# Copyright The Royal Society of Chemistry, 1998 data_CRYSTALS_cif # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' linda.doerrer@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? #choose from: FI FM FO CI CM CO AD# _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 ; 'Studies of Ansa-bis(cyclopentadienyl)tungsten Derivatives' # Title of paper ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Conway, Stephen L. J.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR # Address for author 1 ; ; ? #footnote for author 1 ; 'Doerrer, Linda H.' # Author 2 ; South Parks Road Inorganic Chemistry Laboratory Oxford OX1 3QR # Address 2 ; ; ? # footnote 2 ; 'Green, Malcolm L.H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ; ? ; 'Stephens, Adam H. H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ; ? ; #============================================================================== # 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_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _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 # Add your own references - in alphabetic order ; 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite # choose from: _diffrn_measurement_device-type ' Enraf-nonius DIP2000 ' _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) ; # end_choice #========================================================================== # 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) ; # choose one of the following two lines _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _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 noref #**************************************************************************** _cell_length_a 8.064(6) _cell_angle_alpha 90. _cell_length_b 14.807(7) _cell_angle_beta 98.853(4) _cell_length_c 11.212(7) _cell_angle_gamma 90. _cell_volume 1322.8 _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 'W ' -1.4210 6.8720 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 'International_Tables_Vol_IV_Table_2.2B' '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' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 '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' _chemical_formula_sum ' C14 H20 W1 SI1 ' _chemical_formula_moiety ' C14 H20 W1 SI1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 400.25 _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 ' rhombus ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 2.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 762.98 _exptl_absorpt_coefficient_mu 8.98 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature '100 K' _diffrn_reflns_number 2715 _reflns_number_total 2715 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 2715 # Number of reflections without Friedels Law is 0 _reflns_number_observed 2318 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -10 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -1.57 _refine_diff_density_max 1.54 _refine_ls_number_reflns 2318 _refine_ls_number_parameters 145 _refine_ls_R_factor_obs 0.0335 _refine_ls_wR_factor_obs 0.0407 _refine_ls_goodness_of_fit_obs 0.8863 _refine_ls_shift/su_max 0.021644 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 4.80 0.569 3.64 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _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 W1 0.52564(2) 0.237729(15) 0.053411(16) 0.0179 1.0000 Uani Si1 0.36753(19) 0.4005(1) 0.17308(13) 0.0224 1.0000 Uani C1 0.3667(7) 0.2755(4) 0.1941(5) 0.0229 1.0000 Uani C2 0.2691(6) 0.2144(4) 0.1089(5) 0.0254 1.0000 Uani C3 0.3489(8) 0.1291(4) 0.1235(5) 0.0298 1.0000 Uani C4 0.4933(8) 0.1342(4) 0.2093(5) 0.0302 1.0000 Uani C5 0.5111(7) 0.2239(4) 0.2535(5) 0.0253 1.0000 Uani C6 0.5030(7) 0.3894(4) 0.0534(4) 0.0234 1.0000 Uani C7 0.4393(7) 0.3581(4) -0.0677(5) 0.0275 1.0000 Uani C8 0.5810(8) 0.3230(4) -0.1156(5) 0.0310 1.0000 Uani C9 0.7240(7) 0.3276(4) -0.0274(5) 0.0285 1.0000 Uani C10 0.6813(7) 0.3670(4) 0.0795(5) 0.0250 1.0000 Uani C21 0.1573(7) 0.4448(4) 0.1114(6) 0.0333 1.0000 Uani C22 0.4722(8) 0.4603(4) 0.3085(5) 0.0319 1.0000 Uani C31 0.4702(9) 0.1408(4) -0.1020(6) 0.0348 1.0000 Uani C32 0.7565(8) 0.1522(5) 0.0726(6) 0.0357 1.0000 Uani H21 0.1667 0.2290 0.0500 0.0600 1.0000 Uiso H31 0.3035 0.0734 0.0756 0.0600 1.0000 Uiso H41 0.6018 0.1169 0.2668 0.0600 1.0000 Uiso H51 0.4981 0.1763 0.3151 0.0600 1.0000 Uiso H71 0.3178 0.3601 -0.1086 0.0600 1.0000 Uiso H81 0.5792 0.3001 -0.1995 0.0600 1.0000 Uiso H91 0.8418 0.3052 -0.0354 0.0600 1.0000 Uiso H101 0.7587 0.3783 0.1583 0.0600 1.0000 Uiso H211 0.1636 0.5122 0.1007 0.0600 1.0000 Uiso H212 0.0758 0.4304 0.1664 0.0600 1.0000 Uiso H213 0.1185 0.4169 0.0297 0.0600 1.0000 Uiso H221 0.4733 0.5271 0.2951 0.0600 1.0000 Uiso H222 0.5947 0.4395 0.3286 0.0600 1.0000 Uiso H223 0.4167 0.4469 0.3804 0.0600 1.0000 Uiso H311 0.4895 0.1651 -0.1807 0.0600 1.0000 Uiso H312 0.5624 0.1045 -0.0644 0.0600 1.0000 Uiso H313 0.3642 0.1023 -0.1171 0.0600 1.0000 Uiso H321 0.8001 0.1487 -0.0059 0.0600 1.0000 Uiso H322 0.8472 0.1804 0.1332 0.0600 1.0000 Uiso H323 0.7339 0.0912 0.1000 0.0600 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 W1 0.02073(15) 0.02118(16) 0.01278(15) 0.00096(6) 0.00602(9) -0.00032(7 Si1 0.0253(7) 0.0232(7) 0.0203(7) 0.0010(5) 0.0089(6) 0.0006(5) C1 0.026(3) 0.028(3) 0.017(2) 0.004(2) 0.011(2) -0.002(2) C2 0.021(2) 0.031(3) 0.027(3) 0.002(2) 0.014(2) -0.007(2) C3 0.043(3) 0.021(3) 0.028(3) -0.003(2) 0.014(2) -0.013(2) C4 0.039(3) 0.028(3) 0.027(3) 0.010(2) 0.016(2) -0.002(2) C5 0.034(3) 0.026(3) 0.018(2) 0.007(2) 0.011(2) -0.003(2) C6 0.026(3) 0.025(3) 0.021(3) 0.0061(18) 0.008(2) -0.006(2) C7 0.029(3) 0.033(3) 0.021(3) 0.007(2) 0.004(2) -0.003(2) C8 0.042(3) 0.035(3) 0.019(3) 0.004(2) 0.017(2) -0.003(3) C9 0.026(3) 0.036(3) 0.026(3) 0.000(2) 0.012(2) -0.008(2) C10 0.022(3) 0.030(3) 0.024(3) 0.005(2) 0.008(2) -0.004(2) C21 0.027(3) 0.035(3) 0.039(3) 0.006(2) 0.009(2) 0.002(2) C22 0.040(3) 0.030(3) 0.027(3) -0.006(2) 0.011(2) -0.002(2) C31 0.045(4) 0.035(3) 0.026(3) -0.010(2) 0.011(3) -0.008(3) C32 0.032(3) 0.040(3) 0.037(3) -0.001(3) 0.010(3) 0.011(3) _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 W1 . C1 . 2.250(5) yes W1 . C2 . 2.276(5) yes W1 . C3 . 2.362(5) yes W1 . C4 . 2.370(5) yes W1 . C5 . 2.274(5) yes W1 . C6 . 