#Supplementary Material (ESI) for Dalton Transactions #This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Daran, Jean-Claude' _publ_contact_author_email NATALIABELK@INEOS.AC.RU _publ_section_title ; Hydrogen bonding to carbonyl hydride complex Cp*Mo(PMe3)2(CO)H and its role in proton transfer ; loop_ _publ_author_name 'Natalia Belkova' 'Jean-Claude Daran' 'Pavel A. Dub' 'Lina M. Epstein' 'Oleg Filippov' 'Rinaldo Poli' ; E.S.Shubina ; # Attachment 'MoHCO.cif' data_Pd6 _database_code_depnum_ccdc_archive 'CCDC 742724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 F27 Mo O4 P3' _chemical_formula_weight 1194.52 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P b c a' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.2134(4) _cell_length_b 20.3539(6) _cell_length_c 27.5461(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9090.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17231 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 32.08 _exptl_crystal_description box _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4784 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.558 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm, CrysAlis RED (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean 8.2632 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66640 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9284 _reflns_number_gt 4672 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0656P)^2^+124.5900P] 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 9284 _refine_ls_number_parameters 602 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1917 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2715 _refine_ls_wR_factor_gt 0.1871 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.002 _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 0.77527(4) 0.90685(4) 0.65785(3) 0.0321(2) Uani 1 1 d . . . P1 P 0.76344(19) 0.84145(15) 0.58046(10) 0.0553(8) Uani 1 1 d . . . P2 P 0.63777(16) 0.94906(15) 0.63459(10) 0.0495(7) Uani 1 1 d . . . P3 P 0.78421(19) 0.79794(14) 0.69526(11) 0.0546(7) Uani 1 1 d . . . C1 C 0.7079(7) 0.9075(6) 0.7156(4) 0.059(3) Uani 1 1 d . . . O1 O 0.6715(6) 0.9113(5) 0.7518(3) 0.078(3) Uani 1 1 d . . . C11 C 0.8792(6) 0.9561(5) 0.7023(4) 0.046(2) Uani 1 1 d . . . C12 C 0.8313(5) 1.0057(5) 0.6825(4) 0.047(2) Uani 1 1 d . . . C13 C 0.8396(5) 1.0042(5) 0.6310(4) 0.040(2) Uani 1 1 d . . . C14 C 0.8977(6) 0.9542(5) 0.6213(4) 0.047(3) Uani 1 1 d . . . C15 C 0.9204(6) 0.9226(5) 0.6640(4) 0.048(2) Uani 1 1 d . . . C16 C 0.8996(9) 0.9506(7) 0.7558(4) 0.082(4) Uani 1 1 d . . . H16A H 0.9387 0.9840 0.7645 0.123 Uiso 1 1 calc R . . H16B H 0.9229 0.9081 0.7623 0.123 Uiso 1 1 calc R . . H16C H 0.8502 0.9561 0.7746 0.123 Uiso 1 1 calc R . . C17 C 0.7924(8) 1.0595(5) 0.7124(5) 0.069(3) Uani 1 1 d . . . H17A H 0.7597 1.0404 0.7378 0.103 Uiso 1 1 calc R . . H17B H 0.7580 1.0862 0.6920 0.103 Uiso 1 1 calc R . . H17C H 0.8349 1.0863 0.7265 0.103 