Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method SHELXL _publ_contact_author_name 'Dr Julio Perez' _publ_contact_author_address ; Departamento Quimica Organica e Inorganica Universidad de Oviedo c/ Julian Claveria, no. 8 Oviedo 33006 SPAIN ; _publ_contact_author_phone +34-85-102985 _publ_contact_author_fax +34-85-103446 _publ_contact_author_email japm@sauron.quimica.uniovi.es loop_ _publ_author_name _publ_author_address 'Julio Perez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qumica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Dolores Morales' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qumica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Sonia Nieto' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qumica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Lucia Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qumica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Victor Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qumica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Daniel Miguel' ; Quimica Inorganica Facultad de Ciencias Universidad de Valladolid 47071 Valladolid SPAIN ; _publ_section_title ; New [Mo(h3-allyl)(CO)2L3]+ complexes with monodentate or tridentate nitrogen-donor ligands ; #-------------------------- data section of block --------------------------- data_Compound_2_(lr31am) _database_code_depnum_ccdc_archive 'CCDC 254975' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 F3 Mo N3 O5 S' _chemical_formula_weight 589.39 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 P2(1)/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 8.3982(16) _cell_length_b 24.889(5) _cell_length_c 10.886(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.241(3) _cell_angle_gamma 90.00 _cell_volume 2273.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.791132 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14197 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 23.28 _reflns_number_total 3275 _reflns_number_gt 2989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0339P)^2^+1.5076P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3275 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.73919(2) 0.092082(8) 0.711035(19) 0.03073(10) Uani 1 1 d . . . N1 N 0.6126(2) 0.16529(9) 0.7667(2) 0.0384(5) Uani 1 1 d . . . N2 N 0.8947(2) 0.13384(8) 0.84108(19) 0.0352(5) Uani 1 1 d . . . N3 N 0.9277(2) 0.03481(9) 0.7717(2) 0.0381(5) Uani 1 1 d . . . C1 C 0.6208(3) 0.04861(12) 0.8315(3) 0.0428(7) Uani 1 1 d . . . O1 O 0.5496(3) 0.02078(11) 0.8903(2) 0.0753(7) Uani 1 1 d . . . C2 C 0.5514(3) 0.06383(11) 0.6175(3) 0.0413(6) Uani 1 1 d . . . O2 O 0.4344(2) 0.04753(9) 0.5727(2) 0.0625(6) Uani 1 1 d . . . C3 C 0.8259(4) 0.06204(12) 0.5214(3) 0.0480(7) Uani 1 1 d . . . H3A H 0.8924 0.0302 0.5230 0.058 Uiso 1 1 calc R . . H3B H 0.7477 0.0625 0.4535 0.058 Uiso 1 1 calc R . . C4 C 0.9035(3) 0.11134(12) 0.5492(2) 0.0429(7) Uani 1 1 d . . . C5 C 0.8078(3) 0.15632(11) 0.5610(2) 0.0438(7) Uani 1 1 d . . . H5A H 0.7293 0.1628 0.4949 0.053 Uiso 1 1 calc R . . H5B H 0.8602 0.1887 0.5912 0.053 Uiso 1 1 calc R . . C6 C 1.0810(3) 0.11405(16) 0.5754(3) 0.0645(9) Uani 1 1 d . . . H6A H 1.1339 0.1204 0.5002 0.097 Uiso 1 1 calc R . . H6B H 1.1174 0.0807 0.6106 0.097 Uiso 1 1 calc R . . H6C H 1.1047 0.1428 0.6320 0.097 Uiso 1 1 calc R . . C11 C 0.4628(3) 0.17841(12) 0.7290(3) 0.0492(7) Uani 1 1 d . . . H11 H 0.4033 0.1535 0.6831 0.059 Uiso 1 1 calc R . . C12 C 0.3941(4) 0.22665(13) 0.7552(3) 0.0576(8) Uani 1 1 d . . . H12 H 0.2905 0.2343 0.7272 0.069 Uiso 1 1 calc R . . C13 C 0.4805(4) 0.26347(13) 0.8234(3) 0.0627(9) Uani 1 1 d . . . H13 H 0.4370 0.2968 0.8413 0.075 Uiso 1 1 calc R . . C14 C 0.6315(4) 0.25066(13) 0.8649(3) 0.0570(8) Uani 1 1 d . . . H14 H 0.6907 0.2750 0.9126 0.068 Uiso 1 1 calc R . . C15 C 0.6958(3) 0.20129(11) 0.8354(2) 0.0410(7) Uani 1 1 d . . . C16 C 0.8560(3) 0.18389(11) 0.8783(2) 0.0418(7) Uani 1 1 d . . . C17 C 0.9619(4) 0.21339(13) 0.9519(3) 0.0596(9) Uani 1 1 d . . . H17 H 0.9362 0.2481 0.9758 0.072 Uiso 1 1 calc R . . C18 C 1.1050(4) 0.19103(15) 0.9893(3) 0.0670(10) Uani 1 1 d . . . H18 H 1.1782 0.2109 1.0368 0.080 Uiso 1 1 calc R . . C19 C 1.1402(4) 0.13908(14) 0.9563(3) 0.0564(8) Uani 1 1 d . . . H19 H 1.2356 0.1232 0.9831 0.068 Uiso 1 1 calc R . . C20 C 1.0315(3) 0.11079(12) 0.8827(2) 0.0406(6) Uani 1 1 d . . . C21 C 1.0465(3) 0.05404(12) 0.8483(2) 0.0405(6) Uani 1 1 d . . . C22 C 1.1679(3) 0.02108(14) 0.8935(3) 0.0547(8) Uani 1 1 d . . . H22 H 1.2484 0.0351 0.9451 0.066 Uiso 1 1 calc R . . C23 C 1.1693(4) -0.03228(15) 0.8623(3) 0.0632(9) Uani 1 1 d . . . H23 H 1.2512 -0.0546 0.8916 0.076 Uiso 1 1 calc R . . C24 C 1.0484(4) -0.05234(13) 0.7874(3) 0.0591(9) Uani 1 1 d . . . H24 H 1.0462 -0.0885 0.7662 0.071 Uiso 1 1 calc R . . C25 C 0.9298(4) -0.01802(12) 0.7438(3) 0.0486(7) Uani 1 1 d . . . H25 H 0.8481 -0.0319 0.6932 0.058 Uiso 1 1 calc R . . S1 S 1.04975(10) 0.33473(3) 0.66155(8) 0.0561(2) Uani 1 1 d . . . O11 O 1.2086(3) 0.34038(11) 0.7093(3) 0.0888(9) Uani 1 1 d . . . O12 O 1.0159(3) 0.36484(12) 0.5525(2) 0.0818(8) Uani 1 1 d . . . O13 O 0.9860(4) 0.28196(10) 0.6640(3) 0.0942(9) Uani 1 1 d . . . C51 C 0.9345(4) 0.37025(13) 0.7746(3) 0.0546(8) Uani 1 1 d . . . F1 F 0.9493(3) 0.34765(9) 0.88479(18) 0.0875(7) Uani 1 1 d . . . F2 F 0.7802(2) 0.36951(12) 0.7444(2) 0.0960(8) Uani 1 1 d . . . F3 F 0.9808(3) 0.42066(9) 0.7867(2) 0.0985(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02550(14) 0.03375(15) 0.03287(15) 0.00063(9) 0.00022(9) 0.00114(9) N1 0.0339(12) 0.0388(13) 0.0426(13) -0.0010(10) 0.0036(10) 0.0027(10) N2 0.0325(12) 0.0396(13) 0.0334(12) 0.0026(10) -0.0016(9) -0.0011(10) N3 0.0325(12) 0.0404(13) 0.0415(13) 0.0034(10) 0.0027(10) 0.0031(10) C1 0.0340(15) 0.0502(17) 0.0440(16) 0.0073(14) 0.0000(13) -0.0020(13) O1 0.0674(16) 0.0936(19) 0.0656(15) 0.0255(14) 0.0136(13) -0.0220(14) C2 0.0361(16) 0.0433(16) 0.0444(16) -0.0014(13) 0.0007(13) 0.0040(13) O2 0.0396(12) 0.0696(15) 0.0772(15) -0.0142(12) -0.0138(11) -0.0071(11) C3 0.0500(18) 0.0564(19) 0.0383(16) -0.0046(14) 0.0085(13) 0.0100(15) C4 0.0365(15) 0.0606(19) 0.0322(14) 0.0075(13) 0.0063(12) -0.0016(14) C5 0.0486(17) 0.0474(17) 0.0354(15) 0.0081(13) 0.0014(12) -0.0055(14) C6 0.0362(17) 0.102(3) 0.056(2) 0.0156(19) 0.0110(15) -0.0046(17) C11 0.0371(16) 0.0482(18) 0.0622(19) -0.0022(15) 0.0007(14) 0.0082(13) C12 0.0467(18) 0.058(2) 0.068(2) 0.0028(17) 0.0063(16) 0.0179(16) C13 0.073(2) 0.0484(19) 0.068(2) -0.0061(17) 0.0116(18) 0.0225(17) C14 0.071(2) 0.0447(18) 0.0547(19) -0.0104(15) -0.0001(16) 0.0067(16) C15 0.0500(17) 0.0381(16) 0.0351(14) 0.0000(12) 0.0045(13) 0.0030(13) C16 0.0515(17) 0.0378(16) 0.0360(15) 0.0013(12) -0.0008(13) -0.0043(13) C17 0.078(2) 0.0449(18) 0.0543(19) -0.0059(15) -0.0159(17) -0.0060(17) C18 0.071(2) 0.070(2) 0.058(2) -0.0046(18) -0.0273(18) -0.0189(19) C19 0.0444(17) 0.069(2) 0.0546(19) 0.0064(16) -0.0170(15) -0.0065(15) C20 0.0328(15) 0.0520(17) 0.0368(15) 0.0057(13) -0.0024(12) -0.0020(13) C21 0.0304(14) 0.0547(18) 0.0365(14) 0.0078(13) 0.0014(12) 0.0047(12) C22 0.0373(16) 0.072(2) 0.0546(19) 0.0067(17) -0.0042(14) 0.0129(15) C23 0.055(2) 0.071(2) 0.064(2) 0.0130(18) 0.0028(17) 0.0311(18) C24 0.063(2) 0.0469(18) 0.068(2) 0.0055(16) 0.0095(18) 0.0194(16) C25 0.0464(17) 0.0437(17) 0.0559(18) 0.0029(14) 0.0032(14) 0.0056(13) S1 0.0483(5) 0.0502(5) 0.0692(5) -0.0037(4) -0.0043(4) 0.0020(4) O11 0.0465(14) 0.0789(19) 0.139(3) 0.0040(17) -0.0171(15) 0.0121(12) O12 0.0792(18) 0.107(2) 0.0596(15) 0.0102(14) 0.0046(13) 0.0096(15) O13 0.118(2) 0.0550(15) 0.110(2) -0.0223(15) 0.0135(18) -0.0250(15) C51 0.054(2) 0.056(2) 0.0517(19) 0.0016(15) -0.0142(15) 0.0030(15) F1 0.1048(17) 0.0987(17) 0.0579(12) 0.0048(12) -0.0097(11) -0.0055(13) F2 0.0554(13) 0.142(2) 0.0897(15) -0.0090(15) -0.0030(11) 0.0235(13) F3 0.137(2) 0.0552(13) 0.1033(18) -0.0147(12) 0.0084(16) 0.0019(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.973(3) . ? Mo1 C1 1.995(3) . ? Mo1 N2 2.155(2) . ? Mo1 N1 2.206(2) . ? Mo1 N3 2.212(2) . ? Mo1 C4 2.330(3) . ? Mo1 C3 2.338(3) . ? Mo1 C5 2.373(3) . ? N1 C15 1.346(3) . ? N1 C11 1.348(3) . ? N2 C20 1.346(3) . ? N2 C16 1.353(3) . ? N3 C25 1.350(4) . ? N3 C21 1.362(3) . ? C1 O1 1.130(3) . ? C2 O2 1.154(3) . ? C3 C4 1.417(4) . ? C4 C5 1.387(4) . ? C4 C6 1.508(4) . ? C11 C12 1.367(4) . ? C12 