# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'J. Anderson' 'Warren B. Cross' 'Claire Wilson' _publ_contact_author_name 'J. Anderson' _publ_contact_author_email J.ANDERSON@NOTTINGHAM.AC.UK _publ_section_title ; Nucleophilic reactivity of a d0 molybdenum oxo moiety ; # Attachment '3.cif' data_montip _database_code_depnum_ccdc_archive 'CCDC 704967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 Cl Mo N O4' _chemical_formula_weight 672.17 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' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.400(2) _cell_length_b 10.8824(14) _cell_length_c 21.642(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.411(2) _cell_angle_gamma 90.00 _cell_volume 3460.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3624 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.65 _exptl_crystal_description tablet _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21505 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7886 _reflns_number_gt 5956 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _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^)+(0.0475P)^2^+1.1945P] 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 7886 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl 0.38312(5) 0.85504(7) 0.23201(3) 0.02652(17) Uani 1 1 d . . . Mo1 Mo 0.329629(16) 0.88751(2) 0.116340(11) 0.01668(8) Uani 1 1 d . . . O1 O 0.39801(13) 1.05525(18) 0.14229(9) 0.0215(4) Uani 1 1 d . . . N1 N 0.22447(16) 0.9397(2) 0.11386(11) 0.0208(5) Uani 1 1 d . . . C1 C 0.13945(19) 1.0031(3) 0.11093(14) 0.0227(6) Uani 1 1 d . . . O2 O 0.32283(13) 0.92028(17) 0.02811(9) 0.0192(4) Uani 1 1 d . . . C2 C 0.0607(2) 0.9207(3) 0.07364(15) 0.0283(7) Uani 1 1 d . . . H2A H 0.0626 0.8435 0.0972 0.042 Uiso 1 1 calc R . . H2B H 0.0664 0.9034 0.0306 0.042 Uiso 1 1 calc R . . H2C H 0.0029 0.9626 0.0692 0.042 Uiso 1 1 calc R . . O3 O 0.32166(13) 0.71708(17) 0.11008(9) 0.0210(4) Uani 1 1 d . . . C3 C 0.1384(2) 1.1251(3) 0.07523(17) 0.0326(7) Uani 1 1 d . . . H3A H 0.1893 1.1764 0.0999 0.049 Uiso 1 1 calc R . . H3B H 0.0809 1.1680 0.0709 0.049 Uiso 1 1 calc R . . H3C H 0.1443 1.1089 0.0321 0.049 Uiso 1 1 calc R . . O4 O 0.47973(13) 0.90239(17) 0.12700(9) 0.0215(4) Uani 1 1 d . . . C4 C 0.1379(2) 1.0243(4) 0.18015(16) 0.0393(9) Uani 1 1 d . . . H4A H 0.1388 0.9450 0.2017 0.059 Uiso 1 1 calc R . . H4B H 0.0826 1.0694 0.1796 0.059 Uiso 1 1 calc R . . H4C H 0.1915 1.0723 0.2037 0.059 Uiso 1 1 calc R . . C5 C 0.2568(2) 0.9560(3) -0.02744(13) 0.0206(6) Uani 1 1 d . . . C6 C 0.2523(2) 1.0800(3) -0.04631(14) 0.0237(6) Uani 1 1 d . . . C7 C 0.1878(2) 1.1111(3) -0.10453(14) 0.0305(7) Uani 1 1 d . . . H7A H 0.1827 1.1943 -0.1184 0.037 Uiso 1 1 calc R . . C8 C 0.1312(2) 1.0243(3) -0.14251(15) 0.0327(8) Uani 1 1 d . . . H8A H 0.0881 1.0479 -0.1822 0.039 Uiso 1 1 calc R . . C9 C 0.1371(2) 0.9033(3) -0.12287(14) 0.0299(7) Uani 1 1 d . . . H9A H 0.0977 0.8443 -0.1495 0.036 Uiso 1 1 calc R . . C10 C 0.1993(2) 0.8653(3) -0.06508(14) 0.0229(6) Uani 1 1 d . . . C11 C 0.3162(2) 1.1756(3) -0.00496(15) 0.0254(7) Uani 1 1 d . . . H11A H 0.3235 1.1551 0.0414 0.030 Uiso 1 1 calc R . . C12 C 0.2798(3) 1.3067(3) -0.01640(17) 0.0351(8) Uani 1 1 d . . . H12A H 0.2196 1.3105 -0.0099 0.053 Uiso 1 1 calc R . . H12B H 0.2750 1.3315 -0.0608 0.053 Uiso 1 1 calc R . . H12C H 0.3214 1.3623 0.0141 0.053 Uiso 1 1 calc R . . C13 C 0.4100(2) 1.1659(3) -0.01475(17) 0.0367(8) Uani 1 1 d . . . H13A H 0.4319 1.0810 -0.0071 0.055 Uiso 1 1 calc R . . H13B H 0.4525 1.2207 0.0157 0.055 Uiso 1 1 calc R . . H13C H 0.4060 1.1897 -0.0592 0.055 Uiso 1 1 calc R . . C14 C 0.2085(2) 0.7326(3) -0.04342(15) 0.0253(7) Uani 1 1 d . . . H14A H 0.2153 0.7323 0.0040 0.030 Uiso 1 1 calc R . . C15 C 0.1264(3) 0.6532(3) -0.07611(18) 0.0445(9) Uani 1 1 d . . . H15A H 0.0715 0.6906 -0.0703 0.067 Uiso 1 1 calc R . . H15B H 0.1348 0.5710 -0.0567 0.067 Uiso 1 1 calc R . . H15C H 0.1199 0.6467 -0.1224 0.067 Uiso 1 1 calc R . . C16 C 0.2954(2) 0.6758(3) -0.05181(17) 0.0375(8) Uani 1 1 d . . . H16A H 