# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1355 data_CRYSTALS_cif _audit_creation_date 97-07-04 _audit_creation_method CRYSTALS # icl11 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_author ; Linda H. Doerrer Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; _publ_contact_author_phone ' 01865 272 675 ' _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_coeditor_name 'P.P. Edwards ' _publ_contact_letter ; Please consider this CIF submission for publication as a Full Paper in Journal of the Chemical Society, Dalton Transactions. Full text and all other figures have been sent by post under separate cover. ; #============================================================================= # 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 ; 'Adducts of the Lewis Acid B(C6F5)3 with Transition Metal Oxo Compounds' ; # 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 'Barrado, Georgina' #<--'Last name, first name' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Green, Malcolm L. H.' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Doerrer, Linda H.' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Leech, Michael A.' ; Chemical Crystallography Laboratory 9 Parks Road OXFORD OX1 3PD ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; 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 Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (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. Otwinowski, Z. & Minor, W. (1996) DENZO - Processing of X-ray Diffraction data collected in oscillation mode. Methods in Enzymology (276). ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #========================================================================== # Now, all the strucure specific goodies #========================================================================== _computing_data_collection 'DIP2000 software (Enraf-Nonius)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO (Otwinowski & Minor, 1996) ; _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 'SHELXS86 (Sheldrick, 1986)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius DIP2020 ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment noref #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 16.157(1) _cell_angle_alpha 90 _cell_length_b 21.204(1) _cell_angle_beta 92.731(2) _cell_length_c 23.912(1) _cell_angle_gamma 90 _cell_volume 8182.78 _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 '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' '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' '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' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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 ' C78 H56 W1 F45 O4 N2 B3 ' _chemical_formula_moiety ' C78 H56 W1 F45 O4 N2 B3 ' _chemical_compound_source ; ? ; _chemical_formula_weight 2156.51 _cell_measurement_reflns_used 58107 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 26.69 _cell_measurement_temperature 100 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.21 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.75 _exptl_crystal_density_meas none _exptl_crystal_F_000 4253.09 _exptl_absorpt_coefficient_mu 1.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 #_diffrn_standards_interval_time ? #_diffrn_standards_interval_count ? #_diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 100 _diffrn_reflns_number 58107 _reflns_number_total 16848 _diffrn_reflns_av_R_equivalents 0.03 _reflns_number_observed 14377 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.69 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.42 _refine_diff_density_max 0.98 _refine_ls_number_reflns 14377 _refine_ls_number_parameters 1198 _refine_ls_R_factor_obs 0.0303 _refine_ls_wR_factor_obs 0.0301 _refine_ls_goodness_of_fit_obs 1.0941 _refine_ls_shift/esd_max 0.004452 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type W1 0.251598(5) 0.168204(4) 0.223820(3) 0.0109 1.0000 Uani F111 0.08706(9) 0.16785(7) 0.27284(6) 0.0237 1.0000 Uani F112 -0.0409(1) 0.18508(9) 0.33463(7) 0.0341 1.0000 Uani F113 -0.1945(1) 0.20757(9) 0.28707(8) 0.0370 1.0000 Uani F114 -0.21732(9) 0.20540(8) 0.17315(7) 0.0300 1.0000 Uani F115 -0.08966(9) 0.18129(7) 0.10925(6) 0.0215 1.0000 Uani F121 0.0305(1) 0.19010(8) 0.01949(6) 0.0281 1.0000 Uani F122 0.0369(1) 0.30024(9) -0.03319(7) 0.0379 1.0000 Uani F123 0.0935(1) 0.40508(9) 0.02128(9) 0.0458 1.0000 Uani F124 0.1371(1) 0.39842(7) 0.13342(8) 0.0378 1.0000 Uani F125 0.1262(1) 0.29053(7) 0.18731(6) 0.0244 1.0000 Uani F131 0.20654(9) 0.14003(7) 0.06661(6) 0.0224 1.0000 Uani F132 0.22262(9) 0.03632(8) 0.00510(6) 0.0276 1.0000 Uani F133 0.1081(1) -0.05752(7) 0.00804(6) 0.0255 1.0000 Uani F134 -0.02375(9) -0.04489(7) 0.07408(6) 0.0223 1.0000 Uani F135 -0.03911(8) 0.05579(7) 0.13800(6) 0.0202 1.0000 Uani F211 0.2875(1) 0.27691(9) 0.1379(1) 0.0466 1.0000 Uani F212 0.3013(1) 0.3868(1) 0.0876(1) 0.0604 1.0000 Uani F213 0.4501(1) 0.42841(8) 0.05365(8) 0.0385 1.0000 Uani F214 0.5873(1) 0.35587(8) 0.07380(7) 0.0314 1.0000 Uani F215 0.57533(9) 0.24371(8) 0.12284(7) 0.0276 1.0000 Uani F221 0.42610(9) 0.24410(8) 0.27009(6) 0.0269 1.0000 Uani F222 0.5365(1) 0.23189(9) 0.35554(7) 0.0350 1.0000 Uani F223 0.6734(1) 0.15877(9) 0.34590(7) 0.0337 1.0000 Uani F224 0.6982(1) 0.09885(8) 0.24735(7) 0.0311 1.0000 Uani F225 0.59023(9) 0.11108(8) 0.16110(6) 0.0263 1.0000 Uani F231 0.4097(1) 0.19563(7) 0.03361(6) 0.0249 1.0000 Uani F232 0.3997(1) 0.10066(8) -0.03757(6) 0.0298 1.0000 Uani F233 0.4094(1) -0.02033(8) -0.00137(7) 0.0314 1.0000 Uani F234 0.4339(1) -0.04471(7) 0.11051(8) 0.0337 1.0000 Uani F235 0.4391(1) 0.05006(7) 0.18412(6) 0.0263 1.0000 Uani F311 0.22297(9) 0.00490(7) 0.41914(6) 0.0243 1.0000 Uani F312 0.0717(1) -0.00617(8) 0.45755(7) 0.0334 1.0000 Uani F313 -0.0646(1) 0.01309(8) 0.38881(8) 0.0381 1.0000 Uani F314 -0.0471(1) 0.03047(8) 0.27709(8) 0.0348 1.0000 Uani F315 0.10338(9) 0.03851(7) 0.23671(6) 0.0245 1.0000 Uani F321 0.25807(9) 0.12909(7) 0.38761(7) 0.0256 1.0000 Uani F322 0.3852(1) 0.16723(8) 0.45473(8) 0.0390 1.0000 Uani F323 0.5389(1) 0.11777(9) 0.44393(8) 0.0383 1.0000 Uani F324 0.56271(9) 0.02971(9) 0.36329(7) 0.0338 1.0000 Uani F325 0.43763(9) -0.01181(8) 0.29883(6) 0.0264 1.0000 Uani F331 0.3019(1) -0.08545(7) 0.33616(6) 0.0233 1.0000 Uani F332 0.3197(1) -0.19029(7) 0.27564(7) 0.0354 1.0000 Uani F333 0.2998(1) -0.18585(8) 0.16162(7) 0.0352 1.0000 Uani F334 0.2614(1) -0.07405(8) 0.11036(6) 0.0327 1.0000 Uani F335 0.2486(1) 0.03078(7) 0.16919(6) 0.0252 1.0000 Uani O1 0.2466(1) 0.23201(8) 0.26764(7) 0.0210 1.0000 Uani O101 0.1639(1) 0.16753(7) 0.17535(7) 0.0155 1.0000 Uani O201 0.3459(1) 0.17317(8) 0.18820(7) 0.0167 1.0000 Uani O301 0.2519(1) 0.09783(8) 0.26465(7) 0.0171 1.0000 Uani N1 0.2181(1) 0.3985(1) 0.33331(8) 0.0180 1.0000 Uani N2 0.2210(1) 0.70311(9) 0.00787(8) 0.0128 1.0000 Uani C1 0.2083(2) 0.4693(1) 0.3437(1) 0.0183 1.0000 Uani C2 0.2802(1) 0.5010(1) 0.3763(1) 0.0207 1.0000 Uani C3 0.2523(2) 0.5664(1) 0.3938(1) 0.0248 1.0000 Uani C4 0.2129(2) 0.3651(1) 0.3896(1) 0.0193 1.0000 Uani C5 0.2098(2) 0.2936(1) 0.3883(1) 0.0283 1.0000 Uani C6 0.2190(2) 0.2696(1) 0.4481(1) 0.0305 1.0000 Uani C7 0.3016(1) 0.3835(1) 0.3097(1) 0.0196 1.0000 Uani C8 0.3202(2) 0.4164(1) 0.2552(1) 0.0272 1.0000 Uani C9 0.4107(2) 0.4066(2) 0.2430(1) 0.0363 1.0000 Uani C10 0.1500(2) 0.3766(1) 0.2917(1) 0.0196 1.0000 Uani C11 0.0622(2) 0.3873(1) 0.3100(1) 0.0249 1.0000 Uani C12 -0.0003(2) 0.3649(1) 0.2642(1) 0.0284 1.0000 Uani C13 0.2854(1) 0.7485(1) -0.0129(1) 0.0160 1.0000 Uani C14 0.3549(1) 0.7652(1) 0.0296(1) 0.0195 1.0000 Uani C15 0.3967(2) 0.8260(1) 0.0119(1) 0.0325 1.0000 Uani C16 0.2631(1) 0.6414(1) 0.0253(1) 0.0157 1.0000 Uani C17 0.2057(2) 0.5903(1) 0.0450(1) 0.0243 1.0000 Uani C18 0.2553(2) 0.5310(1) 0.0597(1) 0.0257 1.0000 Uani C19 0.1555(1) 0.6923(1) -0.0388(1) 0.0156 1.0000 Uani C20 0.1856(2) 0.6601(1) -0.0909(1) 0.0221 1.0000 Uani C21 0.1127(2) 0.6499(1) -0.1329(1) 0.0221 1.0000 Uani C22 0.1785(1) 0.7306(1) 0.05799(9) 0.0154 1.0000 Uani C23 0.1531(2) 0.7995(1) 0.0528(1) 0.0189 1.0000 Uani C24 0.1007(2) 0.8169(1) 0.1020(1) 0.0256 1.0000 Uani C110 0.0060(1) 0.1739(1) 0.1868(1) 0.0158 1.0000 Uani C111 0.0133(1) 0.1756(1) 0.2447(1) 0.0186 1.0000 Uani C112 -0.0532(2) 0.1852(1) 0.2788(1) 0.0239 1.0000 Uani C113 -0.1304(2) 0.1958(1) 0.2547(1) 0.0255 1.0000 Uani C114 -0.1421(2) 0.1945(1) 0.1975(1) 0.0226 1.0000 Uani C115 -0.0745(1) 0.1829(1) 0.1654(1) 0.0175 1.0000 Uani C120 0.0807(1) 0.2335(1) 0.1062(1) 0.0178 1.0000 Uani C121 0.0578(1) 0.2402(1) 0.0498(1) 0.0210 1.0000 Uani C122 0.0612(2) 0.2970(1) 0.0215(1) 0.0268 1.0000 Uani C123 0.0892(2) 0.3505(1) 0.0488(1) 0.0303 1.0000 Uani C124 0.1115(2) 0.3469(1) 0.1049(1) 0.0271 1.0000 Uani C125 0.1058(1) 0.2900(1) 0.1318(1) 0.0205 1.0000 Uani C130 0.0828(1) 0.1042(1) 0.10548(9) 0.0161 1.0000 Uani C131 0.1480(1) 0.0949(1) 0.0706(1) 0.0177 1.0000 Uani C132 0.1575(2) 0.0418(1) 0.0382(1) 0.0205 1.0000 Uani C133 0.1006(2) -0.0058(1) 0.03960(9) 0.0198 1.0000 Uani C134 0.0340(1) 0.0006(1) 0.0735(1) 0.0179 1.0000 Uani C135 0.0271(1) 0.0545(1) 0.10533(9) 0.0161 1.0000 Uani C210 0.4314(1) 0.2546(1) 0.1347(1) 0.0162 1.0000 Uani C211 0.3643(2) 0.2941(1) 0.1237(1) 0.0256 1.0000 Uani C212 0.3692(2) 0.3518(1) 0.0972(1) 0.0314 1.0000 Uani C213 0.4442(2) 0.3731(1) 0.0803(1) 0.0256 1.0000 Uani C214 0.5135(2) 0.3363(1) 0.0907(1) 0.0206 1.0000 Uani C215 0.5055(1) 0.2788(1) 0.1169(1) 0.0181 1.0000 Uani C220 0.5003(1) 0.1762(1) 0.2115(1) 0.0165 1.0000 Uani C221 0.4923(1) 0.2067(1) 0.2624(1) 0.0187 1.0000 Uani C222 0.5490(2) 0.2018(1) 0.3073(1) 0.0232 1.0000 Uani C223 0.6182(2) 0.1650(1) 0.3024(1) 0.0238 1.0000 Uani C224 0.6304(2) 0.1347(1) 0.2527(1) 0.0227 1.0000 Uani C225 0.5725(2) 0.1414(1) 0.2086(1) 0.0199 1.0000 Uani C230 0.4273(1) 0.1280(1) 0.1131(1) 0.0171 1.0000 Uani C231 0.4160(1) 0.1375(1) 0.0562(1) 0.0176 1.0000 Uani C232 0.4101(2) 0.0882(1) 0.0176(1) 0.0218 1.0000 Uani C233 0.4151(2) 0.0271(1) 0.0358(1) 0.0231 1.0000 Uani C234 0.4264(2) 0.0151(1) 0.0924(1) 0.0223 1.0000 Uani C235 0.4310(1) 