Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'M. Whiteley' 'Roy L. Beddoes' 'Madeleine Helliwell' 'Dale M. Spencer' _publ_contact_author_name 'Dr M Whiteley' _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL U.K. ; _publ_contact_author_phone ' 0161 275 4634 ' _publ_contact_author_email ' Mark.Whiteley@man,ac.uk ' _publ_section_title ; Synthesis, Structure and Hapticity Interconversion Reactions of Pentahapto-bonded Cyclooctadienyl Complexes of Molybdenum ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; data_Complex_6b _database_code_CSD 195204 _audit_creation_date 1996-11-11 _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 B F4 Mo N3 O' _chemical_formula_weight 567.32 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z _cell_length_a 13.396(2) _cell_length_b 13.653(19) _cell_length_c 15.810(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.126(12) _cell_angle_gamma 90.00 _cell_volume 2884(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 12.3 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -3.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -5 0 -1 -1 -5 0 1 1 -6 _diffrn_reflns_number 5342 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01955 _diffrn_orient_matrix_UB_12 -0.02095 _diffrn_orient_matrix_UB_13 -0.05951 _diffrn_orient_matrix_UB_21 0.06867 _diffrn_orient_matrix_UB_22 0.01633 _diffrn_orient_matrix_UB_23 -0.01663 _diffrn_orient_matrix_UB_31 0.02242 _diffrn_orient_matrix_UB_32 -0.06826 _diffrn_orient_matrix_UB_33 0.01426 _reflns_number_total 5111 _reflns_number_gt 3774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan (MSC, 1995)' _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^)+(0.0960P)^2^+2.4970P] 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 5111 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 1.03450(3) 0.09880(3) 0.23639(2) 0.04363(18) Uani 1 1 d . . . O1 O 1.2494(3) 0.0286(4) 0.2959(3) 0.0827(13) Uani 1 1 d . . . N1 N 0.9011(3) 0.0515(3) 0.3942(3) 0.0537(10) Uani 1 1 d . . . N2 N 1.0152(4) -0.1374(4) 0.2270(3) 0.0612(12) Uani 1 1 d . . . N3 N 1.0993(3) 0.2856(3) 0.3560(3) 0.0554(11) Uani 1 1 d . . . C1 C 1.0615(5) 0.1124(5) 0.0949(3) 0.0706(17) Uani 1 1 d . . . H1 H 1.1006 0.0739 0.0617 0.085 Uiso 1 1 calc R . . C2 C 0.9629(5) 0.0825(5) 0.1000(3) 0.0702(17) Uani 1 1 d . . . H2 H 0.9424 0.0307 0.0647 0.084 Uiso 1 1 calc R . . C3 C 0.8895(4) 0.1197(4) 0.1513(4) 0.0638(15) Uani 1 1 d . . . H3 H 0.8313 0.0826 0.1526 0.077 Uiso 1 1 calc R . . C4 C 0.8932(4) 0.2054(4) 0.2005(4) 0.0622(14) Uani 1 1 d . . . H4 H 0.8833 0.1969 0.2576 0.075 Uiso 1 1 calc R . . C5 C 0.9109(6) 0.3083(5) 0.1732(4) 0.0811(19) Uani 1 1 d . . . H5A H 0.9434 0.3433 0.2210 0.097 Uiso 1 1 calc R . . H5B H 0.8463 0.3390 0.1602 0.097 Uiso 1 1 calc R . . C6 C 0.9721(6) 0.3223(5) 0.0987(5) 0.092(2) Uani 1 1 d . . . H6A H 0.9661 0.3897 0.0798 0.110 Uiso 1 1 calc R . . H6B H 0.9457 0.2807 0.0527 0.110 Uiso 1 1 calc R . . C7 C 1.0804(6) 0.2987(5) 0.1182(4) 0.085(2) Uani 1 1 d . . . H7A H 1.1168 0.3221 0.0713 0.102 Uiso 1 1 calc R . . H7B H 1.1038 0.3363 0.1679 0.102 Uiso 1 1 calc R . . C8 C 1.1093(5) 0.1945(5) 0.1340(4) 0.0676(16) Uani 1 1 d . . . H8 H 1.1632 0.1826 0.1730 0.081 Uiso 1 1 calc R . . C9 C 1.1704(4) 0.0539(4) 0.2747(3) 0.0557(13) Uani 1 1 d . . . C10 C 0.9530(4) 0.0676(4) 0.3414(3) 0.0473(11) Uani 1 1 d . . . C11 C 0.8261(4) 0.0368(4) 0.4540(3) 0.0527(12) Uani 1 1 d . . . C12 C 0.8509(5) 0.1028(5) 0.5297(4) 0.0739(17) Uani 1 1 d . . . H12A H 0.9126 0.0819 0.5587 0.111 Uiso 1 1 calc R . . H12B H 0.7982 0.0991 0.5677 0.111 Uiso 1 1 calc R . . H12C H 0.8575 0.1691 0.5107 0.111 Uiso 1 1 calc R . . C13 C 0.7261(5) 0.0641(6) 0.4080(5) 0.083(2) Uani 1 1 d . . . H13A H 0.7238 0.1336 0.3984 0.125 Uiso 1 1 calc R . . H13B H 0.6726 0.0455 0.4421 0.125 Uiso 1 1 calc R . . H13C H 0.7187 0.0305 0.3546 0.125 Uiso 1 1 calc R . . C14 C 0.8286(5) -0.0707(4) 0.4792(4) 0.0714(17) Uani 1 1 d . . . H14A H 0.8182 -0.1106 0.4293 0.107 Uiso 1 1 calc R . . H14B H 0.7768 -0.0835 0.5166 0.107 Uiso 1 1 calc R . . H14C H 0.8925 -0.0859 0.5076 0.107 Uiso 1 1 calc R . . C15 C 1.0185(4) -0.0545(4) 0.2267(3) 0.0538(13) Uani 1 1 d . . . C16 C 1.0122(5) -0.2446(4) 0.2315(4) 0.0650(16) Uani 1 1 d . . . C17 C 0.9200(7) -0.2726(6) 0.2728(5) 0.103(3) Uani 1 1 d . . . H17A H 0.9241 -0.2486 0.3300 0.155 Uiso 1 1 calc R . . H17B H 0.9138 -0.3427 0.2731 0.155 Uiso 1 1 calc R . . H17C H 0.8627 -0.2446 0.2419 0.155 Uiso 1 1 calc R . . C18 C 1.0078(6) -0.2807(5) 0.1415(4) 0.091(2) Uani 1 1 d . . . H18A H 0.9485 -0.2558 0.1111 0.137 Uiso 1 1 calc R . . H18B H 1.0063 -0.3510 0.1411 0.137 Uiso 1 1 calc R . . H18C H 1.0658 -0.2583 0.1149 0.137 Uiso 1 1 calc R . . C19 C 1.1066(7) -0.2756(5) 0.2807(7) 0.127(4) Uani 1 1 d . . . H19A H 1.1630 -0.2468 0.2560 0.190 Uiso 1 1 calc R . . H19B H 1.1122 -0.3456 0.2793 0.190 Uiso 1 1 calc R . . H19C H 1.1051 -0.2541 0.3384 0.190 Uiso 1 1 calc R . . C20 C 1.0756(4) 0.2212(4) 0.3130(3) 0.0477(11) Uani 1 1 d . . . C21 C 1.1259(4) 0.3672(4) 0.4128(4) 0.0572(13) Uani 1 1 d . . . C22 