2.254(6) yes W1 . C7 . 2.284(6) yes W1 . C8 . 2.375(5) yes W1 . C9 . 2.366(5) yes W1 . C10 . 2.282(5) yes W1 . C31 . 2.249(6) yes W1 . C32 . 2.235(6) yes Si1 . C1 . 1.867(6) yes Si1 . C6 . 1.863(5) yes Si1 . C21 . 1.850(6) yes Si1 . C22 . 1.845(6) yes C1 . C2 . 1.455(8) yes C1 . C5 . 1.465(8) yes C2 . C3 . 1.415(9) yes C2 . H21 . 0.999(6) no C3 . C4 . 1.394(9) yes C3 . H31 . 1.021(5) no C4 . C5 . 1.417(8) yes C4 . H41 . 1.036(6) no C5 . H51 . 1.004(5) no C6 . C7 . 1.452(8) yes C6 . C10 . 1.461(7) yes C7 . C8 . 1.433(8) yes C7 . H71 . 1.016(6) no C8 . C9 . 1.401(8) yes C8 . H81 . 0.998(5) no C9 . C10 . 1.421(8) yes C9 . H91 . 1.023(6) no C10 . H101 . 1.015(6) no C21 . H211 . 1.006(6) no C21 . H212 . 0.991(6) no C21 . H213 . 1.009(7) no C22 . H221 . 1.001(6) no C22 . H222 . 1.026(6) no C22 . H223 . 1.000(6) no C31 . H311 . 0.988(6) no C31 . H312 . 0.960(7) no C31 . H313 . 1.019(6) no C32 . H321 . 0.997(6) no C32 . H322 . 1.009(7) no C32 . H323 . 0.980(7) 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 C1 . W1 . C2 . 37.5(2) yes C1 . W1 . C3 . 59.86(19) yes C2 . W1 . C3 . 35.5(2) yes C1 . W1 . C4 . 60.3(2) yes C2 . W1 . C4 . 59.5(2) yes C3 . W1 . C4 . 34.3(2) yes C1 . W1 . C5 . 37.8(2) yes C2 . W1 . C5 . 61.9(2) yes C3 . W1 . C5 . 59.0(2) yes C4 . W1 . C5 . 35.5(2) yes C1 . W1 . C6 . 72.39(19) yes C2 . W1 . C6 . 94.3(2) yes C3 . W1 . C6 . 128.7(2) yes C4 . W1 . C6 . 128.80(18) yes C5 . W1 . C6 . 94.21(19) yes C1 . W1 . C7 . 93.9(2) yes C2 . W1 . C7 . 94.3(2) yes C3 . W1 . C7 . 125.8(2) yes C4 . W1 . C7 . 152.3(2) yes C5 . W1 . C7 . 126.9(2) yes C1 . W1 . C8 . 128.6(2) yes C2 . W1 . C8 . 126.1(2) yes C3 . W1 . C8 . 145.5(2) yes C4 . W1 . C8 . 171.0(2) yes C5 . W1 . C8 . 151.6(2) yes C1 . W1 . C9 . 128.3(2) yes C2 . W1 . C9 . 152.4(2) yes C3 . W1 . C9 . 171.3(2) yes C4 . W1 . C9 . 143.5(2) yes C5 . W1 . C9 . 124.7(2) yes C1 . W1 . C10 . 93.62(19) yes C2 . W1 . C10 . 126.7(2) yes C3 . W1 . C10 . 151.17(19) yes C4 . W1 . C10 . 124.7(2) yes C5 . W1 . C10 . 93.44(19) yes C1 . W1 . C31 . 129.4(2) yes C2 . W1 . C31 . 92.0(2) yes C3 . W1 . C31 . 76.4(2) yes C4 . W1 . C31 . 97.3(2) yes C5 . W1 . C31 . 132.3(2) yes C1 . W1 . C32 . 129.0(2) yes C2 . W1 . C32 . 131.8(2) yes C3 . W1 . C32 . 96.8(2) yes C4 . W1 . C32 . 75.3(2) yes C5 . W1 . C32 . 91.3(2) yes C6 . W1 . C7 . 37.3(2) yes C6 . W1 . C8 . 59.71(19) yes C7 . W1 . C8 . 35.7(2) yes C6 . W1 . C9 . 59.9(2) yes C7 . W1 . C9 . 59.7(2) yes C8 . W1 . C9 . 34.4(2) yes C6 . W1 . C10 . 37.57(19) yes C7 . W1 . C10 . 62.2(2) yes C8 . W1 . C10 . 59.3(2) yes C9 . W1 . C10 . 35.55(19) yes C6 . W1 . C31 . 129.1(2) yes C7 . W1 . C31 . 91.8(2) yes C8 . W1 . C31 . 76.2(2) yes C9 . W1 . C31 . 97.4(2) yes C10 . W1 . C31 . 132.4(2) yes C6 . W1 . C32 . 129.2(2) yes C7 . W1 . C32 . 132.3(2) yes C8 . W1 . C32 . 97.0(2) yes C9 . W1 . C32 . 75.7(2) yes C10 . W1 . C32 . 91.7(2) yes C31 . W1 . C32 . 77.0(2) yes C1 . Si1 . C6 . 91.0(2) yes C1 . Si1 . C21 . 112.2(3) yes C6 . Si1 . C21 . 111.5(3) yes C1 . Si1 . C22 . 112.4(3) yes C6 . Si1 . C22 . 113.0(3) yes C21 . Si1 . C22 . 114.5(3) yes W1 . C1 . Si1 . 98.3(2) yes W1 . C1 . C2 . 72.2(3) yes Si1 . C1 . C2 . 