0.3477 0.7281 -0.0305 0.056 Uiso 1 1 calc R . . H16B H 0.2896 0.6693 -0.0980 0.056 Uiso 1 1 calc R . . H16C H 0.3046 0.5938 -0.0322 0.056 Uiso 1 1 calc R . . C17 C 0.3256(2) 0.5974(2) 0.12828(13) 0.0197(6) Uani 1 1 d . . . C18 C 0.2468(2) 0.5412(3) 0.13555(13) 0.0206(6) Uani 1 1 d . . . C19 C 0.2537(2) 0.4188(3) 0.15483(14) 0.0279(7) Uani 1 1 d . . . H19A H 0.2021 0.3787 0.1609 0.033 Uiso 1 1 calc R . . C20 C 0.3347(2) 0.3540(3) 0.16534(15) 0.0312(8) Uani 1 1 d . . . H20A H 0.3381 0.2703 0.1783 0.037 Uiso 1 1 calc R . . C21 C 0.4102(2) 0.4116(3) 0.15682(15) 0.0279(7) Uani 1 1 d . . . H21A H 0.4652 0.3665 0.1644 0.033 Uiso 1 1 calc R . . C22 C 0.4081(2) 0.5338(3) 0.13743(13) 0.0211(6) Uani 1 1 d . . . C23 C 0.1601(2) 0.6131(3) 0.12568(14) 0.0261(6) Uani 1 1 d . . . H23A H 0.1616 0.6839 0.0966 0.031 Uiso 1 1 calc R . . C24 C 0.0746(2) 0.5385(4) 0.09352(18) 0.0450(9) Uani 1 1 d . . . H24A H 0.0783 0.5056 0.0522 0.067 Uiso 1 1 calc R . . H24B H 0.0210 0.5916 0.0856 0.067 Uiso 1 1 calc R . . H24C H 0.0697 0.4706 0.1220 0.067 Uiso 1 1 calc R . . C25 C 0.1563(2) 0.6658(3) 0.19031(15) 0.0299(7) Uani 1 1 d . . . H25A H 0.2116 0.7136 0.2101 0.045 Uiso 1 1 calc R . . H25B H 0.1520 0.5984 0.2193 0.045 Uiso 1 1 calc R . . H25C H 0.1029 0.7192 0.1830 0.045 Uiso 1 1 calc R . . C26 C 0.4906(2) 0.5946(3) 0.12715(15) 0.0251(7) Uani 1 1 d . . . H26A H 0.4693 0.6673 0.0984 0.030 Uiso 1 1 calc R . . C27 C 0.5547(2) 0.6406(3) 0.19034(17) 0.0394(9) Uani 1 1 d . . . H27A H 0.5218 0.6953 0.2115 0.059 Uiso 1 1 calc R . . H27B H 0.6050 0.6858 0.1817 0.059 Uiso 1 1 calc R . . H27C H 0.5791 0.5706 0.2187 0.059 Uiso 1 1 calc R . . C28 C 0.5411(3) 0.5093(4) 0.0937(2) 0.0488(10) Uani 1 1 d . . . H28A H 0.5943 0.5520 0.0881 0.073 Uiso 1 1 calc R . . H28B H 0.5005 0.4854 0.0512 0.073 Uiso 1 1 calc R . . H28C H 0.5610 0.4357 0.1202 0.073 Uiso 1 1 calc R . . C29 C 0.47580(19) 1.0141(3) 0.13990(13) 0.0203(6) Uani 1 1 d . . . C30 C 0.5560(2) 1.0983(3) 0.15302(14) 0.0240(6) Uani 1 1 d . . . H30A H 0.5339 1.1832 0.1418 0.029 Uiso 1 1 calc R . . H30B H 0.5928 1.0752 0.1243 0.029 Uiso 1 1 calc R . . C31 C 0.6182(2) 1.0964(3) 0.22428(15) 0.0268(7) Uani 1 1 d . . . C32 C 0.5623(2) 1.1223(3) 0.27018(16) 0.0368(8) Uani 1 1 d . . . H32A H 0.6022 1.1209 0.3150 0.055 Uiso 1 1 calc R . . H32B H 0.5151 1.0594 0.2646 0.055 Uiso 1 1 calc R . . H32C H 0.5338 1.2034 0.2606 0.055 Uiso 1 1 calc R . . C33 C 0.6650(3) 0.9726(3) 0.23972(18) 0.0424(9) Uani 1 1 d . . . H33A H 0.7040 0.9721 0.2848 0.064 Uiso 1 1 calc R . . H33B H 0.7023 0.9580 0.2108 0.064 Uiso 1 1 calc R . . H33C H 0.6191 0.9077 0.2336 0.064 Uiso 1 1 calc R . . C34 C 0.6892(2) 1.1978(3) 0.23064(18) 0.0388(9) Uani 1 1 d . . . H34A H 0.7299 1.1997 0.2752 0.058 Uiso 1 1 calc R . . H34B H 0.6585 1.2773 0.2200 0.058 Uiso 1 1 calc R . . H34C H 0.7247 1.1813 0.2008 0.058 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 Cl 0.0268(4) 0.0315(4) 0.0206(3) 0.0011(3) 0.0060(3) -0.0012(3) Mo1 0.01546(12) 0.01429(12) 0.01932(12) 0.00027(10) 0.00371(9) 0.00010(10) O1 0.0183(10) 0.0189(11) 0.0251(11) -0.0015(8) 0.0033(9) 0.0003(8) N1 0.0181(13) 0.0205(13) 0.0226(12) 0.0009(10) 0.0043(10) 0.0008(10) C1 0.0157(14) 0.0265(16) 0.0241(15) 0.0005(12) 0.0032(12) 0.0047(12) O2 0.0207(10) 0.0155(10) 0.0204(10) 0.0038(8) 0.0048(8) 0.0021(8) C2 0.0185(15) 0.0321(18) 0.0313(17) 0.0059(13) 0.0028(13) 0.0020(13) O3 0.0225(11) 0.0158(10) 0.0227(10) 0.0014(8) 0.0037(9) -0.0008(8) C3 0.0245(17) 0.0254(18) 0.047(2) 0.0000(15) 0.0096(15) 0.0037(14) O4 0.0191(10) 0.0168(11) 0.0272(11) -0.0018(8) 0.0046(9) 0.0000(8) C4 0.0329(19) 0.055(2) 0.0279(18) -0.0065(16) 0.0063(15) 0.0098(17) C5 0.0228(15) 0.0209(15) 0.0183(14) 0.0008(11) 0.0067(12) 0.0027(12) C6 0.0282(17) 0.0231(16) 0.0223(15) 0.0024(12) 0.0113(13) 0.0051(12) C7 0.0364(19) 0.0290(17) 0.0259(16) 0.0069(14) 0.0093(14) 0.0092(15) C8 0.0313(18) 0.041(2) 0.0222(16) 0.0052(14) 0.0028(14) 0.0092(15) C9 0.0268(16) 0.036(2) 0.0248(16) -0.0054(14) 0.0040(13) 0.0014(14) C10 0.0243(16) 0.0229(16) 0.0237(15) -0.0028(12) 