C13 1.369(5) . ? C13 C14 1.367(5) . ? C14 C15 1.385(4) . ? C15 C16 1.472(4) . ? C16 C17 1.384(4) . ? C17 C18 1.372(5) . ? C18 C19 1.377(5) . ? C19 C20 1.383(4) . ? C20 C21 1.468(4) . ? C21 C22 1.384(4) . ? C22 C23 1.371(5) . ? C23 C24 1.372(5) . ? C24 C25 1.382(4) . ? S1 O13 1.419(3) . ? S1 O11 1.420(3) . ? S1 O12 1.423(3) . ? S1 C51 1.824(3) . ? C51 F3 1.319(4) . ? C51 F2 1.324(4) . ? C51 F1 1.326(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 C2 Mo1 C1 74.76(11) . . ? C2 Mo1 N2 164.25(10) . . ? C1 Mo1 N2 97.73(10) . . ? C2 Mo1 N1 92.98(10) . . ? C1 Mo1 N1 90.54(10) . . ? N2 Mo1 N1 73.01(8) . . ? C2 Mo1 N3 118.21(10) . . ? C1 Mo1 N3 79.83(10) . . ? N2 Mo1 N3 72.92(8) . . ? N1 Mo1 N3 142.86(8) . . ? C2 Mo1 C4 99.69(11) . . ? C1 Mo1 C4 159.02(11) . . ? N2 Mo1 C4 92.05(9) . . ? N1 Mo1 C4 110.10(9) . . ? N3 Mo1 C4 85.42(9) . . ? C2 Mo1 C3 72.58(11) . . ? C1 Mo1 C3 125.96(12) . . ? N2 Mo1 C3 122.17(9) . . ? N1 Mo1 C3 132.56(9) . . ? N3 Mo1 C3 79.27(9) . . ? C4 Mo1 C3 35.33(10) . . ? C2 Mo1 C5 95.49(11) . . ? C1 Mo1 C5 163.45(11) . . ? N2 Mo1 C5 88.28(9) . . ? N1 Mo1 C5 76.42(9) . . ? N3 Mo1 C5 116.71(9) . . ? C4 Mo1 C5 34.29(10) . . ? C3 Mo1 C5 61.00(10) . . ? C15 N1 C11 117.8(2) . . ? C15 N1 Mo1 117.20(17) . . ? C11 N1 Mo1 124.80(19) . . ? C20 N2 C16 120.2(2) . . ? C20 N2 Mo1 120.18(18) . . ? C16 N2 Mo1 119.58(17) . . ? C25 N3 C21 117.7(2) . . ? C25 N3 Mo1 125.17(19) . . ? C21 N3 Mo1 117.08(18) . . ? O1 C1 Mo1 173.2(3) . . ? O2 C2 Mo1 173.8(2) . . ? C4 C3 Mo1 72.00(15) . . ? C5 C4 C3 117.1(3) . . ? C5 C4 C6 121.2(3) . . ? C3 C4 C6 121.5(3) . . ? C5 C4 Mo1 74.56(15) . . ? C3 C4 Mo1 72.67(15) . . ? C6 C4 Mo1 118.47(19) . . ? C4 C5 Mo1 71.15(15) . . ? N1 C11 C12 123.1(3) . . ? C11 C12 C13 118.8(3) . . ? C14 C13 C12 119.2(3) . . ? C13 C14 C15 119.7(3) . . ? N1 C15 C14 121.4(3) . . ? N1 C15 C16 115.4(2) . . ? C14 C15 C16 123.2(3) . . ? N2 C16 C17 120.3(3) . . ? N2 C16 C15 113.8(2) . . ? C17 C16 C15 125.9(3) . . ? C18 C17 C16 119.5(3) . . ? C17 C18 C19 119.9(3) . . ? C18 C19 C20 119.0(3) . . ? N2 C20 C19 120.9(3) . . ? N2 C20 C21 113.9(2) . . ? C19 C20 C21 125.2(3) . . ? N3 C21 C22 121.4(3) . . ? N3 C21 C20 115.2(2) . . ? C22 C21 C20 123.3(3) . . ? C23 C22 C21 120.0(3) . . ? C22 C23 C24 119.1(3) . . ? C23 C24 C25 119.1(3) . . ? N3 C25 C24 122.7(3) . . ? O13 S1 O11 115.77(18) . . ? O13 S1 O12 116.11(18) . . ? O11 S1 O12 114.04(17) . . ? O13 S1 C51 103.01(17) . . ? O11 S1 C51 102.77(16) . . ? O12 S1 C51 102.33(15) . . ? F3 C51 F2 108.7(3) . . ? F3 C51 F1 107.2(3) . . ? F2 C51 F1 106.0(3) . . ? F3 C51 S1 111.5(2) . . ? F2 C51 S1 111.5(2) . . ? F1 C51 S1 111.8(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.264 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.048 #===END data_Compound_3_(sn130k) _database_code_depnum_ccdc_archive 'CCDC 254976' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H34 B F24 Mo N3 O2' _chemical_formula_weight 1199.49 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' B B 0.0013 0.0007 '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 Trigonal _symmetry_space_group_name_H-M P3(2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 16.224(6) _cell_length_b 16.224(6) _cell_length_c 15.949(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3636(3) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1794 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.655101 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17474 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 23.46 _reflns_number_total 7015 _reflns_number_gt 3425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1093P)^2^+4.9080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0067(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 7015 _refine_ls_number_parameters 678 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1555 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2559 _refine_ls_wR_factor_gt 0.2042 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.007 _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 0.14388(9) 0.16962(12) 0.22119(11) 0.1277(7) Uani 1 1 d . . . C1 C 0.052(2) 0.158(4) 0.144(2) 0.34(3) Uani 1 1 d . . . O1 O 0.000(2) 0.150(4) 0.095(2) 0.56(5) Uani 1 1 d . . . C2 C 0.0402(17) 0.062(3) 0.264(4) 0.33(3) Uani 1 1 d . . . O2 O -0.0215(15) -0.013(2) 0.296(4) 0.57(4) Uani 1 1 d . . . N1 N 0.2710(16) 0.285(2) 0.1617(16) 0.278(18) Uani 1 1 d . . . H1A H 0.2516 0.2967 0.1124 0.334 Uiso 1 1 calc R . . H1B H 0.2888 0.3370 0.1937 0.334 Uiso 1 1 calc R . . N2 N 0.1833(15) 0.085(2) 0.1422(19) 0.32(2) Uani 1 1 d . . . H2A H 0.1394 0.0235 0.1513 0.388 Uiso 1 1 calc R . . H2B H 0.1758 0.0976 0.0888 0.388 Uiso 1 1 calc R . . N3 N 0.2495(15) 0.1621(14) 0.3017(9) 0.154(7) Uani 1 1 d . . . H3A H 0.2621 0.2040 0.3436 0.184 Uiso 1 1 calc R . . H3B H 0.2200 0.1039 0.3252 0.184 Uiso 1 1 calc R . . C5 C 0.1020(16) 0.2851(17) 0.2336(19) 0.188(11) Uani 1 1 d . . . H5A H 0.1393 0.3435 0.2021 0.226 Uiso 1 1 calc R . . H5B H 0.0346 0.2640 0.2363 0.226 Uiso 1 1 calc R . . C6 C 0.143(3) 0.273(3) 0.3030(18) 0.171(10) Uani 1 1 d . . . C7 C 0.087(2) 0.197(3) 0.344(2) 0.219(16) Uani 1 1 d . . . H7A H 0.0201 0.1784 0.3455 0.262 Uiso 1 1 calc R . . H7B H 0.1111 0.1864 0.3959 0.262 Uiso 1 1 calc R . . C8 C 0.229(2) 0.352(2) 0.346(2) 0.26(2) Uani 1 1 d . . . H8A H 0.2854 0.3532 0.3253 0.396 Uiso 1 1 calc R . . H8B H 0.2243 0.3400 0.4056 0.396 Uiso 1 1 calc R . . H8C H 0.2327 0.4114 0.3354 0.396 Uiso 1 1 calc R . . C11 C 0.3624(15) 0.282(3) 0.143(3) 0.30(3) Uani 1 1 d . . . H11 H 0.4102 0.3365 0.1106 0.362 Uiso 1 1 calc R . . C12 C 0.333(3) 0.186(4) 0.1032(19) 0.26(3) Uani 1 1 d . . . H12A H 0.2942 0.1813 0.0549 0.312 Uiso 1 1 calc R . . H12B H 0.3904 0.1904 0.0814 0.312 Uiso 1 1 calc R . . C13 C 0.280(2) 0.091(4) 0.147(3) 0.31(3) Uani 1 1 d . . . H13 H 0.2799 0.0419 0.1117 0.369 Uiso 1 1 calc R . . C14 C 0.335(2) 0.105(2) 0.216(3) 0.233(16) Uani 1 1 d . . . H14A H 0.3986 0.1235 0.1982 0.279 Uiso 1 1 calc R . . H14B H 0.3094 0.0457 0.2464 0.279 Uiso 1 1 calc R . . C15 C 0.3390(17) 0.1777(14) 0.2723(12) 0.128(6) Uani 1 1 d . . . H15 H 0.3747 0.1776 0.3218 0.154 Uiso 1 1 calc R . . C16 C 0.3948(12) 0.2733(18) 0.2332(19) 0.179(10) Uani 1 1 d . . . H16A H 0.4611 0.2898 0.2309 0.215 Uiso 1 1 calc R . . H16B H 0.3908 0.3195 0.2689 0.215 Uiso 1 1 calc R . . B51 B 0.4958(9) -0.0059(9) 0.4146(8) 0.066(3) Uani 1 1 d . . . C51 C 0.5093(7) 0.1019(8) 0.4241(7) 0.066(3) Uani 1 1 d . . . C52 C 0.4430(8) 0.1155(8) 0.4698(7) 0.071(3) Uani 1 1 d . . . H52 H 0.3919 0.0635 0.4954 0.086 Uiso 1 1 calc R . . C53 C 0.4521(9) 0.2045(9) 0.4776(7) 0.073(3) Uani 1 1 d . . . C54 C 0.5247(11) 0.2812(10) 0.4389(8) 0.087(4) Uani 1 1 d . . . H54 H 0.5295 0.3406 0.4430 0.104 Uiso 1 1 calc R . . C55 C 0.5915(9) 0.2705(8) 0.3936(8) 0.074(3) Uani 1 1 d . . . C56 C 0.5799(9) 0.1820(10) 0.3880(8) 0.086(4) Uani 1 1 d . . . H56 H 0.6246 0.1755 0.3565 0.103 Uiso 1 1 calc R . . C57 C 0.3843(13) 0.2155(13) 0.5243(11) 0.097(4) Uani 1 1 d . . . C58 C 0.6668(13) 0.3460(13) 0.3538(16) 0.120(6) Uani 1 1 d . . . C61 C 0.4478(7) -0.0697(8) 0.4986(8) 0.072(3) Uani 1 1 d . . . C62 C 0.4592(8) -0.0317(8) 0.5790(8) 0.074(3) Uani 1 1 d . . . H62 H 0.4926 0.0342 0.5841 0.089 Uiso 1 1 calc R . . C63 C 0.4247(10) -0.0846(9) 0.6519(9) 0.084(4) Uani 1 1 d . . . C64 C 0.3766(9) -0.1809(10) 0.6464(8) 0.084(4) Uani 1 1 d . . . H64 H 0.3508 -0.2176 0.6943 0.100 Uiso 1 1 calc R . . C65 C 0.3660(9) -0.2251(8) 0.5687(8) 0.079(3) Uani 1 1 d . . . C66 C 0.4013(8) -0.1670(8) 0.4968(8) 0.077(3) Uani 1 1 d . . . H66 H 0.3924 -0.1967 0.4450 0.092 Uiso 1 1 calc R . . C67 C 0.428(2) -0.0336(16) 0.7295(10) 0.184(12) Uani 1 1 d . . . C68 C 0.3138(13) -0.3274(11) 0.5631(11) 0.101(4) Uani 1 1 d . . . C71 C 0.5957(9) -0.0007(9) 0.4052(7) 0.072(3) Uani 1 1 d . . . C72 C 0.6063(10) -0.0668(11) 0.3579(9) 0.096(4) Uani 1 1 d . . . H72 H 0.5549 -0.1132 0.3278 0.116 Uiso 1 1 calc R . . C73 C 0.6950(12) -0.0640(12) 0.3553(10) 0.096(4) Uani 1 1 d . . . C74 C 0.7698(11) 0.0009(15) 0.3978(11) 0.105(5) Uani 1 1 d . . . H74 H 0.8280 0.0033 0.3929 0.126 Uiso 1 1 calc R . . C75 C 0.7615(10) 0.0655(14) 0.4495(10) 0.099(5) Uani 1 1 d . . . C76 C 0.6747(9) 0.0643(9) 0.4512(8) 0.082(3) Uani 1 1 d . . . H76 H 0.6695 0.1087 0.4844 0.098 Uiso 1 1 calc R . . C77 C 0.700(2) -0.134(2) 0.3010(18) 0.163(10) Uani 1 1 d . . . C78 C 0.8386(16) 