C 1.0814(6) 0.3475(5) 0.4959(4) 0.087(2) Uani 1 1 d . . . H22A H 1.0103 0.3393 0.4863 0.131 Uiso 1 1 calc R . . H22B H 1.0952 0.4017 0.5336 0.131 Uiso 1 1 calc R . . H22C H 1.1103 0.2890 0.5208 0.131 Uiso 1 1 calc R . . C23 C 1.0815(7) 0.4584(5) 0.3714(5) 0.094(2) Uani 1 1 d . . . H23A H 1.1039 0.4645 0.3153 0.141 Uiso 1 1 calc R . . H23B H 1.1027 0.5147 0.4044 0.141 Uiso 1 1 calc R . . H23C H 1.0099 0.4541 0.3682 0.141 Uiso 1 1 calc R . . C24 C 1.2385(6) 0.3714(7) 0.4230(6) 0.111(3) Uani 1 1 d . . . H24A H 1.2639 0.3108 0.4467 0.166 Uiso 1 1 calc R . . H24B H 1.2590 0.4244 0.4602 0.166 Uiso 1 1 calc R . . H24C H 1.2645 0.3816 0.3686 0.166 Uiso 1 1 calc R . . F1 F 0.3195(6) 0.1989(4) 0.8809(5) 0.185(3) Uani 1 1 d . . . F2 F 0.1858(6) 0.1177(8) 0.9156(7) 0.237(5) Uani 1 1 d . . . F3 F 0.3102(10) 0.0994(13) 0.9710(12) 0.467(15) Uani 1 1 d . . . F4 F 0.2988(11) 0.0565(10) 0.8521(11) 0.386(11) Uani 1 1 d . . . B1 B 0.2764(9) 0.1236(9) 0.9051(8) 0.103(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0519(3) 0.0430(3) 0.0359(2) -0.00451(18) 0.00270(17) 0.0016(2) O1 0.061(3) 0.099(4) 0.089(3) 0.013(3) 0.005(2) 0.017(2) N1 0.063(3) 0.049(2) 0.049(2) -0.001(2) 0.007(2) 0.001(2) N2 0.077(3) 0.046(3) 0.060(3) -0.010(2) 0.000(2) 0.002(2) N3 0.071(3) 0.045(2) 0.051(2) -0.003(2) 0.007(2) -0.002(2) C1 0.084(4) 0.092(5) 0.036(3) -0.005(3) 0.010(3) 0.003(4) C2 0.084(4) 0.085(4) 0.039(3) -0.012(3) -0.014(3) 0.004(3) C3 0.058(3) 0.078(4) 0.053(3) 0.004(3) -0.014(3) 0.001(3) C4 0.071(4) 0.064(3) 0.051(3) 0.008(3) -0.002(3) 0.011(3) C5 0.099(5) 0.073(4) 0.071(4) 0.014(3) -0.001(4) 0.029(4) C6 0.124(6) 0.072(4) 0.077(5) 0.030(4) -0.009(4) -0.001(4) C7 0.105(5) 0.081(5) 0.070(4) 0.025(4) 0.013(4) -0.016(4) C8 0.077(4) 0.080(4) 0.046(3) 0.009(3) 0.007(3) -0.007(3) C9 0.063(3) 0.052(3) 0.053(3) -0.002(2) 0.006(3) -0.002(3) C10 0.055(3) 0.043(3) 0.043(3) 0.001(2) -0.001(2) 0.000(2) C11 0.051(3) 0.055(3) 0.053(3) 0.005(2) 0.011(2) 0.003(2) C12 0.086(4) 0.074(4) 0.063(4) -0.006(3) 0.016(3) 0.007(3) C13 0.058(4) 0.087(5) 0.104(5) 0.010(4) -0.003(4) 0.013(3) C14 0.081(4) 0.060(4) 0.074(4) 0.012(3) 0.011(3) -0.002(3) C15 0.057(3) 0.054(3) 0.049(3) -0.012(2) -0.002(2) 0.001(3) C16 0.087(4) 0.048(3) 0.059(3) -0.012(3) -0.002(3) -0.003(3) C17 0.148(7) 0.081(5) 0.087(5) 0.001(4) 0.046(5) -0.009(5) C18 0.113(6) 0.080(5) 0.082(5) -0.039(4) 0.019(4) -0.021(4) C19 0.150(8) 0.061(4) 0.159(9) -0.012(5) -0.064(7) 0.024(5) C20 0.058(3) 0.043(3) 0.042(2) 0.001(2) 0.005(2) 0.002(2) C21 0.071(4) 0.044(3) 0.057(3) -0.012(2) 0.008(3) -0.003(3) C22 0.139(7) 0.064(4) 0.060(4) -0.007(3) 0.023(4) -0.009(4) C23 0.144(7) 0.050(4) 0.088(5) -0.003(3) 0.009(5) 0.006(4) C24 0.071(5) 0.119(6) 0.141(8) -0.064(6) 0.002(5) -0.015(4) F1 0.284(9) 0.099(4) 0.180(6) 0.028(4) 0.081(6) -0.048(5) F2 0.112(5) 0.368(14) 0.239(10) -0.039(9) 0.057(6) -0.049(6) F3 0.232(12) 0.59(3) 0.58(3) 0.47(3) -0.014(15) 0.075(15) F4 0.419(19) 0.285(12) 0.49(2) -0.217(14) 0.299(18) -0.235(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 C9 1.974(6) . ? Mo1 C10 2.095(5) . ? Mo1 C15 2.108(7) . ? Mo1 C20 2.113(5) . ? Mo1 C1 2.300(6) . ? Mo1 C3 2.300(5) . ? Mo1 C2 2.307(5) . ? Mo1 C8 2.359(6) . ? Mo1 C4 2.422(6) . ? O1 C9 1.140(7) . ? N1 C10 1.145(6) . ? N1 C11 1.443(7) . ? N2 C15 1.133(8) . ? N2 C16 1.466(8) . ? N3 C20 1.142(6) . ? N3 C21 1.460(7) . ? C1 C2 1.391(9) . ? C1 C8 1.412(9) . ? C1 H1 0.9300 . ? C2 C3 1.413(9) . ? C2 H2 0.9300 . ? C3 C4 1.404(8) . ? C3 H3 0.9300 . ? C4 C5 1.494(9) . ? C4 H4 0.9300 . ? C5 C6 1.494(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.496(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.490(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9300 . ? C11 C12 1.515(8) . ? C11 C14 1.521(8) . ? C11 C13 1.524(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 C17 1.487(10) . ? C16 C19 1.498(10) . ? C16 C18 1.503(8) . ? 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 . ? C21 C22 1.506(8) . ? C21 C24 1.507(9) . ? C21 C23 1.508(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? F1 B1 1.253(13) . ? F2 B1 1.239(13) . ? F3 B1 1.153(17) . ? F4 B1 1.292(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 C9 Mo1 C10 102.5(2) . . ? C9 Mo1 C15 78.5(2) . . ? C10 Mo1 C15 78.4(2) . . ? C9 Mo1 C20 82.7(2) . . ? C10 Mo1 C20 80.57(19) . . ? C15 Mo1 C20 147.94(19) . . ? C9 Mo1 C1 96.7(2) . . ? C10 Mo1 C1 156.2(2) . . ? C15 Mo1 C1 91.8(2) . . ? C20 Mo1 C1 116.1(2) . . ? C9 Mo1 C3 159.9(2) . . ? C10 Mo1 C3 91.3(2) . . ? C15 Mo1 C3 90.2(2) . . ? C20 Mo1 C3 114.3(2) . . ? C1 Mo1 C3 66.8(2) . . ? C9 Mo1 C2 124.7(2) . . ? C10 Mo1 C2 121.0(2) . . ? C15 Mo1 C2 78.6(2) . . ? C20 Mo1 C2 133.3(2) . . ? C1 Mo1 C2 35.1(2) . . ? C3 Mo1 C2 35.7(2) . . ? C9 Mo1 C8 87.4(2) . . ? C10 Mo1 C8 158.0(2) . . ? C15 Mo1 C8 123.1(2) . . ? C20 Mo1 C8 81.3(2) . . ? C1 Mo1 C8 35.2(2) . . ? C3 Mo1 C8 85.0(2) . . ? C2 Mo1 C8 65.2(2) . . ? C9 Mo1 C4 161.1(2) . . ? C10 Mo1 C4 82.2(2) . . ? C15 Mo1 C4 120.4(2) . . ? C20 Mo1 C4 80.0(2) . . ? C1 Mo1 C4 84.2(2) . . ? C3 Mo1 C4 34.5(2) . . ? C2 Mo1 C4 