0.0104(13) 0.0022(12) C11 0.0313(17) 0.0194(16) 0.0258(16) 0.0018(12) 0.0092(14) 0.0007(13) C12 0.048(2) 0.0189(17) 0.0389(19) 0.0057(14) 0.0139(17) 0.0020(15) C13 0.0334(19) 0.0318(19) 0.046(2) 0.0009(16) 0.0133(17) -0.0033(15) C14 0.0305(17) 0.0203(16) 0.0258(16) -0.0036(12) 0.0094(14) -0.0041(13) C15 0.049(2) 0.031(2) 0.046(2) -0.0069(16) 0.0029(19) -0.0134(17) C16 0.045(2) 0.0220(18) 0.046(2) -0.0008(15) 0.0153(18) 0.0065(15) C17 0.0284(16) 0.0129(14) 0.0167(13) -0.0011(10) 0.0049(12) -0.0022(12) C18 0.0257(16) 0.0194(15) 0.0159(14) -0.0034(11) 0.0050(12) -0.0020(12) C19 0.0369(19) 0.0235(17) 0.0268(16) -0.0030(12) 0.0151(15) -0.0074(13) C20 0.047(2) 0.0184(16) 0.0330(18) 0.0022(13) 0.0195(16) 0.0007(14) C21 0.0358(18) 0.0208(17) 0.0304(16) 0.0019(13) 0.0148(15) 0.0050(13) C22 0.0282(16) 0.0178(15) 0.0165(14) 0.0009(11) 0.0056(12) 0.0007(12) C23 0.0234(15) 0.0284(17) 0.0253(15) 0.0014(13) 0.0055(13) -0.0062(13) C24 0.029(2) 0.052(3) 0.046(2) -0.0013(18) -0.0001(17) -0.0104(17) C25 0.0287(18) 0.0306(18) 0.0345(18) 0.0029(14) 0.0156(15) 0.0015(14) C26 0.0247(16) 0.0203(16) 0.0322(16) 0.0030(13) 0.0113(14) 0.0039(12) C27 0.0327(19) 0.037(2) 0.042(2) -0.0011(16) 0.0019(16) -0.0054(16) C28 0.054(2) 0.039(2) 0.069(3) -0.001(2) 0.042(2) -0.0010(19) C29 0.0204(15) 0.0211(15) 0.0175(14) 0.0033(11) 0.0030(12) 0.0011(12) C30 0.0220(15) 0.0185(15) 0.0309(16) -0.0006(12) 0.0071(13) -0.0038(12) C31 0.0182(15) 0.0279(17) 0.0325(16) -0.0052(13) 0.0050(13) -0.0042(13) C32 0.0334(19) 0.045(2) 0.0317(17) -0.0109(16) 0.0100(15) -0.0108(17) C33 0.038(2) 0.037(2) 0.044(2) 0.0021(17) -0.0008(17) 0.0050(16) C34 0.0250(18) 0.041(2) 0.047(2) -0.0035(17) 0.0063(16) -0.0116(15) _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 Cl Mo1 2.4157(8) . ? Mo1 N1 1.702(2) . ? Mo1 O3 1.8610(19) . ? Mo1 O2 1.9144(19) . ? Mo1 O1 2.098(2) . ? Mo1 O4 2.259(2) . ? Mo1 C29 2.557(3) . ? O1 C29 1.294(3) . ? N1 C1 1.464(4) . ? C1 C4 1.523(4) . ? C1 C2 1.529(4) . ? C1 C3 1.534(4) . ? O2 C5 1.378(3) . ? O3 C17 1.357(3) . ? O4 C29 1.253(3) . ? C5 C6 1.406(4) . ? C5 C10 1.410(4) . ? C6 C7 1.393(4) . ? C6 C11 1.524(4) . ? C7 C8 1.378(5) . ? C8 C9 1.379(5) . ? C9 C10 1.391(4) . ? C10 C14 1.512(4) . ? C11 C12 1.525(4) . ? C11 C13 1.526(4) . ? C14 C15 1.521(4) . ? C14 C16 1.534(4) . ? C17 C22 1.407(4) . ? C17 C18 1.409(4) . ? C18 C19 1.390(4) . ? C18 C23 1.508(4) . ? C19 C20 1.392(5) . ? C20 C21 1.380(4) . ? C21 C22 1.392(4) . ? C22 C26 1.507(4) . ? C23 C24 1.525(4) . ? C23 C25 1.529(4) . ? C26 C27 1.513(5) . ? C26 C28 1.526(4) . ? C29 C30 1.495(4) . ? C30 C31 1.553(4) . ? C31 C33 1.518(5) . ? C31 C32 1.522(4) . ? C31 C34 1.531(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O3 106.80(10) . . ? N1 Mo1 O2 97.99(10) . . ? O3 Mo1 O2 97.49(8) . . ? N1 Mo1 O1 96.58(10) . . ? O3 Mo1 O1 154.61(8) . . ? O2 Mo1 O1 88.75(8) . . ? N1 Mo1 O4 156.10(10) . . ? O3 Mo1 O4 97.01(8) . . ? O2 Mo1 O4 80.64(8) . . ? O1 Mo1 O4 59.61(7) . . ? N1 Mo1 Cl 96.18(8) . . ? O3 Mo1 Cl 85.65(6) . . ? O2 Mo1 Cl 163.90(6) . . ? O1 Mo1 Cl 82.05(6) . . ? O4 Mo1 Cl 83.31(5) . . ? N1 Mo1 C29 126.80(10) . . ? O3 Mo1 C29 125.90(9) . . ? O2 Mo1 C29 83.15(8) . . ? O1 Mo1 C29 30.29(8) . . ? O4 Mo1 C29 29.33(8) . . ? Cl Mo1 C29 82.26(6) . . ? C29 O1 Mo1 94.86(17) . . ? C1 N1 Mo1 171.4(2) . . ? N1 C1 C4 107.8(2) . . ? N1 C1 C2 107.7(2) . . ? C4 C1 C2 111.4(3) . . ? N1 C1 C3 107.7(2) . . ? C4 C1 C3 111.3(3) . . ? C2 C1 C3 110.8(2) . . ? C5 O2 Mo1 136.76(17) . . ? C17 O3 Mo1 159.95(18) . . ? C29 O4 Mo1 88.63(17) . . ? O2 C5 C6 118.9(3) . . ? O2 C5 C10 118.5(2) . . ? C6 C5 C10 122.4(3) . . ? C7 C6 C5 117.1(3) . . ? C7 C6 C11 121.7(3) . . ? C5 C6 C11 121.2(3) . . ? C8 C7 C6 121.7(3) . . ? C7 C8 C9 119.9(3) . . ? C8 C9 C10 121.7(3) . . ? C9 C10 C5 117.1(3) . . ? C9 C10 C14 122.5(3) . . ? C5 C10 C14 120.4(3) . . ? C6 C11 C12 113.7(3) . . ? C6 C11 C13 110.1(2) . . ? C12 C11 C13 111.0(3) . . ? C10 C14 C15 114.3(3) . . ? C10 C14 C16 110.6(3) . . ? C15 C14 C16 110.5(3) . . ? O3 C17 C22 118.3(2) . . ? O3 C17 C18 118.9(3) . . ? C22 C17 C18 