0.135(2) 0.4946(16) 0.153(9) Uani 1 1 d . . . C81 C 0.4272(8) -0.0515(7) 0.3348(7) 0.068(3) Uani 1 1 d . . . C82 C 0.3278(8) -0.1047(9) 0.3411(7) 0.078(3) Uani 1 1 d . . . H82 H 0.2995 -0.1155 0.3937 0.094 Uiso 1 1 calc R . . C83 C 0.2697(9) -0.1423(10) 0.2693(9) 0.083(3) Uani 1 1 d . . . C84 C 0.3090(10) -0.1269(10) 0.1919(8) 0.089(4) Uani 1 1 d . . . H84 H 0.2707 -0.1533 0.1449 0.107 Uiso 1 1 calc R . . C85 C 0.4072(9) -0.0712(9) 0.1833(8) 0.080(3) Uani 1 1 d . . . C86 C 0.4623(9) -0.0338(9) 0.2538(8) 0.080(3) Uani 1 1 d . . . H86 H 0.5274 0.0061 0.2466 0.096 Uiso 1 1 calc R . . C87 C 0.1667(11) -0.1973(14) 0.2790(12) 0.116(6) Uani 1 1 d . . . C88 C 0.4438(15) -0.0526(16) 0.1013(13) 0.131(7) Uani 1 1 d . . . F1 F 0.4144(10) 0.2931(11) 0.5641(12) 0.232(9) Uani 1 1 d . . . F2 F 0.3196(14) 0.210(2) 0.4897(9) 0.310(16) Uani 1 1 d . . . F3 F 0.3474(15) 0.1624(13) 0.5856(13) 0.265(11) Uani 1 1 d . . . F4 F 0.6994(16) 0.4254(11) 0.3845(16) 0.302(15) Uani 1 1 d . . . F5 F 0.7416(10) 0.3494(11) 0.3421(18) 0.287(13) Uani 1 1 d . . . F6 F 0.6534(15) 0.363(2) 0.2805(17) 0.343(19) Uani 1 1 d . . . F7 F 0.4828(16) 0.0495(9) 0.7328(6) 0.239(9) Uani 1 1 d . . . F8 F 0.3679(13) -0.0775(13) 0.7798(10) 0.213(7) Uani 1 1 d . . . F9 F 0.4934(15) -0.0550(12) 0.7807(10) 0.219(7) Uani 1 1 d . . . F10 F 0.2205(9) -0.3644(7) 0.5614(10) 0.177(5) Uani 1 1 d . . . F11 F 0.3314(8) -0.3613(6) 0.4954(7) 0.153(4) Uani 1 1 d . . . F12 F 0.3281(9) -0.3706(6) 0.6230(7) 0.162(5) Uani 1 1 d . . . F13 F 0.6294(13) -0.2048(15) 0.2795(19) 0.315(17) Uani 1 1 d . . . F14 F 0.7523(14) -0.1674(13) 0.3364(11) 0.225(7) Uani 1 1 d . . . F15 F 0.7564(19) -0.0944(14) 0.2394(11) 0.266(11) Uani 1 1 d . . . F16 F 0.8565(18) 0.1003(16) 0.5638(14) 0.304(13) Uani 1 1 d . . . F17 F 0.8299(11) 0.1995(16) 0.5356(15) 0.250(10) Uani 1 1 d . . . F18 F 0.9133(12) 0.1795(17) 0.4658(11) 0.291(13) Uani 1 1 d . . . F19 F 0.1385(7) -0.2488(9) 0.3498(7) 0.166(5) Uani 1 1 d . . . F20 F 0.1235(6) -0.2609(9) 0.2236(7) 0.156(4) Uani 1 1 d . . . F21 F 0.1272(7) -0.1471(8) 0.2826(15) 0.256(10) Uani 1 1 d . . . F22 F 0.466(2) 0.0278(17) 0.0743(11) 0.309(15) Uani 1 1 d . . . F23 F 0.5291(13) -0.036(2) 0.0949(8) 0.289(14) Uani 1 1 d . . . F24 F 0.4026(9) -0.1039(13) 0.0425(7) 0.240(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0717(9) 0.1452(15) 0.1297(11) -0.0359(10) 0.0050(8) 0.0268(9) C1 0.17(2) 0.72(9) 0.19(3) -0.28(4) -0.13(2) 0.28(4) O1 0.32(4) 1.18(13) 0.34(4) -0.46(6) -0.22(3) 0.48(6) C2 0.064(15) 0.21(3) 0.59(8) -0.10(4) 0.04(3) -0.021(18) O2 0.102(15) 0.20(2) 1.25(13) 0.08(4) 0.15(3) -0.044(16) N1 0.19(2) 0.39(4) 0.30(3) 0.27(3) 0.071(19) 0.18(2) N2 0.125(16) 0.47(5) 0.36(4) -0.28(4) -0.068(19) 0.13(2) N3 0.234(19) 0.213(18) 0.099(10) 0.051(11) 0.035(11) 0.176(17) C5 0.129(17) 0.17(2) 0.28(3) 0.06(2) -0.019(18) 0.085(16) C6 0.22(3) 0.21(3) 0.14(2) -0.06(2) -0.06(2) 0.16(3) C7 0.21(3) 0.32(5) 0.19(3) 0.04(3) 0.07(2) 0.18(3) C8 0.34(4) 0.25(3) 0.32(4) -0.17(3) -0.20(4) 0.24(3) C11 0.045(11) 0.28(4) 0.56(7) 0.29(5) 0.06(2) 0.066(18) C12 0.20(4) 0.54(8) 0.15(2) 0.16(4) 0.08(2) 0.27(5) C13 0.15(3) 0.42(7) 0.32(5) -0.25(5) -0.02(3) 0.12(4) C14 0.15(2) 0.19(3) 0.38(5) -0.12(3) -0.05(3) 0.09(2) C15 0.19(2) 0.134(15) 0.101(12) -0.012(11) -0.052(13) 0.112(16) C16 0.064(11) 0.16(2) 0.30(3) -0.02(2) -0.042(15) 0.049(13) B51 0.064(8) 0.064(8) 0.075(9) 0.004(6) 0.008(6) 0.037(7) C51 0.054(7) 0.063(7) 0.065(7) -0.012(5) -0.005(5) 0.018(6) C52 0.073(7) 0.051(7) 0.082(8) -0.003(6) 0.000(6) 0.024(6) C53 0.072(8) 0.081(9) 0.064(7) -0.021(6) -0.001(6) 0.036(7) C54 0.102(10) 0.068(8) 0.091(9) -0.013(7) -0.012(8) 0.042(8) C55 0.073(8) 0.049(7) 0.084(8) -0.010(6) -0.003(6) 0.019(6) C56 0.067(8) 0.081(10) 0.087(9) 0.004(7) -0.001(7) 0.021(7) C57 0.115(12) 0.118(12) 0.090(10) -0.001(9) -0.002(9) 0.083(10) C58 0.087(13) 0.085(13) 0.169(18) 0.027(12) 0.027(12) 0.027(10) C61 0.055(6) 0.062(7) 0.080(8) -0.004(6) 0.003(5) 0.015(6) C62 0.058(7) 0.055(7) 0.087(9) -0.003(6) -0.008(6) 0.012(5) C63 0.093(9) 0.072(9) 0.080(10) 0.007(7) -0.004(7) 0.036(7) C64 0.087(9) 0.090(10) 0.072(9) 0.018(7) 0.010(7) 0.042(8) C65 0.075(8) 0.063(8) 0.088(9) 0.009(7) 0.001(6) 0.025(6) C66 0.082(8) 0.058(7) 0.077(8) -0.004(6) 0.011(6) 0.024(6) C67 0.23(3) 0.116(16) 0.044(10) 0.022(10) -0.006(12) -0.033(15) C68 0.118(14) 0.079(10) 0.097(11) 0.005(9) 0.012(9) 0.043(10) C71 0.085(8) 0.074(7) 0.064(7) 0.008(6) 0.009(6) 0.044(7) C72 0.092(10) 0.099(10) 0.102(10) 0.021(8) 0.022(8) 0.050(8) C73 0.086(11) 0.108(11) 0.110(11) 0.027(9) 0.029(9) 0.061(10) C74 0.072(10) 0.140(15) 0.116(12) 0.055(11) 0.029(9) 0.063(11) C75 0.064(10) 0.141(14) 0.082(10) 0.034(10) 0.007(8) 0.044(10) C76 0.064(8) 0.085(9) 0.085(9) 0.007(7) 0.002(6) 0.029(7) C77 0.20(3) 0.16(2) 0.20(2) 0.048(18) 0.11(2) 0.14(2) C78 0.088(15) 0.25(3) 0.135(18) 0.04(2) 0.013(14) 0.10(2) C81 0.070(8) 0.048(6) 0.074(8) -0.002(5) 0.004(6) 0.022(6) C82 0.065(8) 0.099(9) 0.063(7) -0.001(6) 0.008(6) 0.036(7) C83 0.066(8) 0.102(10) 0.079(9) -0.001(7) 0.007(7) 0.040(8) C84 0.093(11) 0.090(9) 0.074(9) -0.007(7) 0.008(7) 0.037(8) C85 0.069(8) 0.083(8) 0.073(8) -0.019(7) 0.005(7) 0.027(7) C86 0.068(7) 0.076(8) 0.085(9) -0.003(7) 0.008(7) 0.026(6) C87 0.073(10) 0.128(14) 0.113(13) -0.045(11) 0.005(10) 0.025(10) C88 0.115(15) 0.117(14) 0.108(15) 0.003(12) 0.046(11) 0.019(11) F1 0.181(12) 0.169(12) 0.31(2) -0.112(13) 0.077(13) 0.062(10) F2 0.31(2) 0.71(5) 0.135(11) -0.089(18) -0.043(13) 0.42(3) F3 0.37(2) 0.259(18) 0.266(18) 0.101(16) 0.21(2) 0.236(19) F4 0.26(2) 0.094(9) 0.37(3) -0.057(12) 0.16(2) -0.044(11) F5 0.103(9) 0.160(13) 0.57(4) 0.178(19) 0.128(16) 0.045(9) F6 0.199(18) 0.33(3) 0.31(3) 0.22(3) 0.045(17) -0.004(18) F7 0.44(3) 0.106(9) 0.093(8) -0.020(6) 0.035(11) 0.074(13) F8 0.231(17) 0.219(16) 0.135(10) -0.049(11) 0.053(11) 0.071(12) F9 0.30(2) 0.220(15) 0.141(10) -0.062(10) -0.073(13) 0.134(15) F10 0.107(8) 0.097(7) 0.279(15) -0.013(8) -0.019(8) 0.015(6) F11 0.207(11) 0.085(6) 0.141(9) 0.008(6) 0.021(8) 0.054(7) F12 0.222(12) 0.083(6) 0.144(9) 0.028(6) -0.039(8) 0.050(7) F13 0.170(14) 0.202(17) 0.57(4) -0.20(2) 0.04(2) 0.087(13) F14 0.30(2) 0.262(17) 0.245(16) -0.033(13) -0.008(13) 0.237(18) F15 0.44(3) 0.243(16) 0.209(15) 0.053(13) 0.157(19) 0.24(2) F16 0.34(3) 0.27(2) 0.236(18) -0.006(17) -0.17(2) 0.10(2) F17 0.117(10) 0.30(2) 0.31(2) -0.14(2) -0.069(11) 0.088(12) F18 0.131(12) 0.38(3) 0.174(14) -0.093(16) 0.003(10) -0.009(14) F19 0.084(6) 0.205(12) 0.128(8) 0.000(8) 0.022(6) 0.011(7) F20 0.075(5) 0.178(10) 0.142(8) -0.032(8) -0.006(5) 0.007(6) F21 0.072(6) 0.121(8) 0.58(3) 0.028(13) 0.048(11) 0.053(6) F22 0.49(4) 0.24(2) 0.164(14) 0.081(14) 0.18(2) 0.16(2) F23 0.163(13) 0.60(4) 0.107(9) 0.002(14) 0.042(8) 0.194(19) F24 0.174(11) 0.280(18) 0.101(8) -0.086(10) 0.031(7) -0.012(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.85(4) . ? Mo1 C1 1.86(3) . ? Mo1 C6 2.13(2) . ? Mo1 N2 2.18(2) . ? Mo1 N1 2.19(2) . ? Mo1 N3 2.192(16) . ? Mo1 C5 2.30(2) . ? Mo1 C7 2.30(3) . ? C1 O1 1.12(3) . ? C2 O2 1.24(5) . ? N1 C11 1.54(4) . ? N2 C13 1.52(4) . ? N3 C15 1.42(2) . ? C5 C6 1.35(3) . ? C6 C7 1.28(4) . ? C6 C8 1.51(4) . ? C11 C12 1.52(6) . ? C11 C16 1.57(5) . ? C12 C13 1.51(6) . ? C13 C14 1.36(5) . ? C14 C15 1.45(3) . ? C15 C16 1.49(3) . ? B51 C71 1.586(18) . ? B51 C81 1.608(18) . ? B51 C61 1.633(18) . ? B51 C51 1.658(17) . ? C51 C56 1.359(16) . ? C51 C52 1.405(16) . ? C52 C53 1.382(16) . ? C53 C54 1.360(18) . ? C53 C57 1.411(19) . ? C54 C55 1.383(18) . ? C55 C56 1.355(17) . ? C55 C58 1.38(2) . ? C57 F2 1.151(17) . ? C57 F3 1.242(19) . ? C57 F1 1.270(18) . ? C58 F5 1.20(2) . ? C58 F4 1.22(2) . ? C58 F6 1.24(3) . ? C61 C66 1.369(16) . ? C61 C62 1.394(16) . ? C62 C63 1.385(17) . ? C63 C64 1.357(18) . ? C63 C67 1.48(3) . ? C64 C65 1.399(17) . ? C65 C66 1.411(16) . ? C65 C68 1.440(18) . ? C67 F8 1.18(2) . ? C67 F7 1.189(19) . ? C67 F9 1.52(3) . ? C68 F12 1.273(17) . ? C68 F11 1.307(17) . ? C68 F10 1.321(19) . ? C71 C72 1.391(18) . ? C71 C76 1.394(17) . ? C72 C73 1.42(2) . ? C73 C74 1.33(2) . ? C73 C77 1.46(3) . ? C74 C75 1.39(2) . ? C75 C78 1.39(3) . ? C75 C76 1.400(19) . ? C77 F13 1.19(3) . ? C77 F15 1.28(2) . ? C77 F14 1.34(3) . ? C78 F18 1.15(2) . ? C78 F17 1.30(3) . ? C78 F16 1.33(3) . ? C81 C86 1.382(16) . ? C81 C82 1.401(16) . ? C82 C83 1.414(17) . ? C83 C84 1.355(17) . ? C83 C87 1.456(19) . ? C84 C85 1.391(18) . ? C85 C86 