 0.0545(17) 0.0462(16) 0.0467(16) 0.0147(13) 0.0097(13) -0.0002(13) C24 0.0482(16) 0.0559(17) 0.0334(13) 0.0103(12) 0.0039(11) 0.0054(13) C25 0.066(2) 0.0560(19) 0.0364(15) 0.0030(13) -0.0053(14) -0.0088(15) C26 0.0630(19) 0.0431(15) 0.0387(15) 0.0071(12) 0.0026(13) -0.0095(14) C27 0.064(2) 0.083(3) 0.062(2) 0.0376(19) 0.0033(17) -0.0013(19) C1 0.0441(14) 0.0337(12) 0.0382(13) -0.0010(11) 0.0155(11) 0.0009(11) C2 0.0527(16) 0.0416(14) 0.0408(14) -0.0007(12) 0.0132(12) 0.0039(12) C3 0.0617(19) 0.0377(14) 0.0618(19) 0.0068(14) 0.0223(15) 0.0099(14) C4 0.069(2) 0.0356(15) 0.065(2) -0.0107(14) 0.0271(16) 0.0005(14) C5 0.0624(19) 0.0495(17) 0.0474(17) -0.0130(13) 0.0158(14) -0.0052(14) C6 0.0485(15) 0.0401(14) 0.0423(14) -0.0006(12) 0.0127(12) 0.0013(12) _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 Mo1 2.0895(4) 7_666 ? Mo1 O2 2.1131(16) 7_666 ? Mo1 O1 2.1259(17) . ? Mo1 N2 2.127(2) . ? Mo1 N1 2.143(2) . ? N1 C10 1.326(3) . ? N1 C11 1.430(3) . ? N2 C10 1.324(3) 7_666 ? N2 C21 1.428(3) . ? O3 C14 1.378(3) . ? O3 C17 1.407(4) . ? O4 C24 1.375(3) . ? O4 C27 1.424(4) . ? O1 C7 1.265(3) . ? O2 C7 1.268(3) . ? O2 Mo1 2.1131(16) 7_666 ? F1 C2 1.343(3) . ? F2 C3 1.338(3) . ? F3 C4 1.336(3) . ? F4 C5 1.344(3) . ? F5 C6 1.337(3) . ? C10 N2 1.324(3) 7_666 ? C7 C1 1.492(3) . ? C11 C16 1.378(4) . ? C11 C12 1.394(4) . ? C12 C13 1.374(4) . ? C13 C14 1.380(4) . ? C14 C15 1.385(4) . ? C15 C16 1.396(4) . ? C21 C22 1.379(4) . ? C21 C26 1.388(4) . ? C22 C23 1.392(4) . ? C23 C24 1.376(4) . ? C24 C25 1.383(4) . ? C25 C26 1.388(4) . ? C1 C2 1.385(4) . ? C1 C6 1.386(4) . ? C2 C3 1.371(4) . ? C3 C4 1.373(5) . ? C4 C5 1.368(5) . ? C5 C6 1.380(4) . ? Cl3 Cl4 0.709(15) . ? Cl3 C2S 1.623(12) . ? C2S Cl3 1.623(12) 2_656 ? C2S Cl4 1.904(12) 2_656 ? C2S Cl4 1.904(12) . ? Cl1 C1S 1.256(18) 2_656 ? Cl1 C1S 1.827(16) . ? Cl1 Cl2 2.307(14) . ? C1S Cl1 1.256(18) 2_656 ? C1S C1S 1.34(4) 2_656 ? C1S Cl2 1.730(17) . ? 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 Mo1 Mo1 O2 92.61(5) 7_666 7_666 ? Mo1 Mo1 O1 91.34(5) 7_666 . ? O2 Mo1 O1 176.03(6) 7_666 . ? Mo1 Mo1 N2 92.65(6) 7_666 . ? O2 Mo1 N2 90.66(7) 7_666 . ? O1 Mo1 N2 88.70(7) . . ? Mo1 Mo1 N1 92.79(6) 7_666 . ? O2 Mo1 N1 87.51(7) 7_666 . ? O1 Mo1 N1 92.76(7) . . ? N2 Mo1 N1 174.33(7) . . ? C10 N1 C11 118.7(2) . . ? C10 N1 Mo1 116.86(17) . . ? C11 N1 Mo1 124.27(16) . . ? C10 N2 C21 118.9(2) 7_666 . ? C10 N2 Mo1 117.77(17) 7_666 . ? C21 N2 Mo1 122.92(16) . . ? C14 O3 C17 117.7(3) . . ? C24 O4 C27 117.1(3) . . ? C7 O1 Mo1 116.35(15) . . ? C7 O2 Mo1 115.75(15) . 