0.0649(1) 0.1290(1) 0.0196 1.0000 Uani C310 0.1713(1) 0.0264(1) 0.3263(1) 0.0159 1.0000 Uani C311 0.1583(2) 0.0135(1) 0.3821(1) 0.0191 1.0000 Uani C312 0.0802(2) 0.0082(1) 0.4033(1) 0.0231 1.0000 Uani C313 0.0109(2) 0.0158(1) 0.3686(1) 0.0262 1.0000 Uani C314 0.0198(2) 0.0254(1) 0.3122(1) 0.0245 1.0000 Uani C315 0.0992(2) 0.0298(1) 0.2925(1) 0.0199 1.0000 Uani C320 0.3395(1) 0.0544(1) 0.34116(9) 0.0164 1.0000 Uani C321 0.3322(2) 0.1012(1) 0.3817(1) 0.0205 1.0000 Uani C322 0.3969(2) 0.1227(1) 0.4163(1) 0.0260 1.0000 Uani C323 0.4748(2) 0.0975(1) 0.4108(1) 0.0270 1.0000 Uani C324 0.4866(2) 0.0528(1) 0.3707(1) 0.0238 1.0000 Uani C325 0.4197(2) 0.0321(1) 0.3373(1) 0.0191 1.0000 Uani C330 0.2746(1) -0.0219(1) 0.2564(1) 0.0164 1.0000 Uani C331 0.2915(2) -0.0809(1) 0.2799(1) 0.0185 1.0000 Uani C332 0.3010(2) -0.1354(1) 0.2499(1) 0.0234 1.0000 Uani C333 0.2909(2) -0.1333(1) 0.1922(1) 0.0257 1.0000 Uani C334 0.2724(2) -0.0766(1) 0.1667(1) 0.0234 1.0000 Uani C335 0.2654(1) -0.0225(1) 0.1984(1) 0.0191 1.0000 Uani B101 0.0823(2) 0.1684(1) 0.1437(1) 0.0152 1.0000 Uani B201 0.4271(2) 0.1836(1) 0.1612(1) 0.0144 1.0000 Uani B301 0.2610(2) 0.0382(1) 0.2979(1) 0.0153 1.0000 Uani H11 0.1571 0.4754 0.3650 0.0201 1.0000 Uiso H12 0.2012 0.4904 0.3064 0.0201 1.0000 Uiso H21 0.2963 0.4753 0.4103 0.0210 1.0000 Uiso H22 0.3288 0.5045 0.3521 0.0210 1.0000 Uiso H31 0.2990 0.5879 0.4154 0.0250 1.0000 Uiso H32 0.2039 0.5625 0.4181 0.0250 1.0000 Uiso H33 0.2364 0.5918 0.3599 0.0250 1.0000 Uiso H41 0.2623 0.3779 0.4134 0.0206 1.0000 Uiso H42 0.1612 0.3802 0.4068 0.0206 1.0000 Uiso H51 0.2563 0.2771 0.3664 0.0291 1.0000 Uiso H52 0.1558 0.2792 0.3708 0.0291 1.0000 Uiso H61 0.2173 0.2225 0.4482 0.0308 1.0000 Uiso H62 0.2731 0.2843 0.4657 0.0308 1.0000 Uiso H63 0.1726 0.2864 0.4701 0.0308 1.0000 Uiso H71 0.3456 0.3958 0.3384 0.0209 1.0000 Uiso H72 0.3038 0.3370 0.3031 0.0209 1.0000 Uiso H81 0.3086 0.4625 0.2586 0.0288 1.0000 Uiso H82 0.2843 0.3982 0.2239 0.0288 1.0000 Uiso H91 0.4230 0.4281 0.2073 0.0369 1.0000 Uiso H92 0.4465 0.4247 0.2744 0.0369 1.0000 Uiso H93 0.4222 0.3604 0.2397 0.0369 1.0000 Uiso H101 0.1563 0.4000 0.2559 0.0208 1.0000 Uiso H102 0.1573 0.3305 0.2853 0.0208 1.0000 Uiso H111 0.0536 0.4332 0.3170 0.0256 1.0000 Uiso H112 0.0536 0.3629 0.3449 0.0256 1.0000 Uiso H121 -0.0577 0.3722 0.2765 0.0289 1.0000 Uiso H122 0.0080 0.3893 0.2290 0.0289 1.0000 Uiso H123 0.0081 0.3191 0.2570 0.0289 1.0000 Uiso H131 0.2566 0.7884 -0.0245 0.0171 1.0000 Uiso H132 0.3107 0.7289 -0.0460 0.0171 1.0000 Uiso H141 0.3317 0.7712 0.0672 0.0207 1.0000 Uiso H142 0.3966 0.7302 0.0315 0.0207 1.0000 Uiso H151 0.4424 0.8367 0.0398 0.0333 1.0000 Uiso H152 0.3550 0.8607 0.0099 0.0333 1.0000 Uiso H153 0.4199 0.8197 -0.0258 0.0333 1.0000 Uiso H161 0.3046 0.6509 0.0565 0.0167 1.0000 Uiso H162 0.2919 0.6248 -0.0076 0.0167 1.0000 Uiso H171 0.1777 0.6054 0.0791 0.0249 1.0000 Uiso H172 0.1629 0.5805 0.0148 0.0249 1.0000 Uiso H181 0.2173 0.4976 0.0727 0.0254 1.0000 Uiso H182 0.2980 0.5409 0.0901 0.0254 1.0000 Uiso H183 0.2833 0.5160 0.0258 0.0254 1.0000 Uiso H191 0.1320 0.7342 -0.0503 0.0161 1.0000 Uiso H192 0.1109 0.6655 -0.0237 0.0161 1.0000 Uiso H201 0.2280 0.6873 -0.1081 0.0228 1.0000 Uiso H202 0.2108 0.6185 -0.0803 0.0228 1.0000 Uiso H211 0.1327 0.6287 -0.1672 0.0229 1.0000 Uiso H212 0.0874 0.6916 -0.1436 0.0229 1.0000 Uiso H213 0.0702 0.6227 -0.1158 0.0229 1.0000 Uiso H221 0.2172 0.7265 0.0916 0.0169 1.0000 Uiso H222 0.1273 0.7053 0.0637 0.0169 1.0000 Uiso H231 0.2037 0.8268 0.0531 0.0203 1.0000 Uiso H232 0.1200 0.8062 0.0167 0.0203 1.0000 Uiso H241 0.0838 0.8621 0.0987 0.0265 1.0000 Uiso H242 0.1340 0.8102 0.1377 0.0265 1.0000 Uiso H243 0.0502 0.7896 0.1013 0.0265 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 0.01115(5) 0.01021(5) 0.01130(5) -0.00012(3) 0.00095(3) 0.00099(3) F111 0.0217(7) 0.0324(8) 0.0173(7) 0.0011(6) 0.0024(5) 0.0030(6) F112 0.038(1) 0.042(1) 0.0231(8) -0.0055(7) 0.0145(7) -0.0006(7) F113 0.0232(9) 0.041(1) 0.049(1) -0.0151(8) 0.0213(7) -0.0029(7) F114 0.0128(7) 0.0269(8) 0.050(1) -0.0029(7) 0.0030(7) 0.0031(6) F115 0.0158(7) 0.0220(7) 0.0263(7) 0.0063(6) -0.0022(5) 0.0011(5) F121 0.0281(8) 0.0350(8) 0.0203(7) 0.0081(6) -0.0090(6) -0.0064(7) F122 0.035(1) 0.050(1) 0.0280(9) 0.0217(8) -0.0057(7) 0.0032(8) F123 0.057(1) 0.0269(9) 0.053(1) 0.0268(8) 0.0052(9) 0.0046(8) F124 0.047(1) 0.0151(7) 0.051(1) 0.0028(7) 0.0058(8) -0.0001(7) F125 0.0315(8) 0.0186(7) 0.0230(7) -0.0014(6) 0.0014(6) 0.0048(6) F131 0.0162(7) 0.0292(8) 0.0223(7) -0.0014(6) 0.0060(5) -0.0059(6) F132 0.0228(8) 0.0371(9) 0.0238(8) -0.0059(6) 0.0114(6) -0.0008(6) F133 0.0321(8) 0.0232(8) 0.0217(7) -0.0055(6) 0.0045(6) 0.0027(6) F134 0.0243(8) 0.0181(7) 0.0247(7) -0.0007(6) 0.0028(6) -0.0054(6) F135 0.0171(7) 0.0195(7) 0.0246(7) -0.0003(6) 0.0082(5) -0.0022(5) F211 0.0165(8) 0.043(1) 0.082(1) 0.035(1) 0.0146(8) 0.0095(7) F212 0.037(1) 0.042(1) 0.104(2) 0.041(1) 0.025(1) 0.0237(9) F213 0.050(1) 0.0183(8) 0.049(1) 0.0115(7) 0.0187(9) 0.0038(7) F214 0.0261(8) 0.0324(8) 0.0365(9) 0.0062(7) 0.0104(7) -0.0091(7) F215 0.0150(7) 0.0328(8) 0.0356(9) 0.0109(7) 0.0071(6) 0.0043(6) F221 0.0216(8) 0.0311(8) 0.0279(8) -0.0129(6) 0.0006(6) 0.0040(6) F222 0.0302(9) 0.056(1) 0.0193(8) -0.0139(7) 0.0004(6) -0.0076(8) F223 0.0238(8) 0.055(1) 0.0214(8) 0.0083(7) -0.0084(6) -0.0072(7) F224 0.0208(8) 0.0346(9) 0.0370(9) 0.0042(7) -0.0081(6) 0.0089(6) F225 0.0203(7) 0.0335(8) 0.0249(8) -0.0095(6) -0.0021(6) 0.0086(6) F231 0.0348(9) 0.0205(7) 0.0186(7) 0.0003(6) -0.0058(6) 0.0013(6) F232 0.0347(9) 0.0359(9) 0.0183(7) -0.0066(6) -0.0041(6) -0.0046(7) F233 0.0315(9) 0.0282(8) 0.0347(9) -0.0171(7) 0.0044(7) -0.0058(7) F234 0.044(1) 0.0160(7) 0.042(1) -0.0026(7) 0.0062(8) -0.0004(7) F235 0.0376(9) 0.0193(7) 0.0220(7) 0.0044(6) 0.0024(6) -0.0008(6) F311 0.0301(8) 0.0265(8) 0.0162(7) 0.0010(6) -0.0003(6) -0.0014(6) F312 0.047(1) 0.0287(8) 0.0263(8) -0.0038(7) 0.0194(7) -0.0078(7) F313 0.0254(9) 0.0303(9) 0.061(1) -0.0067(8) 0.0243(8) -0.0056(7) F314 0.0158(8) 0.0334(9) 0.055(1) 0.0037(8) -0.0047(7) -0.0011(6) F315 0.0210(8) 0.0296(8) 0.0224(7) 0.0032(6) -0.0043(6) -0.0024(6) F321 0.0236(8) 0.0222(7) 0.0307(8) -0.0084(6) -0.0014(6) 0.0030(6) F322 0.043(1) 0.0348(9) 0.038(1) -0.0182(8) -0.0071(8) -0.0050(8) F323 0.0299(9) 0.044(1) 0.039(1) -0.0051(8) -0.0147(7) -0.0137(8) F324 0.0148(8) 0.044(1) 0.042(1) 0.0003(8) -0.0053(6) 0.0004(7) F325 0.0172(7) 0.0330(9) 0.0289(8) -0.0071(6) 0.0010(6) 0.0042(6) F331 0.0342(8) 0.0196(7) 0.0160(7) 0.0043(5) 0.0020(6) 0.0012(6) F332 0.054(1) 0.0152(7) 0.0373(9) 0.0011(7) 0.0032(8) 0.0046(7) F333 0.045(1) 0.0260(8) 0.0352(9) -0.0157(7) 0.0043(8) 0.0013(7) F334 0.041(1) 0.042(1) 0.0154(7) -0.0086(7) -0.0018(6) 0.0014(7) F335 0.0328(8) 0.0271(8) 0.0155(7) 0.0042(6) -0.0013(6) 0.0048(6) O1 0.0220(9) 0.0185(8) 0.0224(9) -0.0087(7) 0.0022(7) 0.0005(7) O101 0.0139(8) 0.0163(8) 0.0164(7) 0.0000(6) 0.0009(6) 0.0020(6) O201 0.0145(8) 0.0188(8) 0.0167(8) -0.0005(6) 0.0012(6) 0.0008(6) O301 0.0177(8) 0.0159(8) 0.0177(8) 0.0049(6) -0.0002(6) 0.0011(6) N1 0.019(1) 0.017(1) 0.018(1) -0.0009(8) 0.0018(8) -0.0011(8) N2 0.0133(9) 0.0117(9) 0.0132(9) 0.0004(7) 0.0003(7) 0.0028(7) C1 0.021(1) 0.014(1) 0.020(1) -0.0002(9) 0.0013(9) 0.0024(9) C2 0.019(1) 0.017(1) 0.026(1) 0.000(1) 0.0002(9) -0.0029(9) C3 0.028(1) 0.019(1) 0.028(1) -0.004(1) 0.005(1) -0.004(1) C4 0.021(1) 0.021(1) 0.016(1) -0.0008(9) 0.0020(9) -0.0020(9) C5 0.039(2) 0.021(1) 0.025(1) -0.003(1) 0.006(1) -0.004(1) C6 0.046(2) 0.020(1) 0.026(1) 0.003(1) 0.009(1) 0.000(1) C7 0.018(1) 0.018(1) 0.023(1) -0.0000(9) 0.0037(9) 0.0027(9) C8 0.029(1) 0.025(1) 0.028(1) 0.000(1) 0.009(1) -0.001(1) C9 0.029(2) 0.037(2) 0.044(2) 0.000(1) 0.013(1) -0.007(1) C10 0.019(1) 0.022(1) 0.017(1) -0.0038(9) 0.0001(9) -0.0045(9) C11 0.020(1) 0.033(1) 0.022(1) -0.005(1) 0.002(1) -0.004(1) C12 0.024(1) 0.034(2) 0.027(1) -0.005(1) -0.003(1) -0.005(1) C13 0.016(1) 0.017(1) 0.016(1) 0.0008(8) 0.0031(8) -0.0002(8) C14 0.016(1) 0.019(1) 0.023(1) 0.0004(9) 0.0002(9) -0.0022(9) C15 0.035(2) 0.029(1) 0.034(1) -0.001(1) 0.001(1) -0.014(1) C16 0.016(1) 0.013(1) 0.018(1) -0.0011(8) -0.0019(8) 0.0034(8) C17 0.020(1) 0.019(1) 0.034(1) 0.007(1) 0.001(1) 0.0010(9) C18 0.024(1) 0.017(1) 0.035(1) 0.006(1) -0.002(1) 0.002(1) C19 0.013(1) 0.017(1) 0.016(1) -0.0004(9) -0.0029(8) 0.0030(8) C20 0.023(1) 0.025(1) 0.018(1) -0.0046(9) -0.0035(9) 0.004(1) C21 0.027(1) 0.019(1) 0.020(1) -0.0024(9) -0.008(1) 0.0029(9) C22 0.015(1) 0.017(1) 0.015(1) -0.0028(8) 0.0040(8) 0.0031(8) C23 0.021(1) 0.015(1) 0.021(1) -0.0009(9) 0.0021(9) 0.0054(9) C24 0.028(1) 0.023(1) 0.027(1) -0.003(1) 0.009(1) 0.006(1) C110 0.015(1) 0.010(1) 0.023(1) 0.0023(9) 0.0043(9) 0.0019(8) C111 0.016(1) 0.017(1) 0.024(1) 0.0012(9) 0.0047(9) -0.0002(9) C112 0.029(1) 0.019(1) 0.024(1) -0.004(1) 0.010(1) -0.002(1) C113 0.020(1) 0.020(1) 0.038(2) -0.006(1) 0.017(1) -0.001(1) C114 0.014(1) 0.015(1) 0.039(1) -0.001(1) 0.005(1) 0.0008(9) C115 0.017(1) 0.011(1) 0.025(1) 0.0023(9) 0.0026(9) 0.0000(8) C120 0.010(1) 0.019(1) 0.024(1) 0.0051(9) 0.0032(9) 0.0020(8) C121 0.013(1) 0.024(1) 0.026(1) 0.006(1) -0.0014(9) 0.0005(9) C122 0.016(1) 0.038(2) 0.026(1) 0.016(1) 0.001(1) 0.007(1) C123 0.026(1) 0.022(1) 0.043(2) 0.018(1) 0.006(1) 0.007(1) C124 0.023(1) 0.020(1) 0.039(2) 0.004(1) 0.004(1) 0.005(1) C125 0.015(1) 0.020(1) 0.027(1) 0.005(1) 0.0027(9) 0.0041(9) C130 0.018(1) 0.019(1) 0.011(1) 0.0051(8) -0.0014(8) 0.0018(9) C131 0.013(1) 0.022(1) 0.018(1) 0.0053(9) -0.0009(8) -0.0015(9) C132 0.018(1) 0.029(1) 0.015(1) 0.0005(9) 0.0037(9) 0.003(1) C133 0.025(1) 0.021(1) 0.013(1) -0.0021(9) 0.0001(9) 0.004(1) C134 0.018(1) 0.018(1) 0.017(1) 0.0046(9) -0.0029(8) -0.0011(9) C135 0.012(1) 0.021(1) 0.016(1) 0.0027(9) 0.0024(8) 0.0023(8) C210 0.016(1) 0.016(1) 0.016(1) -0.0016(8) 0.0014(8) 0.0007(8) C211 0.018(1) 0.023(1) 0.036(1) 0.005(1) 0.007(1) 0.001(1) C212 0.028(1) 0.023(1) 0.044(2) 0.010(1) 0.010(1) 0.011(1) C213 0.035(1) 0.015(1) 0.027(1) 0.003(1) 0.010(1) 0.000(1) C214 0.022(1) 0.021(1) 0.019(1) -0.0039(9) 0.0049(9) -0.0057(9) C215 0.017(1) 0.021(1) 0.016(1) -0.0035(9) 