64.7(2) . . ? C8 Mo1 C4 82.5(2) . . ? C10 N1 C11 173.0(5) . . ? C15 N2 C16 177.5(6) . . ? C20 N3 C21 177.7(5) . . ? C2 C1 C8 127.6(6) . . ? C2 C1 Mo1 72.7(3) . . ? C8 C1 Mo1 74.6(3) . . ? C2 C1 H1 116.2 . . ? C8 C1 H1 116.2 . . ? Mo1 C1 H1 129.5 . . ? C1 C2 C3 129.2(6) . . ? C1 C2 Mo1 72.1(3) . . ? C3 C2 Mo1 71.9(3) . . ? C1 C2 H2 115.4 . . ? C3 C2 H2 115.4 . . ? Mo1 C2 H2 136.0 . . ? C4 C3 C2 128.2(6) . . ? C4 C3 Mo1 77.5(3) . . ? C2 C3 Mo1 72.4(3) . . ? C4 C3 H3 115.9 . . ? C2 C3 H3 115.9 . . ? Mo1 C3 H3 126.4 . . ? C3 C4 C5 128.6(5) . . ? C3 C4 Mo1 68.0(3) . . ? C5 C4 Mo1 119.7(4) . . ? C3 C4 H4 115.7 . . ? C5 C4 H4 115.7 . . ? Mo1 C4 H4 82.0 . . ? C4 C5 C6 117.0(6) . . ? C4 C5 H5A 108.0 . . ? C6 C5 H5A 108.0 . . ? C4 C5 H5B 108.0 . . ? C6 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C7 112.9(6) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 118.4(6) . . ? C8 C7 H7A 107.7 . . ? C6 C7 H7A 107.7 . . ? C8 C7 H7B 107.7 . . ? C6 C7 H7B 107.7 . . ? H7A C7 H7B 107.1 . . ? C1 C8 C7 125.5(6) . . ? C1 C8 Mo1 70.1(3) . . ? C7 C8 Mo1 121.8(4) . . ? C1 C8 H8 117.3 . . ? C7 C8 H8 117.3 . . ? Mo1 C8 H8 78.3 . . ? O1 C9 Mo1 179.1(5) . . ? N1 C10 Mo1 174.0(4) . . ? N1 C11 C12 108.2(5) . . ? N1 C11 C14 107.6(4) . . ? C12 C11 C14 111.6(5) . . ? N1 C11 C13 106.4(5) . . ? C12 C11 C13 111.5(5) . . ? C14 C11 C13 111.3(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 Mo1 174.5(5) . . ? N2 C16 C17 107.8(5) . . ? N2 C16 C19 106.3(5) . . ? C17 C16 C19 113.4(7) . . ? N2 C16 C18 106.3(5) . . ? C17 C16 C18 110.7(6) . . ? C19 C16 C18 111.9(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 Mo1 178.0(5) . . ? N3 C21 C22 107.8(5) . . ? N3 C21 C24 107.1(5) . . ? C22 C21 C24 111.7(6) . . ? N3 C21 C23 107.0(5) . . ? C22 C21 C23 111.0(5) . . ? C24 C21 C23 112.0(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F3 B1 F2 100.6(13) . . ? F3 B1 F1 110.5(14) . . ? F2 B1 F1 124.9(12) . . ? F3 B1 F4 106.7(15) . . ? F2 B1 F4 108.5(12) . . ? F1 B1 F4 104.5(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Mo1 C1 C2 145.8(4) . . . . ? C10 Mo1 C1 C2 2.3(8) . . . . ? C15 Mo1 C1 C2 67.2(4) . . . . ? C20 Mo1 C1 C2 -129.0(4) . . . . ? C3 Mo1 C1 C2 -22.2(4) . . . . ? C8 Mo1 C1 C2 -138.4(6) . . . . ? C4 Mo1 C1 C2 -53.2(4) . . . . ? C9 Mo1 C1 C8 -75.7(4) . . . . ? C10 Mo1 C1 C8 140.7(5) . . . . ? C15 Mo1 C1 C8 -154.4(4) . . . . ? C20 Mo1 C1 C8 9.4(5) . . . . ? C3 Mo1 C1 C8 116.2(4) . . . . ? C2 Mo1 C1 C8 138.4(6) . . . . ? C4 Mo1 C1 C8 85.3(4) . . . . ? C8 C1 C2 C3 -7.0(11) . . . . ? Mo1 C1 C2 C3 46.9(6) . . . . ? C8 C1 C2 Mo1 -53.9(6) . . . . ? C9 Mo1 C2 C1 -42.7(5) . . . . ? C10 Mo1 C2 C1 -178.9(4) . . . . ? C15 Mo1 C2 C1 -110.0(4) . . . . ? C20 Mo1 C2 C1 73.4(5) . . . . ? C3 Mo1 C2 C1 143.5(6) . . . . ? C8 Mo1 C2 C1 25.0(4) . . . . ? C4 Mo1 C2 C1 118.3(4) . . . . ? C9 Mo1 C2 C3 173.9(3) . . . . ? C10 Mo1 C2 C3 37.6(5) . . . . ? C15 Mo1 C2 C3 106.5(4) . . . . ? C20 Mo1 C2 C3 -70.1(5) . . . . ? C1 Mo1 C2 C3 -143.5(6) . . . . ? C8 Mo1 C2 C3 -118.5(4) . . . . ? C4 Mo1 C2 C3 -25.1(4) . . . . ? C1 C2 C3 C4 10.5(11) . . . . ? Mo1 C2 C3 C4 57.5(6) . . . . ? C1 C2 C3 Mo1 -47.0(6) . . . . ? C9 Mo1 C3 C4 -152.1(6) . . . . ? C10 Mo1 C3 C4 74.3(4) . . . . ? C15 Mo1 C3 C4 152.7(4) . . . . ? C20 Mo1 C3 C4 -6.0(4) . . . . ? C1 Mo1 C3 C4 -115.4(4) . . . . ? C2 Mo1 C3 C4 -137.3(6) . . . . ? C8 Mo1 C3 C4 -84.0(4) . . . . ? C9 Mo1 C3 C2 -14.9(8) . . . . ? C10 Mo1 C3 C2 -148.5(4) . . . . ? C15 Mo1 C3 C2 -70.0(4) . . . . ? C20 Mo1 C3 C2 131.3(4) . . . . ? C1 Mo1 C3 C2 21.9(4) . . . . ? C8 Mo1 C3 C2 53.2(4) . . . . ? C4 Mo1 C3 C2 137.3(6) . . . . ? C2 C3 C4 C5 55.7(9) . . . . ? Mo1 C3 C4 C5 111.1(6) . . . . ? C2 C3 C4 Mo1 -55.4(6) . . . . ? C9 Mo1 C4 C3 150.3(6) . . . . ? C10 Mo1 C4 C3 -103.8(4) . . . . ? C15 Mo1 C4 C3 -32.1(4) . . . . ? C20 Mo1 C4 C3 174.5(4) . . . . ? C1 Mo1 C4 C3 56.6(4) . . . . ? C2 Mo1 C4 C3 26.0(4) . . . . ? C8 Mo1 C4 C3 92.1(4) . . . . ? C9 Mo1 C4 C5 27.3(9) . . . . ? C10 Mo1 C4 C5 133.2(5) . . . . ? C15 Mo1 C4 C5 -155.1(4) . . . . ? C20 Mo1 C4 C5 51.5(5) . . . . ? C1 Mo1 C4 C5 -66.4(5) . . . . ? C3 Mo1 C4 C5 -123.0(6) . . . . ? C2 Mo1 C4 C5 -97.0(5) . . . . ? C8 Mo1 C4 C5 -31.0(5) . . . . ? C3 C4 C5 C6 -28.0(10) . . . . ? Mo1 C4 C5 C6 56.5(7) . . . . ? C4 C5 C6 C7 -71.0(9) . . . . ? C5 C6 C7 C8 69.2(9) . . . . ? C2 C1 C8 C7 -62.3(9) . . . . ? Mo1 C1 C8 C7 -115.4(6) . . . . ? C2 C1 C8 Mo1 53.1(6) . . . . ? C6 C7 C8 C1 33.4(9) . . . . ? C6 C7 C8 Mo1 -53.7(8) . . . . ? C9 Mo1 C8 C1 105.5(4) . . . . ? C10 Mo1 C8 C1 -136.8(5) . . . . ? C15 Mo1 C8 C1 31.0(5) . . . . ? C20 Mo1 C8 C1 -171.5(4) . . . . ? C3 Mo1 C8 C1 -55.9(4) . . . . ? C2 Mo1 C8 C1 -24.9(4) . . . . ? C4 Mo1 C8 C1 -90.5(4) . . . . ? C9 Mo1 C8 C7 -134.3(5) . . . . ? C10 Mo1 C8 C7 -16.6(9) . . . . ? C15 Mo1 C8 C7 151.2(5) . . . . ? C20 Mo1 C8 C7 -51.3(5) . . . . ? C1 Mo1 C8 C7 120.2(7) . . . . ? C3 Mo1 C8 C7 64.3(5) . . . . ? C2 Mo1 C8 C7 95.3(6) . . . . ? C4 Mo1 C8 C7 29.7(5) . . . . ? C10 Mo1 C9 O1 -171(100) . . . . ? C15 Mo1 C9 O1 114(39) . . . . ? C20 Mo1 C9 O1 -92(39) . . . . ? C1 Mo1 C9 O1 