7_666 ? N2 C10 N1 119.8(2) 7_666 . ? O1 C7 O2 123.9(2) . . ? O1 C7 C1 118.5(2) . . ? O2 C7 C1 117.5(2) . . ? C16 C11 C12 118.2(2) . . ? C16 C11 N1 123.6(2) . . ? C12 C11 N1 118.2(2) . . ? C13 C12 C11 120.9(3) . . ? C12 C13 C14 120.5(3) . . ? O3 C14 C13 115.7(3) . . ? O3 C14 C15 124.6(3) . . ? C13 C14 C15 119.7(3) . . ? C14 C15 C16 119.2(3) . . ? C11 C16 C15 121.4(3) . . ? C22 C21 C26 118.5(2) . . ? C22 C21 N2 119.4(2) . . ? C26 C21 N2 122.0(2) . . ? C21 C22 C23 121.2(3) . . ? C24 C23 C22 119.9(3) . . ? O4 C24 C23 125.4(3) . . ? O4 C24 C25 115.1(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 120.4(3) . . ? C2 C1 C6 116.5(2) . . ? C2 C1 C7 121.7(2) . . ? C6 C1 C7 121.9(2) . . ? F1 C2 C3 117.4(3) . . ? F1 C2 C1 120.3(2) . . ? C3 C2 C1 122.3(3) . . ? F2 C3 C2 120.5(3) . . ? F2 C3 C4 119.8(3) . . ? C2 C3 C4 119.6(3) . . ? F3 C4 C5 120.0(3) . . ? F3 C4 C3 120.0(3) . . ? C5 C4 C3 120.1(3) . . ? F4 C5 C4 120.2(3) . . ? F4 C5 C6 120.3(3) . . ? C4 C5 C6 119.5(3) . . ? F5 C6 C5 118.0(3) . . ? F5 C6 C1 119.9(2) . . ? C5 C6 C1 122.1(3) . . ? Cl4 Cl3 C2S 102.2(16) . . ? Cl3 C2S Cl3 112.2(12) 2_656 . ? Cl3 C2S Cl4 21.3(5) 2_656 2_656 ? Cl3 C2S Cl4 102.9(8) . 2_656 ? Cl3 C2S Cl4 102.9(8) 2_656 . ? Cl3 C2S Cl4 21.3(5) . . ? Cl4 C2S Cl4 101.1(10) 2_656 . ? Cl3 Cl4 C2S 56.4(13) . . ? C1S Cl1 C1S 47.4(15) 2_656 . ? C1S Cl1 Cl2 79.1(11) 2_656 . ? C1S Cl1 Cl2 47.8(6) . . ? Cl1 C1S C1S 89.2(18) 2_656 2_656 ? Cl1 C1S Cl2 146.3(16) 2_656 . ? C1S C1S Cl2 102.4(12) 2_656 . ? Cl1 C1S Cl1 125.8(13) 2_656 . ? C1S C1S Cl1 43.4(10) 2_656 . ? Cl2 C1S Cl1 80.8(9) . . ? C1S Cl2 Cl1 51.4(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.585 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.069 #====end data_Mo2C52H46N4F10O10 _database_code_depnum_ccdc_archive 'CCDC 825962' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-Mo2(DAniF)2(OOCC6F5)2(THF)2 _chemical_melting_point ? _chemical_formula_moiety 'Mo2 C52 H46 N4 F10 O10' _chemical_formula_sum 'C52 H46 F10 Mo2 N4 O10' _chemical_formula_weight 1268.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.2255(13) _cell_length_b 11.9204(17) _cell_length_c 12.8568(18) _cell_angle_alpha 76.551(2) _cell_angle_beta 82.545(2) _cell_angle_gamma 72.299(2) _cell_volume 1307.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2299 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.63 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 0.901 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6821 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4527 _reflns_number_gt 3699 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _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^)+(0.0413P)^2^+0.8069P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4527 