1.374(17) . ? C85 C88 1.41(2) . ? C87 F21 1.26(2) . ? C87 F20 1.269(17) . ? C87 F19 1.34(2) . ? C88 F24 1.21(2) . ? C88 F22 1.25(3) . ? C88 F23 1.28(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 81(2) . . ? C2 Mo1 C6 98.9(17) . . ? C1 Mo1 C6 99.5(14) . . ? C2 Mo1 N2 91.9(16) . . ? C1 Mo1 N2 91.3(12) . . ? C6 Mo1 N2 165.8(10) . . ? C2 Mo1 N1 172.8(16) . . ? C1 Mo1 N1 99.4(18) . . ? C6 Mo1 N1 88.2(15) . . ? N2 Mo1 N1 80.9(13) . . ? C2 Mo1 N3 95.6(18) . . ? C1 Mo1 N3 170.2(14) . . ? C6 Mo1 N3 90.0(8) . . ? N2 Mo1 N3 79.6(9) . . ? N1 Mo1 N3 82.7(7) . . ? C2 Mo1 C5 103.8(13) . . ? C1 Mo1 C5 66.2(15) . . ? C6 Mo1 C5 35.3(9) . . ? N2 Mo1 C5 149.6(13) . . ? N1 Mo1 C5 82.8(10) . . ? N3 Mo1 C5 123.5(8) . . ? C2 Mo1 C7 66.7(17) . . ? C1 Mo1 C7 101.9(12) . . ? C6 Mo1 C7 33.3(11) . . ? N2 Mo1 C7 152.3(15) . . ? N1 Mo1 C7 120.0(14) . . ? N3 Mo1 C7 85.0(10) . . ? C5 Mo1 C7 57.2(11) . . ? O1 C1 Mo1 177(3) . . ? O2 C2 Mo1 172(4) . . ? C11 N1 Mo1 124.5(15) . . ? C13 N2 Mo1 123.0(15) . . ? C15 N3 Mo1 123.6(11) . . ? C6 C5 Mo1 65.5(13) . . ? C7 C6 C5 113(3) . . ? C7 C6 C8 119(3) . . ? C5 C6 C8 124(3) . . ? C7 C6 Mo1 81(2) . . ? C5 C6 Mo1 79.1(16) . . ? C8 C6 Mo1 125(2) . . ? C6 C7 Mo1 66.1(17) . . ? C12 C11 N1 107(3) . . ? C12 C11 C16 104(2) . . ? N1 C11 C16 101(3) . . ? C13 C12 C11 126(3) . . ? C14 C13 C12 102(3) . . ? C14 C13 N2 128(3) . . ? C12 C13 N2 95(5) . . ? C13 C14 C15 114(3) . . ? N3 C15 C14 115(2) . . ? N3 C15 C16 111.0(16) . . ? C14 C15 C16 110(2) . . ? C15 C16 C11 115.1(19) . . ? C71 B51 C81 113.8(10) . . ? C71 B51 C61 105.2(9) . . ? C81 B51 C61 110.9(9) . . ? C71 B51 C51 111.1(9) . . ? C81 B51 C51 104.7(9) . . ? C61 B51 C51 111.2(9) . . ? C56 C51 C52 114.6(11) . . ? C56 C51 B51 125.0(11) . . ? C52 C51 B51 120.4(9) . . ? C53 C52 C51 121.4(11) . . ? C54 C53 C52 120.3(11) . . ? C54 C53 C57 119.8(13) . . ? C52 C53 C57 119.8(13) . . ? C53 C54 C55 119.9(12) . . ? C56 C55 C58 120.1(14) . . ? C56 C55 C54 117.7(12) . . ? C58 C55 C54 122.1(14) . . ? C55 C56 C51 126.1(13) . . ? F2 C57 F3 103(2) . . ? F2 C57 F1 101.2(17) . . ? F3 C57 F1 96.1(16) . . ? F2 C57 C53 118.6(15) . . ? F3 C57 C53 117.7(14) . . ? F1 C57 C53 116.8(16) . . ? F5 C58 F4 97(2) . . ? F5 C58 F6 97(2) . . ? F4 C58 F6 100(2) . . ? F5 C58 C55 122.7(18) . . ? F4 C58 C55 118(2) . . ? F6 C58 C55 117(2) . . ? C66 C61 C62 113.8(11) . . ? C66 C61 B51 121.8(11) . . ? C62 C61 B51 124.0(10) . . ? C63 C62 C61 125.1(11) . . ? C64 C63 C62 118.7(12) . . ? C64 C63 C67 122.6(13) . . ? C62 C63 C67 117.8(13) . . ? C63 C64 C65 120.0(12) . . ? C64 C65 C66 118.2(11) . . ? C64 C65 C68 119.7(12) . . ? C66 C65 C68 121.9(13) . . ? C61 C66 C65 124.0(11) . . ? F8 C67 F7 125(3) . . ? F8 C67 C63 116.3(17) . . ? F7 C67 C63 117.9(18) . . ? F8 C67 F9 87.4(16) . . ? F7 C67 F9 91(2) . . ? C63 C67 F9 99(2) . . ? F12 C68 F11 104.5(14) . . ? F12 C68 F10 104.4(14) . . ? F11 C68 F10 103.5(15) . . ? F12 C68 C65 115.1(14) . . ? F11 C68 C65 114.2(13) . . ? F10 C68 C65 113.9(14) . . ? C72 C71 C76 116.6(12) . . ? C72 C71 B51 121.8(12) . . ? C76 C71 B51 121.3(11) . . ? C71 C72 C73 120.4(14) . . ? C74 C73 C72 121.4(15) . . ? C74 C73 C77 122(2) . . ? C72 C73 C77 116(2) . . ? C73 C74 C75 120.4(14) . . ? C74 C75 C78 121.9(18) . . ? C74 C75 C76 118.5(15) . . ? C78 C75 C76 119(2) . . ? C71 C76 C75 122.6(14) . . ? F13 C77 F15 111(3) . . ? F13 C77 F14 103(2) . . ? F15 C77 F14 95.0(19) . . ? F13 C77 C73 121(2) . . ? F15 C77 C73 111(2) . . ? F14 C77 C73 111(3) . . ? F18 C78 F17 101(3) . . ? F18 C78 F16 102(2) . . ? F17 C78 F16 93(2) . . ? F18 C78 C75 123(2) . . ? F17 C78 C75 119.6(18) . . ? F16 C78 C75 113(3) . . ? C86 C81 C82 115.1(11) . . ? C86 C81 B51 121.7(10) . . ? C82 C81 B51 123.0(10) . . ? C81 C82 C83 121.4(11) . . ? C84 C83 C82 120.5(12) . . ? C84 C83 C87 120.0(14) . . ? C82 C83 C87 119.5(13) . . ? C83 C84 C85 119.3(13) . . ? C86 C85 C84 119.2(11) . . ? C86 C85 C88 123.8(14) . . ? C84 C85 C88 117.0(14) . . ? C85 C86 C81 124.3(12) . . ? F21 C87 F20 107.6(18) . . ? F21 C87 F19 103.8(16) . . ? F20 C87 F19 101.6(16) . . ? F21 C87 C83 113.9(16) . . ? F20 C87 C83 115.0(14) . . ? F19 C87 C83 113.6(16) . . ? F24 C88 F22 103(2) . . ? F24 C88 F23 104(2) . . ? F22 C88 F23 92.4(19) . . ? F24 C88 C85 123.1(17) . . ? F22 C88 C85 115(2) . . ? F23 C88 C85 115(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.46 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.484 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.068 #===END data_Compound_5_(sn51a) _database_code_depnum_ccdc_archive 'CCDC 254977' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H17 F3 Mo N6 O5 S' _chemical_formula_weight 546.35 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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 21.900(5) _cell_length_b 26.529(6) _cell_length_c 7.3441(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4266.8(16) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.766737 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18771 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6065 _reflns_number_gt 4827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 6065 _refine_ls_number_parameters 559 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.52000(3) 0.36999(2) 0.6879(2) 0.04439(18) Uani 1 1 d D . . C2 C 0.5973(4) 0.3928(3) 0.7853(13) 0.066(3) Uani 1 1 d D . . O2 O 0.6426(3) 0.4076(3) 0.8299(13) 0.108(3) Uani 1 1 d D . . N1 N 0.5744(3) 0.3130(2) 0.5341(9) 0.0421(15) Uani 1 1 d . . . N2 N 0.6500(4) 0.2791(4) 0.3882(12) 0.087(3) Uani 1 1 d . . . H2 H 0.6834 0.2764 0.3276 0.104 Uiso 1 1 calc R . . N3 N 0.4413(3) 0.3355(2) 0.5231(10) 0.0483(16) Uani 1 1 d . . . N4 N 0.3890(3) 0.3012(3) 0.3047(11) 0.065(2) Uani 1 1 d . . . H4 H 0.3806 0.2874 0.2018 0.077 Uiso 1 1 calc R . . N5 N 0.5088(3) 0.3017(3) 0.8739(9) 0.0549(18) Uani 1 1 d . . . N6 N 0.4798(5) 0.2304(3) 0.9872(11) 0.082(3) Uani 1 1 d . . . H6 H 0.4567 0.2052 1.0125 0.099 Uiso 1 1 calc R . . C1 C 0.5392(4) 0.4205(3) 0.5056(15) 0.064(3) Uani 1 1 d . . . O1 O 0.5531(4) 0.4504(3) 0.3983(14) 0.114(3) Uani 1 1 d . . . C3 C 0.5053(5) 0.4131(4) 0.9596(15) 0.089(3) Uani 1 1 d D . . H3A H 0.5093 0.3937 1.0709 0.107 Uiso 1 1 calc R . . H3B H 0.5222 0.4468 0.9673 0.107 Uiso 1 1 calc R . . C4 C 0.4555(5) 0.4082(4) 0.8718(16) 0.080(3) Uani 1 1 d D . . H4A H 0.4204 0.3904 0.9241 0.096 Uiso 1 1 calc R . . C5 C 0.4505(4) 0.4360(4) 0.7059(19) 0.095(4) Uani 1 1 d D . . H5A H 0.4671 0.4699 0.7054 0.113 Uiso 1 1 calc R . . H5B H 0.4128 0.4325 0.6377 0.113 Uiso 1 1 calc R . . C11 C 0.5688(4) 0.2629(3) 0.5347(13) 0.057(2) Uani 1 1 d . . . H11 H 0.5374 0.2456 0.5924 0.068 Uiso 1 1 calc R . . C12 C 0.6143(4) 0.2403(4) 0.4418(14) 0.069(3) Uani 1 1 d . . . H12 H 0.6198 0.2061 0.4198 0.083 Uiso 1 1 calc R . . C13 C 0.6253(4) 0.3224(4) 0.4437(12) 0.058(2) Uani 1 1 d . . . H13 H 0.6413 0.3543 0.4222 0.070 Uiso 1 1 calc R . . C14 C 0.3803(4) 0.3310(3) 0.5731(14) 0.067(3) Uani 1 1 d . . . H14 H 0.3638 0.3408 0.6843 0.080 Uiso 1 1 calc R . . C15 C 0.3498(4) 0.3107(4) 0.4380(15) 0.070(3) Uani 1 1 d . . . H15 H 0.3081 0.3042 0.4361 0.084 Uiso 1 1 calc R . . C16 C 0.4440(4) 0.3170(3) 0.3598(12) 0.058(2) Uani 1 1 d . . . H16 H 0.4794 0.3150 0.2903 0.069 Uiso 1 1 calc R . . C17 C 0.5551(5) 0.2817(4) 0.9810(14) 0.069(3) Uani 1 1 d . . . H17 H 0.5925 0.2970 1.0040 0.083 Uiso 1 1 calc R . . C18 C 0.4641(5) 0.2689(3) 0.8847(12) 0.065(2) Uani 1 1 d . . . H18 H 0.4264 0.2724 0.8276 0.078 Uiso 1 1 calc R . . C19 C 0.5373(6) 0.2364(4) 1.0466(15) 0.093(3) Uani 1 1 d . . . H19 H 0.5600 0.2142 1.1174 0.112 Uiso 1 1 calc R . . Mo51 Mo 0.23153(3) 0.44328(2) 0.15586(19) 0.0566(2) Uani 1 1 d D . . C52 C 0.2051(6) 0.3830(5) 0.282(2) 0.236(15) Uani 1 1 d D . . O52 O 0.1911(5) 0.3534(4) 0.3812(15) 0.172(5) Uani 1 1 d D . . N51 N 0.1682(3) 0.5018(2) 0.2828(10) 0.0533(18) Uani 1 1 d . . . N52 N 0.1326(7) 0.5655(4) 0.4296(14) 0.113(5) Uani 1 1 d . . . H52 H 0.1307 0.5947 0.4801 0.135 Uiso 1 1 calc R . . N53 N 0.1533(4) 0.4313(3) -0.0401(11) 0.070(2) Uani 1 1 d . . . N54 N 0.0970(6) 0.3986(5) -0.255(2) 0.144(6) Uani 1 1 d . . . H54 H 0.0852 0.3782 -0.3388 0.173 Uiso 1 1 calc R . . N55 N 0.2539(4) 0.5050(3) -0.0457(10) 0.066(2) Uani 1 1 d . . . N56 N 0.2513(5) 0.5695(3) -0.2220(13) 0.094(3) Uani 1 1 d . . . H56 H 0.2381 0.5967 -0.2714 0.113 Uiso 1 1 calc R . . C51 C 0.2807(4) 0.3945(3) 0.0331(12) 0.057(2) Uani 1 1 d . . . O51 O 