0.0010(8) -0.0014(9) C220 0.015(1) 0.018(1) 0.016(1) 0.0017(9) 0.0011(8) -0.0041(8) C221 0.014(1) 0.022(1) 0.020(1) 0.0002(9) 0.0033(9) -0.0020(9) C222 0.022(1) 0.032(1) 0.015(1) -0.003(1) 0.0023(9) -0.009(1) C223 0.019(1) 0.035(1) 0.017(1) 0.009(1) -0.0052(9) -0.009(1) C224 0.016(1) 0.025(1) 0.026(1) 0.006(1) -0.0018(9) 0.0015(9) C225 0.019(1) 0.022(1) 0.019(1) -0.0007(9) 0.0008(9) -0.0016(9) C230 0.011(1) 0.018(1) 0.022(1) -0.0039(9) 0.0008(8) 0.0003(8) C231 0.015(1) 0.018(1) 0.019(1) -0.0010(9) -0.0032(8) 0.0008(9) C232 0.015(1) 0.031(1) 0.019(1) -0.004(1) 0.0002(9) -0.003(1) C233 0.017(1) 0.023(1) 0.029(1) -0.011(1) 0.004(1) -0.0025(9) C234 0.019(1) 0.014(1) 0.034(1) -0.002(1) 0.007(1) 0.0006(9) C235 0.017(1) 0.019(1) 0.023(1) -0.0002(9) 0.0032(9) -0.0021(9) C310 0.016(1) 0.012(1) 0.019(1) -0.0021(8) 0.0031(8) 0.0009(8) C311 0.023(1) 0.014(1) 0.021(1) -0.0024(9) 0.0050(9) -0.0032(9) C312 0.034(1) 0.012(1) 0.025(1) -0.0040(9) 0.013(1) -0.004(1) C313 0.020(1) 0.014(1) 0.045(2) -0.006(1) 0.016(1) -0.0020(9) C314 0.015(1) 0.017(1) 0.041(2) -0.002(1) -0.001(1) -0.0015(9) C315 0.021(1) 0.017(1) 0.022(1) -0.0012(9) 0.0025(9) -0.0010(9) C320 0.021(1) 0.016(1) 0.013(1) 0.0040(8) 0.0009(8) -0.0009(9) C321 0.021(1) 0.016(1) 0.024(1) 0.0012(9) 0.0002(9) 0.0011(9) C322 0.031(1) 0.023(1) 0.024(1) -0.004(1) -0.004(1) -0.005(1) C323 0.024(1) 0.028(1) 0.028(1) 0.002(1) -0.009(1) -0.008(1) C324 0.013(1) 0.029(1) 0.029(1) 0.006(1) -0.0027(9) -0.0039(9) C325 0.021(1) 0.017(1) 0.019(1) 0.0024(9) 0.0004(9) 0.0012(9) C330 0.012(1) 0.020(1) 0.017(1) 0.0011(9) 0.0012(8) -0.0017(8) C331 0.020(1) 0.018(1) 0.018(1) 0.0044(9) 0.0025(9) -0.0007(9) C332 0.025(1) 0.017(1) 0.028(1) -0.000(1) 0.002(1) -0.0020(9) C333 0.027(1) 0.023(1) 0.027(1) -0.009(1) 0.005(1) -0.004(1) C334 0.024(1) 0.029(1) 0.017(1) -0.006(1) 0.0004(9) -0.002(1) C335 0.018(1) 0.024(1) 0.015(1) 0.0026(9) 0.0018(9) 0.0002(9) B101 0.010(1) 0.019(1) 0.017(1) 0.005(1) 0.0016(9) -0.0015(9) B201 0.013(1) 0.014(1) 0.016(1) -0.0009(9) -0.0000(9) -0.0006(9) B301 0.015(1) 0.017(1) 0.015(1) 0.002(1) 0.0011(9) -0.0001(9) _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 . O1 . 1.716(2) yes W1 . O101 . 1.788(2) yes W1 . O201 . 1.784(2) yes W1 . O301 . 1.783(2) yes F111 . C111 . 1.350(3) yes F112 . C112 . 1.341(3) yes F113 . C113 . 1.346(3) yes F114 . C114 . 1.342(3) yes F115 . C115 . 1.355(3) yes F121 . C121 . 1.349(3) yes F122 . C122 . 1.348(3) yes F123 . C123 . 1.335(3) yes F124 . C124 . 1.342(3) yes F125 . C125 . 1.352(3) yes F131 . C131 . 1.352(3) yes F132 . C132 . 1.352(3) yes F133 . C133 . 1.340(3) yes F134 . C134 . 1.342(3) yes F135 . C135 . 1.355(3) yes F211 . C211 . 1.351(3) yes F212 . C212 . 1.335(3) yes F213 . C213 . 1.341(3) yes F214 . C214 . 1.344(3) yes F215 . C215 . 1.354(3) yes F221 . C221 . 1.352(3) yes F222 . C222 . 1.343(3) yes F223 . C223 . 1.345(3) yes F224 . C224 . 1.345(3) yes F225 . C225 . 1.347(3) yes F231 . C231 . 1.346(3) yes F232 . C232 . 1.347(3) yes F233 . C233 . 1.342(3) yes F234 . C234 . 1.344(3) yes F235 . C235 . 1.356(3) yes F311 . C311 . 1.350(3) yes F312 . C312 . 1.346(3) yes F313 . C313 . 1.334(3) yes F314 . C314 . 1.342(3) yes F315 . C315 . 1.353(3) yes F321 . C321 . 1.348(3) yes F322 . C322 . 1.339(3) yes F323 . C323 . 1.345(3) yes F324 . C324 . 1.344(3) yes F325 . C325 . 1.350(3) yes F331 . C331 . 1.350(3) yes F332 . C332 . 1.345(3) yes F333 . C333 . 1.343(3) yes F334 . C334 . 1.351(3) yes F335 . C335 . 1.349(3) yes O101 . B101 . 1.488(3) yes O201 . B201 . 1.505(3) yes O301 . B301 . 1.497(3) yes N1 . C1 . 1.530(3) yes N1 . C4 . 1.526(3) yes N1 . C7 . 1.521(3) yes N1 . C10 . 1.520(3) yes N2 . C13 . 1.518(3) yes N2 . C16 . 1.523(3) yes N2 . C19 . 1.519(3) yes N2 . C22 . 1.526(3) yes C1 . C2 . 1.525(3) yes C1 . H11 . 1.000(2) no C1 . H12 . 0.999(2) no C2 . C3 . 1.522(4) yes C2 . H21 . 1.003(2) no C2 . H22 . 1.000(2) no C3 . H31 . 1.004(3) no C3 . H32 . 1.000(3) no C3 . H33 . 0.998(3) no C4 . C5 . 1.516(4) yes C4 . H41 . 0.996(2) no C4 . H42 . 1.002(2) no C5 . C6 . 1.520(4) yes C5 . H51 . 0.999(3) no C5 . H52 . 0.997(3) no C6 . H61 . 0.999(3) no C6 . H62 . 1.000(3) no C6 . H63 . 1.002(3) no C7 . C8 . 1.521(4) yes C7 . H71 . 0.999(3) no C7 . H72 . 0.999(2) no C8 . C9 . 1.519(4) yes C8 . H81 . 0.998(3) no C8 . H82 . 1.002(3) no C9 . H91 . 0.998(3) no C9 . H92 . 1.000(3) no C9 . H93 . 1.001(3) no C10 . C11 . 1.521(3) yes C10 . H101 . 1.000(2) no C10 . H102 . 0.997(2) no C11 . C12 . 1.530(4) yes C11 . H111 . 0.998(3) no C11 . H112 . 0.997(3) no C12 . H121 . 0.999(3) no C12 . H122 . 1.004(3) no C12 . H123 . 0.997(3) no C13 . C14 . 1.519(3) yes C13 . H131 . 0.998(2) no C13 . H132 . 1.000(2) no C14 . C15 . 1.524(4) yes C14 . H141 . 0.999(2) no C14 . H142 . 1.002(2) no C15 . H151 . 0.997(3) no C15 . H152 . 0.998(3) no C15 . H153 . 1.001(3) no C16 . C17 . 1.517(3) yes C16 . H161 . 0.999(2) no C16 . H162 . 0.997(2) no C17 . C18 . 1.521(3) yes C17 . H171 . 1.005(3) no C17 . H172 . 0.998(3) no C18 . H181 . 0.998(3) no C18 . H182 . 1.002(3) no C18 . H183 . 0.999(3) no C19 . C20 . 1.519(3) yes C19 . H191 . 1.001(2) no C19 . H192 . 0.999(2) no C20 . C21 . 1.527(3) yes C20 . H201 . 1.000(3) no C20 . H202 . 0.999(3) no C21 . H211 . 1.001(3) no C21 . H212 . 1.000(2) no C21 . H213 . 1.000(3) no C22 . C23 . 1.521(3) yes C22 . H221 . 0.999(2) no C22 . H222 . 1.001(2) no C23 . C24 . 1.527(3) yes C23 . H231 . 1.000(3) no C23 . H232 . 1.003(2) no C24 . H241 . 0.999(3) no C24 . H242 . 0.998(3) no C24 . H243 . 1.000(3) no C110 . C111 . 1.384(3) yes C110 . C115 . 1.387(3) yes C110 . B101 . 1.648(3) yes C111 . C112 . 1.395(3) yes C112 . C113 . 1.367(4) yes C113 . C114 . 1.372(4) yes C114 . C115 . 1.387(3) yes C120 . C121 . 1.388(3) yes C120 . C125 . 1.396(4) yes C120 . B101 . 1.646(3) yes C121 . C122 . 1.384(4) yes C122 . C123 . 1.375(5) yes C123 . C124 . 1.374(4) yes C124 . C125 . 1.373(4) yes C130 . C131 . 1.389(3) yes C130 . C135 . 1.385(3) yes C130 . B101 . 1.640(4) yes C131 . C132 . 1.379(4) yes C132 . C133 . 1.368(4) yes C133 . C134 . 1.384(3) yes C134 . C135 . 1.381(3) yes C210 . C211 . 1.385(3) yes C210 . C215 . 1.388(3) yes C210 . B201 . 1.636(3) yes C211 . C212 . 1.383(4) yes C212 . C213 . 1.372(4) yes C213 . C214 . 1.376(4) yes C214 . C215 . 1.379(3) yes C220 . C221 . 1.389(3) yes C220 . C225 . 1.385(4) yes C220 . B201 . 1.653(3) yes C221 . C222 . 1.382(4) yes C222 . C223 . 1.373(4) yes C223 . C224 . 1.373(4) yes C224 . C225 . 1.384(3) yes C230 . C231 . 1.381(3) yes C230 . C235 . 1.391(3) yes C230 . B201 . 1.648(3) yes C231 . C232 . 1.395(3) yes C232 . C233 . 1.369(4) yes C233 . C234 . 1.382(4) yes C234 . C235 . 1.370(4) yes C310 . C311 . 1.387(3) yes C310 . C315 . 1.387(3) yes C310 . B301 . 1.649(3) yes C311 . C312 . 1.387(3) yes C312 . C313 . 1.371(4) yes C313 . C314 . 1.377(4) yes C314 . C315 . 1.391(4) yes C320 . C321 . 1.398(3) yes C320 . C325 . 1.387(3) yes C320 . B301 . 1.635(3) yes C321 . C322 . 1.377(4) yes C322 . C323 . 1.379(4) yes C323 . C324 . 1.367(4) yes C324 . C325 . 1.384(4) yes C330 . C331 . 1.394(3) yes C330 . C335 . 1.387(3) yes C330 . B301 . 1.636(3) yes C331 . C332 . 1.373(4) yes C332 . C333 . 1.382(4) yes C333 . C334 . 1.376(4) yes C334 . C335 . 1.383(4) yes 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 O1 . W1 . O101 . 110.10(8) yes O1 . W1 . O201 . 108.12(8) yes O101 . W1 . O201 . 111.09(7) yes O1 . W1 . O301 . 108.94(8) yes O101 . W1 . O301 . 109.25(7) yes O201 . W1 . O301 . 109.31(7) yes W1 . O101 . B101 . 170.1(1) yes W1 . O201 . B201 . 174.2(1) yes W1 . O301 . B301 . 174.4(2) yes C1 . N1 . C4 . 107.6(2) yes C1 . N1 . C7 . 111.4(2) yes C4 . N1 . C7 . 108.5(2) yes C1 . N1 . C10 . 109.2(2) yes C4 . N1 . C10 . 111.5(2) yes C7 . N1 . C10 . 108.7(2) yes C13 . N2 . C16 . 109.3(2) yes C13 . N2 . C19 . 108.7(2) yes C16 . N2 . C19 . 111.0(2) yes C13 . N2 . C22 . 110.9(2) yes C16 . N2 . C22 . 109.0(2) yes C19 . N2 . C22 . 108.1(2) yes N1 . C1 . C2 . 115.7(2) yes N1 . C1 . H11 . 107.7(2) no C2 . C1 . H11 . 108.0(2) no N1 . C1 . H12 . 107.7(2) no C2 . C1 . H12 . 108.0(2) no H11 . C1 . H12 . 109.5(2) no C1 . C2 . C3 . 108.4(2) yes C1 . C2 . H21 . 109.6(2) no C3 . C2 . H21 . 109.9(2) no C1 . C2 . H22 . 109.8(2) no C3 . C2 . H22 . 110.0(2) no H21 . C2 . H22 . 109.2(2) no C2 . C3 . H31 . 109.4(2) no C2 . C3 . H32 . 109.7(2) no H31 . C3 . H32 . 109.2(2) no C2 . C3 . H33 . 109.6(2) no H31 . C3 . H33 . 109.3(2) no H32 . C3 . H33 . 109.7(3) no N1 . C4 . C5 . 116.7(2) yes N1 . C4 . H41 . 107.6(2) no C5 . C4 . H41 . 108.0(2) no N1 . C4 . H42 . 107.3(2) no C5 . C4 . H42 . 107.5(2) no H41 . C4 . H42 . 109.7(2) no C4 . C5 . C6 . 108.3(2) yes C4 . C5 . H51 . 109.6(2) no C6 . C5 . H51 . 109.5(3) no C4 . C5 . H52 . 110.0(3) no C6 . C5 . H52 . 109.7(2) no H51 . C5 . H52 . 109.8(3) no C5 . C6 . H61 . 109.5(2) no C5 . C6 . H62 . 109.6(2) no H61 . C6 . H62 . 109.5(3) no C5 . C6 . H63 . 109.5(3) no H61 . C6 . H63 . 109.4(3) no H62 . C6 . H63 . 109.3(3) no N1 . C7 . C8 . 116.0(2) yes N1 . C7 . H71 . 107.8(2) no C8 . C7 . H71 . 107.8(2) no N1 . C7 . H72 . 107.7(2) no C8 . C7 . H72 . 107.9(2) no H71 . C7 . H72 . 109.6(2) no C7 . C8 . C9 . 109.5(2) yes C7 . C8 . H81 . 109.5(2) no C9 . C8 . H81 . 109.7(2) no C7 . C8 . H82 . 109.3(2) no C9 . C8 . H82 . 109.4(2) no H81 . C8 . H82 . 109.5(3) no C8 . C9 . H91 . 109.5(3) no C8 . C9 . H92 . 109.3(3) no H91 . C9 . H92 . 109.6(3) no C8 . C9 . H93 . 109.4(3) no H91 . C9 . H93 . 109.6(3) no H92 . C9 . H93 . 109.4(3) no N1 . C10 . C11 . 115.0(2) yes N1 . C10 . H101 . 108.0(2) no C11 . C10 . H101 . 107.8(2) no N1 . C10 . H102 . 108.3(2) no C11 . C10 . H102 . 108.0(2) no H101 . C10 . H102 . 109.7(2) no C10 . C11 . C12 . 109.9(2) yes C10 . C11 . H111 . 109.5(2) no C12 . C11 . H111 . 109.2(2) no C10 . C11 . H112 . 109.4(2) no C12 . C11 . H112 . 109.0(2) no H111 . C11 . H112 . 109.9(2) no C11 . C12 . H121 . 109.4(2) no C11 . C12 . H122 . 109.2(2) no H121 . C12 . H122 . 109.3(3) no C11 . C12 . H123 . 109.6(2) no H121 . C12 . H123 . 109.8(3) no H122 . C12 . H123 . 109.5(3) no N2 . C13 . C14 . 115.1(2) yes N2 . C13 . H131 . 108.1(2) no C14 . C13 . H131 . 108.0(2) no N2 . C13 . H132 . 