# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2082 data_global #============================================================================ # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Malcolm L.H.Green' _publ_contact_author_address ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; _publ_contact_author_phone '(01865) 272649' _publ_contact_author_fax '(01865) 272690 ' _publ_contact_author_email 'Malcolm.Green@chemistry.ox.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ' ? ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and reactions of bis(eta-Cyclopentadienyl)niobium(tbutylimido) cations: NMR Evidence for d(0) Olefin Cations [Nb{(eta-C5H4)5}(NtBu)(eta-C2H3R)][B(C6F5)4] , R = H,Me ; loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Humphries, Martin J.' ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? #footnote for author 1 ; ; 'Green, Malcolm L. H.' # Author 2 ; ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? # footnote 2 ; ; 'Douthwaite, Richard E.' # Author 2 ; ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? # footnote 2 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references ; # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # Chebychev Weights # Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 # Denzo # Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # Azimutal absorption correction # North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. # DIFABS # Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. # RC93 # Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; data_compound1 #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; [Nb(eta-C5H5)2(NtBu)(OSO2CF3)] ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment refxyz #**************************************************************************** _cell_length_a 8.648(1) _cell_angle_alpha 90. _cell_length_b 24.018(3) _cell_angle_beta 112.71(2) _cell_length_c 9.588(2) _cell_angle_gamma 90. _cell_volume 1837.1(4) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'Nb ' -2.1970 0.6210 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C15 H19 F3 N Nb O3 S' _chemical_formula_moiety 'C15 H19 F3 N Nb O3 S' _chemical_compound_source ; ? ; _chemical_formula_weight 443.28 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 0 _cell_formula_units_Z 4 _exptl_crystal_description 'prism' _exptl_crystal_colour ' yellow' _exptl_crystal_size_min 0.015 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_max 0.020 _exptl_crystal_density_diffrn 1.60 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 887.81 _exptl_absorpt_coefficient_mu 0.78 _exptl_absorpt_correction_type none _exptl_absorpt_correction_t_max ? _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 9039 _reflns_number_total 3859 _diffrn_reflns_av_R_equivalents 0.020 # Number of reflections with Friedels Law is 0 # Number of reflections without Friedels Law is 0 _reflns_number_observed 3456 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -10 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -1.01 _refine_diff_density_max 0.52 _refine_ls_number_reflns 3456 _refine_ls_number_parameters 218 _refine_ls_R_factor_obs 0.0410 _refine_ls_wR_factor_obs 0.0488 _refine_ls_goodness_of_fit_obs 1.0657 _refine_ls_shift/su_max 0.001426 