Uiso 1 1 calc R . . C18 C 0.8091(8) 1.0554(6) 0.5972(5) 0.070(4) Uani 1 1 d . . . H18A H 0.8470 1.0917 0.5968 0.105 Uiso 1 1 calc R . . H18B H 0.7559 1.0704 0.6077 0.105 Uiso 1 1 calc R . . H18C H 0.8048 1.0373 0.5651 0.105 Uiso 1 1 calc R . . C19 C 0.9416(7) 0.9468(7) 0.5734(4) 0.071(4) Uani 1 1 d . . . H19A H 0.9945 0.9679 0.5752 0.107 Uiso 1 1 calc R . . H19B H 0.9094 0.9669 0.5482 0.107 Uiso 1 1 calc R . . H19C H 0.9490 0.9010 0.5663 0.107 Uiso 1 1 calc R . . C20 C 0.9895(6) 0.8755(6) 0.6692(5) 0.074(4) Uani 1 1 d . . . H20A H 0.9911 0.8472 0.6413 0.111 Uiso 1 1 calc R . . H20B H 0.9816 0.8496 0.6979 0.111 Uiso 1 1 calc R . . H20C H 1.0405 0.8992 0.6716 0.111 Uiso 1 1 calc R . . C111 C 0.8516(8) 0.7906(7) 0.5643(5) 0.076(4) Uani 1 1 d . . . H11A H 0.8490 0.7499 0.5818 0.114 Uiso 1 1 calc R . . H11B H 0.9016 0.8133 0.5726 0.114 Uiso 1 1 calc R . . H11C H 0.8507 0.7819 0.5301 0.114 Uiso 1 1 calc R . . C112 C 0.6777(9) 0.7851(8) 0.5707(5) 0.096(5) Uani 1 1 d . . . H11D H 0.6752 0.7732 0.5371 0.144 Uiso 1 1 calc R . . H11E H 0.6271 0.8062 0.5800 0.144 Uiso 1 1 calc R . . H11F H 0.6856 0.7464 0.5901 0.144 Uiso 1 1 calc R . . C113 C 0.7580(9) 0.8899(8) 0.5243(4) 0.086(4) Uani 1 1 d . . . H11G H 0.7631 0.8611 0.4969 0.130 Uiso 1 1 calc R . . H11H H 0.8020 0.9214 0.5239 0.130 Uiso 1 1 calc R . . H11I H 0.7060 0.9123 0.5229 0.130 Uiso 1 1 calc R . . C231 C 0.6048(8) 1.0209(6) 0.6686(5) 0.080(4) Uani 1 1 d . . . H23A H 0.6381 1.0579 0.6596 0.121 Uiso 1 1 calc R . . H23B H 0.6108 1.0125 0.7027 0.121 Uiso 1 1 calc R . . H23C H 0.5480 1.0300 0.6615 0.121 Uiso 1 1 calc R . . C232 C 0.5522(7) 0.8944(7) 0.6481(6) 0.084(4) Uani 1 1 d . . . H23D H 0.5011 0.9174 0.6437 0.127 Uiso 1 1 calc R . . H23E H 0.5564 0.8796 0.6812 0.127 Uiso 1 1 calc R . . H23F H 0.5540 0.8572 0.6267 0.127 Uiso 1 1 calc R . . C233 C 0.6084(8) 0.9734(8) 0.5738(4) 0.086(5) Uani 1 1 d . . . H23G H 0.6073 0.9354 0.5532 0.129 Uiso 1 1 calc R . . H23H H 0.6476 1.0045 0.5615 0.129 Uiso 1 1 calc R . . H23I H 0.5546 0.9931 0.5746 0.129 Uiso 1 1 calc R . . C321 C 0.6862(9) 0.7570(7) 0.7043(6) 0.096(5) Uani 1 1 d . . . H32A H 0.6951 0.7155 0.7201 0.144 Uiso 1 1 calc R . . H32B H 0.6601 0.7498 0.6735 0.144 Uiso 1 1 calc R . . H32C H 0.6513 0.7839 0.7242 0.144 Uiso 1 1 calc R . . C322 C 0.8212(10) 0.7985(7) 0.7576(5) 0.091(5) Uani 1 1 d . . . H32D H 0.7881 0.8280 0.7765 0.137 Uiso 1 1 calc R . . H32E H 0.8776 0.8128 0.7582 0.137 Uiso 1 1 calc R . . H32F H 0.8174 0.7550 0.7709 0.137 Uiso 1 1 calc R . . C323 C 0.8463(10) 0.7297(7) 0.6726(6) 0.099(5) Uani 1 1 d . . . H32G H 0.8504 0.6964 0.6972 0.148 Uiso 1 1 calc R . . H32H H 0.9005 0.7452 0.6644 0.148 Uiso 1 1 calc R . . H32I H 0.8206 0.7115 0.6442 0.148 Uiso 1 1 calc R . . O2 O 0.7592(5) 0.7738(3) 0.9533(2) 0.0503(17) Uani 1 1 d . . . H2 H 0.7274 0.7561 0.9343 0.075 Uiso 1 1 calc R . . C21 C 0.7648(7) 0.8393(5) 0.9426(4) 0.049(3) Uani 1 1 d . . . C211 C 0.6859(10) 0.8744(7) 0.9585(5) 0.079(4) Uani 