123.1(4) yes W1 . C1 . C5 . 72.0(3) yes Si1 . C1 . C5 . 123.8(4) yes C2 . C1 . C5 . 106.6(5) yes W1 . C2 . C1 . 70.3(3) yes W1 . C2 . C3 . 75.6(3) yes C1 . C2 . C3 . 106.7(5) yes W1 . C2 . H21 . 118.7(4) no C1 . C2 . H21 . 127.4(6) no C3 . C2 . H21 . 125.8(6) no W1 . C3 . C2 . 69.0(3) yes W1 . C3 . C4 . 73.2(3) yes C2 . C3 . C4 . 110.4(5) yes W1 . C3 . H31 . 124.1(4) no C2 . C3 . H31 . 122.7(6) no C4 . C3 . H31 . 126.9(6) no W1 . C4 . C3 . 72.6(3) yes W1 . C4 . C5 . 68.6(3) yes C3 . C4 . C5 . 108.7(5) yes W1 . C4 . H41 . 116.2(4) no C3 . C4 . H41 . 162.2(6) no C5 . C4 . H41 . 89.1(5) no W1 . C5 . C1 . 70.3(3) yes W1 . C5 . C4 . 76.0(3) yes C1 . C5 . C4 . 107.4(5) yes W1 . C5 . H51 . 140.3(5) no C1 . C5 . H51 . 121.3(5) no C4 . C5 . H51 . 64.3(4) no W1 . C6 . Si1 . 98.3(2) yes W1 . C6 . C7 . 72.5(3) yes Si1 . C6 . C7 . 122.7(4) yes W1 . C6 . C10 . 72.3(3) yes Si1 . C6 . C10 . 123.0(4) yes C7 . C6 . C10 . 108.0(5) yes W1 . C7 . C6 . 70.2(3) yes W1 . C7 . C8 . 75.6(3) yes C6 . C7 . C8 . 106.2(5) yes W1 . C7 . H71 . 118.4(4) no C6 . C7 . H71 . 126.2(5) no C8 . C7 . H71 . 127.7(6) no W1 . C8 . C7 . 68.6(3) yes W1 . C8 . C9 . 72.4(3) yes C7 . C8 . C9 . 109.6(5) yes W1 . C8 . H81 . 126.5(5) no C7 . C8 . H81 . 125.4(6) no C9 . C8 . H81 . 125.0(6) no W1 . C9 . C8 . 73.2(3) yes W1 . C9 . C10 . 69.0(3) yes C8 . C9 . C10 . 109.6(5) yes W1 . C9 . H91 . 122.9(4) no C8 . C9 . H91 . 126.6(5) no C10 . C9 . H91 . 123.8(5) no W1 . C10 . C6 . 70.1(3) yes W1 . C10 . C9 . 75.4(3) yes C6 . C10 . C9 . 106.5(5) yes W1 . C10 . H101 . 120.2(4) no C6 . C10 . H101 . 126.3(5) no C9 . C10 . H101 . 127.3(5) no Si1 . C21 . H211 . 109.6(4) no Si1 . C21 . H212 . 110.4(5) no H211 . C21 . H212 . 109.7(6) no Si1 . C21 . H213 . 109.4(4) no H211 . C21 . H213 . 108.2(6) no H212 . C21 . H213 . 109.4(6) no Si1 . C22 . H221 . 111.3(5) no Si1 . C22 . H222 . 109.9(4) no H221 . C22 . H222 . 107.3(6) no Si1 . C22 . H223 . 111.4(5) no H221 . C22 . H223 . 109.4(5) no H222 . C22 . H223 . 107.4(6) no W1 . C31 . H311 . 114.8(4) no W1 . C31 . H312 . 88.2(4) no H311 . C31 . H312 . 112.2(6) no W1 . C31 . H313 . 123.2(4) no H311 . C31 . H313 . 107.3(6) no H312 . C31 . H313 . 109.5(6) no W1 . C32 . H321 . 110.2(4) no W1 . C32 . H322 . 109.6(4) no H321 . C32 . H322 . 107.3(6) no W1 . C32 . H323 . 111.1(4) no H321 . C32 . H323 . 109.7(6) no H322 . C32 . H323 . 108.7(6) no #=END data_CRYSTALS2_cif # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' linda.doerrer@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? #choose from: FI FM FO CI CM CO AD# _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 ; 'Studies of Ansa-bis(cyclopentadienyl)tungsten Derivatives' # Title of paper ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Conway, Stephen L. J.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR # Address for author 1 ; ; ? #footnote for author 1 ; 'Doerrer, Linda H.' # Author 2 ; South Parks Road Inorganic Chemistry Laboratory Oxford OX1 3QR # Address 2 ; ; ? # footnote 2 ; 'Green, Malcolm L.H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ; ? ; 'Stephens, Adam H. H.' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ; ? ; #============================================================================== # 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_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _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 # Add your own references - in alphabetic order ; 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite # choose from: _diffrn_measurement_device-type ' Enraf-nonius DIP2000 ' _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) ; # end_choice #========================================================================== # 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) ; # choose one of the following two lines _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _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 noref #**************************************************************************** _cell_length_a 9.350(3) _cell_angle_alpha 90. _cell_length_b 13.145(3) _cell_angle_beta 105.04(2) _cell_length_c 12.739(4) _cell_angle_gamma 90. _cell_volume 1512.0 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-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 'W ' -1.4210 6.8720 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 'International_Tables_Vol_IV_Table_2.2B' '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' _chemical_formula_sum ' C18 H26 W1 ' _chemical_formula_moiety ' C18 H26 W1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 426.26 _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 ' none ' _exptl_crystal_size_min 0.3 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.87 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 826.67 _exptl_absorpt_coefficient_mu 7.79 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 125 _diffrn_reflns_number 3097 _reflns_number_total 3097 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 3097 # Number of reflections without Friedels Law is 0 _reflns_number_observed 2860 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.59 _refine_diff_density_max 0.93 _refine_ls_number_reflns 2860 _refine_ls_number_parameters 173 _refine_ls_R_factor_obs 0.0198 _refine_ls_wR_factor_obs 0.0263 _refine_ls_goodness_of_fit_obs 0.8041 _refine_ls_shift/su_max 0.033162 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 2.32 0.530 1.82 ; _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 W1 0.61592(1) 0.260907(9) 0.083410(7) 0.0124 1.0000 Uani C1 0.8524(3) 0.26468(19) 0.1803(2) 0.0175 1.0000 Uani C2 0.7684(3) 0.3019(2) 0.2523(2) 0.0192 1.0000 Uani C3 0.7025(3) 0.3946(2) 0.2089(2) 0.0245 1.0000 Uani C4 0.7410(3) 0.4165(2) 0.1123(2) 0.0244 1.0000 Uani C5 0.8358(3) 0.3374(2) 0.0924(2) 0.0214 1.0000 Uani C6 0.6986(3) 0.10090(19) 0.1137(2) 0.0163 1.0000 Uani C7 0.6676(3) 0.1174(2) -0.0020(2) 0.0190 1.0000 Uani C8 0.5122(3) 0.1309(2) -0.0415(2) 0.0233 1.0000 Uani C9 0.4470(3) 0.1260(2) 0.0452(2) 0.0235 1.0000 Uani C10 0.5597(3) 0.1076(2) 0.1430(2) 0.0188 1.0000 Uani C21 0.9522(3) 0.1709(2) 0.1964(2) 0.0196 1.0000 Uani C22 0.8487(3) 0.07460(19) 0.19092(19) 0.0180 1.0000 Uani C23 1.0376(3) 0.1682(2) 0.1084(3) 0.0291 1.0000 Uani C24 