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.53819(3) 0.51371(3) 0.91799(2) 0.03328(11) Uani 1 1 d . . . N1 N 0.7615(3) 0.3968(3) 0.9531(2) 0.0378(7) Uani 1 1 d . . . N2 N 0.3208(3) 0.6328(3) 0.8686(2) 0.0378(7) Uani 1 1 d . . . O1 O 0.6063(3) 0.6647(2) 0.92932(19) 0.0397(6) Uani 1 1 d . . . O2 O 0.4722(3) 0.3654(2) 0.89736(19) 0.0400(6) Uani 1 1 d . . . O3 O 1.2475(3) 0.2331(3) 0.6666(2) 0.0709(10) Uani 1 1 d . . . O4 O 0.1443(5) 0.8699(4) 0.4557(3) 0.0975(13) Uani 1 1 d . . . F1 F 0.4416(3) 0.8382(2) 1.17507(19) 0.0610(6) Uani 1 1 d . . . F2 F 0.5268(3) 1.0233(2) 1.1992(2) 0.0696(7) Uani 1 1 d . . . F3 F 0.7573(3) 1.0885(3) 1.0728(3) 0.0869(9) Uani 1 1 d . . . F4 F 0.9030(3) 0.9649(3) 0.9187(3) 0.0841(9) Uani 1 1 d . . . F5 F 0.8219(3) 0.7788(2) 0.8915(2) 0.0632(7) Uani 1 1 d . . . C10 C 0.2129(4) 0.6539(3) 0.9456(3) 0.0405(9) Uani 1 1 d . . . H1A H 0.1171 0.7053 0.9282 0.049 Uiso 1 1 calc R . . C7 C 0.5841(4) 0.6921(3) 1.0205(3) 0.0389(9) Uani 1 1 d . . . C11 C 0.8837(4) 0.3566(3) 0.8781(3) 0.0374(9) Uani 1 1 d . . . C12 C 1.0093(4) 0.4019(4) 0.8566(3) 0.0456(10) Uani 1 1 d . . . H12A H 1.0135 0.4617 0.8904 0.055 Uiso 1 1 calc R . . C13 C 1.1278(4) 0.3589(4) 0.7856(3) 0.0502(11) Uani 1 1 d . . . H13A H 1.2116 0.3893 0.7725 0.060 Uiso 1 1 calc R . . C14 C 1.1221(4) 0.2715(4) 0.7344(3) 0.0482(11) Uani 1 1 d . . . C15 C 0.9986(5) 0.2274(4) 0.7523(4) 0.0598(12) Uani 1 1 d . . . H15A H 0.9943 0.1690 0.7167 0.072 Uiso 1 1 calc R . . C16 C 0.8796(5) 0.2701(4) 0.8238(3) 0.0536(11) Uani 1 1 d . . . H16A H 0.7956 0.2402 0.8355 0.064 Uiso 1 1 calc R . . C17 C 1.2448(6) 0.1418(6) 0.6129(4) 0.097(2) Uani 1 1 d . . . H17A H 1.3368 0.1226 0.5680 0.146 Uiso 1 1 calc R . . H17B H 1.1585 0.1702 0.5696 0.146 Uiso 1 1 calc R . . H17C H 1.2374 0.0712 0.6649 0.146 Uiso 1 1 calc R . . C21 C 0.2782(4) 0.6942(3) 0.7623(3) 0.0413(9) Uani 1 1 d . . . C22 C 0.3600(5) 0.7667(4) 0.7001(3) 0.0519(11) Uani 1 1 d . . . H22A H 0.4433 0.7763 0.7271 0.062 Uiso 1 1 calc R . . C23 C 0.3194(5) 0.8264(4) 0.5959(3) 0.0626(13) Uani 1 1 d . . . H23A H 0.3771 0.8738 0.5535 0.075 Uiso 1 1 calc R . . C24 C 0.1954(6) 0.8151(4) 0.5568(3) 0.0638(13) Uani 1 1 d . . . C25 C 0.1120(6) 0.7436(5) 0.6187(4) 0.0711(14) Uani 1 1 d . . . H25A H 0.0275 0.7355 0.5919 0.085 Uiso 1 1 calc R . . C26 C 0.1529(5) 0.6837(4) 0.7203(3) 0.0562(11) Uani 1 1 d . . . H26A H 0.0956 0.6354 0.7617 0.067 Uiso 1 1 calc R . . C27 C 0.2224(9) 0.9460(6) 0.3892(4) 0.120(3) Uani 1 1 d . . . H27A H 0.1759 0.9777 0.3219 0.180 Uiso 1 1 calc R . . H27B H 0.3268 0.9016 0.3773 0.180 Uiso 1 1 calc R . . H27C H 0.2182 1.0110 0.4228 0.180 Uiso 1 1 calc R . . C1 C 0.6284(4) 0.7988(3) 