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 4.37 2.57 2.99 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_thermal_displace_type Nb1 0.29608(2) 0.370269(8) 0.60892(2) 0.0335 1.0000 Uani N2 0.3709(3) 0.35551(9) 0.4665(2) 0.0410 1.0000 Uani C3 0.4218(4) 0.34359(13) 0.3422(3) 0.0548 1.0000 Uani C4 0.2920(6) 0.3053(2) 0.2315(5) 0.0921 1.0000 Uani C5 0.5869(6) 0.3140(3) 0.4035(6) 0.1165 1.0000 Uani C6 0.4344(11) 0.3973(2) 0.2666(7) 0.1278 1.0000 Uani O7 0.5318(3) 0.38975(12) 0.7863(2) 0.0632 1.0000 Uani S8 0.70596(9) 0.39211(4) 0.80611(9) 0.0574 1.0000 Uani O9 0.7369(5) 0.4260(2) 0.7042(4) 0.1453 1.0000 Uani O10 0.7833(5) 0.34045(18) 0.8315(6) 0.1345 1.0000 Uani C11 0.7934(5) 0.4271(3) 0.9866(5) 0.0965 1.0000 Uani F12 0.9564(3) 0.43426(18) 1.0261(4) 0.1405 1.0000 Uani F13 0.7691(5) 0.4001(3) 1.0911(3) 0.1722 1.0000 Uani F14 0.7267(6) 0.4760(2) 0.9766(6) 0.2004 1.0000 Uani C15 0.1332(7) 0.44625(17) 0.6826(7) 0.0889 1.0000 Uani C16 0.2686(6) 0.46956(16) 0.6799(6) 0.0826 1.0000 Uani C17 0.2681(6) 0.46819(15) 0.5378(6) 0.0796 1.0000 Uani C18 0.1286(8) 0.4422(2) 0.4464(5) 0.1068 1.0000 Uani C19 0.0399(5) 0.42660(18) 0.543(1) 0.1250 1.0000 Uani C20 0.3593(4) 0.27652(14) 0.7205(4) 0.0630 1.0000 Uani C21 0.3122(6) 0.30517(17) 0.8220(4) 0.0771 1.0000 Uani C22 0.1413(7) 0.31820(16) 0.7497(7) 0.0935 1.0000 Uani C23 0.0910(4) 0.29799(15) 0.5980(5) 0.0743 1.0000 Uani C24 0.2232(5) 0.27024(13) 0.5876(4) 0.0626 1.0000 Uani H41 0.3273 0.2963 0.1456 0.0917 1.0000 Uiso H42 0.1808 0.3231 0.1928 0.0917 1.0000 Uiso H43 0.2877 0.2694 0.2848 0.0917 1.0000 Uiso H51 0.6248 0.3054 0.3196 0.1157 1.0000 Uiso H52 0.6730 0.3382 0.4800 0.1157 1.0000 Uiso H53 0.5761 0.2784 0.4536 0.1157 1.0000 Uiso H61 0.4711 0.3890 0.1815 0.1380 1.0000 Uiso H62 0.5213 0.4216 0.3424 0.1380 1.0000 Uiso H63 0.3249 0.4165 0.2279 0.1380 1.0000 Uiso H151 0.1044 0.4432 0.7739 0.0962 1.0000 Uiso H161 0.3601 0.4858 0.7704 0.0783 1.0000 Uiso H171 0.3558 0.4841 0.5060 0.0814 1.0000 Uiso H181 0.0933 0.4350 0.3355 0.0934 1.0000 Uiso H191 -0.0686 0.4057 0.5130 0.0799 1.0000 Uiso H201 0.4748 0.2624 0.7404 0.0643 1.0000 Uiso H211 0.3863 0.3148 0.9284 0.0774 1.0000 Uiso H221 0.0708 0.3379 0.7962 0.1031 1.0000 Uiso H231 -0.0213 0.3035 0.5147 0.0671 1.0000 Uiso H241 0.2210 0.2487 0.4978 0.0642 1.0000 Uiso 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 Nb1 0.02591(15) 0.03617(15) 0.03930(16) -0.00105(7) 0.0135(1) 0.00176(6) N2 0.0390(11) 0.041(1) 0.0448(11) -0.0030(9) 0.0186(9) -0.0019(9) C3 0.0663(18) 0.0570(17) 0.0536(15) -0.0121(12) 0.0370(14) -0.0153(14) C4 0.113(3) 0.113(3) 0.062(2) -0.036(2) 0.046(2) -0.048(3) C5 0.089(3) 0.179(6) 0.097(3) -0.043(4) 0.053(3) 0.029(3) C6 0.229(7) 0.086(3) 0.136(4) -0.005(3) 0.145(5) -0.035(4) O7 0.0329(9) 0.1004(16) 0.0531(11) -0.0228(11) 0.0129(8) -0.010(1) S8 0.0353(3) 0.0818(5) 0.0561(4) -0.0141(4) 0.0188(3) -0.0104(3) O9 0.115(3) 0.236(5) 0.081(2) 0.017(3) 0.033(2) -0.093(3) O10 0.083(2) 0.110(3) 0.184(4) -0.043(3) 0.023(2) 0.035(2) C11 0.056(2) 0.133(4) 0.080(3) -0.027(3) 0.0031(19) -0.024(2) F12 0.0701(16) 0.196(4) 0.111(2) -0.023(2) -0.0146(15) -0.058(2) F13 0.132(3) 0.319(7) 0.0550(15) -0.015(2) 0.0248(17) -0.072(4) F14 0.174(4) 0.171(4) 0.194(5) -0.128(4) 0.003(3) 0.008(3) C15 0.110(4) 0.058(2) 0.132(4) -0.002(2) 0.083(3) 