1.0703(3) 0.1802(2) 0.3067(2) 0.0305 1.0000 Uani C25 0.9088(3) -0.0208(2) 0.1475(2) 0.0260 1.0000 Uani C26 0.8277(3) 0.0457(2) 0.3028(2) 0.0257 1.0000 Uani C31 0.4090(3) 0.3275(2) 0.1137(2) 0.0258 1.0000 Uani C32 0.5157(3) 0.3419(2) -0.0733(2) 0.0252 1.0000 Uani H21 0.7583 0.2681 0.3203 0.0190 1.0000 Uiso H31 0.6376 0.4376 0.2419 0.0233 1.0000 Uiso H41 0.7075 0.4774 0.0651 0.0212 1.0000 Uiso H51 0.8815 0.3333 0.0297 0.0196 1.0000 Uiso H71 0.7426 0.1199 -0.0458 0.0177 1.0000 Uiso H81 0.4585 0.1421 -0.1193 0.0211 1.0000 Uiso H91 0.3385 0.1338 0.0395 0.0209 1.0000 Uiso H101 0.5452 0.1012 0.2180 0.0185 1.0000 Uiso H231 1.1035 0.1065 0.1194 0.0288 1.0000 Uiso H232 1.1010 0.2306 0.1144 0.0288 1.0000 Uiso H233 0.9672 0.1653 0.0350 0.0288 1.0000 Uiso H241 1.1362 0.1193 0.3188 0.0263 1.0000 Uiso H242 1.1309 0.2430 0.3071 0.0263 1.0000 Uiso H243 1.0197 0.1850 0.3674 0.0263 1.0000 Uiso H251 1.0076 -0.0393 0.1966 0.0247 1.0000 Uiso H252 0.9216 -0.0066 0.0726 0.0247 1.0000 Uiso H253 0.8386 -0.0786 0.1432 0.0247 1.0000 Uiso H261 0.9257 0.0284 0.3535 0.0247 1.0000 Uiso H262 0.7827 0.1042 0.3334 0.0247 1.0000 Uiso H263 0.7602 -0.0147 0.2954 0.0247 1.0000 Uiso H311 0.3233 0.3102 0.0525 0.0600 1.0000 Uiso H312 0.4194 0.4025 0.1200 0.0600 1.0000 Uiso H313 0.3939 0.2995 0.1821 0.0600 1.0000 Uiso H321 0.4907 0.4127 -0.0579 0.0600 1.0000 Uiso H322 0.5875 0.3431 -0.1185 0.0600 1.0000 Uiso H323 0.4246 0.3062 -0.1132 0.0600 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 W1 0.0109(1) 0.0106(1) 0.0159(1) -0.00102(3) 0.00351(6) -0.00046(3 C1 0.0127(12) 0.0161(13) 0.0223(13) -0.0023(9) 0.0022(11) -0.0022(9) C2 0.0169(11) 0.0163(14) 0.0233(12) -0.005(1) 0.0033(9) -0.003(1) C3 0.0212(12) 0.0191(14) 0.0296(14) -0.0108(11) -0.000(1) 0.003(1) C4 0.0236(13) 0.0141(12) 0.0302(14) 0.001(1) -0.003(1) -0.003(1) C5 0.0171(11) 0.0192(14) 0.0270(13) -0.0019(11) 0.004(1) -0.007(1) C6 0.0171(11) 0.0114(11) 0.0205(12) -0.0023(9) 0.0051(9) -0.0015(9) C7 0.0253(12) 0.0118(12) 0.0205(12) -0.0036(9) 0.007(1) -0.0000(9) C8 0.0269(13) 0.0170(13) 0.0215(13) -0.005(1) -0.002(1) -0.002(1) C9 0.0159(11) 0.0199(13) 0.0325(14) -0.0050(11) 0.002(1) -0.006(1) C10 0.0218(12) 0.0129(13) 0.0227(12) -0.0006(9) 0.008(1) -0.0049(9) C21 0.0181(11) 0.0133(12) 0.0268(12) -0.000(1) 0.0049(9) 0.0012(9) C22 0.0181(11) 0.0135(12) 0.0216(12) 0.0002(9) 0.0038(9) -0.0004(9) C23 0.0210(12) 0.0249(16) 0.0459(16) -0.0033(13) 0.0171(12) -0.0018(11 C24 0.0222(13) 0.0237(15) 0.0379(15) 0.0007(12) -0.0058(12) 0.0025(11 C25 0.0259(12) 0.0167(13) 0.0337(14) -0.0018(11) 0.0045(11) 0.005(1) C26 0.0264(13) 0.0238(15) 0.0252(13) 0.0041(11) 0.004(1) 0.001(1) C31 0.0168(11) 0.0272(15) 0.0353(14) -0.0057(12) 0.010(1) 0.004(1) C32 0.0214(12) 0.0250(15) 0.0267(13) 0.0057(11) 0.002(1) 0.0026(11 _refine_ls_extinction_coef 97.1(43) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' 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 W1 . C1 . 2.236(3) yes W1 . C2 . 2.315(2) yes W1 . C3 . 2.372(3) yes W1 . C4 . 2.337(3) yes W1 . C5 . 2.264(2) yes W1 . C6 . 2.240(2) yes W1 . C7 . 2.291(3) yes W1 . C8 . 2.365(3) yes W1 . C9 . 2.340(3) yes W1 . C10 . 