1.0323(3) 0.0382(9) Uani 1 1 d . . . C2 C 0.5588(4) 0.8645(4) 1.1110(3) 0.0428(9) Uani 1 1 d . . . C3 C 0.6001(5) 0.9602(4) 1.1250(3) 0.0491(10) Uani 1 1 d . . . C4 C 0.7174(5) 0.9942(4) 1.0613(4) 0.0570(11) Uani 1 1 d . . . C5 C 0.7891(4) 0.9319(4) 0.9827(4) 0.0564(12) Uani 1 1 d . . . C6 C 0.7452(4) 0.8371(4) 0.9683(3) 0.0453(10) Uani 1 1 d . . . O1S O 0.6414(4) 0.5380(3) 0.7172(2) 0.0722(10) Uani 1 1 d . . . C11S C 0.7457(6) 0.6030(6) 0.6640(4) 0.104(2) Uani 1 1 d . . . H11A H 0.8210 0.5987 0.7119 0.125 Uiso 1 1 calc R . . H11B H 0.6924 0.6868 0.6378 0.125 Uiso 1 1 calc R . . C12S C 0.8178(10) 0.5444(9) 0.5751(6) 0.160(4) Uani 1 1 d . . . H12B H 0.8478 0.6012 0.5155 0.192 Uiso 1 1 calc R . . H12C H 0.9073 0.4786 0.5972 0.192 Uiso 1 1 calc R . . C13S C 0.7030(13) 0.5004(12) 0.5456(6) 0.193(5) Uani 1 1 d . . . H13B H 0.7492 0.4243 0.5232 0.232 Uiso 1 1 calc R . . H13C H 0.6475 0.5576 0.4871 0.232 Uiso 1 1 calc R . . C14S C 0.5986(7) 0.4846(7) 0.6432(5) 0.107(2) Uani 1 1 d . . . H14A H 0.4934 0.5240 0.6264 0.128 Uiso 1 1 calc R . . H14B H 0.6100 0.3999 0.6724 0.128 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 0.03191(17) 0.03572(19) 0.03293(16) -0.00855(12) 0.00065(11) -0.01061(12) N1 0.0332(15) 0.0404(18) 0.0388(16) -0.0113(14) 0.0013(12) -0.0080(13) N2 0.0376(16) 0.0372(18) 0.0374(15) -0.0057(13) -0.0043(12) -0.0094(13) O1 0.0405(13) 0.0403(15) 0.0407(14) -0.0094(11) 0.0004(10) -0.0155(11) O2 0.0407(13) 0.0419(15) 0.0412(13) -0.0099(12) -0.0011(10) -0.0167(11) O3 0.0520(17) 0.090(2) 0.0583(18) -0.0233(18) 0.0138(14) -0.0029(16) O4 0.125(3) 0.110(3) 0.0503(19) 0.007(2) -0.030(2) -0.031(3) F1 0.0637(15) 0.0648(16) 0.0644(15) -0.0300(13) 0.0133(12) -0.0275(13) F2 0.0825(18) 0.0585(16) 0.0773(17) -0.0330(14) -0.0115(14) -0.0170(14) F3 0.095(2) 0.0677(19) 0.123(3) -0.0338(18) -0.0077(18) -0.0479(17) F4 0.0694(18) 0.081(2) 0.116(2) -0.0200(18) 0.0148(16) -0.0507(16) F5 0.0509(14) 0.0691(17) 0.0785(16) -0.0290(14) 0.0159(12) -0.0277(12) C10 0.0327(18) 0.039(2) 0.050(2) -0.0114(17) -0.0049(15) -0.0065(16) C7 0.0314(18) 0.035(2) 0.050(2) -0.0103(18) -0.0039(15) -0.0071(16) C11 0.0308(18) 0.039(2) 0.0402(19) -0.0064(17) -0.0026(14) -0.0071(16) C12 0.039(2) 0.050(2) 0.050(2) -0.0124(19) 0.0008(16) -0.0154(18) C13 0.034(2) 0.060(3) 0.053(2) -0.004(2) 0.0040(16) -0.0167(19) C14 0.038(2) 0.057(3) 0.040(2) -0.0110(19) 0.0002(15) 0.0003(19) C15 0.056(3) 0.065(3) 0.064(3) -0.034(2) 0.004(2) -0.013(2) C16 0.044(2) 0.058(3) 0.068(3) -0.030(2) 0.0060(19) -0.019(2) C17 0.074(4) 0.130(5) 0.075(3) -0.057(4) 0.010(3) 0.011(3) C21 0.046(2) 0.036(2) 0.0377(19) -0.0118(16) -0.0016(15) -0.0032(17) C22 0.058(2) 