0.018(2) C16 0.086(3) 0.0521(19) 0.105(3) -0.0125(19) 0.032(2) 0.0100(18) C17 0.093(3) 0.0487(17) 0.118(3) 0.019(2) 0.063(3) 0.0178(18) C18 0.127(4) 0.082(3) 0.076(2) 0.004(2) -0.001(3) 0.067(3) C19 0.0378(18) 0.051(2) 0.257(8) -0.000(3) 0.025(3) 0.0163(15) C20 0.0602(18) 0.0547(17) 0.077(2) 0.0214(15) 0.0291(16) 0.0094(14) C21 0.103(3) 0.075(2) 0.0583(19) 0.0128(16) 0.0368(19) -0.008(2) C22 0.122(4) 0.057(2) 0.159(4) 0.008(2) 0.118(4) 0.002(2) C23 0.0476(17) 0.0563(18) 0.109(3) 0.0121(19) 0.0188(18) -0.0115(14) C24 0.074(2) 0.0462(15) 0.074(2) -0.0004(14) 0.0361(17) -0.0134(15) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 . N2 . 1.758(2) yes Nb1 . O7 . 2.1423(19) yes Nb1 . C15 . 2.565(4) yes Nb1 . C16 . 2.516(4) yes Nb1 . C17 . 2.435(4) yes Nb1 . C18 . 2.402(4) yes Nb1 . C19 . 2.462(4) yes Nb1 . C20 . 2.462(3) yes Nb1 . C21 . 2.533(3) yes Nb1 . C22 . 2.564(3) yes Nb1 . C23 . 2.455(3) yes Nb1 . C24 . 2.472(3) yes N2 . C3 . 1.450(3) yes C3 . C4 . 1.521(5) yes C3 . C5 . 1.497(6) yes C3 . C6 . 1.504(6) yes C4 . H41 . 1.005(4) no C4 . H42 . 0.985(6) no C4 . H43 . 1.010(5) no C5 . H51 . 1.001(4) no C5 . H52 . 1.005(6) no C5 . H53 . 1.003(7) no C6 . H61 . 1.003(4) no C6 . H62 . 1.006(7) no C6 . H63 . 0.987(8) no O7 . S8 . 1.445(2) yes S8 . O9 . 1.376(3) yes S8 . O10 . 1.386(4) yes S8 . C11 . 1.806(5) yes C11 . F12 . 1.322(5) yes C11 . F13 . 1.276(7) yes C11 . F14 . 1.296(7) yes C15 . C16 . 1.307(7) yes C15 . C19 . 1.351(9) yes C15 . H151 . 1.002(5) no C16 . C17 . 1.361(7) yes C16 . H161 . 1.000(5) no C17 . C18 . 1.340(8) yes C17 . H171 . 0.996(4) no C18 . C19 . 1.464(9) yes C18 . H181 . 1.002(5) no C19 . H191 . 1.003(4) no C20 . C21 . 1.376(6) yes C20 . C24 . 1.369(5) yes C20 . H201 . 1.001(3) no C21 . C22 . 1.404(7) yes C21 . H211 . 1.000(4) no C22 . C23 . 1.432(7) yes C22 . H221 . 1.002(4) no C23 . C24 . 1.360(6) yes C23 . H231 . 1.000(4) no C24 . H241 . 0.998(4) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 . Nb1 . O7 . 97.95(9) yes N2 . Nb1 . C16 . 120.18(14) yes O7 . Nb1 . C16 . 74.84(13) yes N2 . Nb1 . C17 . 90.22(13) yes O7 . Nb1 . C17 . 88.43(15) yes C16 . Nb1 . C17 . 31.87(17) yes N2 . Nb1 . C18 . 87.24(16) yes O7 . Nb1 . C18 . 120.55(17) yes C16 . Nb1 . C18 . 52.93(16) yes C17 . Nb1 . C18 . 32.16(19) yes N2 . Nb1 . C19 . 118.5(2) yes O7 . Nb1 . C19 . 124.71(17) yes C16 . Nb1 . C19 . 51.58(16) yes C17 . Nb1 . C19 . 54.21(16) yes C18 . Nb1 . C19 . 35.0(2) yes N2 . Nb1 . C20 . 93.81(11) yes O7 . Nb1 . C20 . 82.60(12) yes C16 . Nb1 . C20 . 141.04(15) yes C17 . Nb1 . C20 . 170.59(16) yes C18 . Nb1 . C20 . 156.49(19) yes N2 . Nb1 . C21 . 125.43(13) yes O7 . Nb1 . C21 . 75.84(13) yes C16 . Nb1 . C21 . 110.38(15) yes C17 . Nb1 . C21 . 142.25(15) yes C18 . Nb1 . C21 . 143.0(2) yes N2 . Nb1 . C23 . 107.50(14) yes O7 . Nb1 . C23 . 129.68(12) yes C16 . Nb1 . C23 . 122.65(15) yes C17 . Nb1 . C23 . 132.77(14) yes C18 . Nb1 . C23 . 103.7(2) yes N2 . Nb1 . C24 . 84.17(11) yes O7 . Nb1 . C24 . 114.33(12) yes C16 . Nb1 . C24 . 153.59(15) yes C17 . Nb1 . C24 . 157.07(16) yes C18 . Nb1 . C24 . 125.10(18) yes C19 . Nb1 . C20 . 129.84(17) yes C19 . Nb1 . C21 . 108.0(2) yes C20 . Nb1 . C21 . 31.93(13) yes C19 . Nb1 . C23 . 79.25(15) yes C20 . Nb1 . C23 . 53.66(12) yes C21 . Nb1 . C23 . 53.97(14) yes C19 . Nb1 . C24 . 