24(39) . . . . ? C3 Mo1 C9 O1 57(40) . . . . ? C2 Mo1 C9 O1 47(39) . . . . ? C8 Mo1 C9 O1 -10(39) . . . . ? C4 Mo1 C9 O1 -68(40) . . . . ? C11 N1 C10 Mo1 -19(8) . . . . ? C9 Mo1 C10 N1 -164(4) . . . . ? C15 Mo1 C10 N1 -89(4) . . . . ? C20 Mo1 C10 N1 116(4) . . . . ? C1 Mo1 C10 N1 -21(5) . . . . ? C3 Mo1 C10 N1 1(4) . . . . ? C2 Mo1 C10 N1 -20(4) . . . . ? C8 Mo1 C10 N1 81(4) . . . . ? C4 Mo1 C10 N1 35(4) . . . . ? C10 N1 C11 C12 -110(4) . . . . ? C10 N1 C11 C14 129(4) . . . . ? C10 N1 C11 C13 9(4) . . . . ? C16 N2 C15 Mo1 27(18) . . . . ? C9 Mo1 C15 N2 34(5) . . . . ? C10 Mo1 C15 N2 -72(5) . . . . ? C20 Mo1 C15 N2 -21(5) . . . . ? C1 Mo1 C15 N2 130(5) . . . . ? C3 Mo1 C15 N2 -163(5) . . . . ? C2 Mo1 C15 N2 163(5) . . . . ? C8 Mo1 C15 N2 113(5) . . . . ? C4 Mo1 C15 N2 -145(5) . . . . ? C15 N2 C16 C17 73(14) . . . . ? C15 N2 C16 C19 -49(14) . . . . ? C15 N2 C16 C18 -168(13) . . . . ? C21 N3 C20 Mo1 -88(21) . . . . ? C9 Mo1 C20 N3 -38(14) . . . . ? C10 Mo1 C20 N3 66(14) . . . . ? C15 Mo1 C20 N3 17(14) . . . . ? C1 Mo1 C20 N3 -132(14) . . . . ? C3 Mo1 C20 N3 153(14) . . . . ? C2 Mo1 C20 N3 -170(14) . . . . ? C8 Mo1 C20 N3 -126(14) . . . . ? C4 Mo1 C20 N3 150(14) . . . . ? C20 N3 C21 C22 28(14) . . . . ? C20 N3 C21 C24 148(14) . . . . ? C20 N3 C21 C23 -92(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.872 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.106 data_Complex_1a _database_code_CSD 195205 #------------------------------------------------------------------------------ _audit_creation_date 19102-07-11 _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 10.182(4) _cell_length_b 16.698(4) _cell_length_c 19.141(6) _cell_angle_alpha 90 _cell_angle_beta 94.86(3) _cell_angle_gamma 90 _cell_volume 3243(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 16.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 730.34 _chemical_formula_analytical ? _chemical_formula_sum 'C35 H33 B F4 Mo O2 P2 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1488.00 _exptl_absorpt_coefficient_mu 4.783 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.874 _exptl_special_details ; The scan width was (1.26+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.60 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 7072 _reflns_number_total 5005 _reflns_number_observed 3808 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.05361 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 60.07 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00118 _diffrn_orient_matrix_UB_12 0.05985 _diffrn_orient_matrix_UB_13 0.00175 _diffrn_orient_matrix_UB_21 -0.09353 _diffrn_orient_matrix_UB_22 0.00130 _diffrn_orient_matrix_UB_23 -0.02066 _diffrn_orient_matrix_UB_31 -0.03108 _diffrn_orient_matrix_UB_32 -0.00164 _diffrn_orient_matrix_UB_33 0.04816 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 140 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B 0 4 0.009 0.004 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 16 0.073 0.053 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mo 0 4 -0.048 2.734 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.295 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Mo1 0.21856(5) 0.68963(3) 0.69168(3) 0.0311(2) 1.000 . Uani d ? P1 0.4621(2) 0.6743(1) 0.70200(9) 0.0312(5) 1.000 . Uani d ? P2 0.3139(2) 0.6920(1) 0.81750(9) 0.0320(5) 1.000 . Uani d ? O9 0.1721(7) 0.5095(3) 0.7173(3) 0.078(2) 1.000 . Uani d ? O10 0.2474(6) 0.6348(4) 0.5365(3) 0.078(2) 1.000 . Uani d ? C1 0.0992(9) 0.8451(5) 0.7385(4) 0.066(3) 1.000 . Uani d ? C2 0.2219(8) 0.8389(4) 0.6985(4) 0.051(2) 1.000 . Uani d ? C3 0.2160(7) 0.8268(4) 0.6301(4) 0.048(2) 1.000 . Uani d ? C4 0.0934(10) 0.8315(6) 0.5812(5) 0.080(3) 1.000 . Uani d ? C5 -0.0021(9) 0.7674(5) 0.5781(5) 0.071(3) 1.000 . Uani d ? C6 0.0100(7) 0.7010(5) 0.6298(4) 0.053(2) 1.000 . Uani d ? C7 -0.0057(7) 0.7067(5) 0.7029(4) 0.057(3) 1.000 . Uani d ? C8 0.0460(7) 0.7633(5) 0.7496(4) 0.053(2) 1.000 . Uani d ? C9 0.1918(7) 0.5769(5) 0.7093(4) 0.045(2) 1.000 . Uani d ? C10 0.2383(7) 0.6576(5) 0.5919(4) 0.045(2) 1.000 . Uani d ? C11 0.3254(6) 0.7790(4) 0.8756(3) 0.034(2) 1.000 . Uani d ? C12 0.2323(7) 0.7887(4) 0.9246(4) 0.044(2) 1.000 . Uani d ? C13 0.2362(8) 0.8542(5) 0.9694(4) 0.059(3) 1.000 . Uani d ? C14 0.3328(9) 0.9106(5) 0.9653(4) 0.059(3) 1.000 . Uani d ? C15 0.4261(9) 0.9013(5) 0.9186(5) 0.063(3) 1.000 . Uani d ? C16 0.4218(8) 0.8367(4) 0.8727(4) 0.049(2) 1.000 . Uani d ? C17 0.2637(7) 0.6136(4) 0.8755(4) 0.039(2) 1.000 . Uani d ? C18 0.1360(8) 0.5843(5) 0.8690(4) 0.052(2) 1.000 . Uani d ? C19 0.0990(9) 0.5245(5) 0.9135(5) 0.061(3) 1.000 . Uani d ? C20 0.1874(10) 0.4954(5) 0.9648(5) 0.059(3) 1.000 . Uani d ? C21 0.3129(9) 0.5243(5) 0.9726(4) 0.056(3) 1.000 . Uani d ? C22 0.3523(7) 0.5839(4) 0.9289(4) 0.044(2) 1.000 . Uani d ? C23 0.5513(7) 0.5888(4) 0.6694(4) 0.039(2) 1.000 . Uani d ? C24 0.4911(8) 0.5261(5) 0.6320(5) 0.061(3) 1.000 . Uani d ? C25 0.5635(10) 0.4637(5) 0.6100(5) 0.075(3) 1.000 . Uani d ? C26 0.6959(8) 0.4600(5) 0.6246(4) 0.058(3) 1.000 . Uani d ? C27 0.7573(8) 0.5214(5) 0.6626(5) 0.065(3) 1.000 . Uani d ? C28 0.6862(8) 0.5848(5) 0.6848(5) 0.063(3) 1.000 . Uani d ? C29 0.5620(6) 0.7582(4) 0.6767(3) 0.031(2) 1.000 . Uani d ? C30 0.6474(7) 0.8013(4) 0.7227(4) 0.048(2) 1.000 . Uani d ? C31 0.7160(8) 0.8651(5) 0.6987(4) 0.058(3) 1.000 . Uani d ? C32 0.7018(8) 0.8866(5) 0.6291(5) 0.055(3) 1.000 . Uani d ? C33 0.6217(8) 0.8435(5) 0.5823(4) 0.052(2) 1.000 . Uani d ? C34 0.5512(7) 0.7798(4) 0.6065(4) 0.042(2) 1.000 . Uani d ? C35 0.4827(6) 0.6651(4) 0.7973(3) 0.035(2) 1.000 . Uani d ? H1A 0.0344 0.8762 0.7122 0.079 1.000 . Uiso c ? H1B 0.1212 0.8698 0.7826 0.079 1.000 . Uiso c ? H2 0.3059 0.8439 0.7238 0.061 1.000 . Uiso c ? H3 0.2959 0.8142 0.6103 0.057 1.000 . Uiso c ? H4A 0.1211 0.8370 0.5352 0.096 1.000 . Uiso c ? H4B 0.0482 0.8787 0.5933 0.096 1.000 . Uiso c ? H5A -0.0855 0.7916 0.5822 0.086 1.000 . Uiso c ? H5B -0.0008 0.7437 0.5331 0.086 1.000 . Uiso c ? H6 0.0301 0.6495 0.6125 0.064 1.000 . Uiso c ? H7 -0.0584 0.6665 0.7217 0.068 1.000 . Uiso c ? H8 0.0483 0.7475 0.7974 0.064 1.000 . Uiso c ? H12 0.1650 0.7497 0.9273 0.053 1.000 . Uiso c ? H13 0.1725 0.8599 1.0026 0.070 1.000 . Uiso c ? H14 0.3350 0.9562 0.9950 0.070 1.000 . Uiso c ? H15 0.4949 0.9397 0.9175 0.076 1.000 . Uiso c ? H16 0.4853 0.8322 0.8393 0.058 1.000 . Uiso c ? H18 0.0736 0.6053 0.8340 0.063 1.000 . Uiso c ? H19 0.0119 0.5036 0.9082 0.074 1.000 . Uiso c ? H20 0.1612 0.4546 0.9953 0.071 1.000 . Uiso c ? H21 0.3736 0.5034 1.0085 0.067 1.000 . Uiso c ? H22 0.4394 0.6045 0.9352 0.053 1.000 . Uiso c ? H24 0.3983 0.5265 0.6214 0.073 1.000 . Uiso c ? H25 0.5200 0.4218 0.5836 0.090 1.000 . Uiso c ? H26 0.7451 0.4161 0.6091 0.069 1.000 . Uiso c ? H27 0.8501 0.5198 0.6735 0.078 1.000 . Uiso c ? H28 0.7302 0.6266 0.7111 0.076 1.000 . Uiso c ? H30 0.6584 0.7868 0.7708 0.058 1.000 . Uiso c ? H31 0.7739 0.8947 0.7306 0.069 1.000 . Uiso c ? H32 0.7481 0.9318 0.6135 0.067 1.000 . Uiso c ? H33 0.6144 0.8570 0.5339 0.063 1.000 . Uiso c ? H34 0.4941 0.7501 0.5742 0.051 1.000 . Uiso c ? H35A 0.5056 0.6121 0.8117 0.042 1.000 . Uiso c ? H35B 0.5466 0.7015 0.8177 0.042 1.000 . Uiso c ? F1 0.2718(9) 0.2423(4) 0.1042(4) 0.180(4) 1.000 . Uani d ? F2 0.1010(8) 0.3043(5) 0.0462(4) 0.178(4) 1.000 . Uani d ? F3 0.280(1) 0.3552(8) 0.0743(6) 0.259(7) 1.000 . Uani d ? F4 0.1713(7) 0.3364(6) 0.1544(4) 0.157(4) 1.000 . Uani d ? B1 0.189(1) 0.3004(9) 0.0965(6) 0.081(4) 1.000 . Uani 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo1 0.0274(3) 0.0314(3) 0.0332(3) -0.0034(2) -0.0051(2) -0.0003(2) P1 0.0303(9) 0.0320(9) 0.0306(9) -0.0017(7) -0.0014(7) -0.0005(7) P2 0.0297(9) 0.0331(9) 0.0325(9) -0.0031(7) -0.0012(7) 0.0010(8) O9 0.122(6) 0.038(3) 0.075(4) -0.027(4) 0.006(4) -0.001(3) O10 0.095(5) 0.096(5) 0.043(4) 0.016(4) 0.000(3) -0.015(3) C1 0.080(7) 0.057(5) 0.060(6) 0.024(5) 0.005(5) -0.004(4) C2 0.053(5) 0.033(4) 0.064(6) 0.003(4) -0.014(4) 0.001(4) C3 0.043(4) 0.036(4) 0.062(5) 0.003(3) -0.005(4) 0.011(4) C4 0.073(7) 0.090(7) 0.072(6) -0.009(5) -0.027(5) 0.035(6) C5 0.068(6) 0.063(6) 0.079(7) 0.004(5) -0.018(5) 0.017(5) C6 0.039(4) 0.051(5) 0.065(5) -0.002(4) -0.019(4) -0.001(4) C7 0.032(4) 0.079(6) 0.058(5) -0.005(4) -0.003(4) 0.004(5) C8 0.038(4) 0.065(6) 0.054(5) 0.009(4) -0.004(4) 0.001(4) C9 0.052(5) 0.049(5) 0.033(4) -0.012(4) -0.003(3) 0.001(3) C10 0.053(5) 0.047(4) 0.035(4) 0.003(4) -0.004(4) -0.001(3) C11 0.033(4) 0.036(4) 0.032(4) -0.001(3) -0.008(3) 0.004(3) C12 0.041(4) 0.048(4) 0.043(4) 0.001(3) 0.002(3) -0.004(3) C13 0.063(6) 0.068(6) 0.045(5) 0.019(5) 0.006(4) -0.008(4) C14 0.082(6) 0.048(5) 0.045(5) 0.005(5) -0.001(4) -0.011(4) C15 0.078(6) 0.049(5) 0.061(5) -0.020(4) -0.003(5) -0.004(4) C16 0.057(5) 0.045(4) 0.044(4) -0.003(4) 0.004(4) -0.008(4) C17 0.046(4) 0.033(4) 0.039(4) -0.004(3) 0.003(3) 0.001(3) C18 0.054(5) 0.051(5) 0.052(5) -0.008(4) 0.004(4) 0.000(4) C19 0.068(6) 0.045(5) 0.075(6) -0.027(4) 0.026(5) -0.013(4) C20 0.089(7) 0.032(4) 0.063(6) -0.001(4) 0.035(5) 0.008(4) C21 0.082(6) 0.042(5) 0.045(5) 0.025(4) 0.020(4) 0.011(4) C22 0.051(5) 0.042(4) 0.040(4) 0.003(4) 0.011(3) -0.001(3) C23 0.038(4) 0.035(4) 0.043(4) 0.000(3) 0.003(3) 0.000(3) C24 0.048(5) 0.053(5) 0.079(6) 0.001(4) -0.013(4) -0.019(4) C25 0.076(7) 0.058(6) 0.088(7) 0.006(5) -0.011(5) -0.031(5) C26 0.062(5) 0.044(5) 0.067(6) 0.016(4) 0.010(4) -0.002(4) C27 0.043(5) 0.054(5) 0.099(7) 0.006(4) 0.008(5) -0.018(5) C28 0.041(5) 0.050(5) 0.096(7) -0.001(4) -0.003(5) -0.014(5) C29 0.026(3) 0.033(4) 0.034(4) -0.001(3) 0.001(3) 0.000(3) C30 0.043(4) 0.053(5) 0.047(4) -0.007(4) -0.002(3) -0.003(4) C31 0.054(5) 0.058(5) 0.062(6) -0.026(4) 0.007(4) -0.010(4) C32 0.049(5) 0.047(5) 0.072(6) -0.015(4) 0.017(4) 0.005(4) C33 0.054(5) 0.052(5) 0.050(5) -0.002(4) 0.002(4) 0.007(4) C34 0.039(4) 0.043(4) 0.043(4) -0.007(3) -0.003(3) 0.003(3) C35 0.029(4) 0.041(4) 0.036(4) -0.002(3) 0.001(3) 0.004(3) F1 0.240(10) 0.110(6) 0.164(7) 0.060(6) -0.138(7) -0.038(5) F2 0.129(6) 0.230(9) 0.157(7) 0.063(6) -0.103(6) -0.069(6) F3 0.24(1) 0.34(2) 0.20(1) -0.04(1) 0.013(9) 