0.3109(3) 0.3629(3) -0.0331(12) 0.091(2) Uani 1 1 d . . . C53 C 0.3431(5) 0.4547(4) 0.252(2) 0.140(8) Uani 1 1 d D . . H53A H 0.3638 0.4263 0.3076 0.168 Uiso 1 1 calc R . . H53B H 0.3687 0.4766 0.1791 0.168 Uiso 1 1 calc R . . C54 C 0.2988(6) 0.4745(5) 0.338(2) 0.178(10) Uani 1 1 d D . . H54A H 0.2990 0.5108 0.3632 0.214 Uiso 1 1 calc R . . C55 C 0.2637(8) 0.4414(7) 0.451(2) 0.41(3) Uani 1 1 d D . . H55A H 0.2373 0.4569 0.5410 0.493 Uiso 1 1 calc R . . H55B H 0.2835 0.4108 0.4924 0.493 Uiso 1 1 calc R . . C61 C 0.1110(5) 0.4922(4) 0.3463(16) 0.082(3) Uani 1 1 d . . . H61 H 0.0897 0.4622 0.3298 0.099 Uiso 1 1 calc R . . C62 C 0.0906(7) 0.5317(7) 0.4343(19) 0.122(6) Uani 1 1 d . . . H62 H 0.0526 0.5347 0.4900 0.146 Uiso 1 1 calc R . . C63 C 0.1795(5) 0.5476(4) 0.3330(15) 0.081(3) Uani 1 1 d . . . H63 H 0.2150 0.5654 0.3059 0.097 Uiso 1 1 calc R . . C64 C 0.1470(6) 0.3927(5) -0.146(3) 0.142(7) Uani 1 1 d . . . H64 H 0.1729 0.3649 -0.1472 0.171 Uiso 1 1 calc R . . C65 C 0.0717(7) 0.4389(6) -0.2116(18) 0.113(5) Uani 1 1 d . . . H65 H 0.0356 0.4513 -0.2613 0.136 Uiso 1 1 calc R . . C66 C 0.1041(7) 0.4611(5) -0.0844(18) 0.120(5) Uani 1 1 d . . . H66 H 0.0952 0.4922 -0.0322 0.144 Uiso 1 1 calc R . . C67 C 0.2236(7) 0.5434(6) -0.0945(19) 0.144(7) Uani 1 1 d . . . H67 H 0.1859 0.5522 -0.0454 0.172 Uiso 1 1 calc R . . C68 C 0.2997(6) 0.5479(6) -0.258(2) 0.133(6) Uani 1 1 d . . . H68 H 0.3283 0.5580 -0.3443 0.159 Uiso 1 1 calc R . . C69 C 0.3035(6) 0.5070(5) -0.150(2) 0.124(6) Uani 1 1 d . . . H69 H 0.3354 0.4839 -0.1490 0.148 Uiso 1 1 calc R . . S1 S 0.47680(12) 0.11836(9) 0.3471(4) 0.0723(7) Uani 1 1 d . . . O91 O 0.5332(3) 0.1401(3) 0.3901(14) 0.104(3) Uani 1 1 d . . . O92 O 0.4704(5) 0.0681(3) 0.3997(17) 0.141(4) Uani 1 1 d . . . O93 O 0.4550(4) 0.1310(3) 0.1684(13) 0.108(2) Uani 1 1 d . . . C90 C 0.4230(5) 0.1499(4) 0.4892(19) 0.085(3) Uani 1 1 d . . . F1 F 0.4387(4) 0.1444(3) 0.6638(13) 0.150(3) Uani 1 1 d . . . F2 F 0.4241(3) 0.1989(3) 0.4654(13) 0.132(3) Uani 1 1 d . . . F3 F 0.3689(3) 0.1340(4) 0.4762(16) 0.167(4) Uani 1 1 d . . . S2 S 0.79032(11) 0.29527(10) 1.0373(4) 0.0634(6) Uani 1 1 d . . . O94 O 0.7800(8) 0.3426(4) 1.0711(19) 0.260(10) Uani 1 1 d . . . O95 O 0.7636(5) 0.2645(5) 1.1633(18) 0.183(5) Uani 1 1 d . . . O96 O 0.8475(4) 0.2786(7) 1.0143(16) 0.219(8) Uani 1 1 d . . . C91 C 0.7510(5) 0.2807(5) 0.8302(18) 0.082(3) Uani 1 1 d . . . F4 F 0.6955(4) 0.2856(5) 0.8380(17) 0.215(6) Uani 1 1 d . . . F5 F 0.7697(5) 0.3056(6) 0.6999(13) 0.232(7) Uani 1 1 d . . . F6 F 0.7584(7) 0.2369(5) 0.780(2) 0.240(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0487(3) 0.0360(3) 0.0486(4) -0.0074(3) -0.0001(4) -0.0011(3) C2 0.070(6) 0.054(5) 0.072(7) -0.013(5) -0.019(5) -0.015(5) O2 0.100(6) 0.099(6) 0.125(7) -0.035(5) -0.021(6) -0.033(5) N1 0.042(4) 0.040(4) 0.045(4) -0.005(3) 0.003(3) 0.001(3) N2 0.054(5) 0.131(8) 0.075(6) -0.025(6) 0.007(4) 0.043(6) N3 0.042(4) 0.049(4) 0.054(5) -0.003(3) 0.002(3) -0.002(3) N4 0.060(5) 0.074(5) 0.059(5) -0.012(4) -0.013(4) -0.011(4) N5 0.065(5) 0.058(4) 0.042(4) 0.002(3) 0.005(4) -0.001(4) N6 0.134(8) 0.059(5) 0.054(5) 0.009(4) 0.013(6) -0.018(5) C1 0.057(5) 0.046(5) 0.090(8) -0.010(5) -0.001(5) -0.003(4) O1 0.143(7) 0.065(5) 0.136(8) 0.046(5) 0.002(6) -0.026(5) C3 0.113(9) 0.075(7) 0.079(8) -0.040(6) 0.012(8) -0.011(6) C4 0.063(7) 0.097(8) 0.079(8) -0.039(7) 0.011(6) -0.001(6) C5 0.089(7) 0.064(6) 0.131(12) -0.059(8) -0.021(8) 0.038(5) C11 0.051(5) 0.051(5) 0.067(6) -0.008(5) 0.010(5) 0.001(4) C12 0.070(6) 0.072(7) 0.065(7) -0.006(5) 0.017(5) 0.007(5) C13 0.040(5) 0.075(6) 0.059(6) 0.003(5) 0.001(5) -0.014(4) C14 0.043(5) 0.081(7) 0.077(7) -0.025(5) 0.001(5) 0.003(4) C15 0.042(5) 0.076(7) 0.093(8) -0.005(6) -0.014(6) -0.010(5) C16 0.059(6) 0.065(6) 0.049(6) -0.004(5) 0.004(5) -0.009(4) C17 0.079(6) 0.070(7) 0.057(6) 0.002(5) -0.006(6) 0.002(5) C18 0.090(7) 0.069(6) 0.036(5) 0.003(5) 0.006(5) -0.025(5) C19 0.146(11) 0.091(9) 0.043(6) 0.007(6) -0.020(7) 0.005(8) Mo51 0.0704(4) 0.0486(4) 0.0508(4) 0.0077(4) 0.0142(5) 0.0166(3) C52 0.074(8) 0.28(2) 0.35(3) 0.28(2) 0.053(13) 0.048(11) O52 0.143(9) 0.216(12) 0.159(11) 0.001(10) 0.016(8) -0.064(9) N51 0.065(5) 0.040(4) 0.055(4) 0.000(3) 0.000(4) 0.005(3) N52 0.191(14) 0.091(8) 0.057(6) -0.032(6) -0.031(8) 0.079(8) N53 0.075(5) 0.072(5) 0.064(5) 0.001(4) 0.024(4) 0.003(4) N54 0.094(8) 0.151(11) 0.188(15) -0.077(11) -0.003(9) -0.027(7) N55 0.085(6) 0.063(5) 0.049(5) 0.011(4) 0.003(4) 0.016(4) N56 0.144(10) 0.071(6) 0.068(6) 0.019(5) -0.008(6) 0.008(6) C51 0.064(5) 0.049(5) 0.057(6) 0.008(4) 0.015(5) -0.002(4) O51 0.085(5) 0.084(5) 0.106(6) -0.007(5) 0.019(5) 0.020(4) C53 0.055(6) 0.079(8) 0.29(3) 0.041(10) 0.018(10) -0.008(6) C54 0.105(11) 0.28(2) 0.154(16) 0.164(17) -0.008(11) 0.023(14) C55 0.78(7) 0.35(4) 0.104(15) -0.058(19) -0.17(3) 0.46(5) C61 0.087(8) 0.082(7) 0.077(8) 0.013(6) 0.025(6) 0.022(6) C62 0.123(12) 0.169(16) 0.073(9) 0.000(11) 0.019(9) 0.088(11) C63 0.109(9) 0.065(7) 0.068(7) -0.008(5) -0.008(7) 0.002(6) C64 0.065(8) 0.096(9) 0.27(2) -0.062(12) -0.026(11) 0.013(7) C65 0.135(12) 0.148(13) 0.058(8) 0.004(8) -0.007(8) 0.021(10) C66 0.184(14) 0.100(10) 0.076(9) -0.002(7) -0.049(10) 0.057(9) C67 0.197(15) 0.140(12) 0.094(10) 0.084(10) 0.065(11) 0.082(11) C68 0.106(10) 0.149(13) 0.143(15) 0.079(11) 0.033(10) -0.012(9) C69 0.088(8) 0.139(12) 0.143(12) 0.079(10) 0.056(9) 0.025(8) S1 0.0792(17) 0.0526(14) 0.0851(19) 0.0083(12) -0.0147(15) -0.0057(12) O91 0.054(4) 0.101(5) 0.159(9) 0.021(5) -0.017(5) -0.013(4) O92 0.174(9) 0.063(5) 0.186(11) 0.024(6) 0.001(8) 0.004(5) O93 0.140(6) 0.102(5) 0.081(5) -0.009(6) -0.018(6) -0.022(4) C90 0.074(7) 0.078(8) 0.105(10) 0.015(7) 0.000(7) -0.012(6) F1 0.180(7) 0.182(7) 0.087(6) 0.027(7) 0.021(7) -0.001(6) F2 0.135(6) 0.077(5) 0.184(9) 0.003(5) 0.023(6) 0.018(4) F3 0.073(5) 0.190(9) 0.237(12) -0.043(8) 0.018(6) -0.039(5) S2 0.0613(14) 0.0688(16) 0.0602(16) -0.0017(12) -0.0046(12) 0.0146(11) O94 0.45(2) 0.140(9) 0.188(13) -0.097(9) -0.184(15) 0.164(13) O95 0.212(11) 0.226(11) 0.111(8) 0.064(10) -0.056(10) -0.046(9) O96 0.080(6) 0.46(2) 0.116(9) -0.088(12) -0.026(6) 0.052(9) C91 0.066(7) 0.093(8) 0.087(9) -0.010(7) -0.018(6) 0.024(6) F4 0.074(5) 0.393(17) 0.178(10) -0.058(11) -0.056(6) 0.019(8) F5 0.258(12) 0.357(17) 0.081(7) 0.070(9) -0.059(8) -0.163(12) F6 0.327(15) 0.171(10) 0.224(13) -0.117(10) -0.139(12) 0.083(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.936(8) . ? Mo1 C1 1.941(11) . ? Mo1 C4 2.202(10) . ? Mo1 N1 2.232(6) . ? Mo1 N5 2.283(7) . ? Mo1 N3 2.296(6) . ? Mo1 C3 2.322(10) . ? Mo1 C5 2.325(8) . ? C2 O2 1.116(8) . ? N1 C13 1.322(9) . ? N1 C11 1.334(10) . ? N2 C13 1.333(11) . ? N2 C12 1.352(12) . ? N3 C16 1.298(11) . ? N3 C14 1.389(10) . ? N4 C15 1.325(12) . ? N4 C16 1.338(10) . ? N5 C18 1.313(10) . ? N5 C17 1.388(11) . ? N6 C18 1.314(12) . ? N6 C19 1.343(13) . ? C1 O1 1.157(12) . ? C3 C4 1.273(12) . ? C4 C5 1.430(15) . ? C11 C12 1.347(12) . ? C14 C15 1.312(12) . ? C17 C19 1.351(14) . ? Mo51 C51 1.908(9) . ? Mo51 C52 1.936(8) . ? Mo51 C54 2.156(18) . ? Mo51 N53 2.260(9) . ? Mo51 N55 2.261(7) . ? Mo51 C55 2.280(17) . ? Mo51 N51 2.281(7) . ? Mo51 C53 2.562(12) . ? C52 O52 1.115(8) . ? N51 C63 1.294(11) . ? N51 C61 1.361(12) . ? N52 C62 1.286(18) . ? N52 C63 1.337(15) . ? N53 C64 1.292(15) . ? N53 C66 1.375(14) . ? N54 C65 1.247(15) . ? N54 C64 1.366(18) . ? N55 C67 1.269(13) . ? N55 C69 1.330(13) . ? N56 C68 1.233(15) . ? N56 C67 1.312(15) . ? C51 O51 1.174(10) . ? C53 C54 1.270(12) . ? C54 C55 1.431(15) . ? C61 C62 1.309(17) . ? C65 C66 1.312(18) . ? C68 C69 1.347(16) . ? S1 O92 1.394(8) . ? S1 O91 1.401(7) . ? S1 O93 1.437(10) . ? S1 C90 1.782(12) . ? C90 F3 1.262(12) . ? C90 F2 1.312(12) . ? C90 F1 1.336(15) . ? S2 O94 1.299(10) . ? S2 O96 1.339(9) . ? S2 O95 1.364(11) . ? S2 C91 1.790(12) . ? C91 F4 1.224(12) . ? C91 F6 1.229(14) . ? C91 F5 1.232(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 C2 Mo1 C1 81.3(4) . . ? C2 Mo1 C4 101.0(4) . . ? C1 Mo1 C4 104.2(4) . . ? C2 Mo1 N1 86.1(3) . . ? C1 Mo1 N1 90.2(3) . . ? C4 Mo1 N1 164.7(3) . . ? C2 Mo1 N5 96.9(3) . . ? C1 Mo1 N5 169.9(3) . . ? C4 Mo1 N5 85.9(4) . . ? N1 Mo1 N5 79.7(2) . . ? C2 Mo1 N3 167.5(3) . . ? C1 Mo1 N3 94.3(3) . . ? C4 Mo1 N3 91.4(3) . . ? N1 Mo1 N3 82.2(2) . . ? N5 Mo1 N3 85.3(2) . . ? C2 Mo1 C3 69.5(4) . . ? C1 Mo1 C3 106.4(4) . . ? C4 Mo1 C3 