109.71(14) yes C20 . Nb1 . C24 . 32.21(12) yes C21 . Nb1 . C24 . 53.11(13) yes C23 . Nb1 . C24 . 32.04(13) yes Nb1 . N2 . C3 . 176.4(2) yes N2 . C3 . C4 . 108.5(2) yes N2 . C3 . C5 . 108.5(3) yes C4 . C3 . C5 . 108.8(4) yes N2 . C3 . C6 . 109.2(3) yes C4 . C3 . C6 . 110.7(4) yes C5 . C3 . C6 . 111.2(5) yes C3 . C4 . H41 . 109.0(4) no C3 . C4 . H42 . 110.5(4) no H41 . C4 . H42 . 110.2(4) no C3 . C4 . H43 . 108.9(4) no H41 . C4 . H43 . 108.3(5) no H42 . C4 . H43 . 109.9(4) no C3 . C5 . H51 . 109.9(5) no C3 . C5 . H52 . 109.7(5) no H51 . C5 . H52 . 109.0(5) no C3 . C5 . H53 . 110.0(4) no H51 . C5 . H53 . 109.2(5) no H52 . C5 . H53 . 108.9(5) no C3 . C6 . H61 . 109.0(5) no C3 . C6 . H62 . 108.8(6) no H61 . C6 . H62 . 108.7(6) no C3 . C6 . H63 . 110.1(5) no H61 . C6 . H63 . 110.2(7) no H62 . C6 . H63 . 110.0(5) no Nb1 . O7 . S8 . 137.46(14) yes O7 . S8 . O9 . 114.1(2) yes O7 . S8 . O10 . 113.3(2) yes O9 . S8 . O10 . 116.2(4) yes O7 . S8 . C11 . 99.98(18) yes O9 . S8 . C11 . 106.3(3) yes O10 . S8 . C11 . 104.7(3) yes S8 . C11 . F12 . 109.9(4) yes S8 . C11 . F13 . 112.4(4) yes F12 . C11 . F13 . 108.8(4) yes S8 . C11 . F14 . 109.9(4) yes F12 . C11 . F14 . 107.3(5) yes F13 . C11 . F14 . 108.4(6) yes C16 . C15 . C19 . 109.2(5) yes C16 . C15 . H151 . 125.2(6) no C19 . C15 . H151 . 125.6(6) no Nb1 . C16 . C15 . 77.2(2) yes Nb1 . C16 . C17 . 70.8(2) yes C15 . C16 . C17 . 110.6(5) yes Nb1 . C16 . H161 . 118.6(3) no C15 . C16 . H161 . 124.4(5) no C17 . C16 . H161 . 125.0(5) no Nb1 . C17 . C16 . 77.4(2) yes Nb1 . C17 . C18 . 72.6(2) yes C16 . C17 . C18 . 108.6(4) yes Nb1 . C17 . H171 . 116.8(3) no C16 . C17 . H171 . 126.0(5) no C18 . C17 . H171 . 125.3(6) no Nb1 . C18 . C17 . 75.3(2) yes Nb1 . C18 . C19 . 74.7(2) yes C17 . C18 . C19 . 105.4(4) yes Nb1 . C18 . H181 . 115.1(3) no C17 . C18 . H181 . 127.1(7) no C19 . C18 . H181 . 127.5(7) no Nb1 . C19 . C15 . 78.7(2) yes Nb1 . C19 . C18 . 70.3(2) yes C15 . C19 . C18 . 106.1(4) yes Nb1 . C19 . H191 . 116.6(3) no C15 . C19 . H191 . 126.6(9) no C18 . C19 . H191 . 127.3(9) no Nb1 . C20 . C21 . 76.9(2) yes Nb1 . C20 . C24 . 74.31(18) yes C21 . C20 . C24 . 109.3(3) yes Nb1 . C20 . H201 . 115.5(2) no C21 . C20 . H201 . 125.5(4) no C24 . C20 . H201 . 125.2(4) no Nb1 . C21 . C20 . 71.17(19) yes Nb1 . C21 . C22 . 75.2(2) yes C20 . C21 . C22 . 107.8(4) yes Nb1 . C21 . H211 . 119.6(3) no C20 . C21 . H211 . 126.1(5) no C22 . C21 . H211 . 126.2(5) no C21 . C22 . C23 . 106.0(3) yes C21 . C22 . H221 . 126.2(6) no C23 . C22 . H221 . 127.8(6) no Nb1 . C23 . C22 . 77.6(2) yes Nb1 . C23 . C24 . 74.67(19) yes C22 . C23 . C24 . 107.8(4) yes Nb1 . C23 . H231 . 113.8(3) no C22 . C23 . H231 . 126.0(4) no C24 . C23 . H231 . 126.2(5) no Nb1 . C24 . C20 . 73.48(19) yes Nb1 . C24 . C23 . 73.3(2) yes C20 . C24 . C23 . 108.9(3) yes Nb1 . C24 . H241 . 119.6(2) no C20 . C24 . H241 . 125.6(4) no C23 . C24 . H241 . 