0.15(1) F4 0.095(5) 0.27(1) 0.102(5) 0.040(6) -0.004(4) -0.052(6) B1 0.076(8) 0.13(1) 0.036(6) 0.043(8) -0.001(6) 0.025(7) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3808 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0555 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0695 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.383 _refine_ls_shift/esd_max 0.1530 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.63 _refine_diff_density_max 1.22 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MO1 P1 2.484(2) . . yes MO1 P2 2.519(2) . . yes MO1 C2 2.495(7) . . yes MO1 C3 2.576(7) . . yes MO1 C6 2.350(7) . . yes MO1 C7 2.329(8) . . yes MO1 C8 2.482(8) . . yes MO1 C9 1.935(8) . . yes MO1 C10 2.010(8) . . yes P1 C23 1.831(7) . . yes P1 C29 1.821(6) . . yes P1 C35 1.824(7) . . yes P2 C11 1.827(7) . . yes P2 C17 1.816(7) . . yes P2 C35 1.849(7) . . yes O9 C9 1.157(10) . . yes O10 C10 1.138(10) . . yes C1 C2 1.52(1) . . yes C1 C8 1.49(1) . . yes C1 H1A 0.95 . . no C1 H1B 0.95 . . no C2 C3 1.32(1) . . yes C2 H2 0.95 . . no C3 C4 1.50(1) . . yes C3 H3 0.95 . . no C4 C5 1.44(1) . . yes C4 H4A 0.95 . . no C4 H4B 0.95 . . no C5 C6 1.49(1) . . yes C5 H5A 0.95 . . no C5 H5B 0.95 . . no C6 C7 1.42(1) . . yes C6 H6 0.95 . . no C7 C8 1.37(1) . . yes C7 H7 0.95 . . no C8 H8 0.95 . . no C11 C12 1.40(1) . . yes C11 C16 1.380(10) . . yes C12 C13 1.39(1) . . yes C12 H12 0.95 . . no C13 C14 1.37(1) . . yes C13 H13 0.95 . . no C14 C15 1.37(1) . . yes C14 H14 0.95 . . no C15 C16 1.39(1) . . yes C15 H15 0.95 . . no C16 H16 0.95 . . no C17 C18 1.39(1) . . yes C17 C22 1.396(9) . . yes C18 C19 1.39(1) . . yes C18 H18 0.95 . . no C19 C20 1.36(1) . . yes C19 H19 0.95 . . no C20 C21 1.36(1) . . yes C20 H20 0.95 . . no C21 C22 1.38(1) . . yes C21 H21 0.95 . . no C22 H22 0.95 . . no C23 C24 1.38(1) . . yes C23 C28 1.38(1) . . yes C24 C25 1.36(1) . . yes C24 H24 0.95 . . no C25 C26 1.35(1) . . yes C25 H25 0.95 . . no C26 C27 1.38(1) . . yes C26 H26 0.95 . . no C27 C28 1.37(1) . . yes C27 H27 0.95 . . no C28 H28 0.95 . . no C29 C30 1.385(9) . . yes C29 C34 1.386(9) . . yes C30 C31 1.37(1) . . yes C30 H30 0.95 . . no C31 C32 1.38(1) . . yes C31 H31 0.95 . . no C32 C33 1.37(1) . . yes C32 H32 0.95 . . no C33 C34 1.39(1) . . yes C33 H33 0.95 . . no C34 H34 0.95 . . no C35 H35A 0.95 . . no C35 H35B 0.95 . . no F1 B1 1.29(2) . . yes F2 B1 1.26(1) . . yes F3 B1 1.40(2) . . yes F4 B1 1.29(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 MO1 P2 67.95(6) . . . yes P1 MO1 C2 95.2(2) . . . yes P1 MO1 C3 95.7(2) . . . yes P1 MO1 C6 154.4(2) . . . yes P1 MO1 C7 170.1(2) . . . yes P1 MO1 C8 139.0(2) . . . yes P1 MO1 C9 92.3(2) . . . yes P1 MO1 C10 82.5(2) . . . yes P2 MO1 C2 86.1(2) . . . yes P2 MO1 C3 114.3(2) . . . yes P2 MO1 C6 137.6(2) . . . yes P2 MO1 C7 102.2(2) . . . yes P2 MO1 C8 78.2(2) . . . yes P2 MO1 C9 84.1(2) . . . yes P2 MO1 C10 148.3(2) . . . yes C2 MO1 C3 30.2(3) . . . yes C2 MO1 C6 87.3(3) . . . yes C2 MO1 C7 83.2(3) . . . yes C2 MO1 C8 59.2(3) . . . yes C2 MO1 C9 164.4(3) . . . yes C2 MO1 C10 108.3(3) . . . yes C3 MO1 C6 74.0(3) . . . yes C3 MO1 C7 87.8(3) . . . yes C3 MO1 C8 77.5(3) . . . yes C3 MO1 C9 161.6(3) . . . yes C3 MO1 C10 78.4(3) . . . yes C6 MO1 C7 35.4(3) . . . yes C6 MO1 C8 62.7(3) . . . yes C6 MO1 C9 91.8(3) . . . yes C6 MO1 C10 72.6(3) . . . yes C7 MO1 C8 33.0(3) . . . yes C7 MO1 C9 87.1(3) . . . yes C7 MO1 C10 107.3(3) . . . yes C8 MO1 C9 106.8(3) . . . yes C8 MO1 C10 133.5(3) . . . yes C9 MO1 C10 86.2(3) . . . yes MO1 P1 C23 125.0(2) . . . yes MO1 P1 C29 118.4(2) . . . yes MO1 P1 C35 96.8(2) . . . yes C23 P1 C29 101.8(3) . . . yes C23 P1 C35 104.9(3) . . . yes C29 P1 C35 108.1(3) . . . yes MO1 P2 C11 126.4(2) . . . yes MO1 P2 C17 117.8(2) . . . yes MO1 P2 C35 94.9(2) . . . yes C11 P2 C17 102.0(3) . . . yes C11 P2 C35 107.9(3) . . . yes C17 P2 C35 105.5(3) . . . yes C2 C1 C8 109.5(7) . . . yes C2 C1 H1A 109.5 . . . no C2 C1 H1B 109.5 . . . no C8 C1 H1A 109.5 . . . no C8 C1 H1B 109.5 . . . no H1A C1 H1B 109.5 . . . no MO1 C2 C1 94.9(5) . . . yes MO1 C2 C3 78.3(4) . . . yes MO1 C2 H2 97.0 . . . no C1 C2 C3 122.5(7) . . . yes C1 C2 H2 118.7 . . . no C3 C2 H2 118.7 . . . no MO1 C3 C2 71.6(4) . . . yes MO1 C3 C4 108.0(5) . . . yes MO1 C3 H3 90.5 . . . no C2 C3 C4 125.2(8) . . . yes C2 C3 H3 117.4 . . . no C4 C3 H3 117.4 . . . no C3 C4 C5 120.6(8) . . . yes C3 C4 H4A 106.6 . . . no C3 C4 H4B 106.6 . . . no C5 C4 H4A 106.6 . . . no C5 C4 H4B 106.6 . . . no H4A C4 H4B 109.5 . . . no C4 C5 C6 120.6(8) . . . yes C4 C5 H5A 106.6 . . . no C4 C5 H5B 106.6 . . . no C6 C5 H5A 106.6 . . . no C6 C5 H5B 106.6 . . . no H5A C5 H5B 109.5 . . . no MO1 C6 C5 114.6(5) . . . yes MO1 C6 C7 71.5(4) . . . yes MO1 C6 H6 83.7 . . . no C5 C6 C7 126.4(7) . . . yes C5 C6 H6 116.8 . . . no C7 C6 H6 116.8 . . . no MO1 C7 C6 73.1(4) . . . yes MO1 C7 C8 79.6(5) . . . yes MO1 C7 H7 122.6 . . . no C6 C7 C8 128.1(8) . . . yes C6 C7 H7 116.0 . . . no C8 C7 H7 115.9 . . . no MO1 C8 C1 96.3(5) . . . yes MO1 C8 C7 67.4(4) . . . yes MO1 C8 H8 109.4 . . . no