1 1 d . . . C212 C 0.8395(9) 0.8653(6) 0.9732(5) 0.074(4) Uani 1 1 d . . . C213 C 0.7826(10) 0.8508(6) 0.8888(4) 0.070(4) Uani 1 1 d . . . F21 F 0.6290(5) 0.8679(5) 0.9245(3) 0.108(3) Uani 1 1 d . . . F22 F 0.7005(6) 0.9385(4) 0.9641(3) 0.107(3) Uani 1 1 d . . . F23 F 0.6584(5) 0.8531(4) 0.9993(3) 0.097(3) Uani 1 1 d . . . F24 F 0.8627(6) 0.9237(4) 0.9611(4) 0.120(4) Uani 1 1 d . . . F25 F 0.8171(5) 0.8650(4) 1.0200(3) 0.088(2) Uani 1 1 d . . . F26 F 0.9012(5) 0.8259(4) 0.9697(3) 0.094(2) Uani 1 1 d . . . F27 F 0.7306(5) 0.8177(3) 0.8618(2) 0.082(2) Uani 1 1 d . . . F28 F 0.7730(6) 0.9140(3) 0.8773(2) 0.101(3) Uani 1 1 d . . . F29 F 0.8611(6) 0.8338(4) 0.8779(3) 0.098(3) Uani 1 1 d . . . O3 O 0.7110(4) 0.6809(3) 0.8997(2) 0.0396(15) Uani 1 1 d . . . C31 C 0.6377(5) 0.6538(5) 0.8892(4) 0.041(2) Uani 1 1 d . . . C311 C 0.6093(6) 0.6752(6) 0.8377(4) 0.052(3) Uani 1 1 d . . . C312 C 0.5716(6) 0.6744(8) 0.9255(5) 0.067(3) Uani 1 1 d . . . C313 C 0.6460(7) 0.5782(6) 0.8885(5) 0.063(3) Uani 1 1 d . . . F31 F 0.6710(5) 0.6709(5) 0.8064(2) 0.093(3) Uani 1 1 d . . . F32 F 0.5489(5) 0.6403(4) 0.8187(3) 0.088(2) Uani 1 1 d . . . F33 F 0.5847(5) 0.7359(3) 0.8369(3) 0.094(3) Uani 1 1 d . . . F34 F 0.4954(4) 0.6601(4) 0.9108(3) 0.088(2) Uani 1 1 d . . . F35 F 0.5726(5) 0.7365(5) 0.9328(4) 0.124(4) Uani 1 1 d . . . F36 F 0.5810(5) 0.6446(7) 0.9667(3) 0.135(4) Uani 1 1 d . . . F37 F 0.6868(5) 0.5575(3) 0.8497(3) 0.087(2) Uani 1 1 d . . . F38 F 0.6866(5) 0.5577(3) 0.9261(3) 0.093(3) Uani 1 1 d . . . F39 F 0.5750(5) 0.5469(4) 0.8877(3) 0.096(3) Uani 1 1 d . . . O4 O 0.8393(4) 0.6800(4) 0.8468(3) 0.0551(19) Uani 1 1 d D A . H4 H 0.8045 0.6725 0.8676 0.083 Uiso 1 1 calc R . . C41 C 0.9075(6) 0.6435(5) 0.8557(4) 0.054(3) Uani 1 1 d D . . C421 C 0.8950(11) 0.5685(10) 0.8422(6) 0.133(6) Uani 0.50 1 d PD A 1 C422 C 0.9395(11) 0.6504(9) 0.9099(7) 0.133(6) Uani 0.50 1 d PD A 1 C423 C 0.9797(11) 0.6769(9) 0.8252(7) 0.133(6) Uani 0.50 1 d PD A 1 F41 F 0.8565(10) 0.5734(8) 0.7987(6) 0.0928(15) Uani 0.50 1 d PD A 1 F42 F 0.8538(10) 0.5414(8) 0.8815(7) 0.0928(15) Uani 0.50 1 d PD A 1 F43 F 0.9714(9) 0.5472(8) 0.8281(6) 0.0928(15) Uani 0.50 1 d PD A 1 F44 F 0.8740(10) 0.6420(8) 0.9392(6) 0.0928(15) Uani 0.50 1 d PD A 1 F45 F 0.9733(10) 0.7124(8) 0.9180(7) 0.0928(15) Uani 0.50 1 d PD A 1 F46 F 0.9874(10) 0.5963(8) 0.9207(7) 0.0928(15) Uani 0.50 1 d PD A 1 F47 F 0.9768(10) 0.7412(8) 0.8308(7) 0.0928(15) Uani 0.50 1 d PD A 1 F48 F 0.9620(10) 0.6668(9) 0.7781(6) 0.0928(15) Uani 0.50 1 d PD A 1 F49 F 1.0518(9) 0.6592(9) 0.8439(7) 0.0928(15) Uani 0.50 1 d PD A 1 C424 C 0.8867(11) 0.5670(9) 0.8632(6) 0.133(6) Uani 0.50 1 d PD A 2 C425 C 0.9539(11) 0.6696(9) 0.9023(7) 0.133(6) Uani 0.50 1 d PD A 2 C426 C 0.9684(11) 0.6516(10) 0.8107(7) 0.133(6) Uani 0.50 1 d PD A 2 F41B F 0.8383(10) 0.5529(8) 0.8236(6) 0.0928(15) Uani 0.50 1 d PD A 2 F42B F 0.8595(10) 0.5663(8) 0.9119(6) 0.0928(15) Uani 0.50 1 d PD A 2 F43B F 0.9579(10) 0.5342(8) 