125.5(4) no #===end data_compound2 #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic ; [Nb(eta-C5H5)2(NtBu)(PMe3)][CF3SO3] ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 8.868(1) _cell_angle_alpha 90. _cell_length_b 18.934(2) _cell_angle_beta 92.12(2) _cell_length_c 13.641(2) _cell_angle_gamma 90. _cell_volume 2288.9(4) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Nb ' -2.1970 0.6210 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International_Tables_Vol_IV_Table_2.2B' 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C18 H28 F3 N Nb O3 P S' _chemical_formula_moiety 'C18 H28 F3 N Nb O3 P S' _chemical_compound_source ; ? ; _chemical_formula_weight 519.36 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 0 _cell_formula_units_Z 4 _exptl_crystal_description ' box ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.02 _exptl_crystal_density_diffrn 1.51 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1056.18 _exptl_absorpt_coefficient_mu 0.70 _exptl_absorpt_correction_type none _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 11019 _reflns_number_total 4777 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections with Friedels Law is 0 # Number of reflections without Friedels Law is 0 _reflns_number_observed 3510 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.34 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.92 _refine_diff_density_max 0.83 _refine_ls_number_reflns 3510 _refine_ls_number_parameters 254 _refine_ls_R_factor_obs 0.0327 _refine_ls_wR_factor_obs 0.0396 _refine_ls_goodness_of_fit_obs 0.9767 _refine_ls_shift/su_max 0.000859 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 2.54 0.640 2.06 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_thermal_displace_type Nb1 0.55906(2) 0.25231(1) 0.371684(14) 0.0179 1.0000 Uani S7 0.18911(8) 0.50597(3) 0.31606(5) 0.0313 1.0000 Uani P15 0.73988(8) 0.36020(4) 0.37029(5) 0.0288 1.0000 Uani F12 0.3564(3) 0.48514(12) 0.16171(17) 0.0625 1.0000 Uani F13 0.1323(3) 0.44429(12) 0.14433(16) 0.0669 1.0000 Uani F14 0.1722(3) 0.55582(11) 0.13365(16) 0.0645 1.0000 Uani O8 0.0323(2) 0.52125(12) 0.32257(17) 0.0449 1.0000 Uani O9 0.2355(3) 0.43859(12) 0.35326(19) 0.0558 1.0000 Uani O10 0.2888(3) 0.56386(12) 0.34209(18) 0.0476 1.0000 Uani N2 0.7151(2) 0.19337(12) 0.37032(15) 0.0256 1.0000 Uani C3 0.8270(3) 0.13909(15) 0.3618(2) 0.0337 1.0000 Uani C4 0.7521(5) 0.0676(2) 0.3719(4) 0.0736 1.0000 Uani C5 0.8969(7) 0.1443(4) 0.2625(4) 0.1290 1.0000 Uani C6 0.9420(5) 0.1457(3) 0.4488(4) 0.0895 1.0000 Uani C11 0.2140(4) 0.49777(15) 0.1824(2) 0.0387 1.0000 Uani C16 0.8955(3) 0.35475(17) 0.4610(2) 0.0422 1.0000 Uani C17 0.6610(4) 0.44701(16) 0.3912(3) 0.0463 1.0000 Uani C18 0.8360(5) 0.3702(2) 0.2538(3) 0.0582 1.0000 Uani C19 0.4784(3) 0.19838(14) 0.21270(19) 0.0342 1.0000 Uani C20 0.3445(3) 0.21864(16) 0.2589(2) 0.0372 1.0000 Uani C21 0.3369(4) 0.29299(16) 0.2603(2) 0.0398 1.0000 Uani C22 0.4688(4) 0.31838(15) 0.2205(2) 0.0401 1.0000 Uani C23 0.5564(4) 0.26003(16) 0.1898(2) 0.0374 1.0000 Uani C24 0.5413(4) 0.30475(18) 0.5404(2) 0.0421 1.0000 Uani C25 0.3948(4) 0.3132(2) 0.4980(2) 0.0530 1.0000 Uani C26 0.3368(4) 0.2461(3) 0.4824(3) 0.0604 1.0000 Uani C27 0.4479(5) 0.19689(18) 0.5126(2) 0.0525 1.0000 Uani C28 0.5684(4) 0.2332(2) 0.5523(2) 0.0425 1.0000 Uani H41 0.8280 0.0292 0.3661 0.0759 1.0000 Uiso H42 0.7046 0.0644 0.4374 0.0759 1.0000 Uiso H43 0.6711 0.0618 0.3189 0.0759 1.0000 Uiso H51 0.9761 0.1070 0.2582 0.1627 1.0000 Uiso H52 0.9464 0.1922 0.2579 0.1627 1.0000 Uiso H53 0.8187 0.1388 0.2105 0.1627 1.0000 Uiso H61 1.0222 0.1086 0.4430 0.0976 1.0000 Uiso H62 0.9920 0.1936 0.4463 0.0976 1.0000 Uiso H63 0.8911 0.1403 0.5115 0.0976 1.0000 Uiso H191 0.5115 