122.8(3) . . ? C19 C18 C17 117.3(3) . . ? C19 C18 C23 121.6(3) . . ? C17 C18 C23 121.0(3) . . ? C18 C19 C20 121.2(3) . . ? C21 C20 C19 119.8(3) . . ? C20 C21 C22 122.0(3) . . ? C21 C22 C17 116.8(3) . . ? C21 C22 C26 121.3(3) . . ? C17 C22 C26 121.9(3) . . ? C18 C23 C24 113.3(3) . . ? C18 C23 C25 109.8(2) . . ? C24 C23 C25 110.7(3) . . ? C22 C26 C27 111.3(3) . . ? C22 C26 C28 112.0(3) . . ? C27 C26 C28 110.0(3) . . ? O4 C29 O1 116.8(3) . . ? O4 C29 C30 123.0(3) . . ? O1 C29 C30 120.2(3) . . ? O4 C29 Mo1 62.04(15) . . ? O1 C29 Mo1 54.85(14) . . ? C30 C29 Mo1 174.8(2) . . ? C29 C30 C31 114.1(2) . . ? C33 C31 C32 110.2(3) . . ? C33 C31 C34 109.9(3) . . ? C32 C31 C34 109.6(3) . . ? C33 C31 C30 110.0(3) . . ? C32 C31 C30 110.2(3) . . ? C34 C31 C30 106.9(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.503 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.085 # Attachment '4.CIF' data_mobntf _database_code_depnum_ccdc_archive 'CCDC 704968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 F6 Mo2 N2 O11 S2' _chemical_formula_weight 1210.98 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' S S 0.1246 0.1234 '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 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 26.410(8) _cell_length_b 10.589(3) _cell_length_c 19.751(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.462(5) _cell_angle_gamma 90.00 _cell_volume 5297(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7255 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.3 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_process_details 'Bruker SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ' sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 37049 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10481 _reflns_number_gt 6334 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _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^)+(0.0617P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difamp' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10481 _refine_ls_number_parameters 655 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.004 _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 0.435107(15) 0.63995(4) 0.267886(19) 0.01838(11) Uani 1 1 d . . . S1 S 0.53817(5) 0.81513(12) 0.36450(6) 0.0261(3) Uani 1 1 d . . . O1 O 0.5000 0.5962(4) 0.2500 0.0201(10) Uani 1 2 d S . . N1 N 0.42822(14) 0.5124(3) 0.31821(18) 0.0207(8) Uani 1 1 d . . . F1 F 0.55461(14) 1.0572(3) 0.3667(2) 0.0656(11) Uani 1 1 d . . . C1 C 0.41353(17) 0.4054(4) 0.3558(2) 0.0241(11) Uani 1 1 d . . . O2 O 0.38875(11) 0.5876(3) 0.18111(15) 0.0197(7) Uani 1 1 d . . . F2 F 0.50063(14) 0.9985(3) 0.42354(18) 0.0589(10) Uani 1 1 d . . . C2 C 0.44809(19) 0.4114(5) 0.4334(2) 0.0327(12) Uani 1 1 d . . . H2A H 0.4854 0.4053 0.4349 0.049 Uiso 1 1 calc R . . H2B H 0.4389 0.3410 0.4599 0.049 Uiso 1 1 calc R . . H2C H 0.4418 0.4915 0.4545 0.049 Uiso 1 1 calc R . . O3 O 0.38761(12) 0.7510(3) 0.29313(16) 0.0263(8) Uani 1 1 d . . . F3 F 0.47611(13) 1.0043(3) 0.31030(17) 0.0484(8) Uani 1 1 d . . . C3 C 0.4230(2) 0.2847(4) 0.3196(3) 0.0336(12) Uani 1 1 d . . . H3A H 0.3999 0.2833 0.2710 0.050 Uiso 1 1 calc R . . H3B H 0.4151 0.2116 0.3454 0.050 Uiso 1 1 calc R . . H3C H 0.4599 0.2811 0.3191 0.050 Uiso 1 1 calc R . . O4 O 0.49024(12) 0.7414(3) 0.35736(15) 0.0263(8) Uani 1 1 d . . . C4 C 0.35515(18) 0.4221(5) 0.3527(3) 0.0349(13) Uani 1 1 d . . . H4A H 0.3331 0.4090 0.3042 0.052 Uiso 1 1 calc R . . H4B H 0.3495 0.5076 0.3681 0.052 Uiso 1 1 calc R . . H4C H 0.3456 0.3603 0.3840 0.052 Uiso 1 1 calc R . . C5 C 0.35765(17) 0.4828(4) 0.1600(2) 0.0214(10) Uani 1 1 d . . . O5 O 0.55560(12) 0.8108(3) 0.30075(15) 0.0241(7) Uani 1 1 d . . . O6 O 0.57736(13) 0.7985(4) 0.42982(16) 0.0394(9) Uani 1 1 d . . . C6 C 0.37884(18) 0.3811(4) 0.1325(2) 0.0261(11) Uani 1 1 d . . . C7 C 0.34646(19) 0.2768(5) 0.1093(3) 0.0331(12) Uani 1 1 d . . . H7A H 0.3600 0.2067 0.0899 0.040 Uiso 1 1 calc R . . C8 C 0.2956(2) 0.2724(5) 0.1137(3) 0.0388(14) Uani 1 1 d . . . H8A H 0.2743 0.1996 