107.9(2) no C14 . C13 . H132 . 108.0(2) no H131 . C13 . H132 . 109.6(2) no C13 . C14 . C15 . 109.6(2) yes C13 . C14 . H141 . 109.6(2) no C15 . C14 . H141 . 109.5(2) no C13 . C14 . H142 . 109.4(2) no C15 . C14 . H142 . 109.4(2) no H141 . C14 . H142 . 109.4(2) no C14 . C15 . H151 . 109.4(3) no C14 . C15 . H152 . 109.2(3) no H151 . C15 . H152 . 110.0(3) no C14 . C15 . H153 . 109.1(2) no H151 . C15 . H153 . 109.6(3) no H152 . C15 . H153 . 109.6(3) no N2 . C16 . C17 . 115.3(2) yes N2 . C16 . H161 . 107.9(2) no C17 . C16 . H161 . 108.0(2) no N2 . C16 . H162 . 107.9(2) no C17 . C16 . H162 . 107.9(2) no H161 . C16 . H162 . 109.8(2) no C16 . C17 . C18 . 109.9(2) yes C16 . C17 . H171 . 109.3(2) no C18 . C17 . H171 . 109.3(2) no C16 . C17 . H172 . 109.6(2) no C18 . C17 . H172 . 109.6(2) no H171 . C17 . H172 . 109.3(2) no C17 . C18 . H181 . 109.5(2) no C17 . C18 . H182 . 109.4(2) no H181 . C18 . H182 . 109.5(3) no C17 . C18 . H183 . 109.3(2) no H181 . C18 . H183 . 109.7(3) no H182 . C18 . H183 . 109.4(3) no N2 . C19 . C20 . 115.5(2) yes N2 . C19 . H191 . 108.0(2) no C20 . C19 . H191 . 107.8(2) no N2 . C19 . H192 . 108.0(2) no C20 . C19 . H192 . 107.9(2) no H191 . C19 . H192 . 109.4(2) no C19 . C20 . C21 . 109.6(2) yes C19 . C20 . H201 . 109.4(2) no C21 . C20 . H201 . 109.4(2) no C19 . C20 . H202 . 109.3(2) no C21 . C20 . H202 . 109.5(2) no H201 . C20 . H202 . 109.6(2) no C20 . C21 . H211 . 109.4(2) no C20 . C21 . H212 . 109.6(2) no H211 . C21 . H212 . 109.4(2) no C20 . C21 . H213 . 109.6(2) no H211 . C21 . H213 . 109.4(2) no H212 . C21 . H213 . 109.5(3) no N2 . C22 . C23 . 115.6(2) yes N2 . C22 . H221 . 108.1(2) no C23 . C22 . H221 . 107.9(2) no N2 . C22 . H222 . 107.9(2) no C23 . C22 . H222 . 107.8(2) no H221 . C22 . H222 . 109.5(2) no C22 . C23 . C24 . 109.0(2) yes C22 . C23 . H231 . 109.7(2) no C24 . C23 . H231 . 109.7(2) no C22 . C23 . H232 . 109.6(2) no C24 . C23 . H232 . 109.6(2) no H231 . C23 . H232 . 109.2(2) no C23 . C24 . H241 . 109.4(2) no C23 . C24 . H242 . 109.2(2) no H241 . C24 . H242 . 109.8(3) no C23 . C24 . H243 . 109.2(2) no H241 . C24 . H243 . 109.6(3) no H242 . C24 . H243 . 109.7(3) no C111 . C110 . C115 . 113.5(2) yes C111 . C110 . B101 . 126.6(2) yes C115 . C110 . B101 . 119.7(2) yes F111 . C111 . C110 . 121.8(2) yes F111 . C111 . C112 . 114.4(2) yes C110 . C111 . C112 . 123.8(2) yes F112 . C112 . C111 . 120.0(2) yes F112 . C112 . C113 . 120.6(2) yes C111 . C112 . C113 . 119.4(2) yes F113 . C113 . C112 . 119.9(3) yes F113 . C113 . C114 . 120.3(2) yes C112 . C113 . C114 . 119.8(2) yes F114 . C114 . C113 . 120.6(2) yes F114 . C114 . C115 . 120.8(2) yes C113 . C114 . C115 . 118.6(2) yes F115 . C115 . C110 . 118.9(2) yes F115 . C115 . C114 . 116.2(2) yes C110 . C115 . C114 . 124.8(2) yes C121 . C120 . C125 . 113.4(2) yes C121 . C120 . B101 . 127.6(2) yes C125 . C120 . B101 . 118.9(2) yes F121 . C121 . C120 . 120.5(2) yes F121 . C121 . C122 . 116.2(2) yes C120 . C121 . C122 . 123.3(3) yes F122 . C122 . C121 . 120.1(3) yes F122 . C122 . C123 . 119.5(2) yes C121 . C122 . C123 . 120.3(3) yes F123 . C123 . C122 . 120.3(3) yes F123 . C123 . C124 . 120.8(3) yes C122 . C123 . C124 . 118.9(2) yes F124 . C124 . C123 . 120.7(2) yes F124 . C124 . C125 . 120.2(3) yes C123 . C124 . C125 . 119.1(3) yes F125 . C125 . C120 . 119.3(2) yes F125 . C125 . C124 . 115.7(2) yes C120 . C125 . C124 . 124.9(2) yes C131 . C130 . C135 . 113.7(2) yes C131 . C130 . B101 . 118.4(2) yes C135 . C130 . B101 . 127.8(2) yes F131 . C131 . C130 . 119.7(2) yes F131 . C131 . C132 . 116.2(2) yes C130 . C131 . C132 . 124.1(2) yes F132 . C132 . C131 . 120.7(2) yes F132 . C132 . C133 . 119.5(2) yes C131 . C132 . C133 . 119.8(2) yes F133 . C133 . C132 . 120.8(2) yes F133 . C133 . C134 . 120.2(2) yes C132 . C133 . C134 . 119.0(2) yes F134 . C134 . C133 . 119.7(2) yes F134 . C134 . C135 . 121.0(2) yes C133 . C134 . C135 . 119.3(2) yes F135 . C135 . C130 . 120.9(2) yes F135 . C135 . C134 . 114.9(2) yes C130 . C135 . C134 . 124.2(2) yes C211 . C210 . C215 . 113.3(2) yes C211 . C210 . B201 . 125.6(2) yes C215 . C210 . B201 . 120.8(2) yes F211 . C211 . C210 . 120.6(2) yes F211 . C211 . C212 . 115.2(2) yes C210 . C211 . C212 . 124.2(2) yes F212 . C212 . C211 . 120.4(3) yes F212 . C212 . C213 . 119.8(3) yes C211 . C212 . C213 . 119.8(2) yes F213 . C213 . C212 . 120.7(2) yes F213 . C213 . C214 . 120.4(2) yes C212 . C213 . C214 . 118.8(2) yes F214 . C214 . C213 . 119.8(2) yes F214 . C214 . C215 . 120.9(2) yes C213 . C214 . C215 . 119.3(2) yes F215 . C215 . C210 . 119.4(2) yes F215 . C215 . C214 . 116.0(2) yes C210 . C215 . C214 . 124.6(2) yes C221 . C220 . C225 . 114.0(2) yes C221 . C220 . B201 . 119.9(2) yes C225 . C220 . B201 . 126.1(2) yes F221 . C221 . C220 . 120.1(2) yes F221 . C221 . C222 . 115.9(2) yes C220 . C221 . C222 . 124.0(2) yes F222 . C222 . C221 . 120.8(2) yes F222 . C222 . C223 . 120.0(2) yes C221 . C222 . C223 . 119.2(2) yes F223 . C223 . C222 . 120.2(2) yes F223 . C223 . C224 . 120.4(2) yes C222 . C223 . C224 . 119.4(2) yes F224 . C224 . C223 . 119.9(2) yes F224 . C224 . C225 . 120.6(2) yes C223 . C224 . C225 . 119.5(2) yes F225 . C225 . C220 . 120.7(2) yes F225 . C225 . C224 . 115.6(2) yes C220 . C225 . C224 . 123.8(2) yes C231 . C230 . C235 . 114.4(2) yes C231 . C230 . B201 . 125.4(2) yes C235 . C230 . B201 . 120.0(2) yes F231 . C231 . C230 . 122.2(2) yes F231 . C231 . C232 . 114.8(2) yes C230 . C231 . C232 . 123.0(2) yes F232 . C232 . C231 . 120.2(2) yes F232 . C232 . C233 . 119.9(2) yes C231 . C232 . C233 . 119.9(2) yes F233 . C233 . C232 . 119.9(2) yes F233 . C233 . C234 . 120.8(2) yes C232 . C233 . C234 . 119.3(2) yes F234 . C234 . C233 . 119.7(2) yes F234 . C234 . C235 . 121.3(2) yes C233 . C234 . C235 . 119.0(2) yes F235 . C235 . C230 . 119.2(2) yes F235 . C235 . C234 . 116.3(2) yes C230 . C235 . C234 . 124.5(2) yes C311 . C310 . C315 . 114.1(2) yes C311 . C310 . B301 . 127.1(2) yes C315 . C310 . B301 . 118.8(2) yes F311 . C311 . C310 . 120.7(2) yes F311 . C311 . C312 . 116.0(2) yes C310 . C311 . C312 . 123.4(2) yes F312 . C312 . C311 . 120.5(2) yes F312 . C312 . C313 . 119.5(2) yes C311 . C312 . C313 . 120.0(2) yes F313 . C313 . C312 . 120.6(3) yes F313 . C313 . C314 . 120.0(3) yes C312 . C313 . C314 . 119.3(2) yes F314 . C314 . C313 . 120.4(2) yes F314 . C314 . C315 . 120.7(3) yes C313 . C314 . C315 . 118.8(2) yes F315 . C315 . C310 . 120.1(2) yes F315 . C315 . C314 . 115.7(2) yes C310 . C315 . C314 . 124.2(2) yes C321 . C320 . C325 . 113.5(2) yes C321 . C320 . B301 . 120.0(2) yes C325 . C320 . B301 . 125.8(2) yes F321 . C321 . C320 . 119.2(2) yes F321 . C321 . C322 . 116.5(2) yes C320 . C321 . C322 . 124.3(2) yes F322 . C322 . C321 . 121.1(2) yes F322 . C322 . C323 . 119.8(2) yes C321 . C322 . C323 . 119.1(2) yes F323 . C323 . C322 . 120.1(3) yes F323 . C323 . C324 . 120.3(3) yes C322 . C323 . C324 . 119.5(2) yes F324 . C324 . C323 . 120.3(2) yes F324 . C324 . C325 . 120.1(2) yes C323 . C324 . C325 . 119.6(2) yes F325 . C325 . C320 . 120.8(2) yes F325 . C325 . C324 . 115.2(2) yes C320 . C325 . C324 . 124.0(2) yes C331 . C330 . C335 . 113.9(2) yes C331 . C330 . B301 . 119.0(2) yes C335 . C330 . B301 . 126.9(2) yes F331 . C331 . C330 . 118.6(2) yes F331 . C331 . C332 . 116.8(2) yes C330 . C331 . C332 . 124.7(2) yes F332 . C332 . C331 . 121.1(2) yes F332 . C332 . C333 . 119.9(2) yes C331 . C332 . C333 . 119.0(2) yes F333 . C333 . C332 . 120.4(3) yes F333 . C333 . C334 . 120.7(2) yes C332 . C333 . C334 . 118.9(2) yes F334 . C334 . C333 . 119.4(2) yes F334 . C334 . C335 . 120.3(2) yes C333 . C334 . C335 . 120.3(2) yes F335 . C335 . C330 . 121.4(2) yes F335 . C335 . C334 . 115.4(2) yes C330 . C335 . C334 . 123.2(2) yes O101 . B101 . C110 . 110.7(2) yes O101 . B101 . C120 . 106.1(2) yes C110 . B101 . C120 . 106.8(2) yes O101 . B101 . C130 . 104.2(2) yes C110 . B101 . C130 . 115.5(2) yes C120 . B101 . C130 . 113.2(2) yes O201 . B201 . C210 . 110.8(2) yes O201 . B201 . C220 . 106.4(2) yes C210 . B201 . C220 . 109.1(2) yes O201 . B201 . C230 . 103.0(2) yes C210 . B201 . C230 . 112.7(2) yes C220 . B201 . C230 . 114.5(2) yes O301 . B301 . C310 . 106.3(2) yes O301 . B301 . C320 . 102.2(2) yes C310 . B301 . C320 . 116.2(2) yes O301 . B301 . C330 . 110.4(2) yes C310 . B301 . C330 . 106.2(2) yes C320 . B301 . C330 . 115.1(2) yes #end data_CRYSTALS2 _audit_creation_date 98-02-03 _audit_creation_method CRYSTALS # mal31 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_author ; Linda H. Doerrer Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; _publ_contact_author_phone ' 01865 272 675 ' _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_coeditor_name 'P.P. Edwards ' _publ_contact_letter ; Please consider this CIF submission for publication as a Full Paper in Journal of the Chemical Society, Dalton Transactions. Full text and all other figures have been sent by post under separate cover. ; #============================================================================= # 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 ; 'Adducts of the Lewis Acid B(C6F5)3 with Transition Metal Oxo Compounds' ; # 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 'Barrado, Georgina' #<--'Last name, first name' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Green, Malcolm L. H.' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Doerrer, Linda H.' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Leech, Michael A.' ; Chemical Crystallography Laboratory 9 Parks Road OXFORD OX1 3PD ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. 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 Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (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. Otwinowski, Z. & Minor, W. (1996) DENZO - Processing of X-ray Diffraction data collected in oscillation mode. Methods in Enzymology (276). ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #========================================================================== # Now, all the strucure specific goodies #========================================================================== _computing_data_collection 'DIP2000 software (Enraf-Nonius)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO (Otwinowski & Minor, 1996) ; _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 'SHELXS86 (Sheldrick, 1986)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius DIP2020 ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment noref #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 11.300(1) _cell_angle_alpha 90 _cell_length_b 9.585(1) _cell_angle_beta 90.648(2) _cell_length_c 20.596(1) _cell_angle_gamma 90 _cell_volume 2230.62 _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' 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 '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' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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 ' C23 H5 Re1 O3 B1 F15 ' _chemical_formula_moiety ' C23 H5 Re1 O3 B1 F15 ' _chemical_compound_source ; ? ; _chemical_formula_weight 811.27 _cell_measurement_reflns_used 14286 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 26.69 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 2.42 _exptl_crystal_density_meas none _exptl_crystal_F_000 1522.69 _exptl_absorpt_coefficient_mu 5.67 _exptl_absorpt_correction_type none #_diffrn_standards_interval_time ? #_diffrn_standards_interval_count ? #_diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 4755 _reflns_number_total 4469 _diffrn_reflns_av_R_equivalents 0.037 _reflns_number_observed 3989 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.69 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -1.80 _refine_diff_density_max 1.80 _refine_ls_number_reflns 3989 _refine_ls_number_parameters 388 _refine_ls_R_factor_obs 0.0346 _refine_ls_wR_factor_obs 0.0362 _refine_ls_goodness_of_fit_obs 1.1246 _refine_ls_shift/esd_max 0.000104 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type RE1 0.56234(1) 0.28359(2) 0.209891(7) 0.0161 1.0000 Uani O2 0.6849(3) 0.1858(4) 0.2268(2) 0.0272 1.0000 Uani O3 0.4953(2) 0.3151(3) 0.2860(1) 0.0170 1.0000 Uani B4 0.5006(4) 0.3835(5) 0.3552(2) 0.0134 1.0000 Uani C5 0.3697(3) 0.3583(5) 0.3862(2) 0.0144 1.0000 Uani C6 0.3064(4) 0.2345(5) 0.3785(2) 0.0148 1.0000 Uani F7 0.3542(2) 0.1291(3) 0.3442(1) 0.0226 1.0000 Uani C8 0.1970(4) 0.2117(5) 0.4039(2) 0.0176 1.0000 Uani F9 0.1413(2) 0.0891(3) 0.3942(1) 0.0259 1.0000 Uani C10 0.1453(4) 0.3128(5) 0.4411(2) 0.0197 1.0000 Uani F11 0.0391(2) 0.2911(3) 0.4686(1) 0.0278 1.0000 Uani C12 0.2028(3) 0.4362(5) 0.4515(2) 0.0163 1.0000 Uani C13 0.3126(4) 0.4572(5) 0.4241(2) 0.0164 1.0000 Uani F14 0.3649(2) 0.5802(3) 0.4389(1) 0.0278 1.0000 Uani F15 0.1534(2) 0.5360(3) 0.4881(1) 0.0259 1.0000 Uani C16 0.5243(3) 0.5483(5) 0.3423(2) 0.0139 1.0000 Uani C17 0.6049(4) 0.6292(5) 0.3771(2) 0.0181 1.0000 Uani F18 0.6742(2) 0.5721(3) 0.4234(1) 0.0239 1.0000 Uani C19 0.6170(4) 0.7718(5) 0.3691(2) 0.0219 1.0000 Uani F20 0.6970(2) 0.8419(3) 0.4051(2) 0.0303 1.0000 Uani C21 0.5484(4) 0.8386(5) 0.3236(2) 0.0261 1.0000 Uani F22 0.5603(3) 0.9772(3) 0.3138(2) 0.0398 1.0000 Uani C23 0.4679(4) 0.7631(6) 0.2880(2) 0.0244 1.0000 Uani C24 0.4581(4) 0.6220(5) 0.2977(2) 0.0209 1.0000 Uani F25 0.3732(2) 0.5565(3) 0.2614(1) 0.0266 1.0000 Uani F26 0.3968(3) 0.8293(4) 0.2441(2) 0.0392 1.0000 Uani C27 0.6066(3) 0.2991(4) 0.3913(2) 0.0140 1.0000 Uani C28 0.5965(4) 0.2121(5) 0.4456(2) 0.0163 1.0000 Uani F29 0.4938(2) 0.2029(3) 0.4777(1) 0.0252 1.0000 Uani C30 0.6879(4) 0.1328(5) 0.4698(2) 0.0195 1.0000 Uani F31 0.6730(3) 0.0518(3) 0.5220(1) 0.0317 1.0000 Uani C32 0.7970(4) 0.1342(5) 0.4400(2) 0.0185 1.0000 Uani F33 0.8848(2) 0.0529(3) 0.4621(1) 0.0284 1.0000 Uani C34 0.8135(4) 0.2199(5) 0.3873(2) 0.0192 1.0000 Uani C35 0.7205(4) 0.3011(5) 0.3654(2) 0.0157 1.0000 Uani F36 0.7444(2) 0.3905(3) 0.3167(1) 0.0206 1.0000 Uani F37 0.9185(2) 0.2273(3) 0.3573(1) 0.0250 1.0000 Uani O1 0.6162(3) 0.4425(4) 0.1871(2) 0.0318 1.0000 Uani C39 0.5321(4) 0.1666(6) 0.1123(2) 0.0289 1.0000 Uani C40 0.4861(5) 0.0769(6) 0.1602(2) 0.0282 1.0000 Uani C41 0.3876(4) 0.1431(6) 0.1876(2) 0.0256 1.0000 Uani C42 0.3705(5) 0.2745(6) 0.1564(2) 0.0291 1.0000 Uani C43 0.4596(5) 0.2879(5) 0.1093(2) 0.0252 1.0000 Uani H391 0.6030 0.1487 0.0866 0.0289 1.0000 Uiso H401 0.5183 -0.0163 0.1715 0.0283 1.0000 Uiso H411 0.3373 0.1058 0.2233 0.0261 1.0000 Uiso H421 0.3094 0.3441 0.1651 0.0285 1.0000 Uiso H431 0.4698 0.3671 0.0791 0.0259 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 RE1 0.0153(1) 0.0182(1) 0.0149(1) -0.00131(7) 0.00301(6) -0.00170(7) O2 0.019(2) 0.026(2) 0.036(2) -0.007(1) 0.003(1) 0.004(1) O3 0.012(1) 0.020(2) 0.019(1) -0.007(1) 0.003(1) -0.001(1) B4 0.011(2) 0.012(2) 0.018(2) -0.000(2) 0.002(2) -0.001(2) C5 0.011(2) 0.020(2) 0.012(2) 0.004(2) -0.001(1) -0.002(2) C6 0.015(2) 0.016(2) 0.013(2) 0.001(1) 0.003(1) 0.000(2) F7 0.022(1) 0.016(1) 0.031(1) -0.006(1) 0.010(1) 0.001(1) C8 0.011(2) 0.023(2) 0.019(2) 0.001(2) -0.003(1) -0.004(2) F9 0.019(1) 0.025(2) 0.034(1) -0.004(1) 0.003(1) -0.011(1) C10 0.009(2) 0.035(3) 0.015(2) -0.000(2) 0.004(1) -0.004(2) F11 0.010(1) 0.049(2) 0.026(1) -0.008(1) 0.008(1) -0.008(1) C12 0.012(2) 0.024(2) 0.012(2) -0.004(2) -0.000(1) 0.007(2) C13 0.016(2) 0.018(2) 0.015(2) 0.000(2) 0.001(1) -0.003(2) F14 0.029(1) 0.021(2) 0.033(1) -0.011(1) 0.013(1) -0.010(1) F15 0.022(1) 0.030(2) 0.026(1) -0.008(1) 0.007(1) 0.008(1) C16 0.010(2) 0.016(2) 0.016(2) -0.000(1) 0.003(1) -0.001(1) C17 0.014(2) 0.020(2) 0.020(2) 0.001(2) 0.000(1) 0.001(2) F18 0.026(1) 0.019(1) 0.026(1) 0.001(1) -0.012(1) -0.004(1) C19 0.017(2) 0.021(3) 0.028(2) -0.006(2) 0.005(2) -0.004(2) F20 0.027(1) 0.019(2) 0.046(2) -0.010(1) 0.000(1) -0.008(1) C21 0.026(2) 0.016(2) 0.036(3) 0.006(2) 0.011(2) 0.002(2) F22 0.044(2) 0.012(2) 0.063(2) 0.008(1) 0.010(2) 0.001(1) C23 0.020(2) 0.026(3) 0.028(2) 0.010(2) 0.006(2) 0.006(2) C24 0.012(2) 0.026(3) 0.025(2) -0.000(2) 0.001(2) 0.000(2) F25 0.019(1) 0.031(2) 0.030(1) 0.000(1) -0.009(1) 0.004(1) F26 0.037(2) 0.034(2) 0.046(2) 0.019(1) -0.005(1) 0.013(1) C27 0.013(2) 0.015(2) 0.015(2) -0.003(1) -0.000(1) -0.000(1) C28 0.015(2) 0.017(2) 0.017(2) -0.002(2) 0.001(1) -0.005(2) F29 0.013(1) 0.036(2) 0.026(1) 0.013(1) 0.003(1) 0.000(1) C30 0.022(2) 0.014(2) 0.022(2) 0.003(2) -0.002(2) -0.003(2) F31 0.028(1) 0.035(2) 0.032(1) 0.018(1) -0.003(1) -0.002(1) C32 0.013(2) 0.015(2) 0.027(2) -0.003(2) -0.004(2) 0.002(2) F33 0.019(1) 0.026(2) 0.040(2) 0.005(1) -0.009(1) 0.009(1) C34 0.009(2) 0.026(3) 0.022(2) -0.006(2) -0.000(2) -0.001(2) C35 0.012(2) 0.019(2) 0.017(2) -0.000(2) -0.000(1) -0.004(1) F36 0.014(1) 0.025(2) 0.023(1) 0.006(1) 0.0038(9) -0.002(1) F37 0.011(1) 0.034(2) 0.030(1) -0.002(1) 0.002(1) 0.003(1) O1 0.039(2) 0.031(2) 0.026(2) -0.000(1) 0.005(1) -0.012(2) C39 0.028(2) 0.028(3) 0.032(3) -0.006(2) 0.001(2) 0.004(2) C40 0.038(3) 0.027(3) 0.019(2) -0.005(2) -0.011(2) -0.001(2) C41 0.024(2) 0.027(3) 0.026(2) -0.000(2) -0.001(2) -0.006(2) C42 0.032(3) 0.032(3) 0.024(2) -0.007(2) -0.009(2) 0.001(2) C43 0.033(3) 0.026(3) 0.016(2) -0.002(2) -0.003(2) -0.001(2) _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 RE1 . O2 . 1.705(3) yes RE1 . O3 . 1.776(3) yes RE1 . O1 . 1.708(4) yes RE1 . C39 . 2.324(5) yes RE1 . C40 . 2.386(5) yes RE1 . C43 . 2.364(5) yes O3 . B4 . 1.569(5) yes B4 . C5 . 1.635(5) yes B4 . C16 . 1.624(6) yes B4 . C27 . 1.619(6) yes C5 . C6 . 1.395(6) yes C5 . C13 . 1.391(6) yes C6 . F7 . 1.349(5) yes C6 . C8 . 1.365(6) yes C8 . F9 . 1.348(5) yes C8 . C10 . 1.369(6) yes C10 . F11 . 1.350(5) yes C10 . C12 . 1.365(7) yes C12 . C13 . 1.383(6) yes C12 . F15 . 1.344(5) yes C13 . F14 . 1.352(5) yes C16 . C17 . 1.390(6) yes C16 . C24 . 1.375(6) yes C17 . F18 . 1.343(5) yes C17 . C19 . 1.384(7) yes C19 . F20 . 1.343(5) yes C19 . C21 . 1.368(7) yes C21 . F22 . 1.351(6) yes C21 . C23 . 1.370(8) yes C23 . C24 . 1.372(7) yes C23 . F26 . 1.359(5) yes C24 . F25 . 1.362(5) yes C27 . C28 . 1.401(6) yes C27 . C35 . 1.399(6) yes C28 . F29 . 1.345(5) yes C28 . C30 . 1.372(6) yes C30 . F31 . 1.337(5) yes C30 . C32 . 1.384(6) yes C32 . F33 . 1.337(5) yes C32 . C34 . 1.375(7) yes C34 . C35 . 1.379(6) yes C34 . F37 . 1.346(5) yes C35 . F36 . 1.350(5) yes C39 . C40 . 1.411(7) yes C39 . C43 . 1.423(7) yes C39 . H391 . 0.980(5) no C40 . C41 . 1.406(7) yes C40 . H401 . 0.992(5) no C41 . C42 . 1.425(8) yes C41 . H411 . 1.002(5) no C42 . C43 . 1.412(7) yes C42 . H421 . 0.978(5) no C43 . H431 . 0.990(5) 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 O2 . RE1 . O3 . 105.5(2) yes O2 . RE1 . O1 . 104.8(2) yes O3 . RE1 . O1 . 104.3(2) yes O2 . RE1 . C39 . 91.3(2) yes O3 . RE1 . C39 . 141.8(2) yes O1 . RE1 . C39 . 104.0(2) yes O2 . RE1 . C40 . 85.4(2) yes O3 . RE1 . C40 . 111.4(2) yes O1 . RE1 . C40 . 138.6(2) yes C39 . RE1 . C40 . 34.8(2) yes O2 . RE1 . C43 . 125.3(2) yes O3 . RE1 . C43 . 124.1(2) yes O1 . RE1 . C43 . 85.2(2) yes C39 . RE1 . C43 . 35.3(2) yes C40 . RE1 . C43 . 57.8(2) yes RE1 . O3 . B4 . 149.4(2) yes O3 . B4 . C5 . 105.5(3) yes O3 . B4 . C16 . 105.3(3) yes C5 . B4 . C16 . 111.0(3) yes O3 . B4 . C27 . 103.2(3) yes C5 . B4 . C27 . 114.5(3) yes C16 . B4 . C27 . 116.0(3) yes B4 . C5 . C6 . 123.1(4) yes B4 . C5 . C13 . 123.1(4) yes C6 . C5 . C13 . 113.8(4) yes C5 . C6 . F7 . 119.3(4) yes C5 . C6 . C8 . 123.9(4) yes F7 . C6 . C8 . 116.8(4) yes C6 . C8 . F9 . 120.4(4) yes C6 . C8 . C10 . 119.7(4) yes F9 . C8 . C10 . 119.9(4) yes C8 . C10 . F11 . 120.9(4) yes C8 . C10 . C12 . 119.7(4) yes F11 . C10 . C12 . 119.4(4) yes C10 . C12 . C13 . 119.3(4) yes C10 . C12 . F15 . 120.3(4) yes C13 . C12 . F15 . 120.4(4) yes C5 . C13 . C12 . 123.6(4) yes C5 . C13 . F14 . 121.1(4) yes C12 . C13 . F14 . 115.2(4) yes B4 . C16 . C17 . 124.5(4) yes B4 . C16 . C24 . 121.3(4) yes C17 . C16 . C24 . 114.0(4) yes C16 . C17 . F18 . 120.8(4) yes C16 . C17 . C19 . 123.7(4) yes F18 . C17 . C19 . 115.5(4) yes C17 . C19 . F20 . 119.6(4) yes C17 . C19 . C21 . 119.2(4) yes F20 . C19 . C21 . 121.2(5) yes C19 . C21 . F22 . 120.4(5) yes C19 . C21 . C23 . 119.2(5) yes F22 . C21 . C23 . 120.5(5) yes C21 . C23 . C24 . 119.8(4) yes C21 . C23 . F26 . 119.6(5) yes C24 . C23 . F26 . 