0.8493(6) 0.0928(15) Uani 0.50 1 d PD A 2 F44B F 0.8938(10) 0.6738(8) 0.9369(6) 0.0928(15) Uani 0.50 1 d PD A 2 F45B F 0.9871(9) 0.7280(7) 0.8850(7) 0.0928(15) Uani 0.50 1 d PD A 2 F46B F 1.0016(10) 0.6189(8) 0.9194(7) 0.0928(15) Uani 0.50 1 d PD A 2 F47B F 0.9718(9) 0.7162(9) 0.8025(6) 0.096(3) Uani 0.50 1 d PD A 2 F48B F 0.9305(9) 0.6164(10) 0.7753(6) 0.096(3) Uani 0.50 1 d PD A 2 F49B F 1.0443(8) 0.6369(10) 0.8246(6) 0.096(3) Uani 0.50 1 d PD A 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 0.0313(4) 0.0362(4) 0.0288(4) 0.0015(3) 0.0012(3) 0.0042(3) P1 0.0594(18) 0.0618(18) 0.0448(15) -0.0150(14) -0.0047(13) 0.0022(15) P2 0.0346(13) 0.0611(18) 0.0529(16) -0.0001(13) -0.0037(12) 0.0088(13) P3 0.0650(18) 0.0476(16) 0.0512(16) 0.0114(13) 0.0046(14) 0.0037(14) C1 0.065(7) 0.063(7) 0.049(6) 0.009(6) -0.001(6) 0.005(6) O1 0.086(6) 0.102(7) 0.047(4) 0.003(5) 0.031(4) 0.014(5) C11 0.049(6) 0.038(5) 0.052(6) -0.001(5) -0.010(5) -0.003(5) C12 0.022(4) 0.045(6) 0.074(7) -0.010(5) 0.004(5) -0.001(4) C13 0.028(4) 0.039(5) 0.053(6) 0.011(5) -0.010(4) -0.007(4) C14 0.043(5) 0.034(5) 0.063(7) -0.012(5) 0.026(5) -0.010(4) C15 0.039(5) 0.053(6) 0.052(6) -0.004(5) -0.002(5) -0.004(5) C16 0.086(10) 0.104(11) 0.056(8) -0.004(7) -0.025(7) -0.001(9) C17 0.069(8) 0.046(6) 0.091(9) -0.019(6) 0.008(7) 0.008(6) C18 0.082(9) 0.058(7) 0.071(8) 0.028(6) -0.021(7) -0.008(7) C19 0.054(7) 0.106(10) 0.053(7) 0.001(7) 0.018(6) -0.013(7) C20 0.036(6) 0.059(7) 0.128(12) -0.002(8) -0.021(7) 0.009(5) C111 0.076(9) 0.088(9) 0.063(8) -0.020(7) 0.001(7) 0.020(8) C112 0.091(10) 0.111(12) 0.085(10) -0.055(9) 0.006(8) -0.041(9) C113 0.102(10) 0.125(13) 0.032(6) 0.004(7) -0.002(6) 0.018(9) C231 0.065(8) 0.077(9) 0.100(10) -0.033(8) -0.005(7) 0.030(7) C232 0.030(5) 0.090(10) 0.133(13) -0.008(9) 0.010(7) -0.013(6) C233 0.056(7) 0.140(13) 0.062(8) 0.015(8) -0.019(6) 0.033(8) C321 0.096(11) 0.082(10) 0.110(12) 0.039(9) -0.009(9) -0.025(9) C322 0.139(14) 0.074(9) 0.060(8) 0.023(7) -0.024(9) 0.004(9) C323 0.128(14) 0.061(8) 0.108(12) -0.001(8) 0.026(11) 0.021(9) O2 0.070(5) 0.042(4) 0.039(4) -0.005(3) -0.007(3) -0.001(3) C21 0.071(7) 0.031(5) 0.045(5) 0.000(4) -0.006(5) -0.002(5) C211 0.116(12) 0.058(8) 0.064(8) 0.004(7) -0.001(8) 0.016(8) C212 0.097(10) 0.055(8) 0.071(9) -0.010(7) -0.026(8) 0.006(8) C213 0.111(11) 0.046(7) 0.054(7) 0.008(5) -0.009(8) -0.021(7) F21 0.092(6) 0.126(7) 0.107(7) -0.012(6) -0.036(5) 0.041(6) F22 0.174(9) 0.050(4) 0.098(6) -0.003(4) 0.017(6) 0.040(5) F23 0.106(6) 0.109(6) 0.075(5) 0.003(5) 0.028(5) 0.027(5) F24 0.152(9) 0.075(6) 0.132(8) 0.025(5) -0.061(7) -0.055(6) F25 0.130(7) 0.076(5) 0.057(4) -0.012(4) -0.034(4) 0.008(5) F26 0.070(5) 0.087(6) 0.125(7) -0.009(5) -0.020(5) -0.008(4) F27 0.140(7) 0.063(4) 0.044(3) 0.004(3) -0.016(4) -0.017(5) F28 0.200(10) 0.048(4) 0.056(4) 0.017(3) -0.009(5) -0.016(5) F29 0.098(6) 0.113(7) 0.082(6) -0.007(5) 0.034(5) -0.014(5) O3 0.031(3) 0.037(3) 0.051(4) -0.006(3) 