2.263(3) yes W1 . C31 . 2.246(2) yes W1 . C32 . 2.242(3) yes C1 . C2 . 1.439(4) yes C1 . C5 . 1.449(4) yes C1 . C21 . 1.527(4) yes C2 . C3 . 1.412(4) yes C2 . H21 . 1.000(3) no C3 . C4 . 1.398(4) yes C3 . H31 . 0.999(3) no C4 . C5 . 1.430(4) yes C4 . H41 . 1.002(3) no C5 . H51 . 1.001(3) no C6 . C7 . 1.443(3) yes C6 . C10 . 1.445(3) yes C6 . C22 . 1.530(3) yes C7 . C8 . 1.420(4) yes C7 . H71 . 1.003(2) no C8 . C9 . 1.395(4) yes C8 . H81 . 0.999(3) no C9 . C10 . 1.428(4) yes C9 . H91 . 1.003(3) no C10 . H101 . 1.003(2) no C21 . C22 . 1.584(3) yes C21 . C23 . 1.537(4) yes C21 . C24 . 1.550(3) yes C22 . C25 . 1.535(4) yes C22 . C26 . 1.536(4) yes C23 . H231 . 1.007(3) no C23 . H232 . 1.003(3) no C23 . H233 . 0.994(3) no C24 . H241 . 0.998(3) no C24 . H242 . 1.002(3) no C24 . H243 . 1.007(3) no C25 . H251 . 1.001(3) no C25 . H252 . 1.009(3) no C25 . H253 . 0.996(3) no C26 . H261 . 1.000(3) no C26 . H262 . 1.003(3) no C26 . H263 . 1.003(3) no C31 . H311 . 0.988(3) no C31 . H312 . 0.991(3) no C31 . H313 . 0.990(3) no C32 . H321 . 0.991(3) no C32 . H322 . 0.991(3) no C32 . H323 . 0.990(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 C1 . W1 . C2 . 36.8(1) yes C1 . W1 . C3 . 59.74(9) yes C2 . W1 . C3 . 35.04(9) yes C1 . W1 . C4 . 60.71(9) yes C2 . W1 . C4 . 59.17(9) yes C3 . W1 . C4 . 34.5(1) yes C1 . W1 . C5 . 37.6(1) yes C2 . W1 . C5 . 61.14(9) yes C3 . W1 . C5 . 59.3(1) yes C4 . W1 . C5 . 36.2(1) yes C1 . W1 . C6 . 71.21(9) yes C2 . W1 . C6 . 87.51(9) yes C3 . W1 . C6 . 122.5(1) yes C4 . W1 . C6 . 131.17(9) yes C5 . W1 . C6 . 98.1(1) yes C1 . W1 . C7 . 88.86(9) yes C2 . W1 . C7 . 118.55(9) yes C3 . W1 . C7 . 148.52(9) yes C4 . W1 . C7 . 129.5(1) yes C5 . W1 . C7 . 95.1(1) yes C1 . W1 . C8 . 124.2(1) yes C2 . W1 . C8 . 147.1(1) yes C3 . W1 . C8 . 175.89(9) yes C4 . W1 . C8 . 147.1(1) yes C5 . W1 . C8 . 124.3(1) yes C1 . W1 . C9 . 130.48(9) yes C2 . W1 . C9 . 126.1(1) yes C3 . W1 . C9 . 142.7(1) yes C4 . W1 . C9 . 168.2(1) yes C5 . W1 . C9 . 154.4(1) yes C1 . W1 . C10 . 96.74(9) yes C2 . W1 . C10 . 92.08(9) yes C3 . W1 . C10 . 120.1(1) yes C4 . W1 . C10 . 151.25(9) yes C5 . W1 . C10 . 131.7(1) yes C1 . W1 . C31 . 132.01(11) yes C2 . W1 . C31 . 95.75(9) yes C3 . W1 . C31 . 75.8(1) yes C4 . W1 . C31 . 92.87(11) yes C5 . W1 . C31 . 128.99(12) yes C1 . W1 . C32 . 127.3(1) yes C2 . W1 . C32 . 137.0(1) yes C3 . W1 . C32 . 103.8(1) yes C4 . W1 . C32 . 78.5(1) yes C5 . W1 . C32 . 89.9(1) yes C6 . W1 . C7 . 37.13(9) yes C6 . W1 . C8 . 60.02(9) yes C7 . W1 . C8 . 35.48(9) yes C6 . W1 . C9 . 60.57(9) yes C7 . W1 . C9 . 59.45(9) yes C8 . W1 . C9 . 34.5(1) yes C6 . W1 . C10 . 37.42(9) yes C7 . W1 . C10 . 61.46(9) yes C8 . W1 . C10 . 59.45(9) yes C9 . W1 . C10 . 36.10(9) yes C6 . W1 . C31 . 127.6(1) yes C7 . W1 . C31 . 134.4(1) yes C8 . W1 . C31 . 100.1(1) yes C9 . W1 . C31 . 76.5(1) yes C10 . W1 . C31 . 90.2(1) yes C6 . W1 . C32 . 130.2(1) yes C7 . W1 . C32 . 93.4(1) yes C8 . W1 . C32 . 75.0(1) yes C9 . W1 . C32 . 94.1(1) yes C10 . W1 . C32 . 129.9(1) yes C31 . W1 . C32 . 77.76(11) yes W1 . C1 . C2 . 74.59(16) yes W1 . C1 . C5 . 72.28(15) yes C2 . C1 . C5 . 107.5(2) yes W1 . C1 . C21 . 