0.1489 0.1986 0.0372 1.0000 Uiso H201 0.2682 0.1856 0.2858 0.0452 1.0000 Uiso H211 0.2521 0.3223 0.2853 0.0419 1.0000 Uiso H221 0.4972 0.3692 0.2148 0.0408 1.0000 Uiso H231 0.6557 0.2629 0.1576 0.0362 1.0000 Uiso H241 0.6141 0.3431 0.5589 0.0451 1.0000 Uiso H251 0.3436 0.3593 0.4836 0.0575 1.0000 Uiso H261 0.2342 0.2352 0.4537 0.0578 1.0000 Uiso H271 0.4402 0.1440 0.5073 0.0535 1.0000 Uiso H281 0.6612 0.2115 0.5839 0.0413 1.0000 Uiso H161 0.9616 0.3972 0.4576 0.0411 1.0000 Uiso H162 0.8552 0.3512 0.5291 0.0411 1.0000 Uiso H163 0.9580 0.3112 0.4491 0.0411 1.0000 Uiso H171 0.7417 0.4841 0.3892 0.0421 1.0000 Uiso H172 0.6146 0.4488 0.4577 0.0421 1.0000 Uiso H173 0.5803 0.4582 0.3400 0.0421 1.0000 Uiso H181 0.9054 0.4124 0.2566 0.0555 1.0000 Uiso H182 0.8992 0.3270 0.2406 0.0555 1.0000 Uiso H183 0.7612 0.3765 0.1977 0.0555 1.0000 Uiso 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 Nb1 0.02019(13) 0.01864(12) 0.01464(13) -0.00056(7) -0.00049(8) -0.00184(8) S7 0.0353(4) 0.0234(3) 0.0352(3) -0.0043(3) 0.0001(3) -0.0020(3) P15 0.0349(4) 0.0279(3) 0.0236(3) -0.0019(3) 0.0015(3) -0.0103(3) F12 0.0595(13) 0.0639(14) 0.0662(14) -0.0082(11) 0.0296(11) -0.0027(11) F13 0.0869(16) 0.0662(14) 0.0480(12) -0.026(1) 0.0084(11) -0.0366(12) F14 0.0895(17) 0.0561(13) 0.0478(12) 0.016(1) 0.0012(11) 0.0121(12) O8 0.0368(11) 0.0444(12) 0.0536(14) -0.003(1) 0.005(1) 0.000(1) O9 0.0772(18) 0.0383(12) 0.0517(15) 0.005(1) -0.0006(13) 0.0165(12) O10 0.0481(13) 0.0448(12) 0.0497(13) -0.018(1) -0.002(1) -0.015(1) N2 0.024(1) 0.0307(11) 0.0226(11) 0.0006(8) 0.0009(8) -0.0035(9) C3 0.0347(15) 0.0355(14) 0.0311(14) -0.0030(11) 0.0038(11) 0.0069(12) C4 0.061(2) 0.040(2) 0.119(4) -0.012(2) -0.005(2) 0.0160(18) C5 0.148(5) 0.142(5) 0.104(4) 0.062(4) 0.092(4) 0.109(5) C6 0.062(3) 0.077(3) 0.125(4) -0.039(3) -0.052(3) 0.035(2) C11 0.0467(17) 0.0305(14) 0.0389(15) -0.0050(12) 0.0001(13) 0.0006(13) C16 0.0340(15) 0.0439(16) 0.0483(18) -0.0066(14) -0.0063(13) -0.0063(13) C17 0.059(2) 0.0269(14) 0.0524(19) -0.0016(13) -0.0069(15) -0.0089(14) C18 0.074(3) 0.061(2) 0.0402(18) -0.0055(16) 0.0200(17) -0.036(2) C19 0.0491(17) 0.0282(13) 0.0242(13) -0.009(1) -0.0125(12) 0.0030(12) C20 0.0371(15) 0.0368(15) 0.0363(15) -0.0030(12) -0.0170(12) -0.0042(13) C21 0.0433(16) 0.0365(15) 0.0381(16) -0.0057(12) -0.0184(13) 0.0083(13) C22 0.069(2) 0.0271(13) 0.0221(13) 0.003(1) -0.0193(13) -0.0031(14) C23 0.0556(19) 0.0403(16) 0.0156(12) -0.000(1) -0.0070(12) -0.0042(13) C24 0.0552(19) 0.0495(17) 0.0230(13) -0.0148(12) 0.0183(13) -0.0208(15) C25 0.065(2) 0.065(2) 0.0306(16) 0.0068(15) 0.0234(15) 0.0337(19) C26 0.0300(16) 0.120(4) 0.0321(17) -0.0042(19) 0.0085(13) -0.023(2) C27 0.085(3) 0.0447(17) 0.0299(16) -0.0008(13) 0.0261(16) -0.0228(18) C28 0.0483(18) 0.063(2) 0.0161(13) 0.0042(13) 0.0062(12) 0.0168(15) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 . P15 . 2.5974(7) yes Nb1 . N2 . 1.779(2) yes Nb1 . C19 . 2.479(2) yes Nb1 . C20 . 2.486(3) yes Nb1 . C21 . 2.562(3) yes Nb1 . C22 . 2.517(3) yes Nb1 . C23 . 2.485(3) yes Nb1 . C24 . 2.517(3) yes Nb1 . C25 . 2.570(3) yes Nb1 . C26 . 2.530(3) yes Nb1 . C27 . 2.431(3) yes Nb1 . C28 . 2.488(3) yes S7 . O8 . 1.426(2) yes S7 . O9 . 1.428(2) yes S7 . O10 . 1.444(2) yes S7 . C11 . 1.851(3) yes P15 . C16 . 1.822(3) yes P15 . C17 . 