0.052(3) 0.045(2) -0.0057(19) -0.0047(18) -0.017(2) C23 0.080(3) 0.050(3) 0.053(2) -0.006(2) 0.011(2) -0.021(2) C24 0.074(3) 0.063(3) 0.051(2) -0.008(2) -0.018(2) -0.012(2) C25 0.068(3) 0.089(4) 0.060(3) -0.010(3) -0.023(2) -0.025(3) C26 0.056(3) 0.064(3) 0.052(2) -0.005(2) -0.0118(19) -0.023(2) C27 0.176(7) 0.119(6) 0.052(3) 0.018(3) -0.018(4) -0.048(5) C1 0.0356(19) 0.038(2) 0.045(2) -0.0091(17) -0.0095(15) -0.0135(16) C2 0.039(2) 0.042(2) 0.051(2) -0.0104(18) -0.0094(16) -0.0132(17) C3 0.054(2) 0.042(2) 0.054(2) -0.015(2) -0.0127(19) -0.009(2) C4 0.057(3) 0.046(3) 0.078(3) -0.015(2) -0.019(2) -0.022(2) C5 0.041(2) 0.054(3) 0.079(3) -0.007(2) -0.007(2) -0.023(2) C6 0.0337(19) 0.045(2) 0.061(2) -0.015(2) -0.0053(17) -0.0117(18) O1S 0.068(2) 0.097(3) 0.0437(16) -0.0114(17) 0.0029(14) -0.0166(18) C11S 0.061(3) 0.145(6) 0.073(3) 0.018(4) 0.007(3) -0.018(3) C12S 0.136(7) 0.175(9) 0.086(5) 0.015(5) 0.049(5) 0.023(6) C13S 0.199(11) 0.313(15) 0.083(5) -0.104(8) 0.018(6) -0.059(11) C14S 0.105(5) 0.133(6) 0.076(4) -0.042(4) -0.003(3) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 2.117(3) . ? Mo1 Mo1 2.1176(6) 2_667 ? Mo1 O1 2.119(3) . ? Mo1 N1 2.143(3) . ? Mo1 N2 2.149(3) . ? Mo1 O1S 2.614(3) . ? N1 C10 1.320(4) 2_667 ? N1 C11 1.426(4) . ? N2 C10 1.321(4) . ? N2 C21 1.434(4) . ? O1 C7 1.264(4) . ? O2 C7 1.261(4) 2_667 ? O3 C14 1.382(4) . ? O3 C17 1.424(6) . ? O4 C24 1.384(5) . ? O4 C27 1.396(7) . ? F1 C2 1.342(4) . ? F2 C3 1.338(5) . ? F3 C4 1.328(5) . ? F4 C5 1.346(5) . ? F5 C6 1.340(4) . ? C10 N1 1.320(4) 2_667 ? C10 H1A 0.9300 . ? C7 O2 1.261(4) 2_667 ? C7 C1 1.494(5) . ? C11 C16 1.384(5) . ? C11 C12 1.392(5) . ? C12 C13 1.382(5) . ? C12 H12A 0.9300 . ? C13 C14 1.372(6) . ? C13 H13A 0.9300 . ? C14 C15 1.367(6) . ? C15 C16 1.388(5) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C21 C22 1.370(5) . ? C21 C26 1.387(5) . ? C22 C23 1.402(6) . ? C22 H22A 0.9300 . ? C23 C24 1.361(6) . ? C23 H23A 0.9300 . ? C24 C25 1.370(7) . ? C25 C26 1.375(6) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C1 C2 1.393(5) . ? C1 C6 1.393(5) . ? C2 C3 1.362(5) . ? C3 C4 1.374(6) . ? C4 C5 1.375(6) . ? C5 C6 1.368(6) . ? O1S C14S 1.414(7) . ? O1S C11S 1.424(6) . ? C11S C12S 1.458(9) . ? C11S H11A 0.9700 . ? C11S H11B 0.9700 . ? C12S C13S 1.441(12) . ? C12S H12B 0.9700 . ? C12S H12C 0.9700 . ? C13S C14S 1.491(10) . ? C13S H13B 0.9700 . ? C13S H13C 0.9700 . ? C14S H14A 0.9700 . ? C14S H14B 0.9700 . ? 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 O2 Mo1 Mo1 91.31(7) . 