0.004(3) -0.001(3) C31 0.030(5) 0.048(6) 0.046(5) -0.003(5) 0.001(4) 0.003(4) C311 0.038(5) 0.058(7) 0.060(7) 0.003(6) -0.004(5) 0.004(5) C312 0.020(5) 0.099(10) 0.081(9) -0.003(8) 0.006(5) -0.001(6) C313 0.053(7) 0.066(8) 0.069(8) 0.008(6) -0.020(6) -0.012(6) F31 0.075(5) 0.149(8) 0.054(4) 0.009(5) -0.004(4) 0.012(5) F32 0.075(5) 0.118(6) 0.072(5) 0.011(5) -0.033(4) -0.019(5) F33 0.089(5) 0.058(4) 0.134(7) 0.027(5) -0.028(5) 0.016(4) F34 0.027(3) 0.137(7) 0.100(6) -0.004(5) 0.002(3) -0.001(4) F35 0.055(5) 0.127(8) 0.189(10) -0.075(8) 0.037(6) 0.004(5) F36 0.072(5) 0.282(14) 0.051(5) 0.027(7) 0.014(4) 0.020(7) F37 0.086(5) 0.056(4) 0.120(7) -0.027(4) 0.000(5) 0.003(4) F38 0.101(6) 0.061(4) 0.118(6) 0.029(4) -0.047(5) -0.016(4) F39 0.068(5) 0.066(5) 0.155(8) 0.027(5) -0.031(5) -0.032(4) O4 0.029(3) 0.065(5) 0.071(5) 0.017(4) 0.010(3) 0.012(3) C41 0.029(5) 0.058(7) 0.074(8) 0.000(6) 0.003(5) 0.007(5) C421 0.082(8) 0.138(13) 0.178(16) 0.000(12) -0.025(9) 0.069(9) C422 0.082(8) 0.138(13) 0.178(16) 0.000(12) -0.025(9) 0.069(9) C423 0.082(8) 0.138(13) 0.178(16) 0.000(12) -0.025(9) 0.069(9) F41 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F42 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F43 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F44 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F45 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F46 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F47 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F48 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F49 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) C424 0.082(8) 0.138(13) 0.178(16) 0.000(12) -0.025(9) 0.069(9) C425 0.082(8) 0.138(13) 0.178(16) 0.000(12) -0.025(9) 0.069(9) C426 0.082(8) 0.138(13) 0.178(16) 0.000(12) -0.025(9) 0.069(9) F41B 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F42B 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F43B 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F44B 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F45B 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F46B 0.077(3) 0.096(4) 0.106(4) 0.007(3) -0.001(3) 0.011(3) F47B 0.060(5) 0.133(9) 0.093(7) -0.001(6) 0.019(5) 0.028(6) F48B 0.060(5) 0.133(9) 0.093(7) -0.001(6) 0.019(5) 0.028(6) F49B 0.060(5) 0.133(9) 0.093(7) -0.001(6) 0.019(5) 0.028(6) _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 1.929(12) . ? Mo1 C12 2.311(10) . ? Mo1 C11 2.311(10) . ? Mo1 C13 2.358(9) . ? Mo1 C15 2.382(10) . ? Mo1 C14 2.426(9) . ? Mo1 P3 2.449(3) . ? Mo1 P2 2.474(3) . ? Mo1 P1 2.521(3) . ? P1 C111 1.819(12) . ? P1 C112 1.821(13) . ? P1 C113 1.835(12) . ? P2 C233 1.809(12) . ? P2 C231 1.817(11) . ? P2 C232 1.817(12) . ? P3 C321 1.812(14) . ? P3 C322 1.818(12) . ? P3 C323 1.826(13) . ? C1 O1 1.161(13) . ? C11 C12 1.385(14) . ? C11 C15 1.422(14) . ? C11 C16 1.516(15) . ? C12 C13 1.426(14) . ? C12 C17 1.508(14) . ? C13 C14 1.413(13) . ? C13 C18 1.483(13) . ? C14 