32.5(3) . . ? N1 Mo1 C3 147.4(3) . . ? N5 Mo1 C3 82.0(3) . . ? N3 Mo1 C3 123.0(3) . . ? C2 Mo1 C5 108.4(4) . . ? C1 Mo1 C5 70.2(4) . . ? C4 Mo1 C5 36.7(4) . . ? N1 Mo1 C5 152.7(4) . . ? N5 Mo1 C5 119.6(4) . . ? N3 Mo1 C5 80.7(3) . . ? C3 Mo1 C5 59.3(4) . . ? O2 C2 Mo1 175.0(10) . . ? C13 N1 C11 105.5(7) . . ? C13 N1 Mo1 125.1(6) . . ? C11 N1 Mo1 128.7(5) . . ? C13 N2 C12 109.4(8) . . ? C16 N3 C14 104.8(7) . . ? C16 N3 Mo1 127.1(5) . . ? C14 N3 Mo1 128.1(6) . . ? C15 N4 C16 107.4(8) . . ? C18 N5 C17 104.9(8) . . ? C18 N5 Mo1 130.0(6) . . ? C17 N5 Mo1 124.4(6) . . ? C18 N6 C19 109.9(9) . . ? O1 C1 Mo1 177.4(9) . . ? C4 C3 Mo1 68.5(6) . . ? C3 C4 C5 116.4(10) . . ? C3 C4 Mo1 78.9(6) . . ? C5 C4 Mo1 76.3(6) . . ? C4 C5 Mo1 67.0(5) . . ? N1 C11 C12 112.0(8) . . ? C11 C12 N2 103.7(9) . . ? N1 C13 N2 109.5(8) . . ? C15 C14 N3 109.0(8) . . ? C14 C15 N4 107.9(8) . . ? N3 C16 N4 110.9(8) . . ? C19 C17 N5 109.4(9) . . ? N5 C18 N6 110.7(9) . . ? N6 C19 C17 105.0(10) . . ? C51 Mo51 C52 80.5(5) . . ? C51 Mo51 C54 99.7(5) . . ? C52 Mo51 C54 103.0(6) . . ? C51 Mo51 N53 91.8(3) . . ? C52 Mo51 N53 87.8(5) . . ? C54 Mo51 N53 165.3(4) . . ? C51 Mo51 N55 93.4(3) . . ? C52 Mo51 N55 167.3(6) . . ? C54 Mo51 N55 88.9(4) . . ? N53 Mo51 N55 81.3(3) . . ? C51 Mo51 C55 105.1(5) . . ? C52 Mo51 C55 67.7(7) . . ? C54 Mo51 C55 37.5(4) . . ? N53 Mo51 C55 146.8(5) . . ? N55 Mo51 C55 124.8(5) . . ? C51 Mo51 N51 175.5(3) . . ? C52 Mo51 N51 100.7(5) . . ? C54 Mo51 N51 84.3(4) . . ? N53 Mo51 N51 84.0(3) . . ? N55 Mo51 N51 84.7(3) . . ? C55 Mo51 N51 79.3(4) . . ? C51 Mo51 C53 70.9(4) . . ? C52 Mo51 C53 104.5(5) . . ? C54 Mo51 C53 29.7(4) . . ? N53 Mo51 C53 156.3(4) . . ? N55 Mo51 C53 83.6(4) . . ? C55 Mo51 C53 56.3(5) . . ? N51 Mo51 C53 112.7(4) . . ? O52 C52 Mo51 167.6(16) . . ? C63 N51 C61 104.8(9) . . ? C63 N51 Mo51 129.7(7) . . ? C61 N51 Mo51 124.9(6) . . ? C62 N52 C63 108.4(11) . . ? C64 N53 C66 103.3(11) . . ? C64 N53 Mo51 125.0(9) . . ? C66 N53 Mo51 131.6(8) . . ? C65 N54 C64 107.7(12) . . ? C67 N55 C69 103.4(10) . . ? C67 N55 Mo51 130.8(8) . . ? C69 N55 Mo51 125.7(7) . . ? C68 N56 C67 107.9(11) . . ? O51 C51 Mo51 176.0(8) . . ? C54 C53 Mo51 57.2(9) . . ? C53 C54 C55 116.4(10) . . ? C53 C54 Mo51 93.1(11) . . ? C55 C54 Mo51 75.9(10) . . ? C54 C55 Mo51 66.6(9) . . ? C62 C61 N51 109.5(12) . . ? N52 C62 C61 107.5(13) . . ? N51 C63 N52 109.7(11) . . ? N53 C64 N54 110.3(11) . . ? N54 C65 C66 109.0(14) . . ? C65 C66 N53 109.6(13) . . ? N55 C67 N56 112.5(12) . . ? N56 C68 C69 107.4(12) . . ? N55 C69 C68 108.8(11) . . ? O92 S1 O91 114.9(6) . . ? O92 S1 O93 116.3(6) . . ? O91 S1 O93 113.7(5) . . ? O92 S1 C90 102.7(6) . . ? O91 S1 C90 104.9(6) . . ? O93 S1 C90 101.9(6) . . ? F3 C90 F2 109.7(10) . . ? F3 C90 F1 106.2(11) . . ? F2 C90 F1 103.4(11) . . ? F3 C90 S1 114.8(10) . . ? F2 C90 S1 112.1(8) . . ? F1 C90 S1 109.9(8) . . ? O94 S2 O96 120.5(11) . . ? O94 S2 O95 111.9(11) . . ? O96 S2 O95 106.8(9) . . ? O94 S2 C91 106.7(6) . . ? O96 S2 C91 105.7(6) . . ? O95 S2 C91 103.9(7) . . ? F4 C91 F6 104.1(13) . . ? F4 C91 F5 108.0(12) . . ? F6 C91 F5 103.3(13) . . ? F4 C91 S2 114.5(10) . . ? F6 C91 S2 113.4(9) . . ? F5 C91 S2 112.6(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.668 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.076 #===END data_Compound_6_(sn131am) _database_code_depnum_ccdc_archive 'CCDC 254978' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H49 B F24 Mo N6 O3' _chemical_formula_weight 1416.76 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' B B 0.0013 0.0007 '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 13.209(3) _cell_length_b 13.564(3) _cell_length_c 17.510(4) _cell_angle_alpha 86.569(4) _cell_angle_beta 79.445(4) _cell_angle_gamma 89.789(5) _cell_volume 3078.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.735995 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13941 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 23.30 _reflns_number_total 8784 _reflns_number_gt 6621 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0946P)^2^+3.3075P] 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 8784 _refine_ls_number_parameters 837 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.49870(4) 0.25353(3) 0.39360(2) 0.04484(18) Uani 1 1 d . . . C1 C 0.5939(5) 0.3554(5) 0.4123(3) 0.0616(16) Uani 1 1 d . . . O1 O 0.6534(4) 0.4103(4) 0.4261(3) 0.0938(16) Uani 1 1 d . . . C2 C 0.5954(5) 0.1722(5) 0.4399(4) 0.0642(16) Uani 1 1 d . . . O2 O 0.6567(4) 0.1266(4) 0.4677(3) 0.1013(17) Uani 1 1 d . . . N1 N 0.4138(3) 0.3567(3) 0.3168(2) 0.0457(10) Uani 1 1 d . . . N2 N 0.3142(4) 0.3487(4) 0.3079(3) 0.0536(12) Uani 1 1 d . . . H2 H 0.270(4) 0.321(4) 0.337(3) 0.053(19) Uiso 1 1 d . . . N3 N 0.4115(3) 0.1176(3) 0.3607(2) 0.0489(11) Uani 1 1 d . . . N4 N 0.3086(4) 0.1027(4) 0.3811(3) 0.0551(13) Uani 1 1 d . . . H4 H 0.272(3) 0.147(3) 0.393(3) 0.023(14) Uiso 1 1 d . . . N5 N 0.5909(3) 0.2342(3) 0.2766(2) 0.0460(10) Uani 1 1 d . . . N6 N 0.5423(4) 0.2171(3) 0.2170(2) 0.0492(12) Uani 1 1 d . . . H6 H 0.483(3) 0.213(3) 0.226(2) 0.005(10) Uiso 1 1 d . . . C3 C 0.4189(5) 0.3585(5) 0.4864(3) 0.0713(18) Uani 1 1 d . . . H3A H 0.4561 0.3735 0.5272 0.086 Uiso 1 1 calc R . . H3B H 0.3818 0.4142 0.4679 0.086 Uiso 1 1 calc R . . C4 C 0.3712(5) 0.2668(5) 0.4927(3) 0.0618(16) Uani 1 1 d . . . H4A H 0.2994 0.2602 0.4865 0.074 Uiso 1 1 calc R . . C5 C 0.4258(5) 0.1856(5) 0.5160(3) 0.0731(19) Uani 1 1 d . . . H5A H 0.3931 0.1213 0.5183 0.088 Uiso 1 1 calc R . . H5B H 0.4634 0.1943 0.5578 0.088 Uiso 1 1 calc R . . C11 C 0.2892(5) 0.4140(4) 0.2535(4) 0.0617(16) Uani 1 1 d . . . C12 C 0.3760(5) 0.4651(4) 0.2244(3) 0.0647(16) Uani 1 1 d . . . H12 H 0.3836 0.5148 0.1848 0.078 Uiso 1 1 calc R . . C13 C 0.4522(4) 0.4306(4) 0.2637(3) 0.0497(13) Uani 1 1 d . . . C14 C 0.1828(6) 0.4224(6) 0.2379(5) 0.095(2) Uani 1 1 d . . . H14A H 0.1592 0.4889 0.2446 0.142 Uiso 1 1 d R . . H14B H 0.1382 0.3779 0.2735 0.142 Uiso 1 1 d R . . H14C H 0.1820 0.4057 0.1855 0.142 Uiso 1 1 d R . . C15 C 0.5592(5) 0.4682(5) 0.2536(4) 0.0769(19) Uani 1 1 d . . . H15A H 0.5741 0.4833 0.3033 0.115 Uiso 1 1 calc R . . H15B H 0.5669 0.5269 0.2195 0.115 Uiso 1 1 calc R . . H15C H 0.6061 0.4188 0.2315 0.115 Uiso 1 1 calc R . . C21 C 0.4472(5) 0.0284(4) 0.3381(3) 0.0561(14) Uani 1 1 d . . . C22 C 0.3656(5) -0.0376(4) 0.3439(4) 0.0687(17) Uani 1 1 d . . . H22 H 0.3701 -0.1029 0.3304 0.082 Uiso 1 1 calc R . . C23 C 0.2788(5) 0.0104(5) 0.3726(4) 0.0645(16) Uani 1 1 d . . . C24 C 0.5573(5) 0.0062(5) 0.3122(4) 0.0782(19) Uani 1 1 d . . . H24A H 0.5783 0.0292 0.2587 0.117 Uiso 1 1 calc R . . H24B H 0.5674 -0.0638 0.3173 0.117 Uiso 1 1 calc R . . H24C H 0.5975 0.0388 0.3437 0.117 Uiso 1 1 calc R . . C25 C 0.1693(6) -0.0237(6) 0.3925(6) 0.109(3) Uani 1 1 d . . . H25A H 0.1448 -0.0198 0.4473 0.164 Uiso 1 1 calc R . . H25B H 0.1647 -0.0908 0.3789 0.164 Uiso 1 1 calc R . . H25C H 0.1279 0.0175 0.3641 0.164 Uiso 1 1 calc R . . C31 C 0.6080(5) 0.2069(5) 0.1499(3) 0.0654(17) Uani 1 1 d . . . C32 C 0.7036(5) 0.2185(5) 0.1665(4) 0.0727(19) Uani 1 1 d . . . H32 H 0.7657 0.2158 0.1317 0.087 Uiso 1 1 calc R . . C33 C 0.6915(4) 0.2348(4) 0.2447(4) 0.0590(15) Uani 1 1 d . . . C34 C 0.5721(6) 0.1858(7) 0.0765(4) 0.105(3) Uani 1 1 d . . . H34A H 0.5324 0.1257 0.0844 0.157 Uiso 1 1 calc R . . H34B H 0.6306 0.1788 0.0357 0.157 Uiso 1 1 calc R . . H34C H 0.5302 0.2393 0.0621 0.157 Uiso 1 1 calc R . . C35 C 0.7753(5) 0.2531(6) 0.2891(5) 0.091(2) Uani 1 1 d . . . H35A H 0.7743 0.3211 0.3017 0.137 Uiso 1 1 calc R . . H35B H 0.8407 0.2386 0.2579 0.137 Uiso 1 1 calc R . . H35C H 0.7648 0.2114 0.3362 0.137 Uiso 1 1 calc R . . B51 B 0.1587(4) 0.7876(4) 0.1413(3) 0.0395(13) Uani 1 1 d . . . C51 C 0.2536(3) 0.7617(3) 0.1889(3) 0.0377(11) Uani 1 1 d . . . C52 C 0.2409(4) 0.7150(3) 0.2624(3) 0.0409(12) Uani 1 1 d . . . H52 H 0.1748 0.6976 0.2881 0.049 Uiso 1 1 calc R . . C53 C 0.3236(4) 0.6931(4) 0.2993(3) 0.0450(12) Uani 1 1 d . . . C54 C 0.4223(4) 0.7168(4) 0.2627(3) 0.0520(14) Uani 1 1 d . . . H54 H 0.4776 0.7017 0.2872 0.062 Uiso 1 1 calc R . . C55 C 0.4385(4) 0.7631(4) 0.1896(3) 0.0472(13) Uani 1 1 d . . . C56 C 0.3555(4) 0.7854(4) 0.1539(3) 0.0437(12) Uani 1 1 d . . . H56 H 0.3677 0.8175 0.1046 0.052 Uiso 1 1 calc R . . C57 C 0.3036(5) 0.6463(5) 0.3793(4) 0.0665(17) Uani 1 1 d . . . C58 C 0.5426(5) 0.7916(6) 0.1487(5) 0.0755(19) Uani 1 1 d . . . C61 