1.813(3) yes P15 . C18 . 1.840(3) yes F12 . C11 . 1.326(4) yes F13 . C11 . 1.339(4) yes F14 . C11 . 1.330(4) yes N2 . C3 . 1.436(3) yes C3 . C4 . 1.516(5) yes C3 . C5 . 1.513(5) yes C3 . C6 . 1.541(5) yes C4 . H41 . 0.996(4) no C4 . H42 . 1.004(6) no C4 . H43 . 1.006(5) no C5 . H51 . 0.998(4) no C5 . H52 . 1.010(8) no C5 . H53 . 0.979(8) no C6 . H61 . 1.006(4) no C6 . H62 . 1.010(6) no C6 . H63 . 0.986(7) no C16 . H161 . 0.997(3) no C16 . H162 . 1.010(3) no C16 . H163 . 1.010(3) no C17 . H171 . 1.003(3) no C17 . H172 . 1.010(4) no C17 . H173 . 1.004(4) no C18 . H181 . 1.008(3) no C18 . H182 . 1.012(4) no C18 . H183 . 1.002(4) no C19 . C20 . 1.417(4) yes C19 . C23 . 1.398(4) yes C19 . H191 . 1.002(3) no C20 . C21 . 1.410(4) yes C20 . H201 . 1.002(3) no C21 . C22 . 1.393(5) yes C21 . H211 . 1.004(3) no C22 . C23 . 1.422(4) yes C22 . H221 . 0.998(3) no C23 . H231 . 1.000(3) no C24 . C25 . 1.412(5) yes C24 . C28 . 1.385(5) yes C24 . H241 . 0.998(3) no C25 . C26 . 1.383(6) yes C25 . H251 . 1.001(3) no C26 . C27 . 1.407(6) yes C26 . H261 . 0.999(3) no C27 . C28 . 1.365(5) yes C27 . H271 . 1.006(3) no C28 . H281 . 1.002(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P15 . Nb1 . N2 . 90.71(7) yes P15 . Nb1 . C19 . 118.42(7) yes N2 . Nb1 . C19 . 86.10(9) yes P15 . Nb1 . C20 . 130.98(7) yes N2 . Nb1 . C20 . 114.3(1) yes C19 . Nb1 . C20 . 33.2(1) yes P15 . Nb1 . C21 . 102.74(7) yes N2 . Nb1 . C21 . 139.83(9) yes C19 . Nb1 . C21 . 54.13(9) yes C20 . Nb1 . C21 . 32.4(1) yes P15 . Nb1 . C22 . 77.34(7) yes N2 . Nb1 . C22 . 121.8(1) yes C19 . Nb1 . C22 . 54.20(9) yes C20 . Nb1 . C22 . 53.7(1) yes C21 . Nb1 . C22 . 31.83(11) yes P15 . Nb1 . C23 . 85.96(7) yes N2 . Nb1 . C23 . 90.3(1) yes C19 . Nb1 . C23 . 32.7(1) yes C20 . Nb1 . C23 . 54.41(11) yes C21 . Nb1 . C23 . 53.93(11) yes P15 . Nb1 . C24 . 75.87(7) yes N2 . Nb1 . C24 . 109.39(11) yes C19 . Nb1 . C24 . 159.53(11) yes C20 . Nb1 . C24 . 126.52(11) yes C21 . Nb1 . C24 . 110.56(11) yes P15 . Nb1 . C26 . 122.4(1) yes N2 . Nb1 . C26 . 126.94(13) yes C19 . Nb1 . C26 . 107.30(11) yes C20 . Nb1 . C26 . 76.26(11) yes C21 . Nb1 . C26 . 76.65(12) yes P15 . Nb1 . C27 . 127.86(8) yes N2 . Nb1 . C27 . 94.35(12) yes C19 . Nb1 . C27 . 113.69(11) yes C20 . Nb1 . C27 . 93.18(12) yes C21 . Nb1 . C27 . 105.88(13) yes P15 . Nb1 . C28 . 97.11(9) yes N2 . Nb1 . C28 . 85.5(1) yes C19 . Nb1 . C28 . 143.54(11) yes C20 . Nb1 . C28 . 124.91(11) yes C21 . Nb1 . C28 . 128.89(11) yes C22 . Nb1 . C23 . 33.0(1) yes C22 . Nb1 . C24 . 121.63(11) yes C23 . Nb1 . C24 . 153.04(11) yes C22 . Nb1 . C26 . 106.33(13) yes C23 . Nb1 . C26 . 128.33(12) yes C24 . Nb1 . C26 . 52.83(11) yes C22 . Nb1 . C27 . 137.44(14) yes C23 . Nb1 . C27 . 145.69(12) yes C24 . Nb1 . C27 . 53.6(1) yes C26 . Nb1 . C27 . 32.88(14) yes C22 . Nb1 . C28 . 151.81(11) yes C23 . Nb1 . C28 . 174.8(1) yes C24 . Nb1 . C28 . 32.11(11) yes C26 . Nb1 . C28 . 53.15(12) yes C27 . Nb1 . C28 . 32.20(12) yes O8 . S7 . O9 . 115.34(16) yes O8 . S7 . O10 . 114.85(14) yes O9 . S7 . O10 . 115.14(16) yes O8 . S7 . C11 . 103.31(14) yes O9 . S7 . C11 . 103.41(14) yes O10 . S7 . C11 . 102.21(14) yes Nb1 . P15 . C16 . 113.75(11) yes Nb1 . P15 . C17 . 118.03(12) yes C16 . P15 . C17 . 103.38(15) yes Nb1 . P15 . C18 . 113.15(11) yes C16 . P15 . C18 . 103.22(18) yes C17 . P15 . C18 . 