C15 1.391(14) . ? C14 C19 1.506(14) . ? C15 C20 1.480(14) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C111 H11C 0.9600 . ? C112 H11D 0.9600 . ? C112 H11E 0.9600 . ? C112 H11F 0.9600 . ? C113 H11G 0.9600 . ? C113 H11H 0.9600 . ? C113 H11I 0.9600 . ? C231 H23A 0.9600 . ? C231 H23B 0.9600 . ? C231 H23C 0.9600 . ? C232 H23D 0.9600 . ? C232 H23E 0.9600 . ? C232 H23F 0.9600 . ? C233 H23G 0.9600 . ? C233 H23H 0.9600 . ? C233 H23I 0.9600 . ? C321 H32A 0.9600 . ? C321 H32B 0.9600 . ? C321 H32C 0.9600 . ? C322 H32D 0.9600 . ? C322 H32E 0.9600 . ? C322 H32F 0.9600 . ? C323 H32G 0.9600 . ? C323 H32H 0.9600 . ? C323 H32I 0.9600 . ? O2 C21 1.369(11) . ? O2 H2 0.8200 . ? C21 C213 1.526(15) . ? C21 C211 1.529(18) . ? C21 C212 1.567(16) . ? C211 F23 1.284(15) . ? C211 F21 1.323(16) . ? C211 F22 1.335(15) . ? C212 F26 1.286(15) . ? C212 F24 1.291(15) . ? C212 F25 1.340(15) . ? C213 F27 1.311(14) . ? C213 F28 1.334(13) . ? C213 F29 1.352(16) . ? O3 C31 1.342(11) . ? C31 C312 1.523(14) . ? C31 C313 1.544(15) . ? C31 C311 1.556(14) . ? C311 F33 1.297(12) . ? C311 F32 1.317(12) . ? C311 F31 1.323(12) . ? C312 F35 1.280(15) . ? C312 F36 1.296(15) . ? C312 F34 1.332(12) . ? C313 F38 1.298(13) . ? C313 F39 1.315(12) . ? C313 F37 1.325(14) . ? O4 C41 1.354(11) . ? O4 H4 0.8200 . ? C41 C425 1.580(18) . ? C41 C421 1.584(18) . ? C41 C422 1.586(17) . ? C41 C426 1.593(18) . ? C41 C423 1.594(18) . ? C41 C424 1.607(18) . ? C421 F41 1.356(14) . ? C421 F43 1.368(14) . ? C421 F42 1.385(13) . ? C422 F44 1.345(14) . ? C422 F46 1.381(13) . ? C422 F45 1.395(13) . ? C423 F47 1.319(15) . ? C423 F49 1.328(14) . ? C423 F48 1.343(14) . ? C424 F41B 1.373(14) . ? C424 F43B 1.388(14) . ? C424 F42B 1.411(13) . ? C425 F44B 1.366(14) . ? C425 F46B 1.373(13) . ? C425 F45B 1.390(13) . ? C426 F49B 1.322(14) . ? C426 F47B 1.336(15) . ? C426 F48B 1.358(14) . ? 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 C12 88.5(4) . . ? C1 Mo1 C11 88.5(4) . . ? C12 Mo1 C11 34.9(3) . . ? C1 Mo1 C13 120.2(4) . . ? C12 Mo1 C13 35.5(3) . . ? C11 Mo1 C13 58.6(3) . . ? C1 Mo1 C15 120.0(4) . . ? C12 Mo1 C15 58.2(3) . . ? C11 Mo1 C15 35.2(3) . . ? C13 Mo1 C15 58.1(3) . . ? C1 Mo1 C14 143.4(4) . . ? C12 Mo1 C14 56.9(3) . . ? C11 Mo1 C14 56.7(4) . . ? C13 Mo1 C14 34.3(3) . . ? C15 Mo1 C14 33.6(4) . . ? C1 Mo1 P3 72.1(4) . . ? C12 Mo1 P3 129.9(3) . . ? C11 Mo1 P3 97.3(3) . . ? C13 Mo1 P3 150.0(2) . . ? C15 Mo1 P3 91.9(3) . . ? C14 Mo1 P3 119.1(3) . . ? C1 Mo1 P2 72.6(3) . . ? C12 Mo1 P2 97.4(2) . . ? C11 Mo1 P2 130.0(3) . . ? C13 Mo1 P2 91.5(2) . . ? C15 Mo1 P2 149.6(3) . . ? C14 Mo1 P2 119.5(3) . . ? P3 Mo1 P2 118.48(11) . . ? C1 Mo1 P1 131.1(4) . . ? C12 Mo1 P1 137.6(3) . . ? C11 Mo1 P1 137.1(3) . . ? C13 Mo1 P1 102.3(3) . . ? C15 Mo1 P1 101.9(3) . . ? C14 Mo1 P1 85.5(2) . . ? P3 Mo1 P1 83.24(10) . . ? P2 Mo1 P1 84.01(10) . . ? C111 P1 C112 101.9(7) . . ? C111 P1 C113 97.9(6) . . ? C112 P1 C113 100.2(7) . . ? C111 P1 Mo1 116.5(4) . . ? C112 P1 Mo1 