0.0986 0.047 Uiso 1 1 calc R . . C9 C 0.27568(19) 0.3764(5) 0.1405(3) 0.0334(13) Uani 1 1 d . . . H9A H 0.2404 0.3737 0.1436 0.040 Uiso 1 1 calc R . . C10 C 0.30569(18) 0.4845(5) 0.1631(2) 0.0253(11) Uani 1 1 d . . . C11 C 0.28247(19) 0.5999(5) 0.1859(3) 0.0337(12) Uani 1 1 d . . . H11A H 0.2468 0.5811 0.1886 0.051 Uiso 1 1 calc R . . H11B H 0.2808 0.6678 0.1515 0.051 Uiso 1 1 calc R . . H11C H 0.3046 0.6268 0.2323 0.051 Uiso 1 1 calc R . . C12 C 0.43451(19) 0.3873(5) 0.1275(3) 0.0377(14) Uani 1 1 d . . . H12A H 0.4425 0.3100 0.1052 0.056 Uiso 1 1 calc R . . H12B H 0.4590 0.3952 0.1749 0.056 Uiso 1 1 calc R . . H12C H 0.4383 0.4606 0.0990 0.056 Uiso 1 1 calc R . . C13 C 0.36883(18) 0.8530(4) 0.3206(2) 0.0226(10) Uani 1 1 d . . . C14 C 0.37624(19) 0.8618(5) 0.3935(2) 0.0287(11) Uani 1 1 d . . . C15 C 0.3557(2) 0.9652(5) 0.4187(3) 0.0376(13) Uani 1 1 d . . . H15A H 0.3610 0.9738 0.4681 0.045 Uiso 1 1 calc R . . C16 C 0.3277(2) 1.0564(5) 0.3739(3) 0.0420(15) Uani 1 1 d . . . H16A H 0.3134 1.1263 0.3925 0.050 Uiso 1 1 calc R . . C17 C 0.32003(19) 1.0466(5) 0.3014(3) 0.0329(12) Uani 1 1 d . . . H17A H 0.3006 1.1099 0.2708 0.039 Uiso 1 1 calc R . . C18 C 0.34053(17) 0.9459(4) 0.2739(2) 0.0235(11) Uani 1 1 d . . . C19 C 0.3315(2) 0.9364(5) 0.1949(3) 0.0418(14) Uani 1 1 d . . . H19A H 0.2950 0.9601 0.1706 0.063 Uiso 1 1 calc R . . H19B H 0.3379 0.8495 0.1824 0.063 Uiso 1 1 calc R . . H19C H 0.3557 0.9936 0.1805 0.063 Uiso 1 1 calc R . . C20 C 0.4044(2) 0.7604(5) 0.4437(3) 0.0402(14) Uani 1 1 d . . . H20A H 0.3785 0.7093 0.4585 0.060 Uiso 1 1 calc R . . H20B H 0.4288 0.7997 0.4853 0.060 Uiso 1 1 calc R . . H20C H 0.4243 0.7063 0.4201 0.060 Uiso 1 1 calc R . . C21 C 0.5158(2) 0.9775(5) 0.3656(3) 0.0394(14) Uani 1 1 d . . . Mo1A Mo 0.066829(15) 0.52873(4) 0.23836(2) 0.01908(11) Uani 1 1 d . . . S1A S -0.03365(5) 0.35496(11) 0.13534(6) 0.0248(3) Uani 1 1 d . . . O1A O 0.0000 0.5742(4) 0.2500 0.0212(10) Uani 1 2 d S . . F1A F 0.00869(12) 0.1741(3) 0.08057(16) 0.0496(9) Uani 1 1 d . . . N1A N 0.07641(14) 0.6584(4) 0.19262(19) 0.0221(9) Uani 1 1 d . . . C1A C 0.09097(18) 0.7703(4) 0.1593(2) 0.0247(11) Uani 1 1 d . . . O2A O 0.11046(11) 0.5772(3) 0.32798(15) 0.0207(7) Uani 1 1 d . . . F2A F -0.05149(14) 0.1135(3) 0.1273(2) 0.0657(11) Uani 1 1 d . . . C2A C 0.05966(19) 0.7698(5) 0.0808(2) 0.0324(12) Uani 1 1 d . . . H2AA H 0.0678 0.6928 0.0584 0.049 Uiso 1 1 calc R . . H2AB H 0.0694 0.8439 0.0575 0.049 Uiso 1 1 calc R . . H2AC H 0.0218 0.7725 0.0764 0.049 Uiso 1 1 calc R . . O3A O 0.11562(12) 0.4172(3) 0.21614(15) 0.0262(7) Uani 1 1 d . . . F3A F 0.02578(13) 0.1638(3) 0.19334(16) 0.0454(8) Uani 1 1 d . . . C3A C 0.0780(2) 0.8877(5) 0.1965(3) 0.0341(13) Uani 1 1 d . . . H3AA H 0.0994 0.8875 0.2460 0.051 Uiso 1 1 calc R . . H3AB H 0.0405 0.8870 0.1943 0.051 Uiso 1 1 calc R . . H3AC H 0.0859 0.9637 0.1731 0.051 Uiso 1 1 calc R . . O4A O 0.01488(12) 0.4278(3) 0.14609(15) 0.0256(7) Uani 1 1 d . . . C4A C 0.15030(18) 0.7653(5) 0.1669(3) 0.0308(12) Uani 1 1 d . . . H4AA H 0.1700 0.7680 0.2171 0.046 Uiso 1 1 calc R . . H4AB H 0.1602 0.8378 0.1426 0.046 Uiso 1 1 calc R . . H4AC H 0.1586 0.6869 0.1460 0.046 Uiso 1 1 calc R . . O5A O -0.05377(12) 0.3579(3) 0.19687(15) 0.0220(7) Uani 1 1 d . . . C5A C 0.14352(18) 0.6785(4) 0.3525(2) 0.0233(10) Uani 1 1 d . . . O6A O -0.07089(13) 0.3739(3) 0.06857(17) 0.0377(9) Uani 1 1 d . . . C6A C 0.12418(19) 0.7826(4) 0.3797(2) 0.0273(11) Uani 1 1 d . . . C7A C 0.1579(2) 0.8841(5) 0.4034(3) 0.0346(13) Uani 1 1 d . . . H7AA H 0.1452 0.9572 0.4213 0.042 Uiso 1 1 calc R . . C8A C 0.2096(2) 0.8794(5) 0.4013(3) 0.0414(14) Uani 1 1 d . . . H8AA H 0.2323 0.9494 0.4174 0.050 Uiso 1 1 calc R . . C9A C 0.2283(2) 0.7746(6) 0.3762(3) 0.0389(14) Uani 1 1 d . . . H9AA H 0.2641 0.7729 0.3754 0.047 Uiso 1 1 calc R . . C10A C 0.19630(19) 0.6698(5) 0.3517(2) 0.0282(11) Uani 1 1 d . . . C11A C 0.21637(19) 0.5536(5) 0.3248(3) 0.0380(13) Uani 1 1 d . . . H11D H 0.2544 0.5617 0.3316 0.057 Uiso 1 1 calc R . . H11E H 0.1983 0.5431 0.2745 0.057 Uiso 1 1 calc