C 0.1785(3) 0.8995(4) 0.1007(3) 0.0397(11) Uani 1 1 d . . . C62 C 0.2109(4) 0.9758(4) 0.1407(3) 0.0436(12) Uani 1 1 d . . . H62 H 0.2235 0.9612 0.1907 0.052 Uiso 1 1 calc R . . C63 C 0.2253(4) 1.0719(4) 0.1100(3) 0.0482(13) Uani 1 1 d . . . C64 C 0.2099(4) 1.0968(4) 0.0355(3) 0.0516(13) Uani 1 1 d . . . H64 H 0.2207 1.1612 0.0141 0.062 Uiso 1 1 calc R . . C65 C 0.1784(4) 1.0243(4) -0.0061(3) 0.0439(12) Uani 1 1 d . . . C66 C 0.1633(4) 0.9282(4) 0.0258(3) 0.0407(11) Uani 1 1 d . . . H66 H 0.1419 0.8807 -0.0041 0.049 Uiso 1 1 calc R . . C67 C 0.2562(6) 1.1486(5) 0.1589(4) 0.0691(17) Uani 1 1 d . . . C68 C 0.1616(5) 1.0474(4) -0.0868(3) 0.0568(14) Uani 1 1 d . . . C71 C 0.0479(3) 0.7801(4) 0.2026(3) 0.0390(11) Uani 1 1 d . . . C72 C 0.0053(4) 0.8605(4) 0.2435(3) 0.0445(12) Uani 1 1 d . . . H72 H 0.0394 0.9211 0.2342 0.053 Uiso 1 1 calc R . . C73 C -0.0857(4) 0.8533(4) 0.2973(3) 0.0524(14) Uani 1 1 d . . . C74 C -0.1384(4) 0.7656(5) 0.3119(3) 0.0658(17) Uani 1 1 d . . . H74 H -0.2003 0.7608 0.3472 0.079 Uiso 1 1 calc R . . C75 C -0.0983(4) 0.6845(5) 0.2736(3) 0.0636(16) Uani 1 1 d . . . C76 C -0.0065(4) 0.6924(4) 0.2201(3) 0.0528(14) Uani 1 1 d . . . H76 H 0.0192 0.6365 0.1951 0.063 Uiso 1 1 calc R . . C77 C -0.1271(5) 0.9409(6) 0.3373(5) 0.083(2) Uani 1 1 d . . . C78 C -0.1529(9) 0.5901(7) 0.2872(6) 0.114(3) Uani 1 1 d . . . C81 C 0.1581(4) 0.7070(3) 0.0746(3) 0.0396(11) Uani 1 1 d . . . C82 C 0.0776(4) 0.7059(4) 0.0331(3) 0.0436(12) Uani 1 1 d . . . H82 H 0.0225 0.7483 0.0461 0.052 Uiso 1 1 calc R . . C83 C 0.0770(4) 0.6430(4) -0.0274(3) 0.0482(13) Uani 1 1 d . . . C84 C 0.1552(4) 0.5767(4) -0.0458(3) 0.0545(14) Uani 1 1 d . . . H84 H 0.1549 0.5347 -0.0858 0.065 Uiso 1 1 calc R . . C85 C 0.2336(4) 0.5733(4) -0.0042(3) 0.0481(13) Uani 1 1 d . . . C86 C 0.2349(4) 0.6381(4) 0.0542(3) 0.0445(12) Uani 1 1 d . . . H86 H 0.2897 0.6351 0.0808 0.053 Uiso 1 1 calc R . . C87 C -0.0089(5) 0.6515(5) -0.0723(4) 0.0693(18) Uani 1 1 d . . . C88 C 0.3182(5) 0.5006(5) -0.0211(4) 0.0675(17) Uani 1 1 d . . . F1 F 0.3856(4) 0.5990(4) 0.3981(3) 0.1225(18) Uani 1 1 d . . . F2 F 0.2737(5) 0.7086(3) 0.4323(2) 0.1236(18) Uani 1 1 d . . . F3 F 0.2334(4) 0.5772(4) 0.3913(2) 0.1139(16) Uani 1 1 d . . . F4 F 0.6148(3) 0.7689(6) 0.1869(4) 0.169(3) Uani 1 1 d . . . F5 F 0.5529(3) 0.8841(4) 0.1283(4) 0.146(2) Uani 1 1 d . . . F6 F 0.5697(4) 0.7498(5) 0.0817(4) 0.151(2) Uani 1 1 d . . . F7 F 0.3398(4) 1.1228(3) 0.1885(3) 0.1052(15) Uani 1 1 d . . . F8 F 0.1862(4) 1.1635(4) 0.2205(3) 0.1220(18) Uani 1 1 d . . . F9 F 0.2798(4) 1.2348(3) 0.1215(3) 0.1148(17) Uani 1 1 d . . . F10 F 0.1497(5) 1.1413(3) -0.1040(3) 0.134(2) Uani 1 1 d . . . F11 F 0.0819(4) 1.0017(5) -0.1034(3) 0.139(2) Uani 1 1 d . . . F12 F 0.2367(3) 1.0205(4) -0.1399(2) 0.1046(14) Uani 1 1 d . . . F13 F -0.0799(6) 1.0196(5) 0.3213(6) 0.217(5) Uani 1 1 d . . . F14 F -0.1199(11) 0.9344(7) 0.4085(4) 0.269(6) Uani 1 1 d . . . F15 F -0.2163(5) 0.9580(6) 0.3420(7) 0.256(6) Uani 1 1 d . . . F16 F -0.1672(9) 0.5469(7) 0.2319(5) 0.265(7) Uani 1 1 d . . . F17 F -0.2400(7) 0.5902(6) 0.3310(6) 0.250(6) Uani 1 1 d . . . F18 F -0.1078(9) 0.5264(8) 0.3216(10) 0.320(9) Uani 1 1 d . . . F19 F -0.0994(3) 0.6608(4) -0.0293(3) 0.1062(15) Uani 1 1 d . . . F20 F 0.0022(4) 0.7271(5) -0.1214(3) 0.153(3) Uani 1 1 d . . . F21 F -0.0181(4) 0.5727(4) -0.1108(3) 0.140(2) Uani 1 1 d . . . F22 F 0.3066(4) 0.4403(3) -0.0742(3) 0.1138(16) Uani 1 1 d . . . F23 F 0.4076(3) 0.5436(4) -0.0478(4) 0.1272(19) Uani 1 1 d . . . F24 F 0.3311(4) 0.4457(4) 0.0401(3) 0.132(2) Uani 1 1 d . . . O90 O 0.1359(4) 0.2591(4) 0.4189(3) 0.0995(16) Uani 1 1 d . . . C91 C 0.1029(9) 0.3318(10) 0.4776(7) 0.156(4) Uani 1 1 d . . . H91A H 0.1288 0.3134 0.5248 0.187 Uiso 1 1 calc R . . H91B H 0.1303 0.3966 0.4581 0.187 Uiso 1 1 calc R . . C92 C -0.0016(10) 0.3343(17) 0.4931(12) 0.309(15) Uani 1 1 d . . . H92A H -0.0253 0.4015 0.4866 0.371 Uiso 1 1 calc R . . H92B H -0.0273 0.3095 0.5462 0.371 Uiso 1 1 calc R . . C93 C -0.0397(10) 0.2700(16) 0.4366(11) 0.247(10) Uani 1 1 d . . . H93A H -0.0890 0.2212 0.4637 0.296 Uiso 1 1 calc R . . H93B H -0.0715 0.3094 0.3995 0.296 Uiso 1 1 calc R . . C94 C 0.0440(9) 0.2278(11) 0.4019(8) 0.171(5) Uani 1 1 d . . . H94A H 0.0474 0.2378 0.3461 0.205 Uiso 1 1 calc R . . H94B H 0.0374 0.1573 0.4148 0.205 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 0.0581(3) 0.0462(3) 0.0324(3) -0.00056(19) -0.0147(2) -0.0053(2) C1 0.078(4) 0.076(4) 0.034(3) 0.004(3) -0.021(3) -0.020(3) O1 0.126(4) 0.098(4) 0.066(3) 0.001(3) -0.042(3) -0.061(3) C2 0.077(4) 0.068(4) 0.052(4) -0.003(3) -0.022(3) 0.001(3) O2 0.119(4) 0.109(4) 0.086(4) 0.010(3) -0.050(3) 0.031(3) N1 0.052(3) 0.050(3) 0.038(2) -0.007(2) -0.0130(19) 0.001(2) N2 0.059(3) 0.055(3) 0.049(3) -0.004(3) -0.016(3) 0.001(3) N3 0.058(3) 0.048(3) 0.042(3) -0.004(2) -0.012(2) -0.006(2) N4 0.061(3) 0.051(3) 0.055(3) -0.011(2) -0.011(2) -0.007(3) N5 0.056(3) 0.046(3) 0.036(2) -0.0017(19) -0.011(2) -0.001(2) N6 0.047(3) 0.062(3) 0.036(3) -0.006(2) 0.000(2) -0.006(2) C3 0.105(5) 0.072(4) 0.037(3) -0.015(3) -0.010(3) 0.010(4) C4 0.067(4) 0.076(4) 0.038(3) -0.007(3) 0.002(3) -0.003(3) C5 0.098(5) 0.083(5) 0.035(3) 0.002(3) -0.004(3) -0.021(4) C11 0.078(4) 0.055(4) 0.064(4) -0.015(3) -0.039(3) 0.012(3) C12 0.096(5) 0.051(4) 0.050(4) 0.001(3) -0.022(3) 0.004(3) C13 0.068(4) 0.043(3) 0.039(3) -0.001(2) -0.014(3) 0.001(3) C14 0.102(6) 0.091(5) 0.106(6) -0.007(5) -0.057(5) 0.015(4) C15 0.082(5) 0.065(4) 0.079(5) 0.024(4) -0.009(3) -0.010(3) C21 0.077(4) 0.043(3) 0.048(3) -0.003(3) -0.010(3) -0.004(3) C22 0.099(5) 0.042(3) 0.065(4) -0.005(3) -0.011(4) -0.016(3) C23 0.079(4) 0.055(4) 0.058(4) 0.002(3) -0.010(3) -0.022(3) C24 0.083(5) 0.049(4) 0.101(5) -0.003(4) -0.014(4) 0.013(3) C25 0.095(6) 0.095(6) 0.135(8) -0.014(5) -0.009(5) -0.043(5) C31 0.083(5) 0.066(4) 0.043(4) -0.007(3) 0.001(3) -0.005(3) C32 0.059(4) 0.077(5) 0.073(5) -0.016(4) 0.015(3) -0.003(3) C33 0.050(4) 0.056(4) 0.068(4) -0.006(3) -0.003(3) 0.001(3) C34 0.121(6) 0.145(8) 0.046(4) -0.027(5) -0.002(4) -0.023(6) C35 0.056(4) 0.113(6) 0.106(6) -0.008(5) -0.014(4) -0.001(4) B51 0.040(3) 0.042(3) 0.037(3) -0.001(3) -0.010(2) 0.001(2) C51 0.042(3) 0.038(3) 0.035(3) -0.005(2) -0.011(2) 0.002(2) C52 0.047(3) 0.040(3) 0.038(3) -0.006(2) -0.012(2) 0.001(2) C53 0.058(3) 0.040(3) 0.042(3) -0.007(2) -0.020(2) 0.004(2) C54 0.056(3) 0.047(3) 0.063(4) -0.017(3) -0.032(3) 0.007(3) C55 0.050(3) 0.046(3) 0.049(3) -0.011(3) -0.016(2) 0.001(2) C56 0.046(3) 0.049(3) 0.037(3) -0.005(2) -0.010(2) -0.001(2) C57 0.091(5) 0.066(4) 0.046(4) -0.003(3) -0.023(3) 0.006(4) C58 0.051(4) 0.084(5) 0.097(5) -0.017(4) -0.023(4) 0.002(3) C61 0.036(3) 0.049(3) 0.034(3) -0.003(2) -0.008(2) 0.003(2) C62 0.050(3) 0.047(3) 0.034(3) 0.003(2) -0.012(2) -0.002(2) C63 0.049(3) 0.048(3) 0.049(3) -0.002(3) -0.010(2) -0.004(2) C64 0.058(3) 0.044(3) 0.051(3) 0.010(3) -0.009(3) 0.004(3) C65 0.041(3) 0.055(3) 0.035(3) 0.005(2) -0.008(2) 0.005(2) C66 0.042(3) 0.044(3) 0.036(3) -0.004(2) -0.009(2) 0.003(2) C67 0.098(5) 0.051(4) 0.063(4) -0.002(3) -0.029(4) -0.012(3) C68 0.062(4) 0.061(4) 0.048(3) 0.010(3) -0.015(3) 0.002(3) C71 0.038(3) 0.047(3) 0.033(3) 0.000(2) -0.011(2) -0.001(2) C72 0.039(3) 0.049(3) 0.047(3) -0.004(2) -0.013(2) 0.001(2) C73 0.041(3) 0.068(4) 0.050(3) -0.013(3) -0.011(2) 0.006(3) C74 0.048(3) 0.092(5) 0.053(4) -0.015(3) 0.004(3) -0.012(3) C75 0.061(4) 0.070(4) 0.056(4) -0.004(3) 0.001(3) -0.023(3) C76 0.061(3) 0.053(3) 0.044(3) -0.008(3) -0.005(3) -0.005(3) C77 0.051(4) 0.108(6) 0.083(5) -0.054(5) 0.019(3) -0.001(4) C78 0.143(8) 0.086(6) 0.093(6) -0.007(5) 0.033(6) -0.054(6) C81 0.041(3) 0.040(3) 0.038(3) -0.002(2) -0.008(2) -0.002(2) C82 0.042(3) 0.043(3) 0.046(3) -0.006(2) -0.010(2) 0.001(2) C83 0.050(3) 0.052(3) 0.045(3) -0.003(3) -0.014(2) -0.003(3) C84 0.068(4) 0.052(3) 0.047(3) -0.016(3) -0.015(3) -0.002(3) C85 0.053(3) 0.048(3) 0.044(3) -0.005(3) -0.007(2) 0.005(2) C86 0.045(3) 0.052(3) 0.039(3) -0.001(2) -0.014(2) 0.000(2) C87 0.066(4) 0.083(5) 0.070(4) -0.020(4) -0.037(4) -0.002(3) C88 0.066(4) 0.088(5) 0.050(4) -0.018(4) -0.010(3) 0.015(4) F1 0.123(4) 0.167(5) 0.080(3) 0.036(3) -0.038(3) 0.045(3) F2 0.231(6) 0.091(3) 0.047(2) -0.013(2) -0.018(3) 0.025(3) F3 0.166(4) 0.109(4) 0.067(3) 0.034(2) -0.033(3) -0.046(3) F4 0.048(3) 0.273(8) 0.181(6) 0.081(5) -0.041(3) -0.027(3) F5 0.069(3) 