C1 C8 C7 131.3(7) . . . yes C1 C8 H8 114.4 . . . no C7 C8 H8 114.3 . . . no MO1 C9 O9 177.1(6) . . . yes MO1 C10 O10 175.7(7) . . . yes P2 C11 C12 119.2(5) . . . yes P2 C11 C16 122.6(5) . . . yes C12 C11 C16 118.1(6) . . . yes C11 C12 C13 121.3(7) . . . yes C11 C12 H12 119.3 . . . no C13 C12 H12 119.3 . . . no C12 C13 C14 119.3(8) . . . yes C12 C13 H13 120.4 . . . no C14 C13 H13 120.3 . . . no C13 C14 C15 120.2(8) . . . yes C13 C14 H14 119.9 . . . no C15 C14 H14 119.9 . . . no C14 C15 C16 120.9(8) . . . yes C14 C15 H15 119.5 . . . no C16 C15 H15 119.5 . . . no C11 C16 C15 120.1(7) . . . yes C11 C16 H16 120.0 . . . no C15 C16 H16 120.0 . . . no P2 C17 C18 120.7(5) . . . yes P2 C17 C22 120.4(5) . . . yes C18 C17 C22 118.9(6) . . . yes C17 C18 C19 120.1(7) . . . yes C17 C18 H18 120.0 . . . no C19 C18 H18 120.0 . . . no C18 C19 C20 120.2(8) . . . yes C18 C19 H19 119.9 . . . no C20 C19 H19 119.9 . . . no C19 C20 C21 120.6(8) . . . yes C19 C20 H20 119.7 . . . no C21 C20 H20 119.7 . . . no C20 C21 C22 120.4(7) . . . yes C20 C21 H21 119.8 . . . no C22 C21 H21 119.8 . . . no C17 C22 C21 119.8(7) . . . yes C17 C22 H22 120.1 . . . no C21 C22 H22 120.1 . . . no P1 C23 C24 123.8(5) . . . yes P1 C23 C28 118.6(5) . . . yes C24 C23 C28 117.6(7) . . . yes C23 C24 C25 120.7(7) . . . yes C23 C24 H24 119.6 . . . no C25 C24 H24 119.6 . . . no C24 C25 C26 121.7(8) . . . yes C24 C25 H25 119.1 . . . no C26 C25 H25 119.2 . . . no C25 C26 C27 118.4(8) . . . yes C25 C26 H26 120.8 . . . no C27 C26 H26 120.8 . . . no C26 C27 C28 120.7(7) . . . yes C26 C27 H27 119.7 . . . no C28 C27 H27 119.7 . . . no C23 C28 C27 120.9(7) . . . yes C23 C28 H28 119.6 . . . no C27 C28 H28 119.6 . . . no P1 C29 C30 124.4(5) . . . yes P1 C29 C34 117.2(5) . . . yes C30 C29 C34 118.4(6) . . . yes C29 C30 C31 120.0(7) . . . yes C29 C30 H30 120.0 . . . no C31 C30 H30 120.0 . . . no C30 C31 C32 120.8(7) . . . yes C30 C31 H31 119.6 . . . no C32 C31 H31 119.6 . . . no C31 C32 C33 120.4(7) . . . yes C31 C32 H32 119.8 . . . no C33 C32 H32 119.8 . . . no C32 C33 C34 118.9(7) . . . yes C32 C33 H33 120.5 . . . no C34 C33 H33 120.5 . . . no C29 C34 C33 121.5(6) . . . yes C29 C34 H34 119.2 . . . no C33 C34 H34 119.2 . . . no P1 C35 P2 99.1(3) . . . yes P1 C35 H35A 112.0 . . . no P1 C35 H35B 112.0 . . . no P2 C35 H35A 112.0 . . . no P2 C35 H35B 112.0 . . . no H35A C35 H35B 109.5 . . . no F1 B1 F2 123(1) . . . yes F1 B1 F3 94(1) . . . yes F1 B1 F4 113.0(10) . . . yes F2 B1 F3 100(1) . . . yes F2 B1 F4 119(1) . . . yes F3 B1 F4 95(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O9 C15 3.25(1) . 2_546 no O10 F1 3.230(10) . 2 no C20 F3 3.23(2) . 1_556 no C33 F2 3.27(1) . 2 no C34 F2 3.22(1) . 2 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag MO1 P1 C23 C24 . . . . 3.9(8) no MO1 P1 C23 C28 . . . . -173.9(5) no MO1 P1 C29 C30 . . . . 114.1(6) no MO1 P1 C29 C34 . . . . -66.0(6) no MO1 P1 C35 P2 . . . . -9.7(3) no MO1 P2 C11 C12 . . . . 100.2(5) no MO1 P2 C11 C16 . . . . -78.9(6) no MO1 P2 C17 C18 . . . . -36.4(7) no MO1 P2 C17 C22 . . . . 145.8(5) no MO1 P2 C35 P1 . . . . 9.5(3) no MO1 C2 C1 C8 . . . . -1.1(6) no MO1 C2 C3 C4 . . . . 99.3(8) no MO1 C3 C2 C1 . . . . -88.4(7) no MO1 C3 C4 C5 . . . . 3(1) no MO1 C6 C5 C4 . . . . -16(1) no MO1 C6 C7 C8 . . . . 61.5(8) no MO1 C7 C6 C5 . . . . -107.3(8) no MO1 C7 C8 C1 . . . . 78.1(9) no MO1 C8 C1 C2 . . . . 1.1(7) no MO1 C8 C7 C6 . . . . -58.7(8) no P1 MO1 P2 C11 . . . . 109.1(3) no P1 MO1 P2 C17 . . . . -117.9(3) no P1 MO1 P2 C35 . . . . -7.4(2) no P1 MO1 C2 C1 . . . . -145.3(4) no P1 MO1 C2 C3 . . . . 92.5(5) no P1 MO1 C3 C2 . . . . -90.4(5) no P1 MO1 C3 C4 . . . . 147.5(5) no P1 MO1 C6 C5 . . . . -56.0(8) no P1 MO1 C6 C7 . . . . -178.4(4) no P1 MO1 C7 C6 . . . . 175(1) no P1 MO1 C7 C8 . . . . 40(1) no P1 MO1 C8 C1 . . . . 57.5(6) no P1 MO1 C8 C7 . . . . -170.2(4) no P1 MO1 C9 O9 . . . . -129(13) no P1 MO1 C10 O10 . . . . 98(8) no P1 C23 C24 C25 . . . . -179.2(7) no P1 C23 C28 C27 . . . . 179.0(7) no P1 C29 C30 C31 . . . . -178.3(6) no P1 C29 C34 C33 . . . . 179.0(6) no P1 C35 P2 C11 . . . . -121.3(3) no P1 C35 P2 C17 . . . . 130.2(3) no P2 MO1 P1 C23 . . . . 121.1(3) no P2 MO1 P1 C29 . . . . -107.3(2) no P2 MO1 P1 C35 . . . . 7.6(2) no P2 MO1 C2 C1 . . . . -77.9(4) no P2 MO1 C2 C3 . . . . 159.9(5) no P2 MO1 C3 C2 . . . . -22.1(5) no P2 MO1 C3 C4 . . . . -144.2(5) no P2 MO1 C6 C5 . . . . 121.6(6) no P2 MO1 C6 C7 . . . . -0.8(6) no P2 MO1 C7 C6 . . . . 179.5(4) no P2 MO1 C7 C8 . . . . 44.1(5) no P2 MO1 C8 C1 . . . . 91.8(4) no P2 MO1 C8 C7 . . . . -135.9(5) no P2 MO1 C9 O9 . . . . 163(13) no P2 MO1 C10 O10 . . . . 78(8) no P2 C11 C12 C13 . . . . -179.4(6) no P2 C11 C16 C15 . . . . -179.6(6) no P2 C17 C18 C19 . . . . 179.9(6) no P2 C17 C22 C21 . . . . 180.0(6) no P2 C35 P1 C23 . . . . -138.7(3) no P2 C35 P1 C29 . . . . 113.2(3) no O9 C9 MO1 C2 . . . . 111(13) no O9 C9 MO1 C3 . . . . -13(13) no O9 C9 MO1 C6 . . . . 25(13) no O9 C9 MO1 C7 . . . . 60(13) no O9 C9 MO1 C8 . . . . 