R . . H11F H 0.2095 0.4798 0.3509 0.057 Uiso 1 1 calc R . . C12A C 0.06767(18) 0.7823(5) 0.3821(3) 0.0337(13) Uani 1 1 d . . . H12D H 0.0441 0.7739 0.3341 0.051 Uiso 1 1 calc R . . H12E H 0.0601 0.8616 0.4029 0.051 Uiso 1 1 calc R . . H12F H 0.0621 0.7112 0.4109 0.051 Uiso 1 1 calc R . . C13A C 0.13375(17) 0.3170(4) 0.1862(2) 0.0210(10) Uani 1 1 d . . . C14A C 0.12998(18) 0.3195(5) 0.1140(2) 0.0255(11) Uani 1 1 d . . . C15A C 0.1495(2) 0.2174(5) 0.0861(3) 0.0363(13) Uani 1 1 d . . . H15B H 0.1462 0.2154 0.0369 0.044 Uiso 1 1 calc R . . C16A C 0.1737(2) 0.1186(5) 0.1277(3) 0.0405(14) Uani 1 1 d . . . H16B H 0.1874 0.0498 0.1075 0.049 Uiso 1 1 calc R . . C17A C 0.17812(19) 0.1194(5) 0.1991(3) 0.0340(13) Uani 1 1 d . . . H17B H 0.1952 0.0511 0.2278 0.041 Uiso 1 1 calc R . . C18A C 0.15806(18) 0.2178(4) 0.2296(3) 0.0285(11) Uani 1 1 d . . . C19A C 0.1642(2) 0.2162(5) 0.3090(3) 0.0441(15) Uani 1 1 d . . . H19D H 0.1475 0.1401 0.3210 0.066 Uiso 1 1 calc R . . H19E H 0.1473 0.2913 0.3219 0.066 Uiso 1 1 calc R . . H19F H 0.2018 0.2162 0.3349 0.066 Uiso 1 1 calc R . . C20A C 0.1069(2) 0.4306(5) 0.0679(2) 0.0361(13) Uani 1 1 d . . . H20D H 0.1120 0.4191 0.0210 0.054 Uiso 1 1 calc R . . H20E H 0.1245 0.5083 0.0892 0.054 Uiso 1 1 calc R . . H20F H 0.0690 0.4366 0.0634 0.054 Uiso 1 1 calc R . . C21A C -0.0116(2) 0.1916(5) 0.1346(3) 0.0360(13) Uani 1 1 d . . . C1S C 0.1968(3) 0.7354(9) -0.0026(3) 0.066(2) Uani 1 1 d . . . H1SA H 0.1608 0.7560 -0.0080 0.079 Uiso 1 1 calc R . . C2S C 0.2100(3) 0.6133(8) -0.0124(3) 0.064(2) Uani 1 1 d . . . H2SA H 0.1835 0.5498 -0.0249 0.076 Uiso 1 1 calc R . . C3S C 0.2621(3) 0.5838(6) -0.0038(3) 0.0546(17) Uani 1 1 d . . . H3SA H 0.2719 0.4991 -0.0099 0.065 Uiso 1 1 calc R . . C4S C 0.2998(2) 0.6759(7) 0.0133(3) 0.0494(17) Uani 1 1 d . . . H4SA H 0.3358 0.6550 0.0189 0.059 Uiso 1 1 calc R . . C5S C 0.2863(3) 0.7972(7) 0.0225(3) 0.0487(16) Uani 1 1 d . . . H5SA H 0.3128 0.8606 0.0342 0.058 Uiso 1 1 calc R . . C6S C 0.2342(3) 0.8287(7) 0.0150(3) 0.0593(19) Uani 1 1 d . . . H6SA H 0.2246 0.9132 0.0219 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 0.0207(2) 0.0230(2) 0.0132(2) 0.00071(17) 0.00765(16) 0.00145(17) S1 0.0280(7) 0.0299(7) 0.0209(6) -0.0082(5) 0.0078(5) -0.0011(5) O1 0.017(2) 0.031(3) 0.014(2) 0.000 0.0052(18) 0.000 N1 0.020(2) 0.027(2) 0.017(2) 0.0029(16) 0.0079(16) 0.0005(16) F1 0.062(2) 0.0346(19) 0.109(3) -0.027(2) 0.039(2) -0.0173(17) C1 0.022(2) 0.031(3) 0.024(3) 0.012(2) 0.013(2) 0.002(2) O2 0.0190(16) 0.0244(17) 0.0178(16) 0.0004(13) 0.0087(13) 0.0003(13) F2 0.073(3) 0.059(2) 0.053(2) -0.0267(18) 0.031(2) 0.0026(19) C2 0.026(3) 0.050(3) 0.025(3) 0.011(2) 0.012(2) 0.005(2) O3 0.0303(18) 0.0298(18) 0.0206(17) 0.0006(15) 0.0103(14) 0.0091(15) F3 0.057(2) 0.0360(18) 0.054(2) -0.0016(16) 0.0201(18) 0.0113(16) C3 0.034(3) 0.023(3) 0.045(3) 0.004(2) 0.014(2) -0.003(2) O4 0.0311(19) 0.0340(19) 0.0173(17) -0.0050(14) 0.0123(14) -0.0037(15) C4 0.025(3) 0.048(3) 0.035(3) 0.014(3) 0.014(2) 0.000(2) C5 0.021(2) 0.024(2) 0.019(2) 0.005(2) 0.0050(19) -0.001(2) O5 0.0277(18) 0.0275(18) 0.0196(17) -0.0034(14) 0.0107(14) 0.0006(15) O6 0.034(2) 0.062(3) 0.0188(18) -0.0091(18) 0.0025(16) 0.0022(19) C6 0.023(3) 0.030(3) 0.024(3) 0.000(2) 0.004(2) 0.001(2) C7 0.033(3) 0.029(3) 0.036(3) -0.004(2) 0.008(2) -0.003(2) C8 0.032(3) 0.036(3) 0.045(3) 0.001(3) 0.006(3) -0.013(2) C9 0.017(3) 0.047(3) 0.038(3) 0.006(3) 0.012(2) -0.007(2) C10 0.022(2) 0.037(3) 0.020(3) 0.005(2) 0.011(2) 0.001(2) C11 0.025(3) 0.054(3) 0.025(3) 0.008(3) 0.013(2) 0.003(2) C12 0.027(3) 0.044(3) 0.042(3) -0.017(3) 0.010(2) -0.003(2) C13 0.024(2) 0.024(3) 0.023(3) -0.006(2) 0.012(2) 0.001(2) C14 0.030(3) 0.035(3) 0.023(3) -0.005(2) 0.012(2) 0.000(2) C15 0.045(3) 0.050(4) 0.025(3) -0.011(3) 0.021(3) -0.006(3) C16 0.050(4) 0.031(3) 0.055(4) -0.018(3) 0.032(3) -0.010(3) C17 0.032(3) 0.023(3) 0.045(3) 0.001(2) 0.015(3) 0.004(2) C18 0.020(2) 0.028(3) 0.027(3) -0.001(2) 0.013(2) 0.002(2) C19 0.044(3) 0.054(4) 0.027(3) 0.011(3) 0.011(3) 0.016(3) C20 0.045(3) 