0.110(4) 0.238(7) 0.035(4) 0.013(3) -0.022(3) F6 0.081(3) 0.220(7) 0.141(5) -0.069(5) 0.033(3) -0.020(4) F7 0.135(4) 0.088(3) 0.114(3) -0.011(3) -0.076(3) -0.027(3) F8 0.154(4) 0.109(4) 0.100(3) -0.057(3) 0.002(3) -0.022(3) F9 0.206(5) 0.050(2) 0.100(3) 0.009(2) -0.064(3) -0.040(3) F10 0.256(7) 0.082(3) 0.079(3) 0.012(2) -0.073(4) 0.043(4) F11 0.113(3) 0.231(6) 0.082(3) 0.065(4) -0.063(3) -0.072(4) F12 0.112(3) 0.151(4) 0.046(2) -0.002(2) -0.005(2) 0.025(3) F13 0.177(6) 0.103(4) 0.324(12) -0.109(6) 0.107(7) -0.014(4) F14 0.520(19) 0.183(8) 0.109(6) -0.081(6) -0.053(8) 0.160(10) F15 0.092(4) 0.240(8) 0.471(16) -0.238(10) -0.074(6) 0.089(5) F16 0.371(14) 0.206(8) 0.184(7) -0.094(7) 0.066(8) -0.211(10) F17 0.205(8) 0.172(7) 0.307(10) -0.081(7) 0.149(8) -0.131(6) F18 0.270(12) 0.147(7) 0.56(2) 0.180(12) -0.187(14) -0.140(8) F19 0.058(2) 0.148(4) 0.124(4) -0.032(3) -0.039(2) 0.004(2) F20 0.130(4) 0.197(6) 0.147(5) 0.098(5) -0.096(4) -0.051(4) F21 0.138(4) 0.157(5) 0.164(5) -0.097(4) -0.109(4) 0.044(3) F22 0.128(4) 0.112(3) 0.114(4) -0.068(3) -0.036(3) 0.054(3) F23 0.067(3) 0.116(4) 0.191(6) -0.029(4) 0.002(3) 0.025(3) F24 0.178(5) 0.136(4) 0.079(3) -0.004(3) -0.020(3) 0.104(4) O90 0.075(3) 0.113(4) 0.105(4) -0.018(3) 0.000(3) -0.005(3) C91 0.131(9) 0.215(13) 0.119(9) -0.040(9) -0.007(7) 0.024(9) C92 0.095(9) 0.49(3) 0.38(3) -0.31(3) -0.037(12) 0.077(14) C93 0.089(9) 0.40(3) 0.26(2) -0.14(2) -0.024(10) -0.007(12) C94 0.078(7) 0.215(14) 0.210(14) -0.032(11) 0.005(8) -0.010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.941(7) . ? Mo1 C1 1.954(6) . ? Mo1 C4 2.201(5) . ? Mo1 N5 2.213(4) . ? Mo1 N1 2.310(4) . ? Mo1 C5 2.321(6) . ? Mo1 C3 2.327(6) . ? Mo1 N3 2.334(4) . ? C1 O1 1.152(7) . ? C2 O2 1.175(7) . ? N1 N2 1.358(6) . ? N1 C13 1.360(7) . ? N2 C11 1.346(8) . ? N3 C21 1.352(7) . ? N3 N4 1.353(6) . ? N4 C23 1.339(7) . ? N5 C33 1.344(7) . ? N5 N6 1.353(6) . ? N6 C31 1.340(7) . ? C3 C4 1.386(9) . ? C4 C5 1.395(9) . ? C11 C12 1.342(9) . ? C11 C14 1.484(9) . ? C12 C13 1.384(8) . ? C13 C15 1.481(8) . ? C21 C22 1.389(8) . ? C21 C24 1.478(9) . ? C22 C23 1.346(9) . ? C23 C25 1.493(9) . ? C31 C32 1.359(9) . ? C31 C34 1.493(9) . ? C32 C33 1.380(9) . ? C33 C35 1.494(9) . ? B51 C61 1.638(8) . ? B51 C71 1.648(7) . ? B51 C81 1.649(7) . ? B51 C51 1.653(7) . ? C51 C52 1.383(7) . ? C51 C56 1.403(7) . ? C52 C53 1.389(7) . ? C53 C54 1.374(8) . ? C53 C57 1.481(8) . ? C54 C55 1.372(8) . ? C55 C56 1.383(7) . ? C55 C58 1.472(9) . ? C57 F2 1.299(7) . ? C57 F3 1.301(7) . ? C57 F1 1.340(7) . ? C58 F5 1.286(8) . ? C58 F4 1.287(8) . ? C58 F6 1.322(8) . ? C61 C62 1.394(7) . ? C61 C66 1.396(7) . ? C62 C63 1.381(7) . ? C63 C64 1.378(7) . ? C63 C67 1.489(8) . ? C64 C65 1.367(7) . ? C65 C66 1.388(7) . ? C65 C68 1.485(7) . ? C67 F8 1.311(8) . ? C67 F9 1.315(7) . ? C67 F7 1.340(8) . ? C68 F12 1.297(7) . ? C68 F10 1.306(7) . ? C68 F11 1.311(7) . ? C71 C76 1.381(7) . ? C71 C72 1.401(7) . ? C72 C73 1.384(7) . ? C73 C74 1.368(8) . ? C73 C77 1.467(9) . ? C74 C75 1.377(8) . ? C75 C76 1.390(8) . ? C75 C78 1.458(10) . ? C77 F15 1.189(8) . ? C77 F13 1.230(9) . ? C77 F14 1.266(10) . ? C78 F16 1.205(11) . ? C78 F18 1.238(14) . ? C78 F17 1.261(11) . ? C81 C86 1.390(7) . ? C81 C82 1.394(7) . ? C82 C83 1.400(7) . ? C83 C84 1.374(7) . ? C83 C87 1.494(8) . ? C84 C85 1.371(8) . ? C85 C86 1.389(7) . ? C85 C88 1.488(8) . ? C87 F20 1.289(8) . ? C87 F19 1.300(7) . ? C87 F21 1.316(7) . ? C88 F24 1.304(8) . ? C88 F22 1.305(7) . ? C88 F23 1.313(8) . ? O90 C94 1.377(12) . ? O90 C91 1.474(11) . ? C91 C92 1.357(14) . ? C92 C93 1.510(17) . ? C93 C94 1.307(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 80.0(3) . . ? C2 Mo1 C4 101.9(3) . . ? C1 Mo1 C4 101.6(2) . . ? C2 Mo1 N5 90.0(2) . . ? C1 Mo1 N5 90.9(2) . . ? C4 Mo1 N5 164.0(2) . . ? C2 Mo1 N1 167.6(2) . . ? C1 Mo1 N1 94.8(2) . . ? C4 Mo1 N1 90.1(2) . . ? N5 Mo1 N1 78.73(15) . . ? C2 Mo1 C5 67.9(3) . . ? C1 Mo1 C5 105.3(2) . . ? C4 Mo1 C5 35.8(2) . . ? N5 Mo1 C5 149.1(2) . . ? N1 Mo1 C5 124.6(2) . . ? C2 Mo1 C3 108.1(2) . . ? C1 Mo1 C3 68.7(3) . . ? C4 Mo1 C3 35.5(2) . . ? N5 Mo1 C3 149.1(2) . . ? N1 Mo1 C3 80.1(2) . . ? C5 Mo1 C3 61.5(2) . . ? C2 Mo1 N3 93.4(2) . . ? C1 Mo1 N3 169.7(2) . . ? C4 Mo1 N3 87.41(19) . . ? N5 Mo1 N3 81.17(15) . . ? N1 Mo1 N3 90.07(15) . . ? C5 Mo1 N3 79.07(19) . . ? C3 Mo1 N3 121.1(2) . . ? O1 C1 Mo1 175.1(6) . . ? O2 C2 Mo1 177.0(6) . . ? N2 N1 C13 103.4(4) . . ? N2 N1 Mo1 126.9(3) . . ? C13 N1 Mo1 129.3(3) . . ? C11 N2 N1 113.2(5) . . ? C21 N3 N4 103.4(4) . . ? C21 N3 Mo1 130.2(4) . . ? N4 N3 Mo1 124.3(3) . . ? C23 N4 N3 113.7(5) . . ? C33 N5 N6 104.5(4) . . ? C33 N5 Mo1 136.1(4) . . ? N6 N5 Mo1 119.4(3) . . ? C31 N6 N5 112.6(5) . . ? C4 C3 Mo1 67.3(3) . . ? C3 C4 C5 117.4(6) . . ? C3 C4 Mo1 77.2(3) . . ? C5 C4 Mo1 76.8(3) . . ? C4 C5 Mo1 67.4(3) . . ? C12 C11 N2 105.7(5) . . ? C12 C11 C14 132.2(7) . . ? N2 C11 C14 122.1(6) . . ? C11 C12 C13 108.0(6) . . ? N1 C13 C12 109.8(5) . . ? N1 C13 C15 123.2(5) . . ? C12 C13 C15 127.0(6) . . ? N3 C21 C22 109.9(5) . . ? N3 C21 C24 124.0(5) . . ? C22 C21 C24 126.1(6) . . ? C23 C22 C21 107.5(5) . . ? N4 C23 C22 105.5(5) . . ? N4 C23 C25 123.3(7) . . ? C22 C23 C25 131.2(6) . . ? N6 C31 C32 105.7(5) . . ? N6 C31 C34 122.2(6) . . ? C32 C31 C34 132.1(6) . . ? C31 C32 C33 107.3(5) . . ? N5 C33 C32 109.9(5) . . ? N5 C33 C35 123.5(6) . . ? C32 C33 C35 126.6(6) . . ? C61 B51 C71 111.0(4) . . ? C61 B51 C81 110.6(4) . . ? C71 B51 C81 108.8(4) . . ? C61 B51 C51 107.7(4) . . ? C71 B51 C51 109.5(4) . . ? C81 B51 C51 109.3(4) . . ? C52 C51 C56 115.6(4) . . ? C52 C51 B51 124.5(4) . . ? C56 C51 B51 119.9(4) . . ? C51 C52 C53 122.2(5) . . ? C54 C53 C52 120.3(5) . . ? C54 C53 C57 120.5(5) . . ? C52 C53 C57 119.1(5) . . ? C55 C54 C53 119.4(5) . . ? C54 C55 C56 119.7(5) . . ? C54 C55 C58 121.3(5) . . ? C56 C55 C58 118.9(5) . . ? C55 C56 C51 122.7(5) . . ? F2 C57 F3 105.3(6) . . ? F2 C57 F1 107.3(5) . . ? F3 C57 F1 102.4(6) . . ? F2 C57 C53 113.2(5) . . ? F3 C57 C53 114.6(5) . . ? F1 C57 C53 113.0(5) . . ? F5 C58 F4 106.8(6) . . ? F5 C58 F6 102.6(7) . . ? F4 C58 F6 104.8(7) . . ? F5 C58 C55 113.8(6) . . ? F4 C58 C55 114.5(7) . . ? F6 C58 C55 113.2(5) . . ? C62 C61 C66 114.2(5) . . ? C62 C61 B51 121.3(4) . . ? C66 C61 B51 124.5(4) . . ? C63 C62 C61 123.4(5) . . ? C64 C63 C62 120.4(5) . . ? C64 C63 C67 120.5(5) . . ? C62 C63 C67 119.0(5) . . ? C65 C64 C63 118.2(5) . . ? C64 C65 C66 120.8(5) . . ? C64 C65 C68 120.1(5) . . ? C66 C65 C68 119.1(5) . . ? C65 C66 C61 123.0(5) . . ? F8 C67 F9 107.6(6) . . ? F8 C67 F7 103.7(6) . . ? F9 C67 F7 104.8(5) . . ? F8 C67 C63 113.1(5) . . ? F9 C67 C63 114.2(5) . . ? F7 C67 C63 112.4(5) . . ? F12 C68 F10 104.6(5) . . ? F12 C68 F11 103.0(5) . . ? F10 C68 F11 106.5(6) . . ? F12 C68 C65 113.7(5) . . ? F10 C68 C65 114.3(5) . . ? F11 C68 C65 113.7(5) . . ? C76 C71 C72 115.4(4) . . ? C76 C71 B51 122.0(4) . . ? C72 C71 B51 122.4(4) . . ? C73 C72 C71 122.6(5) . . ? C74 C73 C72 120.3(5) . . ? C74 C73 C77 119.9(5) . . ? C72 C73 C77 119.8(6) . . ? C73 C74 C75 118.9(5) . . ? C74 C75 C76 120.4(5) . . ? C74 C75 C78 120.3(6) . . ? C76 C75 C78 119.3(6) . . ? C71 C76 C75 122.5(5) . . ? F15 C77 F13 107.6(10) . . ? F15 C77 F14 100.7(8) . . ? F13 C77 F14 96.1(8) . . ? F15 C77 C73 118.3(7) . . ? F13 C77 C73 118.6(6) . . ? F14 C77 C73 111.8(8) . . ? F16 C78 F18 101.2(11) . . ? F16 C78 F17 104.3(11) . . ? F18 C78 F17 101.2(11) . . ? F16 C78 C75 118.7(9) . . ? F18 C78 C75 113.1(11) . . ? F17 C78 C75 116.0(8) . . ? C86 C81 C82 115.2(4) . . ? C86 C81 B51 124.6(4) . . ? C82 C81 B51 120.2(4) . . ? C81 C82 C83 122.2(5) . . ? C84 C83 C82 120.3(5) . . ? C84 C83 C87 121.1(5) . . ? C82 C83 C87 118.6(5) . . ? C85 C84 C83 118.9(5) . . ? C84 C85 C86 120.2(5) . . ? C84 C85 C88 120.5(5) . . ? C86 C85 C88 119.3(5) . . ? C85 C86 C81 123.1(5) . . ? F20 C87 F19 105.6(6) . . ? F20 C87 F21 107.8(6) . . ? F19 C87 F21 104.0(6) . . ? F20 C87 C83 112.2(5) . . ? F19 C87 C83 114.1(6) . . ? F21 C87 C83 112.5(6) . . ? F24 C88 F22 106.4(6) . . ? F24 C88 F23 105.6(6) . . ? F22 C88 F23 104.3(5) . . ? F24 C88 C85 113.3(5) . . ? F22 C88 C85 114.2(5) . . ? F23 C88 C85 112.2(6) . . ? C94 O90 C91 102.7(8) . . ? C92 C91 O90 108.8(11) . . ? C91 C92 C93 107.3(11) . . ? C94 C93 C92 103.6(11) . . ? C93 C94 O90 117.0(12) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.083 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.075 #===END