87(13) no O9 C9 MO1 C10 . . . . -47(13) no O10 C10 MO1 C2 . . . . -168(8) no O10 C10 MO1 C3 . . . . -163(8) no O10 C10 MO1 C6 . . . . -87(8) no O10 C10 MO1 C7 . . . . -80(8) no O10 C10 MO1 C8 . . . . -103(8) no O10 C10 MO1 C9 . . . . 5(8) no C1 C2 MO1 C3 . . . . 122.2(7) no C1 C2 MO1 C6 . . . . 60.3(5) no C1 C2 MO1 C7 . . . . 24.9(5) no C1 C2 MO1 C8 . . . . 0.7(4) no C1 C2 MO1 C9 . . . . -26(1) no C1 C2 MO1 C10 . . . . 131.0(5) no C1 C2 C3 C4 . . . . 10(1) no C1 C8 MO1 C2 . . . . -0.7(4) no C1 C8 MO1 C3 . . . . -26.8(5) no C1 C8 MO1 C6 . . . . -105.0(5) no C1 C8 MO1 C7 . . . . -132.3(7) no C1 C8 MO1 C9 . . . . 171.8(5) no C1 C8 MO1 C10 . . . . -87.2(6) no C1 C8 C7 C6 . . . . 19(1) no C2 MO1 P1 C23 . . . . -155.3(3) no C2 MO1 P1 C29 . . . . -23.7(3) no C2 MO1 P1 C35 . . . . 91.2(3) no C2 MO1 P2 C11 . . . . 12.0(3) no C2 MO1 P2 C17 . . . . 145.0(3) no C2 MO1 P2 C35 . . . . -104.6(3) no C2 MO1 C3 C4 . . . . -122.1(8) no C2 MO1 C6 C5 . . . . 40.4(6) no C2 MO1 C6 C7 . . . . -82.0(5) no C2 MO1 C7 C6 . . . . 95.0(5) no C2 MO1 C7 C8 . . . . -40.3(5) no C2 MO1 C8 C7 . . . . 131.6(6) no C2 C1 C8 C7 . . . . -64(1) no C2 C3 MO1 C6 . . . . 113.5(5) no C2 C3 MO1 C7 . . . . 80.3(5) no C2 C3 MO1 C8 . . . . 48.6(5) no C2 C3 MO1 C9 . . . . 154.3(8) no C2 C3 MO1 C10 . . . . -171.5(5) no C2 C3 C4 C5 . . . . -76(1) no C3 MO1 P1 C23 . . . . -125.0(3) no C3 MO1 P1 C29 . . . . 6.6(3) no C3 MO1 P1 C35 . . . . 121.5(3) no C3 MO1 P2 C11 . . . . 22.9(3) no C3 MO1 P2 C17 . . . . 155.9(3) no C3 MO1 P2 C35 . . . . -93.7(3) no C3 MO1 C6 C5 . . . . 12.9(6) no C3 MO1 C6 C7 . . . . -109.5(5) no C3 MO1 C7 C6 . . . . 65.1(5) no C3 MO1 C7 C8 . . . . -70.3(5) no C3 MO1 C8 C7 . . . . 105.5(5) no C3 C2 MO1 C6 . . . . -62.0(5) no C3 C2 MO1 C7 . . . . -97.3(5) no C3 C2 MO1 C8 . . . . -121.5(5) no C3 C2 MO1 C9 . . . . -149.2(9) no C3 C2 MO1 C10 . . . . 8.8(5) no C3 C2 C1 C8 . . . . 78.2(9) no C3 C4 C5 C6 . . . . 8(1) no C4 C3 MO1 C6 . . . . -8.6(6) no C4 C3 MO1 C7 . . . . -41.8(6) no C4 C3 MO1 C8 . . . . -73.5(6) no C4 C3 MO1 C9 . . . . 32(1) no C4 C3 MO1 C10 . . . . 66.4(6) no C4 C5 C6 C7 . . . . 67(1) no C5 C6 MO1 C7 . . . . 122.4(8) no C5 C6 MO1 C8 . . . . 96.9(6) no C5 C6 MO1 C9 . . . . -155.2(6) no C5 C6 MO1 C10 . . . . -69.7(6) no C5 C6 C7 C8 . . . . -45(1) no C6 MO1 P1 C23 . . . . -60.7(5) no C6 MO1 P1 C29 . . . . 71.0(5) no C6 MO1 P1 C35 . . . . -174.2(5) no C6 MO1 P2 C11 . . . . -69.8(4) no C6 MO1 P2 C17 . . . . 63.2(4) no C6 MO1 P2 C35 . . . . 173.7(3) no C6 MO1 C7 C8 . . . . -135.3(7) no C6 MO1 C8 C7 . . . . 27.3(5) no C6 C7 MO1 C8 . . . . 135.3(7) no C6 C7 MO1 C9 . . . . -97.2(5) no C6 C7 MO1 C10 . . . . -12.1(5) no C7 MO1 P1 C23 . . . . 124(1) no C7 MO1 P1 C29 . . . . -103(1) no C7 MO1 P1 C35 . . . . 11(1) no C7 MO1 P2 C11 . . . . -70.2(3) no C7 MO1 P2 C17 . . . . 62.8(3) no C7 MO1 P2 C35 . . . . 173.2(3) no C7 C6 MO1 C8 . . . . -25.5(5) no C7 C6 MO1 C9 . . . . 82.5(5) no C7 C6 MO1 C10 . . . . 167.9(5) no C7 C8 MO1 C9 . . . . -55.9(5) no C7 C8 MO1 C10 . . . . 45.1(7) no C8 MO1 P1 C23 . . . . 157.5(4) no C8 MO1 P1 C29 . . . . -70.8(4) no C8 MO1 P1 C35 . . . . 44.0(4) no C8 MO1 P2 C11 . . . . -47.4(3) no C8 MO1 P2 C17 . . . . 85.6(3) no C8 MO1 P2 C35 . . . . -164.0(3) no C8 C7 MO1 C9 . . . . 127.5(5) no C8 C7 MO1 C10 . . . . -147.4(5) no C9 MO1 P1 C23 . . . . 38.4(3) no C9 MO1 P1 C29 . . . . 170.0(3) no C9 MO1 P1 C35 . . . . -75.1(3) no C9 MO1 P2 C11 . . . . -155.9(4) no C9 MO1 P2 C17 . . . . -23.0(3) no C9 MO1 P2 C35 . . . . 87.5(3) no C10 MO1 P1 C23 . . . . -47.5(3) no C10 MO1 P1 C29 . . . . 84.1(3) no C10 MO1 P1 C35 . . . . -161.0(3) no C10 MO1 P2 C11 . . . . 131.2(5) no C10 MO1 P2 C17 . . . . -95.9(5) no C10 MO1 P2 C35 . . . . 14.6(5) no C11 P2 C17 C18 . . . . 106.6(6) no C11 P2 C17 C22 . . . . -71.2(6) no C11 C12 C13 C14 . . . . 0(1) no C11 C16 C15 C14 . . . . -2(1) no C12 C11 P2 C17 . . . . -38.4(6) no C12 C11 P2 C35 . . . . -149.2(5) no C12 C11 C16 C15 . . . . 1(1) no C12 C13 C14 C15 . . . . -1(1) no C13 C12 C11 C16 . . . . 0(1) no C13 C14 C15 C16 . . . . 2(1) no C16 C11 P2 C17 . . . . 142.5(6) no C16 C11 P2 C35 . . . . 31.6(6) no C17 C18 C19 C20 . . . . 1(1) no C17 C22 C21 C20 . . . . -1(1) no C18 C17 P2 C35 . . . . -140.7(6) no C18 C17 C22 C21 . . . . 2(1) no C18 C19 C20 C21 . . . . 0(1) no C19 C18 C17 C22 . . . . -2(1) no C19 C20 C21 C22 . . . . 0(1) no C22 C17 P2 C35 . . . . 41.5(6) no C23 P1 C29 C30 . . . . -104.6(6) no C23 P1 C29 C34 . . . . 75.3(6) no C23 C24 C25 C26 . . . . 0(1) no C23 C28 C27 C26 . . . . 0(1) no C24 C23 P1 C29 . . . . -133.9(7) no C24 C23 P1 C35 . . . . 113.5(7) no C24 C23 C28 C27 . . . . 0(1) no C24 C25 C26 C27 . . . . 0(1) no C25 C24 C23 C28 . . . . -1(1) no C25 C26 C27 C28 . . . . 0(1) no C28 C23 P1 C29 . . . . 48.3(7) no C28 C23 P1 C35 . . . . -64.3(7) no C29 C30 C31 C32 . . . . 0(1) no C29 C34 C33 C32 . . . . -1(1) no C30 C29 P1 C35 . . . . 5.5(7) no C30 C29 C34 C33 . . . . -1(1) no C30 C31 C32 C33 . . . . -1(1) no C31 C30 C29 C34 . . . . 1(1) no C31 C32 C33 C34 . . . . 2(1) no C34 C29 P1 C35 . . . . -174.5(5) no #------------------------------------------------------------------------------