120.6(5) yes C16 . C24 . C23 . 124.1(4) yes C16 . C24 . F25 . 120.2(4) yes C23 . C24 . F25 . 115.6(4) yes B4 . C27 . C28 . 126.7(4) yes B4 . C27 . C35 . 119.8(4) yes C28 . C27 . C35 . 113.3(4) yes C27 . C28 . F29 . 120.7(4) yes C27 . C28 . C30 . 123.5(4) yes F29 . C28 . C30 . 115.8(4) yes C28 . C30 . F31 . 120.8(4) yes C28 . C30 . C32 . 120.3(4) yes F31 . C30 . C32 . 118.9(4) yes C30 . C32 . F33 . 120.3(4) yes C30 . C32 . C34 . 119.0(4) yes F33 . C32 . C34 . 120.7(4) yes C32 . C34 . C35 . 119.1(4) yes C32 . C34 . F37 . 121.5(4) yes C35 . C34 . F37 . 119.4(4) yes C27 . C35 . C34 . 124.6(4) yes C27 . C35 . F36 . 119.0(4) yes C34 . C35 . F36 . 116.4(4) yes RE1 . C39 . C40 . 75.0(3) yes RE1 . C39 . C43 . 73.9(3) yes C40 . C39 . C43 . 108.1(4) yes RE1 . C39 . H391 . 115.9(4) no C40 . C39 . H391 . 125.4(5) no C43 . C39 . H391 . 126.4(5) no RE1 . C40 . C39 . 70.2(3) yes RE1 . C40 . C41 . 74.7(3) yes C39 . C40 . C41 . 107.8(5) yes RE1 . C40 . H401 . 121.2(3) no C39 . C40 . H401 . 125.2(5) no C41 . C40 . H401 . 127.0(5) no C40 . C41 . C42 . 108.8(4) yes C40 . C41 . H411 . 126.3(5) no C42 . C41 . H411 . 124.9(5) no C41 . C42 . C43 . 107.2(4) yes C41 . C42 . H421 . 127.9(5) no C43 . C42 . H421 . 125.0(5) no RE1 . C43 . C39 . 70.8(3) yes RE1 . C43 . C42 . 75.1(3) yes C39 . C43 . C42 . 108.1(4) yes RE1 . C43 . H431 . 120.3(4) no C39 . C43 . H431 . 125.7(5) no C42 . C43 . H431 . 126.2(5) no #end data_CRYSTALS3 _audit_creation_date 98-01-22 _audit_creation_method CRYSTALS # mal67 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS # 1. SUBMISSION DETAILS _publ_contact_author ; Linda H. Doerrer Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; _publ_contact_author_phone ' 01865 272 675 ' _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_coeditor_name 'P.P. Edwards ' _publ_contact_letter ; Please consider this CIF submission for publication as a Full Paper in Journal of the Chemical Society, Dalton Transactions. Full text and all other figures have been sent by post under separate cover. ; #============================================================================= # 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 ; 'Adducts of the Lewis Acid B(C6F5)3 with Transition Metal Oxo Compounds' ; # 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 'Barrado, Georgina' #<--'Last name, first name' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Green, Malcolm L. H.' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Doerrer, Linda H.' ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; 'Leech, Michael A.' ; Chemical Crystallography Laboratory 9 Parks Road OXFORD OX1 3PD ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. 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 Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (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. Otwinowski, Z. & Minor, W. (1996) DENZO - Processing of X-ray Diffraction data collected in oscillation mode. Methods in Enzymology (276). ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #========================================================================== # Now, all the strucure specific goodies #========================================================================== _computing_data_collection 'DIP2000 software (Enraf-Nonius)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO (Otwinowski & Minor, 1996) ; _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 'SHELXS86 (Sheldrick, 1986)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius DIP2020 ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment noref #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 13.289(1) _cell_angle_alpha 90 _cell_length_b 14.028(1) _cell_angle_beta 110.256(3) _cell_length_c 18.270(1) _cell_angle_gamma 90 _cell_volume 3195.22 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' 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' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' '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' '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' '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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C56 H46 W2 O6 B2 F30 Cl4 N6 ' _chemical_formula_moiety ' C56 H46 W2 O6 B2 F30 Cl4 N6 ' _chemical_compound_source ; ? ; _chemical_formula_weight 2000.10 _cell_measurement_reflns_used 22644 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 26.72 _cell_measurement_temperature 100 _cell_formula_units_Z 2 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 2.08 _exptl_crystal_density_meas none _exptl_crystal_F_000 1932.41 _exptl_absorpt_coefficient_mu 3.98 _exptl_absorpt_correction_type none #_diffrn_standards_interval_time ? #_diffrn_standards_interval_count ? #_diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 100 _diffrn_reflns_number 22644 _reflns_number_total 6588 _diffrn_reflns_av_R_equivalents 0.019 _reflns_number_observed 6469 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.72 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.92 _refine_diff_density_max 0.73 _refine_ls_number_reflns 6469 _refine_ls_number_parameters 956 _refine_ls_R_factor_obs 0.0189 _refine_ls_wR_factor_obs 0.0220 _refine_ls_goodness_of_fit_obs 1.0705 _refine_ls_shift/esd_max 0.009219 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type W1 0.09731(1) 0.39143(3) 0.496283(9) 0.0092 1.0000 Uani O2 0.2443(2) 0.3739(2) 0.5359(2) 0.0127 1.0000 Uani B3 0.3310(4) 0.3180(4) 0.5205(3) 0.0129 1.0000 Uani C4 0.2900(4) 0.3002(4) 0.4259(3) 0.0145 1.0000 Uani C5 0.3206(4) 0.3561(3) 0.3732(3) 0.0157 1.0000 Uani F6 0.3949(2) 0.4255(2) 0.4002(2) 0.0209 1.0000 Uani C7 0.2790(4) 0.3457(3) 0.2937(3) 0.0174 1.0000 Uani F8 0.3141(2) 0.4017(2) 0.2474(2) 0.0233 1.0000 Uani C9 0.2006(4) 0.2781(3) 0.2602(3) 0.0193 1.0000 Uani C10 0.1662(4) 0.2216(3) 0.3094(3) 0.0166 1.0000 Uani C11 0.2083(4) 0.2361(3) 0.3877(3) 0.0141 1.0000 Uani F12 0.1651(2) 0.1829(2) 0.4320(2) 0.0165 1.0000 Uani F13 0.0896(2) 0.1565(2) 0.2787(2) 0.0235 1.0000 Uani F14 0.1592(2) 0.2677(2) 0.1830(2) 0.0266 1.0000 Uani C15 0.4523(4) 0.3680(3) 0.5542(3) 0.0141 1.0000 Uani C16 0.4841(4) 0.4484(3) 0.5995(3) 0.0168 1.0000 Uani F17 0.4111(2) 0.5034(2) 0.6158(2) 0.0222 1.0000 Uani C18 0.5899(4) 0.4784(3) 0.6321(3) 0.0176 1.0000 Uani F19 0.6140(2) 0.5578(2) 0.6742(2) 0.0299 1.0000 Uani C20 0.6697(4) 0.4269(4) 0.6188(3) 0.0200 1.0000 Uani F21 0.7723(2) 0.4564(2) 0.6491(2) 0.0248 1.0000 Uani C22 0.6436(4) 0.3469(3) 0.5724(3) 0.0179 1.0000 Uani C23 0.5375(4) 0.3202(3) 0.5410(3) 0.0168 1.0000 Uani F24 0.5166(2) 0.2407(2) 0.4957(2) 0.0236 1.0000 Uani F25 0.7198(2) 0.2976(2) 0.5562(2) 0.0270 1.0000 Uani C26 0.3528(3) 0.2196(3) 0.5751(3) 0.0126 1.0000 Uani C27 0.3742(4) 0.2304(3) 0.6552(3) 0.0138 1.0000 Uani F28 0.3733(2) 0.3180(2) 0.6854(2) 0.0165 1.0000 Uani C29 0.3998(4) 0.1575(4) 0.7084(3) 0.0168 1.0000 Uani F30 0.4174(2) 0.1733(2) 0.7846(2) 0.0214 1.0000 Uani C31 0.4068(4) 0.0646(4) 0.6827(3) 0.0178 1.0000 Uani F32 0.4295(2) -0.0089(2) 0.7327(2) 0.0238 1.0000 Uani C33 0.3910(4) 0.0505(3) 0.6056(3) 0.0161 1.0000 Uani C34 0.3659(4) 0.1270(3) 0.5540(3) 0.0140 1.0000 Uani F35 0.3545(2) 0.1045(2) 0.4796(2) 0.0179 1.0000 Uani F36 0.3958(2) -0.0385(2) 0.5793(2) 0.0195 1.0000 Uani O37 0.0397(3) 0.2981(2) 0.5271(2) 0.0165 1.0000 Uani O38 0.0638(2) 0.3790(2) 0.3971(2) 0.0145 1.0000 Uani W39 -0.40643(1) 0.02854(3) 0.001792(9) 0.0096 1.0000 Uani O40 -0.2601(2) 0.0476(2) 0.0488(2) 0.0132 1.0000 Uani B41 -0.1674(4) 0.1010(4) 0.0379(3) 0.0150 1.0000 Uani C42 -0.0499(3) 0.0469(3) 0.0787(3) 0.0163 1.0000 Uani C43 -0.0252(4) -0.0329(3) 0.1260(3) 0.0174 1.0000 Uani F44 -0.1035(2) -0.0820(2) 0.1419(2) 0.0223 1.0000 Uani C45 0.0767(4) -0.0703(4) 0.1598(3) 0.0255 1.0000 Uani F46 0.0942(3) -0.1489(2) 0.2050(2) 0.0349 1.0000 Uani C47 0.1620(4) -0.0258(4) 0.1476(3) 0.0245 1.0000 Uani F48 0.2620(2) -0.0616(2) 0.1796(2) 0.0341 1.0000 Uani C49 0.1433(4) 0.0556(4) 0.1031(3) 0.0232 1.0000 Uani C50 0.0406(4) 0.0899(3) 0.0715(3) 0.0168 1.0000 Uani F51 0.0288(2) 0.1713(2) 0.0296(2) 0.0226 1.0000 Uani F52 0.2261(2) 0.1009(2) 0.0909(2) 0.0275 1.0000 Uani C53 -0.1499(3) 0.2013(3) 0.0886(3) 0.0120 1.0000 Uani C54 -0.1339(4) 0.2932(4) 0.0655(3) 0.0161 1.0000 Uani F55 -0.1336(2) 0.3114(2) -0.0067(2) 0.0178 1.0000 Uani C56 -0.1158(4) 0.3718(3) 0.1148(3) 0.0151 1.0000 Uani F57 -0.1064(2) 0.4589(2) 0.0871(2) 0.0198 1.0000 Uani C58 -0.1109(4) 0.3617(3) 0.1901(3) 0.0157 1.0000 Uani F59 -0.0951(2) 0.4384(2) 0.2370(2) 0.0229 1.0000 Uani C60 -0.1220(4) 0.2717(3) 0.2176(3) 0.0150 1.0000 Uani C61 -0.1413(3) 0.1963(3) 0.1665(3) 0.0144 1.0000 Uani F62 -0.1451(2) 0.1088(2) 0.1992(2) 0.0163 1.0000 Uani F63 -0.1148(2) 0.2578(2) 0.2918(2) 0.0206 1.0000 Uani C64 -0.1967(4) 0.1149(3) -0.0564(3) 0.0143 1.0000 Uani C65 -0.2735(4) 0.1814(4) -0.0990(3) 0.0159 1.0000 Uani F66 -0.3253(2) 0.2334(2) -0.0611(2) 0.0175 1.0000 Uani C67 -0.3034(4) 0.1956(4) -0.1782(3) 0.0208 1.0000 Uani F68 -0.3789(2) 0.2606(2) -0.2149(2) 0.0275 1.0000 Uani C69 -0.2558(4) 0.1420(4) -0.2204(3) 0.0248 1.0000 Uani C70 -0.1813(4) 0.0739(4) -0.1820(3) 0.0237 1.0000 Uani C71 -0.1554(4) 0.0610(4) -0.1037(3) 0.0188 1.0000 Uani F72 -0.0859(2) -0.0116(2) -0.0718(2) 0.0255 1.0000 Uani F73 -0.1345(2) 0.0205(3) -0.2232(2) 0.0331 1.0000 Uani F74 -0.2825(3) 0.1555(3) -0.2977(2) 0.0369 1.0000 Uani O75 -0.4287(2) 0.0430(3) -0.0960(2) 0.0165 1.0000 Uani O76 -0.4650(3) 0.1311(2) 0.0269(2) 0.0174 1.0000 Uani CL77 -0.17375(9) 0.67568(9) 0.23670(7) 0.0240 1.0000 Uani C78 -0.0573(4) 0.6729(5) 0.2109(3) 0.0313 1.0000 Uani CL79 -0.0859(1) 0.68499(9) 0.11050(8) 0.0284 1.0000 Uani CL80 0.57790(9) 0.70076(9) 0.78094(7) 0.0236 1.0000 Uani C81 0.4793(5) 0.7502(4) 0.6987(3) 0.0325 1.0000 Uani CL82 0.3519(1) 0.7531(1) 0.70992(9) 0.0315 1.0000 Uani N83 -0.5759(3) -0.0356(3) -0.0352(2) 0.0133 1.0000 Uani C84 -0.6492(3) 0.0240(4) -0.0991(3) 0.0169 1.0000 Uani C85 -0.6112(4) -0.0303(4) 0.0343(3) 0.0139 1.0000 Uani C86 -0.5296(4) -0.0780(3) 0.1039(3) 0.0175 1.0000 Uani N87 -0.4193(3) -0.0447(3) 0.1126(2) 0.0138 1.0000 Uani C88 -0.3422(4) -0.1265(3) 0.1284(3) 0.0175 1.0000 