121.0(4) . . ? C113 P1 Mo1 115.6(5) . . ? C233 P2 C231 100.3(7) . . ? C233 P2 C232 99.0(7) . . ? C231 P2 C232 99.3(7) . . ? C233 P2 Mo1 124.9(4) . . ? C231 P2 Mo1 114.3(4) . . ? C232 P2 Mo1 114.9(5) . . ? C321 P3 C322 99.3(7) . . ? C321 P3 C323 100.4(8) . . ? C322 P3 C323 98.4(7) . . ? C321 P3 Mo1 115.0(5) . . ? C322 P3 Mo1 114.3(5) . . ? C323 P3 Mo1 125.3(5) . . ? O1 C1 Mo1 174.9(11) . . ? C12 C11 C15 108.8(9) . . ? C12 C11 C16 124.0(10) . . ? C15 C11 C16 125.6(10) . . ? C12 C11 Mo1 72.6(6) . . ? C15 C11 Mo1 75.1(6) . . ? C16 C11 Mo1 129.9(8) . . ? C11 C12 C13 108.8(9) . . ? C11 C12 C17 123.3(10) . . ? C13 C12 C17 126.8(10) . . ? C11 C12 Mo1 72.6(6) . . ? C13 C12 Mo1 74.0(6) . . ? C17 C12 Mo1 129.0(7) . . ? C14 C13 C12 105.5(8) . . ? C14 C13 C18 127.5(10) . . ? C12 C13 C18 125.4(10) . . ? C14 C13 Mo1 75.5(5) . . ? C12 C13 Mo1 70.4(5) . . ? C18 C13 Mo1 129.8(7) . . ? C15 C14 C13 110.4(9) . . ? C15 C14 C19 124.8(10) . . ? C13 C14 C19 123.6(10) . . ? C15 C14 Mo1 71.4(5) . . ? C13 C14 Mo1 70.2(5) . . ? C19 C14 Mo1 135.4(7) . . ? C14 C15 C11 106.3(9) . . ? C14 C15 C20 125.4(10) . . ? C11 C15 C20 126.6(10) . . ? C14 C15 Mo1 74.9(6) . . ? C11 C15 Mo1 69.7(6) . . ? C20 C15 Mo1 131.8(8) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P1 C111 H11A 109.5 . . ? P1 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? P1 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? P1 C112 H11D 109.5 . . ? P1 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? P1 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? P1 C113 H11G 109.5 . . ? P1 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? P1 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? P2 C231 H23A 109.5 . . ? P2 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? P2 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? P2 C232 H23D 109.5 . . ? P2 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? P2 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? P2 C233 H23G 109.5 . . ? P2 C233 H23H 109.5 . . ? H23G C233 H23H 109.5 . . ? P2 C233 H23I 109.5 . . ? H23G C233 H23I 109.5 . . ? H23H C233 H23I 109.5 . . ? P3 C321 H32A 109.5 . . ? P3 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? P3 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? P3 C322 H32D 109.5 . . ? P3 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? P3 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? P3 C323 H32G 109.5 . . ? P3 C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? P3 C323 H32I 109.5 . . ? H32G C323 H32I 109.5 . . ? H32H C323 H32I 109.5 . . ? C21 O2 H2 109.5 . . ? O2 C21 C213 111.8(8) . . ? O2 C21 C211 109.7(10) . . ? C213 C21 C211 111.5(10) . . ? O2 C21 C212 105.2(9) . . ? C213 C21 C212 108.9(10) . . ? C211 C21 C212 109.5(10) . . ? F23 C211 F21 110.2(14) . . ? F23 C211 F22 106.9(12) . . ? F21 C211 F22 107.6(11) . . ? F23 C211 C21 112.7(11) . . ? F21 C211 C21 109.4(11) . . ? F22 C211 C21 109.9(13) . . ? F26 C212 F24 