2_667 ? O2 Mo1 O1 176.84(9) . . ? Mo1 Mo1 O1 91.81(7) 2_667 . ? O2 Mo1 N1 89.57(11) . . ? Mo1 Mo1 N1 91.84(8) 2_667 . ? O1 Mo1 N1 90.89(11) . . ? O2 Mo1 N2 90.15(11) . . ? Mo1 Mo1 N2 93.05(8) 2_667 . ? O1 Mo1 N2 89.14(10) . . ? N1 Mo1 N2 175.11(11) . . ? O2 Mo1 O1S 87.50(11) . . ? Mo1 Mo1 O1S 177.42(8) 2_667 . ? O1 Mo1 O1S 89.41(11) . . ? N1 Mo1 O1S 85.87(10) . . ? N2 Mo1 O1S 89.25(10) . . ? C10 N1 C11 114.8(3) 2_667 . ? C10 N1 Mo1 117.7(2) 2_667 . ? C11 N1 Mo1 127.2(2) . . ? C10 N2 C21 115.5(3) . . ? C10 N2 Mo1 116.3(2) . . ? C21 N2 Mo1 128.3(2) . . ? C7 O1 Mo1 116.0(2) . . ? C7 O2 Mo1 116.6(2) 2_667 . ? C14 O3 C17 116.8(4) . . ? C24 O4 C27 117.9(5) . . ? N1 C10 N2 121.2(3) 2_667 . ? N1 C10 H1A 119.4 2_667 . ? N2 C10 H1A 119.4 . . ? O2 C7 O1 124.3(4) 2_667 . ? O2 C7 C1 117.7(3) 2_667 . ? O1 C7 C1 118.0(3) . . ? C16 C11 C12 117.9(3) . . ? C16 C11 N1 120.0(3) . . ? C12 C11 N1 122.1(4) . . ? C13 C12 C11 120.7(4) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 O3 124.0(4) . . ? C13 C14 O3 115.7(4) . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C11 C16 C15 121.3(4) . . ? C11 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C21 C26 118.2(4) . . ? C22 C21 N2 120.3(4) . . ? C26 C21 N2 121.5(4) . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.0(4) . . ? C23 C24 O4 125.1(5) . . ? C25 C24 O4 114.9(5) . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 121.2(4) . . ? C25 C26 H26A 119.4 . . ? C21 C26 H26A 119.4 . . ? O4 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C2 C1 C6 115.4(4) . . ? C2 C1 C7 122.0(3) . . ? C6 C1 C7 122.5(3) . . ? F1 C2 C3 116.4(4) . . ? F1 C2 C1 120.6(4) . . ? C3 C2 C1 123.0(4) . . ? F2 C3 C2 121.1(4) . . ? F2 C3 C4 119.0(4) . . ? C2 C3 C4 119.9(4) . . ? F3 C4 C3 120.7(4) . . ? F3 C4 C5 120.4(4) . . ? C3 C4 C5 118.9(4) . . ? F4 C5 C6 119.6(4) . . ? F4 C5 C4 119.7(4) . . ? C6 C5 C4 120.6(4) . . ? F5 C6 C5 117.6(4) . . ? F5 C6 C1 120.4(4) . . ? C5 C6 C1 122.0(4) . . ? C14S O1S C11S 108.9(4) . . ? C14S O1S Mo1 122.9(3) . . ? C11S O1S Mo1 128.1(3) . . ? O1S C11S C12S 105.0(7) . . ? O1S C11S H11A 110.7 . . ? C12S C11S H11A 110.7 . . ? O1S C11S H11B 110.7 . . ? C12S C11S H11B 110.7 . . ? H11A C11S H11B 108.8 . . ? C13S C12S C11S 104.9(7) . . ? C13S C12S H12B 110.8 . . ? C11S C12S H12B 110.8 . . ? C13S C12S H12C 110.8 . . ? C11S C12S H12C 110.8 . . ? H12B C12S H12C 108.8 . . ? C12S C13S C14S 106.0(6) . . ? C12S C13S H13B 110.5 . . ? C14S C13S H13B 110.5 . . ? C12S C13S H13C 110.5 . . ? C14S C13S H13C 110.5 . . ? H13B C13S H13C 108.7 . . ? O1S C14S C13S 105.9(6) . . ? O1S C14S H14A 110.6 . . ? C13S C14S H14A 110.6 . . ? O1S C14S H14B 110.6 . . ? C13S C14S H14B 110.6 . . ? H14A C14S H14B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.926 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.074