Uani C89 -0.3667(4) -0.1896(3) 0.0573(3) 0.0167 1.0000 Uani N90 -0.3824(3) -0.1306(2) -0.0145(2) 0.0125 1.0000 Uani C91 -0.4791(4) -0.1615(3) -0.0800(3) 0.0136 1.0000 Uani C92 -0.5800(4) -0.1376(3) -0.0627(3) 0.0155 1.0000 Uani C93 -0.2864(4) -0.1422(3) -0.0393(3) 0.0173 1.0000 Uani C94 -0.3829(3) 0.0242(4) 0.1792(3) 0.0165 1.0000 Uani C95 0.1530(4) 0.6160(3) 0.5462(3) 0.0158 1.0000 Uani C96 0.1818(4) 0.5537(3) 0.6194(3) 0.0152 1.0000 Uani N97 0.1025(3) 0.4760(3) 0.6090(2) 0.0124 1.0000 Uani C98 0.1407(4) 0.4080(4) 0.6752(3) 0.0199 1.0000 Uani C99 -0.0042(4) 0.5152(3) 0.6060(3) 0.0151 1.0000 Uani C100 -0.0936(4) 0.4691(4) 0.5413(3) 0.0152 1.0000 Uani N101 -0.0674(3) 0.4688(3) 0.4674(3) 0.0132 1.0000 Uani C102 -0.0699(4) 0.5687(4) 0.4373(3) 0.0167 1.0000 Uani C103 0.0260(4) 0.5879(4) 0.4130(3) 0.0161 1.0000 Uani N104 0.1276(3) 0.5549(3) 0.4748(2) 0.0127 1.0000 Uani C105 0.2150(4) 0.5596(3) 0.4418(3) 0.0181 1.0000 Uani C106 -0.1479(4) 0.4103(4) 0.4086(3) 0.0186 1.0000 Uani H841 -0.6260 0.0210 -0.1459 0.0153 1.0000 Uiso H842 -0.7241 0.0005 -0.1134 0.0153 1.0000 Uiso H843 -0.6454 0.0922 -0.0813 0.0153 1.0000 Uiso H851 -0.6815 -0.0624 0.0226 0.0141 1.0000 Uiso H852 -0.6176 0.0385 0.0477 0.0141 1.0000 Uiso H861 -0.5453 -0.0614 0.1523 0.0179 1.0000 Uiso H862 -0.5341 -0.1484 0.0962 0.0179 1.0000 Uiso H881 -0.3487 -0.1643 0.1733 0.0172 1.0000 Uiso H882 -0.2677 -0.1005 0.1433 0.0172 1.0000 Uiso H891 -0.4328 -0.2269 0.0511 0.0122 1.0000 Uiso H892 -0.3048 -0.2337 0.0652 0.0122 1.0000 Uiso H911 -0.4759 -0.2316 -0.0872 0.0133 1.0000 Uiso H912 -0.4811 -0.1277 -0.1286 0.0133 1.0000 Uiso H921 -0.6438 -0.1463 -0.1109 0.0135 1.0000 Uiso H922 -0.5853 -0.1806 -0.0207 0.0135 1.0000 Uiso H931 -0.2967 -0.1035 -0.0874 0.0144 1.0000 Uiso H932 -0.2780 -0.2108 -0.0505 0.0144 1.0000 Uiso H933 -0.2210 -0.1197 0.0036 0.0144 1.0000 Uiso H941 -0.3090 0.0471 0.1853 0.0156 1.0000 Uiso H942 -0.3819 -0.0081 0.2279 0.0156 1.0000 Uiso H943 -0.4330 0.0798 0.1679 0.0156 1.0000 Uiso H951 0.0894 0.6560 0.5431 0.0152 1.0000 Uiso H952 0.2156 0.6583 0.5509 0.0152 1.0000 Uiso H961 0.1823 0.5938 0.6652 0.0140 1.0000 Uiso H962 0.2543 0.5251 0.6305 0.0140 1.0000 Uiso H981 0.0868 0.3556 0.6675 0.0186 1.0000 Uiso H982 0.1498 0.4420 0.7250 0.0186 1.0000 Uiso H983 0.2108 0.3802 0.6771 0.0186 1.0000 Uiso H991 -0.0138 0.5013 0.6571 0.0150 1.0000 Uiso H992 -0.0050 0.5853 0.5977 0.0150 1.0000 Uiso H1001 -0.1610 0.5059 0.5324 0.0155 1.0000 Uiso H1002 -0.1031 0.4021 0.5557 0.0155 1.0000 Uiso H1021 -0.0689 0.6142 0.4797 0.0136 1.0000 Uiso H1022 -0.1366 0.5779 0.3914 0.0136 1.0000 Uiso H1031 0.0313 0.6581 0.4051 0.0133 1.0000 Uiso H1032 0.0170 0.5535 0.3635 0.0133 1.0000 Uiso H1051 0.1962 0.5183 0.3945 0.0199 1.0000 Uiso H1052 0.2246 0.6267 0.4279 0.0199 1.0000 Uiso H1053 0.2832 0.5359 0.4819 0.0199 1.0000 Uiso H1061 -0.1320 0.4097 0.3587 0.0170 1.0000 Uiso H1062 -0.2210 0.4381 0.3982 0.0170 1.0000 Uiso H1063 -0.1458 0.3440 0.4284 0.0170 1.0000 Uiso H781 -0.0088 0.7275 0.2387 0.0275 1.0000 Uiso H782 -0.0184 0.6117 0.2293 0.0275 1.0000 Uiso H811 0.5011 0.8173 0.6910 0.0341 1.0000 Uiso H812 0.4745 0.7115 0.6516 0.0341 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 0.00930(8) 0.00712(9) 0.01140(9) -0.00047(6) 0.00392(7) 0.00037(6) O2 0.010(1) 0.013(2) 0.016(2) -0.001(1) 0.006(1) -0.000(1) B3 0.012(2) 0.009(2) 0.016(3) 0.002(2) 0.002(2) 0.002(2) C4 0.012(2) 0.017(2) 0.014(2) -0.003(2) 0.004(2) 0.002(2) C5 0.015(2) 0.013(2) 0.022(3) -0.001(2) 0.011(2) -0.000(2) F6 0.019(1) 0.020(1) 0.022(2) 0.003(1) 0.005(1) -0.006(1) C7 0.021(2) 0.017(2) 0.016(2) 0.005(2) 0.009(2) 0.005(2) F8 0.029(1) 0.025(1) 0.022(2) 0.009(1) 0.016(1) 0.004(1) C9 0.022(2) 0.020(2) 0.018(3) -0.001(2) 0.009(2) 0.007(2) C10 0.012(2) 0.018(2) 0.017(2) -0.003(2) 0.002(2) 0.003(2) C11 0.014(2) 0.014(2) 0.017(2) 0.003(2) 0.008(2) 0.003(2) F12 0.018(1) 0.015(1) 0.017(1) 0.001(1) 0.007(1) -0.004(1) F13 0.019(1) 0.024(2) 0.023(2) -0.004(1) 0.001(1) -0.003(1) F14 0.031(1) 0.033(2) 0.013(1) -0.001(1) 0.005(1) 0.004(1) C15 0.014(2) 0.013(2) 0.015(2) 0.003(1) 0.005(2) 0.002(1) C16 0.015(2) 0.021(2) 0.015(2) 0.002(2) 0.006(2) 0.002(2) F17 0.017(1) 0.021(1) 0.031(2) -0.011(1) 0.011(1) -0.002(1) C18 0.020(2) 0.016(2) 0.018(2) -0.005(2) 0.008(2) -0.006(2) F19 0.023(1) 0.030(2) 0.035(2) -0.019(1) 0.009(1) -0.011(1) C20 0.009(2) 0.024(2) 0.026(3) 0.005(2) 0.005(2) -0.002(2) F21 0.012(1) 0.033(2) 0.026(2) -0.003(1) 0.003(1) -0.007(1) C22 0.015(2) 0.022(2) 0.019(2) 0.006(2) 0.007(2) 0.002(2) C23 0.017(2) 0.011(2) 0.024(3) -0.000(2) 0.010(2) -0.001(2) F24 0.020(1) 0.016(1) 0.036(2) -0.010(1) 0.011(1) -0.001(1) F25 0.018(1) 0.024(1) 0.043(2) -0.004(1) 0.015(1) 0.002(1) C26 0.006(2) 0.019(2) 0.010(2) 0.001(2) 0.000(2) 0.000(2) C27 0.015(2) 0.007(2) 0.021(2) -0.002(2) 0.009(2) -0.000(2) F28 0.022(1) 0.011(1) 0.016(1) -0.002(1) 0.005(1) 0.001(1) C29 0.018(2) 0.021(2) 0.010(2) 0.000(2) 0.002(2) 0.001(2) F30 0.027(1) 0.022(1) 0.016(1) 0.001(1) 0.008(1) -0.000(1) C31 0.014(2) 0.015(2) 0.024(3) 0.004(2) 0.006(2) -0.000(2) F32 0.031(2) 0.014(1) 0.023(2) 0.007(1) 0.005(1) 0.003(1) C33 0.010(2) 0.016(3) 0.021(3) -0.001(2) 0.004(2) 0.001(2) C34 0.016(2) 0.011(2) 0.018(2) -0.002(2) 0.009(2) 0.001(2) F35 0.021(1) 0.016(1) 0.017(1) -0.003(1) 0.007(1) 0.003(1) F36 0.020(1) 0.012(1) 0.028(2) -0.002(1) 0.010(1) 0.003(1) O37 0.018(2) 0.009(2) 0.024(2) -0.000(1) 0.010(1) 0.001(1) O38 0.013(1) 0.015(2) 0.014(2) -0.001(1) 0.003(1) 0.002(1) W39 0.00972(9) 0.00736(9) 0.01161(9) -0.00007(6) 0.00354(7) -0.00028(6) O40 0.014(1) 0.010(2) 0.015(2) -0.003(1) 0.005(1) -0.004(1) B41 0.012(2) 0.018(3) 0.016(3) -0.002(2) 0.005(2) -0.000(2) C42 0.013(2) 0.017(2) 0.017(2) -0.003(2) 0.004(2) -0.001(2) C43 0.014(2) 0.015(2) 0.022(3) -0.003(2) 0.005(2) 0.001(2) F44 0.018(1) 0.018(1) 0.028(2) 0.006(1) 0.005(1) -0.001(1) C45 0.019(2) 0.017(2) 0.035(3) -0.001(2) 0.002(2) 0.003(2) F46 0.025(2) 0.023(2) 0.048(2) 0.010(1) 0.000(1) 0.005(1) C47 0.011(2) 0.027(3) 0.032(3) -0.007(2) 0.004(2) 0.004(2) F48 0.014(1) 0.033(2) 0.048(2) 0.000(1) 0.002(1) 0.009(1) C49 0.016(2) 0.026(3) 0.031(3) -0.009(2) 0.013(2) -0.002(2) C50 0.018(2) 0.018(2) 0.016(2) -0.005(2) 0.007(2) 0.001(2) F51 0.018(1) 0.027(2) 0.025(2) 0.003(1) 0.010(1) -0.003(1) F52 0.013(1) 0.034(2) 0.038(2) -0.003(1) 0.011(1) -0.003(1) C53 0.010(2) 0.010(2) 0.016(2) -0.001(2) 0.006(2) -0.001(2) C54 0.014(2) 0.025(3) 0.008(2) -0.003(2) 0.002(2) -0.001(2) F55 0.021(1) 0.017(1) 0.018(1) 0.001(1) 0.009(1) -0.003(1) C56 0.012(2) 0.008(3) 0.028(3) 0.001(2) 0.011(2) -0.003(2) F57 0.023(2) 0.012(1) 0.025(2) 0.002(1) 0.009(1) -0.001(1) C58 0.017(2) 0.013(2) 0.015(3) -0.008(2) 0.003(2) -0.004(2) F59 0.030(1) 0.014(1) 0.024(2) -0.008(1) 0.008(1) -0.002(1) C60 0.019(2) 0.014(2) 0.014(2) -0.003(2) 0.008(2) 0.001(2) C61 0.008(2) 0.015(2) 0.017(2) -0.002(2) -0.001(2) 0.000(2) F62 0.022(1) 0.011(1) 0.015(1) 0.001(1) 0.006(1) -0.003(1) F63 0.028(1) 0.018(1) 0.015(1) -0.004(1) 0.007(1) -0.003(1) C64 0.013(2) 0.014(2) 0.017(2) -0.005(2) 0.007(2) -0.003(2) C65 0.018(2) 0.018(2) 0.013(2) -0.002(2) 0.007(2) -0.004(2) F66 0.017(1) 0.018(1) 0.018(1) -0.001(1) 0.007(1) 0.002(1) C67 0.021(2) 0.023(2) 0.018(3) 0.004(2) 0.006(2) -0.004(2) F68 0.029(2) 0.027(2) 0.020(2) 0.009(1) 0.001(1) -0.003(1) C69 0.034(3) 0.031(3) 0.008(2) -0.000(2) 0.007(2) -0.010(2) C70 0.023(2) 0.030(3) 0.026(3) -0.014(2) 0.018(2) -0.010(2) C71 0.013(2) 0.027(3) 0.016(3) -0.009(2) 0.004(2) -0.005(2) F72 0.019(1) 0.030(2) 0.028(2) -0.010(1) 0.008(1) 0.004(1) F73 0.033(2) 0.046(2) 0.029(2) -0.022(2) 0.022(1) -0.014(2) F74 0.048(2) 0.050(2) 0.015(2) -0.003(1) 0.013(2) -0.012(2) O75 0.014(1) 0.015(2) 0.020(2) 0.005(1) 0.005(1) -0.002(1) O76 0.014(1) 0.013(2) 0.024(2) -0.000(1) 0.006(1) 0.001(1) CL77 0.0237(5) 0.0257(6) 0.0235(6) -0.0012(4) 0.0091(5) 0.0035(4) C78 0.023(2) 0.044(3) 0.027(3) 0.009(2) 0.009(2) 0.006(2) CL79 0.0401(7) 0.0232(6) 0.0266(7) 0.0016(4) 0.0174(6) 0.0057(5) CL80 0.0225(5) 0.0250(5) 0.0241(6) -0.0041(4) 0.0092(5) 0.0002(4) C81 0.031(3) 0.034(3) 0.032(3) 0.003(2) 0.011(2) -0.001(2) CL82 0.0196(5) 0.0275(6) 0.0434(8) 0.0041(5) 0.0060(5) -0.0027(5) N83 0.014(2) 0.013(2) 0.012(2) -0.000(1) 0.003(2) -0.002(2) C84 0.010(2) 0.017(2) 0.019(2) 0.009(2) -0.001(2) 0.005(2) C85 0.012(2) 0.013(2) 0.020(3) 0.002(2) 0.009(2) -0.001(2) C86 0.018(2) 0.021(2) 0.017(2) 0.000(2) 0.011(2) -0.006(2) N87 0.012(2) 0.014(2) 0.013(2) -0.002(1) 0.002(1) -0.003(1) C88 0.022(2) 0.014(2) 0.018(2) 0.001(2) 0.008(2) -0.003(2) C89 0.022(2) 0.013(2) 0.011(2) 0.005(2) -0.000(2) 0.005(2) N90 0.014(2) 0.008(2) 0.013(2) -0.003(1) 0.001(2) -0.001(1) C91 0.017(2) 0.008(2) 0.013(2) -0.002(2) 0.001(2) -0.002(2) C92 0.017(2) 0.016(2) 0.012(2) -0.000(2) 0.002(2) -0.003(2) C93 0.018(2) 0.016(2) 0.017(3) -0.003(2) 0.004(2) 0.001(2) C94 0.019(2) 0.017(2) 0.013(2) -0.008(2) 0.006(2) -0.005(2) C95 0.019(2) 0.013(2) 0.015(2) -0.000(2) 0.007(2) 0.003(2) C96 0.014(2) 0.015(2) 0.014(2) -0.005(2) 0.001(2) -0.003(2) N97 0.010(2) 0.012(2) 0.015(2) -0.000(1) 0.005(1) 0.001(1) C98 0.023(2) 0.023(3) 0.014(2) 0.005(2) 0.007(2) 0.004(2) C99 0.016(2) 0.015(2) 0.016(2) -0.000(2) 0.007(2) 0.004(2) C100 0.012(2) 0.014(2) 0.022(3) 0.002(2) 0.009(2) 0.002(2) N101 0.012(2) 0.012(2) 0.017(2) -0.004(1) 0.007(2) -0.001(1) C102 0.018(2) 0.012(2) 0.017(3) 0.002(2) 0.002(2) 0.005(2) C103 0.019(2) 0.015(2) 0.013(2) 0.004(2) 0.004(2) 0.004(2) N104 0.013(2) 0.013(2) 0.014(2) -0.001(1) 0.007(2) -0.001(1) C105 0.020(2) 0.018(2) 0.020(3) 0.004(2) 0.012(2) -0.002(2) C106 0.014(2) 0.018(3) 0.024(3) -0.006(2) 0.007(2) 0.001(2) _refine_ls_extinction_coef 52.5(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 . O2 . 1.850(3) yes W1 . O37 . 1.708(3) yes W1 . O38 . 1.719(3) yes W1 . N97 . 2.357(4) yes W1 . N101 . 2.334(4) yes W1 . N104 . 2.384(4) yes O2 . B3 . 1.499(5) yes B3 . C4 . 1.642(7) yes B3 . C15 . 1.668(7) yes B3 . C26 . 1.668(7) yes C4 . C5 . 1.406(6) yes C4 . C11 . 1.395(7) yes C5 . F6 . 1.353(5) yes C5 . C7 . 1.372(7) yes C7 . F8 . 1.349(5) yes C7 . C9 . 1.384(7) yes C9 . C10 . 1.388(7) yes C9 . F14 . 1.334(6) yes C10 . C11 . 1.360(7) yes C10 . F13 . 