109.2(14) . . ? F26 C212 F25 106.2(11) . . ? F24 C212 F25 109.3(11) . . ? F26 C212 C21 110.6(10) . . ? F24 C212 C21 113.4(11) . . ? F25 C212 C21 107.8(12) . . ? F27 C213 F28 106.6(11) . . ? F27 C213 F29 110.4(11) . . ? F28 C213 F29 107.7(11) . . ? F27 C213 C21 110.5(10) . . ? F28 C213 C21 110.8(10) . . ? F29 C213 C21 110.8(11) . . ? O3 C31 C312 111.6(8) . . ? O3 C31 C313 109.6(8) . . ? C312 C31 C313 110.2(10) . . ? O3 C31 C311 110.1(8) . . ? C312 C31 C311 108.2(9) . . ? C313 C31 C311 107.0(8) . . ? F33 C311 F32 106.2(9) . . ? F33 C311 F31 106.5(10) . . ? F32 C311 F31 105.5(9) . . ? F33 C311 C31 111.9(9) . . ? F32 C311 C31 115.5(9) . . ? F31 C311 C31 110.6(8) . . ? F35 C312 F36 108.8(13) . . ? F35 C312 F34 106.0(11) . . ? F36 C312 F34 105.8(11) . . ? F35 C312 C31 111.5(10) . . ? F36 C312 C31 111.3(10) . . ? F34 C312 C31 113.2(11) . . ? F38 C313 F39 107.5(10) . . ? F38 C313 F37 106.7(11) . . ? F39 C313 F37 105.7(10) . . ? F38 C313 C31 110.7(10) . . ? F39 C313 C31 114.0(10) . . ? F37 C313 C31 111.8(10) . . ? C41 O4 H4 109.5 . . ? O4 C41 C425 110.6(10) . . ? O4 C41 C421 112.4(10) . . ? C425 C41 C421 125.1(12) . . ? O4 C41 C422 112.9(10) . . ? C425 C41 C422 18.2(9) . . ? C421 C41 C422 110.4(11) . . ? O4 C41 C426 107.9(10) . . ? C425 C41 C426 107.6(11) . . ? C421 C41 C426 89.8(11) . . ? C422 C41 C426 121.3(11) . . ? O4 C41 C423 105.6(10) . . ? C425 C41 C423 86.3(11) . . ? C421 C41 C423 112.4(11) . . ? C422 C41 C423 102.6(11) . . ? C426 C41 C423 24.5(9) . . ? O4 C41 C424 112.6(9) . . ? C425 C41 C424 108.8(11) . . ? C421 C41 C424 21.4(8) . . ? C422 C41 C424 91.9(11) . . ? C426 C41 C424 109.3(11) . . ? C423 C41 C424 129.5(12) . . ? F41 C421 F43 100.9(14) . . ? F41 C421 F42 119.9(18) . . ? F43 C421 F42 122.1(16) . . ? F41 C421 C41 101.2(14) . . ? F43 C421 C41 104.8(15) . . ? F42 C421 C41 105.2(14) . . ? F44 C422 F46 102.2(15) . . ? F44 C422 F45 109.2(16) . . ? F46 C422 F45 117.8(16) . . ? F44 C422 C41 107.2(14) . . ? F46 C422 C41 108.4(15) . . ? F45 C422 C41 111.1(14) . . ? F47 C423 F49 104.8(16) . . ? F47 C423 F48 104.9(17) . . ? F49 C423 F48 121.4(18) . . ? F47 C423 C41 109.7(15) . . ? F49 C423 C41 109.0(15) . . ? F48 C423 C41 106.7(14) . . ? F41B C424 F43B 99.0(14) . . ? F41B C424 F42B 125.0(18) . . ? F43B C424 F42B 121.1(16) . . ? F41B C424 C41 102.7(14) . . ? F43B C424 C41 104.8(15) . . ? F42B C424 C41 101.3(13) . . ? F44B C425 F46B 102.1(15) . . ? F44B C425 F45B 117.6(17) . . ? F46B C425 F45B 122.8(16) . . ? F44B C425 C41 104.4(14) . . ? F46B C425 C41 107.2(15) . . ? F45B C425 C41 101.1(13) . . ? F49B C426 F47B 103.5(16) . . ? F49B C426 F48B 120.7(17) . . ? F47B C426 F48B 114.5(18) . . ? F49B C426 C41 109.2(15) . . ? F47B C426 C41 105.0(14) . . ? F48B C426 C41 103.0(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O3 0.82 1.82 2.525(9) 142.9 . O4 H4 O3 0.82 1.76 2.541(9) 157.8 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.840 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.157 #====END