0.058(4) 0.022(3) -0.002(3) 0.017(3) 0.005(3) C21 0.042(3) 0.037(3) 0.044(4) -0.015(3) 0.019(3) -0.007(3) Mo1A 0.0209(2) 0.0232(2) 0.0146(2) 0.00084(17) 0.00739(16) 0.00097(17) S1A 0.0267(6) 0.0260(6) 0.0203(6) -0.0051(5) 0.0042(5) 0.0009(5) O1A 0.019(2) 0.031(3) 0.013(2) 0.000 0.0044(18) 0.000 F1A 0.057(2) 0.054(2) 0.0405(19) -0.0171(16) 0.0181(16) 0.0116(17) N1A 0.017(2) 0.034(2) 0.018(2) -0.0021(17) 0.0083(16) -0.0011(17) C1A 0.030(3) 0.027(3) 0.018(2) 0.002(2) 0.008(2) 0.001(2) O2A 0.0232(17) 0.0218(17) 0.0181(16) 0.0013(13) 0.0074(13) -0.0039(13) F2A 0.056(2) 0.0310(18) 0.116(3) -0.028(2) 0.035(2) -0.0135(17) C2A 0.036(3) 0.041(3) 0.020(3) 0.009(2) 0.007(2) 0.004(2) O3A 0.0311(19) 0.0286(18) 0.0196(17) -0.0006(14) 0.0084(14) 0.0064(15) F3A 0.060(2) 0.0352(18) 0.0411(19) 0.0006(14) 0.0145(17) 0.0221(16) C3A 0.036(3) 0.032(3) 0.036(3) -0.004(2) 0.014(2) 0.002(2) O4A 0.0345(19) 0.0307(19) 0.0147(16) -0.0046(14) 0.0118(14) -0.0042(15) C4A 0.027(3) 0.037(3) 0.032(3) 0.001(2) 0.013(2) 0.000(2) O5A 0.0252(17) 0.0265(18) 0.0182(17) -0.0012(14) 0.0123(14) -0.0027(14) C5A 0.025(3) 0.028(3) 0.016(2) 0.002(2) 0.004(2) -0.003(2) O6A 0.036(2) 0.053(2) 0.0204(18) -0.0038(17) 0.0013(16) 0.0063(18) C6A 0.033(3) 0.027(3) 0.021(3) 0.000(2) 0.006(2) -0.005(2) C7A 0.044(3) 0.032(3) 0.028(3) -0.002(2) 0.010(2) -0.002(2) C8A 0.040(3) 0.048(4) 0.034(3) -0.004(3) 0.007(3) -0.020(3) C9A 0.025(3) 0.064(4) 0.028(3) 0.002(3) 0.009(2) -0.012(3) C10A 0.027(3) 0.034(3) 0.024(3) 0.005(2) 0.008(2) -0.001(2) C11A 0.023(3) 0.061(4) 0.033(3) 0.006(3) 0.013(2) 0.008(3) C12A 0.030(3) 0.034(3) 0.038(3) -0.006(2) 0.011(2) 0.002(2) C13A 0.019(2) 0.026(3) 0.025(3) -0.003(2) 0.017(2) -0.004(2) C14A 0.024(3) 0.032(3) 0.026(3) -0.002(2) 0.015(2) -0.004(2) C15A 0.037(3) 0.041(3) 0.035(3) -0.013(3) 0.017(3) -0.011(3) C16A 0.038(3) 0.030(3) 0.062(4) -0.016(3) 0.027(3) -0.004(2) C17A 0.028(3) 0.029(3) 0.049(4) 0.000(3) 0.016(3) 0.001(2) C18A 0.024(3) 0.027(3) 0.035(3) -0.002(2) 0.010(2) 0.000(2) C19A 0.047(4) 0.046(4) 0.039(3) 0.011(3) 0.011(3) 0.017(3) C20A 0.044(3) 0.049(3) 0.019(3) 0.003(2) 0.016(2) 0.001(3) C21A 0.043(3) 0.027(3) 0.041(3) -0.012(3) 0.016(3) -0.002(3) C1S 0.042(4) 0.134(7) 0.021(3) 0.004(4) 0.008(3) 0.010(5) C2S 0.056(5) 0.113(7) 0.022(3) 0.000(4) 0.012(3) -0.040(4) C3S 0.075(5) 0.065(4) 0.026(3) 0.001(3) 0.017(3) -0.006(4) C4S 0.035(3) 0.099(6) 0.016(3) 0.007(3) 0.011(2) -0.002(4) C5S 0.062(4) 0.068(4) 0.020(3) 0.007(3) 0.020(3) -0.022(4) C6S 0.084(5) 0.076(5) 0.020(3) 0.010(3) 0.018(3) 0.015(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 N1 1.717(4) . ? Mo1 O2 1.885(3) . ? Mo1 O3 1.887(3) . ? Mo1 O1 1.9025(12) . ? Mo1 O4 2.222(3) . ? Mo1 O5 2.315(3) 2_655 ? S1 O6 1.418(3) . ? S1 O5 1.459(3) . ? S1 O4 1.460(3) . ? S1 C21 1.820(6) . ? O1 Mo1 1.9025(12) 2_655 ? N1 C1 1.465(5) . ? F1 C21 1.323(6) . ? C1 C3 1.518(7) . ? C1 C4 1.536(6) . ? C1 C2 1.547(6) . ? O2 C5 1.373(5) . ? F2 C21 1.334(6) . ? O3 C13 1.364(5) . ? F3 C21 1.314(6) . ? C5 C10 1.391(6) . ? C5 C6 1.393(6) . ? O5 Mo1 2.315(3) 2_655 ? C6 C7 1.392(6) . ? C6 C12 1.502(7) . ? C7 C8 1.372(7) . ? C8 C9 1.389(7) . ? C9 C10 1.391(7) . ? C10 C11 1.493(7) . ? C13 C14 1.399(6) . ? C13 C18 1.410(6) . ? C14 C15 1.376(7) . ? C14 C20 1.508(7) . ? C15 C16 1.376(8) . ? C16 C17 1.393(7) . ? C17 C18 1.377(6) . ? C18 C19 1.513(6) . ? Mo1A N1A 1.701(4) . ? Mo1A O2A 1.889(3) . ? Mo1A O3A 1.889(3) . ? Mo1A O1A 1.9052(12) . ? Mo1A O4A 2.220(3) . ? Mo1A O5A 2.297(3) 2 ? S1A O6A 1.418(3) . ? S1A O5A 1.458(3) . ? S1A O4A 1.459(3) . ? S1A C21A 1.826(5) . ? O1A Mo1A 1.9052(12) 2 ? F1A C21A 1.336(6) . ? N1A C1A 1.460(6) . ? C1A C3A 1.532(6) . ? C1A C4A 1.532(6) . ? C1A C2A 1.536(6) . ? O2A C5A 1.381(5) . ? F2A C21A 1.314(6) . ? O3A C13A 1.365(5) . ? F3A C21A 1.327(6) . ? O5A Mo1A 2.297(3) 2 ? C5A C6A 1.386(6) . ? C5A C10A 1.401(6) . ? C6A C7A 1.389(7) . ? C6A C12A 1.507(7) . ? C7A C8A 1.380(7) . ? C8A C9A 1.362(7) . ? C9A C10A 1.396(7) . ? C10A C11A 1.495(7) . ? C13A C18A 1.392(6) . ? C13A C14A 1.402(6) . ? C14A C15A 1.379(7) . ? C14A C20A 1.507(7) . ? C15A C16A 1.372(7) . ? C16A C17A 1.381(7) . ? C17A C18A 1.382(7) . ? C18A C19A 1.530(7) . ? C1S C2S 1.367(10) . ? C1S C6S 1.372(9) . ? C2S C3S 1.375(9) . ? C3S C4S 1.367(8) . ? C4S C5S 1.358(9) . ? C5S C6S 1.383(9) . ? 