122.58(16) yes C2 . C1 . C21 . 127.1(2) yes C5 . C1 . C21 . 125.2(3) yes W1 . C2 . C1 . 68.60(15) yes W1 . C2 . C3 . 74.68(15) yes C1 . C2 . C3 . 107.4(2) yes W1 . C2 . H21 . 121.84(18) no C1 . C2 . H21 . 126.3(3) no C3 . C2 . H21 . 126.3(3) no W1 . C3 . C2 . 70.28(15) yes W1 . C3 . C4 . 71.36(15) yes C2 . C3 . C4 . 109.6(2) yes W1 . C3 . H31 . 124.41(19) no C2 . C3 . H31 . 125.1(3) no C4 . C3 . H31 . 125.3(3) no W1 . C4 . C3 . 74.10(16) yes W1 . C4 . C5 . 69.14(14) yes C3 . C4 . C5 . 108.6(2) yes W1 . C4 . H41 . 122.62(19) no C3 . C4 . H41 . 125.5(3) no C5 . C4 . H41 . 125.9(3) no W1 . C5 . C1 . 70.15(15) yes W1 . C5 . C4 . 74.68(14) yes C1 . C5 . C4 . 106.9(2) yes W1 . C5 . H51 . 120.38(19) no C1 . C5 . H51 . 126.7(3) no C4 . C5 . H51 . 126.4(3) no W1 . C6 . C7 . 73.38(15) yes W1 . C6 . C10 . 72.17(15) yes C7 . C6 . C10 . 107.4(2) yes W1 . C6 . C22 . 122.76(16) yes C7 . C6 . C22 . 126.7(2) yes C10 . C6 . C22 . 125.8(2) yes W1 . C7 . C6 . 69.49(14) yes W1 . C7 . C8 . 75.07(15) yes C6 . C7 . C8 . 107.2(2) yes W1 . C7 . H71 . 120.0(2) no C6 . C7 . H71 . 126.1(2) no C8 . C7 . H71 . 126.7(2) no W1 . C8 . C7 . 69.45(14) yes W1 . C8 . C9 . 71.81(15) yes C7 . C8 . C9 . 109.4(2) yes W1 . C8 . H81 . 125.0(2) no C7 . C8 . H81 . 125.0(3) no C9 . C8 . H81 . 125.6(3) no W1 . C9 . C8 . 73.71(15) yes W1 . C9 . C10 . 69.00(14) yes C8 . C9 . C10 . 108.9(2) yes W1 . C9 . H91 . 123.6(2) no C8 . C9 . H91 . 125.4(3) no C10 . C9 . H91 . 125.7(3) no W1 . C10 . C6 . 70.41(14) yes W1 . C10 . C9 . 74.90(15) yes C6 . C10 . C9 . 107.1(2) yes W1 . C10 . H101 . 119.65(19) no C6 . C10 . H101 . 126.4(2) no C9 . C10 . H101 . 126.4(2) no C1 . C21 . C22 . 107.13(19) yes C1 . C21 . C23 . 109.6(2) yes C22 . C21 . C23 . 112.1(2) yes C1 . C21 . C24 . 109.0(2) yes C22 . C21 . C24 . 112.7(2) yes C23 . C21 . C24 . 106.3(2) yes C6 . C22 . C21 . 107.20(19) yes C6 . C22 . C25 . 108.3(2) yes C21 . C22 . C25 . 113.1(2) yes C6 . C22 . C26 . 109.6(2) yes C21 . C22 . C26 . 112.4(2) yes C25 . C22 . C26 . 106.2(2) yes C21 . C23 . H231 . 109.4(3) no C21 . C23 . H232 . 109.5(3) no H231 . C23 . H232 . 108.7(2) no C21 . C23 . H233 . 110.2(2) no H231 . C23 . H233 . 109.4(3) no H232 . C23 . H233 . 109.7(3) no C21 . C24 . H241 . 110.1(3) no C21 . C24 . H242 . 109.8(3) no H241 . C24 . H242 . 109.5(3) no C21 . C24 . H243 . 109.6(2) no H241 . C24 . H243 . 109.1(3) no H242 . C24 . H243 . 108.8(3) no C22 . C25 . H251 . 109.8(2) no C22 . C25 . H252 . 109.5(2) no H251 . C25 . H252 . 108.6(3) no C22 . C25 . H253 . 110.2(2) no H251 . C25 . H253 . 109.7(3) no H252 . C25 . H253 . 109.1(3) no C22 . C26 . H261 . 109.8(2) no C22 . C26 . H262 . 109.8(2) no H261 . C26 . H262 . 109.2(3) no C22 . C26 . H263 . 109.7(2) no H261 . C26 . H263 . 109.2(3) no H262 . C26 . H263 . 109.0(3) no W1 . C31 . H311 . 109.50(19) no W1 . C31 . H312 . 109.34(18) no H311 . C31 . H312 . 109.5(3) no W1 . C31 . H313 . 109.4(2) no H311 . C31 . H313 . 109.7(3) no H312 . C31 . H313 . 109.4(3) no W1 . C32 . H321 . 109.6(2) no W1 . C32 . H322 . 109.58(19) no H321 . C32 . H322 . 109.3(3) no W1 . C32 . H323 . 109.6(2) no H321 . C32 . H323 . 109.4(3) no H322 . C32 . H323 . 109.3(3) no