103.66(18) yes Nb1 . N2 . C3 . 171.90(19) yes N2 . C3 . C4 . 109.0(3) yes N2 . C3 . C5 . 109.5(3) yes C4 . C3 . C5 . 109.5(4) yes N2 . C3 . C6 . 108.6(2) yes C4 . C3 . C6 . 106.4(3) yes C5 . C3 . C6 . 113.8(4) yes C3 . C4 . H41 . 110.1(4) no C3 . C4 . H42 . 109.5(4) no H41 . C4 . H42 . 109.5(5) no C3 . C4 . H43 . 109.6(4) no H41 . C4 . H43 . 109.3(4) no H42 . C4 . H43 . 108.7(5) no C3 . C5 . H51 . 108.6(4) no C3 . C5 . H52 . 107.9(5) no H51 . C5 . H52 . 108.8(6) no C3 . C5 . H53 . 109.8(5) no H51 . C5 . H53 . 111.3(7) no H52 . C5 . H53 . 110.3(5) no C3 . C6 . H61 . 109.3(4) no C3 . C6 . H62 . 109.0(4) no H61 . C6 . H62 . 108.2(5) no C3 . C6 . H63 . 110.3(4) no H61 . C6 . H63 . 110.1(5) no H62 . C6 . H63 . 109.8(4) no S7 . C11 . F12 . 111.9(2) yes S7 . C11 . F13 . 111.3(2) yes F12 . C11 . F13 . 106.7(3) yes S7 . C11 . F14 . 112.5(2) yes F12 . C11 . F14 . 107.0(3) yes F13 . C11 . F14 . 107.1(3) yes P15 . C16 . H161 . 110.8(3) no P15 . C16 . H162 . 110.1(2) no H161 . C16 . H162 . 108.9(3) no P15 . C16 . H163 . 110.1(2) no H161 . C16 . H163 . 108.9(3) no H162 . C16 . H163 . 107.9(3) no P15 . C17 . H171 . 110.5(3) no P15 . C17 . H172 . 110.1(2) no H171 . C17 . H172 . 108.4(3) no P15 . C17 . H173 . 110.5(2) no H171 . C17 . H173 . 108.9(3) no H172 . C17 . H173 . 108.4(4) no P15 . C18 . H181 . 110.6(3) no P15 . C18 . H182 . 110.4(3) no H181 . C18 . H182 . 107.8(4) no P15 . C18 . H183 . 111.0(3) no H181 . C18 . H183 . 108.6(4) no H182 . C18 . H183 . 108.3(3) no Nb1 . C19 . C20 . 73.68(15) yes Nb1 . C19 . C23 . 73.89(15) yes C20 . C19 . C23 . 107.6(3) yes Nb1 . C19 . H191 . 118.39(19) no C20 . C19 . H191 . 126.5(3) no C23 . C19 . H191 . 125.9(3) no Nb1 . C20 . C19 . 73.14(15) yes Nb1 . C20 . C21 . 76.78(15) yes C19 . C20 . C21 . 108.5(3) yes Nb1 . C20 . H201 . 116.4(2) no C19 . C20 . H201 . 125.6(3) no C21 . C20 . H201 . 125.9(3) no Nb1 . C21 . C20 . 70.83(15) yes Nb1 . C21 . C22 . 72.33(16) yes C20 . C21 . C22 . 107.3(3) yes Nb1 . C21 . H211 . 122.3(2) no C20 . C21 . H211 . 126.4(3) no C22 . C21 . H211 . 126.3(3) no Nb1 . C22 . C21 . 75.84(16) yes Nb1 . C22 . C23 . 72.24(15) yes C21 . C22 . C23 . 108.8(3) yes Nb1 . C22 . H221 . 117.97(19) no C21 . C22 . H221 . 125.5(3) no C23 . C22 . H221 . 125.7(3) no Nb1 . C23 . C19 . 73.38(15) yes Nb1 . C23 . C22 . 74.73(15) yes C19 . C23 . C22 . 107.6(3) yes Nb1 . C23 . H231 . 117.7(2) no C19 . C23 . H231 . 126.5(3) no C22 . C23 . H231 . 125.9(3) no Nb1 . C24 . C25 . 75.97(17) yes Nb1 . C24 . C28 . 72.81(16) yes C25 . C24 . C28 . 108.1(3) yes Nb1 . C24 . H241 . 117.16(19) no C25 . C24 . H241 . 126.7(4) no C28 . C24 . H241 . 125.1(4) no C24 . C25 . C26 . 106.9(3) yes C24 . C25 . H251 . 125.6(4) no C26 . C25 . H251 . 127.5(4) no Nb1 . C26 . C25 . 75.86(18) yes Nb1 . C26 . C27 . 69.66(18) yes C25 . C26 . C27 . 108.1(3) yes Nb1 . C26 . H261 . 119.5(2) no C25 . C26 . H261 . 125.3(5) no C27 . C26 . H261 . 126.6(4) no Nb1 . C27 . C26 . 77.46(19) yes Nb1 . C27 . C28 . 76.24(17) yes C26 . C27 . C28 . 108.2(3) yes Nb1 . C27 . H271 . 113.7(2) no C26 . C27 . H271 . 126.4(4) no C28 . C27 . H271 . 125.4(4) no Nb1 . C28 . C24 . 75.07(16) yes Nb1 . C28 . C27 . 71.56(17) yes C24 . C28 . C27 . 108.4(3) yes Nb1 . C28 . H281 . 118.8(2) no C24 . C28 . H281 . 126.0(4) no C27 . C28 . H281 . 125.6(4) no #===end