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 N1 Mo1 O2 98.44(15) . . ? N1 Mo1 O3 98.61(15) . . ? O2 Mo1 O3 96.57(13) . . ? N1 Mo1 O1 99.49(16) . . ? O2 Mo1 O1 98.44(10) . . ? O3 Mo1 O1 154.44(16) . . ? N1 Mo1 O4 94.18(14) . . ? O2 Mo1 O4 167.27(12) . . ? O3 Mo1 O4 79.83(12) . . ? O1 Mo1 O4 81.00(10) . . ? N1 Mo1 O5 179.52(14) . 2_655 ? O2 Mo1 O5 81.19(12) . 2_655 ? O3 Mo1 O5 81.75(12) . 2_655 ? O1 Mo1 O5 80.26(13) . 2_655 ? O4 Mo1 O5 86.19(11) . 2_655 ? O6 S1 O5 117.0(2) . . ? O6 S1 O4 114.3(2) . . ? O5 S1 O4 112.15(18) . . ? O6 S1 C21 105.2(2) . . ? O5 S1 C21 102.9(2) . . ? O4 S1 C21 103.4(2) . . ? Mo1 O1 Mo1 151.8(2) 2_655 . ? C1 N1 Mo1 171.1(3) . . ? N1 C1 C3 108.1(4) . . ? N1 C1 C4 107.3(4) . . ? C3 C1 C4 112.0(4) . . ? N1 C1 C2 107.7(4) . . ? C3 C1 C2 111.8(4) . . ? C4 C1 C2 109.7(4) . . ? C5 O2 Mo1 133.8(3) . . ? C13 O3 Mo1 160.5(3) . . ? S1 O4 Mo1 133.65(18) . . ? O2 C5 C10 119.3(4) . . ? O2 C5 C6 118.1(4) . . ? C10 C5 C6 122.5(4) . . ? S1 O5 Mo1 129.92(19) . 2_655 ? C7 C6 C5 117.6(4) . . ? C7 C6 C12 122.3(5) . . ? C5 C6 C12 120.0(4) . . ? C8 C7 C6 121.9(5) . . ? C7 C8 C9 118.7(5) . . ? C8 C9 C10 122.1(5) . . ? C9 C10 C5 117.1(4) . . ? C9 C10 C11 121.6(4) . . ? C5 C10 C11 121.2(4) . . ? O3 C13 C14 120.1(4) . . ? O3 C13 C18 118.5(4) . . ? C14 C13 C18 121.4(4) . . ? C15 C14 C13 118.1(5) . . ? C15 C14 C20 120.0(4) . . ? C13 C14 C20 121.9(4) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C17 120.3(5) . . ? C18 C17 C16 120.4(5) . . ? C17 C18 C13 118.5(4) . . ? C17 C18 C19 119.6(4) . . ? C13 C18 C19 121.9(4) . . ? F3 C21 F1 107.9(5) . . ? F3 C21 F2 108.3(5) . . ? F1 C21 F2 107.4(4) . . ? F3 C21 S1 112.3(4) . . ? F1 C21 S1 110.6(4) . . ? F2 C21 S1 110.2(4) . . ? N1A Mo1A O2A 97.78(15) . . ? N1A Mo1A O3A 99.64(15) . . ? O2A Mo1A O3A 96.46(13) . . ? N1A Mo1A O1A 98.19(16) . . ? O2A Mo1A O1A 99.11(10) . . ? O3A Mo1A O1A 154.45(15) . . ? N1A Mo1A O4A 95.90(14) . . ? O2A Mo1A O4A 166.16(12) . . ? O3A Mo1A O4A 79.15(12) . . ? O1A Mo1A O4A 80.94(11) . . ? N1A Mo1A O5A 178.13(14) . 2 ? O2A Mo1A O5A 80.81(11) . 2 ? O3A Mo1A O5A 81.77(12) . 2 ? O1A Mo1A O5A 80.88(13) . 2 ? O4A Mo1A O5A 85.56(11) . 2 ? O6A S1A O5A 116.8(2) . . ? O6A S1A O4A 114.2(2) . . ? O5A S1A O4A 112.34(18) . . ? O6A S1A C21A 105.4(2) . . ? O5A S1A C21A 102.7(2) . . ? O4A S1A C21A 103.5(2) . . ? Mo1A O1A Mo1A 150.7(2) 2 . ? C1A N1A Mo1A 173.1(3) . . ? N1A C1A C3A 108.6(4) . . ? N1A C1A C4A 108.7(4) . . ? C3A C1A C4A 110.0(4) . . ? N1A C1A C2A 108.5(4) . . ? C3A C1A C2A 111.0(4) . . ? C4A C1A C2A 110.0(4) . . ? C5A O2A Mo1A 134.1(3) . . ? C13A O3A Mo1A 158.8(3) . . ? S1A O4A Mo1A 133.40(18) . . ? S1A O5A Mo1A 128.93(18) . 2 ? O2A C5A C6A 119.2(4) . . ? O2A C5A C10A 118.5(4) . . ? C6A C5A C10A 122.2(4) . . ? C5A C6A C7A 118.3(5) . . ? C5A C6A C12A 119.2(4) . . ? C7A C6A C12A 122.5(5) . . ? C8A C7A C6A 120.5(5) . . ? C9A C8A C7A 120.2(5) . . ? C8A C9A C10A 121.9(5) . . ? C9A C10A C5A 116.7(5) . . ? C9A C10A C11A 122.5(5) . . ? C5A C10A C11A 120.8(4) . . ? O3A C13A C18A 118.5(4) . . ? O3A C13A C14A 119.5(4) . . ? C18A C13A C14A 121.9(4) . . ? C15A C14A C13A 117.7(5) . . ? C15A C14A C20A 120.2(4) . . ? C13A C14A C20A 122.0(4) . . ? C16A C15A C14A 121.5(5) . . ? C15A C16A C17A 119.8(5) . . ? C16A C17A C18A 121.2(5) . . ? C17A C18A C13A 117.9(5) . . ? C17A C18A C19A 119.7(4) . . ? C13A C18A C19A 122.4(4) . . ? F2A C21A F3A 109.3(5) . . ? F2A C21A F1A 108.4(4) . . ? F3A C21A F1A 107.5(4) . . ? F2A C21A S1A 110.5(4) . . ? F3A C21A S1A 111.3(3) . . ? F1A C21A S1A 109.8(4) . . ? C2S C1S C6S 121.5(7) . . ? C1S C2S C3S 119.0(7) . . ? C4S C3S C2S 120.2(7) . . ? C5S C4S C3S 120.5(6) . . ? C4S C5S C6S 120.3(6) . . ? C1S C6S C5S 118.5(7) . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 1.171 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.112