1.338(5) yes C11 . F12 . 1.365(5) yes C15 . C16 . 1.376(6) yes C15 . C23 . 1.407(6) yes C16 . F17 . 1.350(5) yes C16 . C18 . 1.389(6) yes C18 . F19 . 1.328(5) yes C18 . C20 . 1.373(6) yes C20 . F21 . 1.346(5) yes C20 . C22 . 1.377(7) yes C22 . C23 . 1.377(6) yes C22 . F25 . 1.342(5) yes C23 . F24 . 1.359(5) yes C26 . C27 . 1.398(6) yes C26 . C34 . 1.383(7) yes C27 . F28 . 1.350(5) yes C27 . C29 . 1.370(6) yes C29 . F30 . 1.348(5) yes C29 . C31 . 1.399(7) yes C31 . F32 . 1.340(6) yes C31 . C33 . 1.366(7) yes C33 . C34 . 1.391(7) yes C33 . F36 . 1.347(6) yes C34 . F35 . 1.351(5) yes W39 . O40 . 1.853(3) yes W39 . O75 . 1.720(3) yes W39 . O76 . 1.770(3) yes W39 . N83 . 2.298(4) yes W39 . N87 . 2.329(4) yes W39 . N90 . 2.290(3) yes O40 . B41 . 1.513(5) yes B41 . C42 . 1.662(7) yes B41 . C53 . 1.655(7) yes B41 . C64 . 1.642(7) yes C42 . C43 . 1.383(7) yes C42 . C50 . 1.391(6) yes C43 . F44 . 1.361(5) yes C43 . C45 . 1.382(7) yes C45 . F46 . 1.349(6) yes C45 . C47 . 1.377(7) yes C47 . F48 . 1.350(5) yes C47 . C49 . 1.373(8) yes C49 . C50 . 1.371(7) yes C49 . F52 . 1.355(5) yes C50 . F51 . 1.353(6) yes C53 . C54 . 1.395(7) yes C53 . C61 . 1.389(6) yes C54 . F55 . 1.347(5) yes C54 . C56 . 1.391(7) yes C56 . F57 . 1.343(5) yes C56 . C58 . 1.362(7) yes C58 . F59 . 1.347(5) yes C58 . C60 . 1.385(7) yes C60 . C61 . 1.375(6) yes C60 . F63 . 1.339(5) yes C61 . F62 . 1.373(5) yes C64 . C65 . 1.403(7) yes C64 . C71 . 1.395(6) yes C65 . F66 . 1.348(5) yes C65 . C67 . 1.376(7) yes C67 . F68 . 1.349(6) yes C67 . C69 . 1.378(7) yes C69 . C70 . 1.380(8) yes C69 . F74 . 1.345(6) yes C70 . C71 . 1.362(8) yes C70 . F73 . 1.357(5) yes C71 . F72 . 1.363(6) yes CL77 . C78 . 1.767(5) yes C78 . CL79 . 1.748(6) yes C78 . H781 . 1.016(6) no C78 . H782 . 0.998(6) no CL80 . C81 . 1.758(6) yes C81 . CL82 . 1.775(6) yes C81 . H811 . 1.008(6) no C81 . H812 . 1.000(6) no N83 . C84 . 1.491(6) yes N83 . C85 . 1.498(6) yes N83 . C92 . 1.512(6) yes C84 . H841 . 1.005(4) no C84 . H842 . 0.993(4) no C84 . H843 . 1.006(6) no C85 . C86 . 1.512(7) yes C85 . H851 . 0.992(5) no C85 . H852 . 1.007(5) no C86 . N87 . 1.493(5) yes C86 . H861 . 1.004(4) no C86 . H862 . 0.997(5) no N87 . C88 . 1.498(6) yes N87 . C94 . 1.496(6) yes C88 . C89 . 1.512(7) yes C88 . H881 . 1.005(4) no C88 . H882 . 1.000(5) no C89 . N90 . 1.504(6) yes C89 . H891 . 0.995(5) no C89 . H892 . 0.999(5) no N90 . C91 . 1.485(6) yes N90 . C93 . 1.504(6) yes C91 . C92 . 1.517(6) yes C91 . H911 . 0.996(5) no C91 . H912 . 1.000(5) no C92 . H921 . 0.996(5) no C92 . H922 . 0.998(5) no C93 . H931 . 1.000(5) no C93 . H932 . 0.999(5) no C93 . H933 . 0.999(5) no C94 . H941 . 1.002(4) no C94 . H942 . 0.995(5) no C94 . H943 . 0.999(5) no C95 . C96 . 1.531(7) yes C95 . N104 . 1.498(6) yes C95 . H951 . 1.000(4) no C95 . H952 . 1.001(5) no C96 . N97 . 1.482(6) yes C96 . H961 . 1.006(4) no C96 . H962 . 0.997(4) no N97 . C98 . 1.485(6) yes N97 . C99 . 1.505(5) yes C98 . H981 . 1.003(5) no C98 . H982 . 0.997(5) no C98 . H983 . 1.000(5) no C99 . C100 . 1.501(7) yes C99 . H991 . 1.004(4) no C99 . H992 . 0.995(5) no C100 . N101 . 1.506(6) yes C100 . H1001 . 0.997(5) no C100 . H1002 . 0.996(5) no N101 . C102 . 1.502(6) yes N101 . C106 . 1.474(6) yes C102 . C103 . 1.510(6) yes C102 . H1021 . 1.001(5) no C102 . H1022 . 0.995(5) no C103 . N104 . 1.502(6) yes C103 . H1031 . 1.001(5) no C103 . H1032 . 0.996(5) no N104 . C105 . 1.484(5) yes C105 . H1051 . 0.998(5) no C105 . H1052 . 0.995(5) no C105 . H1053 . 1.004(5) no C106 . H1061 . 1.005(5) no C106 . H1062 . 1.002(4) no C106 . H1063 . 0.995(5) 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 O2 . W1 . O37 . 107.6(1) yes O2 . W1 . O38 . 104.6(1) yes O37 . W1 . O38 . 106.7(2) yes O2 . W1 . N97 . 91.0(1) yes O37 . W1 . N97 . 88.8(1) yes O38 . W1 . N97 . 153.0(1) yes O2 . W1 . N101 . 158.6(1) yes O37 . W1 . N101 . 86.5(1) yes O38 . W1 . N101 . 85.9(1) yes N97 . W1 . N101 . 72.8(1) yes O2 . W1 . N104 . 88.7(1) yes O37 . W1 . N104 . 155.8(1) yes O38 . W1 . N104 . 85.4(1) yes N97 . W1 . N104 . 72.8(1) yes N101 . W1 . N104 . 73.4(1) yes W1 . O2 . B3 . 140.6(3) yes O2 . B3 . C4 . 106.3(4) yes O2 . B3 . C15 . 114.7(4) yes C4 . B3 . C15 . 112.2(4) yes O2 . B3 . C26 . 107.8(3) yes C4 . B3 . C26 . 115.4(4) yes C15 . B3 . C26 . 100.5(3) yes B3 . C4 . C5 . 124.5(4) yes B3 . C4 . C11 . 122.8(4) yes C5 . C4 . C11 . 112.1(4) yes C4 . C5 . F6 . 120.0(5) yes C4 . C5 . C7 . 124.1(4) yes F6 . C5 . C7 . 116.0(4) yes C5 . C7 . F8 . 120.1(4) yes C5 . C7 . C9 . 120.3(4) yes F8 . C7 . C9 . 119.6(4) yes C7 . C9 . C10 . 118.2(5) yes C7 . C9 . F14 . 120.9(4) yes C10 . C9 . F14 . 121.0(5) yes C9 . C10 . C11 . 119.2(5) yes C9 . C10 . F13 . 119.5(4) yes C11 . C10 . F13 . 121.3(4) yes C4 . C11 . C10 . 126.0(4) yes C4 . C11 . F12 . 118.0(4) yes C10 . C11 . F12 . 115.9(4) yes B3 . C15 . C16 . 128.5(4) yes B3 . C15 . C23 . 118.0(4) yes C16 . C15 . C23 . 113.3(4) yes C15 . C16 . F17 . 120.4(4) yes C15 . C16 . C18 . 124.1(4) yes F17 . C16 . C18 . 115.4(4) yes C16 . C18 . F19 . 120.6(4) yes C16 . C18 . C20 . 119.6(4) yes F19 . C18 . C20 . 119.8(4) yes C18 . C20 . F21 . 120.0(4) yes C18 . C20 . C22 . 119.5(4) yes F21 . C20 . C22 . 120.5(4) yes C20 . C22 . C23 . 118.8(4) yes C20 . C22 . F25 . 120.5(4) yes C23 . C22 . F25 . 120.7(4) yes C15 . C23 . C22 . 124.6(4) yes C15 . C23 . F24 . 119.2(4) yes C22 . C23 . F24 . 116.2(4) yes B3 . C26 . C27 . 117.8(4) yes B3 . C26 . C34 . 128.5(4) yes C27 . C26 . C34 . 113.2(4) yes C26 . C27 . F28 . 120.0(4) yes C26 . C27 . C29 . 124.9(4) yes F28 . C27 . C29 . 115.1(4) yes C27 . C29 . F30 . 121.5(4) yes C27 . C29 . C31 . 119.1(4) yes F30 . C29 . C31 . 119.4(4) yes C29 . C31 . F32 . 120.9(4) yes C29 . C31 . C33 . 118.5(5) yes F32 . C31 . C33 . 120.6(5) yes C31 . C33 . C34 . 120.2(5) yes C31 . C33 . F36 . 119.5(4) yes C34 . C33 . F36 . 120.2(4) yes C26 . C34 . C33 . 124.0(4) yes C26 . C34 . F35 . 121.3(4) yes C33 . C34 . F35 . 114.7(4) yes O40 . W39 . O75 . 103.9(1) yes O40 . W39 . O76 . 104.3(1) yes O75 . W39 . O76 . 103.9(2) yes O40 . W39 . N83 . 163.1(1) yes O75 . W39 . N83 . 86.7(1) yes O76 . W39 . N83 . 85.4(1) yes O40 . W39 . N87 . 92.4(1) yes O75 . W39 . N87 . 156.6(2) yes O76 . W39 . N87 . 87.8(1) yes N83 . W39 . N87 . 73.9(1) yes O40 . W39 . N90 . 91.7(1) yes O75 . W39 . N90 . 87.8(2) yes O76 . W39 . N90 . 156.9(1) yes N83 . W39 . N90 . 75.3(1) yes N87 . W39 . N90 . 74.8(1) yes W39 . O40 . B41 . 141.5(3) yes O40 . B41 . C42 . 113.4(4) yes O40 . B41 . C53 . 108.1(3) yes C42 . B41 . C53 . 102.1(4) yes O40 . B41 . C64 . 106.8(4) yes C42 . B41 . C64 . 111.6(3) yes C53 . B41 . C64 . 115.0(4) yes B41 . C42 . C43 . 129.2(4) yes B41 . C42 . C50 . 118.0(4) yes C43 . C42 . C50 . 112.6(4) yes C42 . C43 . F44 . 120.6(4) yes C42 . C43 . C45 . 124.8(4) yes F44 . C43 . C45 . 114.6(4) yes C43 . C45 . F46 . 121.3(5) yes C43 . C45 . C47 . 119.3(5) yes F46 . C45 . C47 . 119.5(4) yes C45 . C47 . F48 . 120.2(5) yes C45 . C47 . C49 . 118.8(4) yes F48 . C47 . C49 . 121.0(5) yes C47 . C49 . C50 . 119.4(4) yes C47 . C49 . F52 . 119.8(4) yes C50 . C49 . F52 . 120.8(5) yes C42 . C50 . C49 . 125.1(5) yes C42 . C50 . F51 . 118.9(4) yes C49 . C50 . F51 . 116.0(4) yes B41 . C53 . C54 . 128.5(4) yes B41 . C53 . C61 . 118.4(4) yes C54 . C53 . C61 . 112.9(4) yes C53 . C54 . F55 . 121.6(4) yes C53 . C54 . C56 . 123.2(4) yes F55 . C54 . C56 . 115.1(4) yes C54 . C56 . F57 . 119.7(5) yes C54 . C56 . C58 . 120.5(4) yes F57 . C56 . C58 . 119.8(4) yes C56 . C58 . F59 . 120.1(4) yes C56 . C58 . C60 . 119.2(4) yes F59 . C58 . C60 . 120.7(4) yes C58 . C60 . C61 . 118.2(4) yes C58 . C60 . F63 . 121.4(4) yes C61 . C60 . F63 . 120.4(4) yes C53 . C61 . C60 . 125.9(4) yes C53 . C61 . F62 . 119.2(4) yes C60 . C61 . F62 . 114.7(4) yes B41 . C64 . C65 . 121.6(4) yes B41 . C64 . C71 . 125.8(4) yes C65 . C64 . C71 . 112.6(4) yes C64 . C65 . F66 . 118.6(4) yes C64 . C65 . C67 . 124.7(4) yes F66 . C65 . C67 . 116.7(4) yes C65 . C67 . F68 . 120.9(4) yes C65 . C67 . C69 . 119.2(5) yes F68 . C67 . C69 . 119.8(5) yes C67 . C69 . C70 . 118.7(5) yes C67 . C69 . F74 . 120.3(5) yes C70 . C69 . F74 . 120.9(5) yes C69 . C70 . C71 . 120.1(4) yes C69 . C70 . F73 . 119.0(5) yes C71 . C70 . F73 . 120.8(5) yes C64 . C71 . C70 . 124.6(5) yes C64 . C71 . F72 . 119.5(5) yes C70 . C71 . F72 . 115.9(4) yes CL77 . C78 . CL79 . 112.6(3) yes CL77 . C78 . H781 . 108.3(4) no CL79 . C78 . H781 . 108.7(4) no CL77 . C78 . H782 . 109.2(4) no CL79 . C78 . H782 . 109.6(5) no H781 . C78 . H782 . 108.4(5) no CL80 . C81 . CL82 . 111.7(3) yes CL80 . C81 . H811 . 108.8(4) no CL82 . C81 . H811 . 109.0(4) no CL80 . C81 . H812 . 109.1(4) no CL82 . C81 . H812 . 109.4(4) no H811 . C81 . H812 . 108.8(5) no W39 . N83 . C84 . 108.6(3) yes W39 . N83 . C85 . 107.1(3) yes C84 . N83 . C85 . 108.9(4) yes W39 . N83 . C92 . 112.8(3) yes C84 . N83 . C92 . 109.3(4) yes C85 . N83 . C92 . 110.0(3) yes N83 . C84 . H841 . 109.4(4) no N83 . C84 . H842 . 110.1(4) no H841 . C84 . H842 . 109.6(5) no N83 . C84 . H843 . 109.4(4) no H841 . C84 . H843 . 108.6(5) no H842 . C84 . H843 . 109.6(4) no N83 . C85 . C86 . 110.3(4) yes N83 . C85 . H851 . 110.0(5) no C86 . C85 . H851 . 109.1(4) no N83 . C85 . H852 . 109.3(4) no C86 . C85 . H852 . 108.4(4) no H851 . C85 . H852 . 109.6(4) no C85 . C86 . N87 . 110.1(4) yes C85 . C86 . H861 . 109.4(4) no N87 . C86 . H861 . 109.2(4) no C85 . C86 . H862 . 109.3(4) no N87 . C86 . H862 . 109.5(4) no H861 . C86 . H862 . 109.4(4) no W39 . N87 . C86 . 114.2(3) yes W39 . N87 . C88 . 104.7(2) yes C86 . N87 . C88 . 111.2(3) yes W39 . N87 . C94 . 108.7(3) yes C86 . N87 . C94 . 108.6(3) yes C88 . N87 . C94 . 109.3(4) yes N87 . C88 . C89 . 110.7(4) yes N87 . C88 . H881 . 108.5(4) no C89 . C88 . H881 . 109.7(4) no N87 . C88 . H882 . 108.7(4) no C89 . C88 . H882 . 110.1(4) no H881 . C88 . H882 . 109.1(5) no C88 . C89 . N90 . 110.6(4) yes C88 . C89 . H891 . 109.0(4) no N90 . C89 . H891 . 109.8(4) no C88 . C89 . H892 . 108.5(4) no N90 . C89 . H892 . 108.9(4) no H891 . C89 . H892 . 110.0(4) no W39 . N90 . C89 . 114.0(3) yes W39 . N90 . C91 . 105.6(3) yes C89 . N90 . C91 . 111.3(3) yes W39 . N90 . C93 . 108.4(3) yes C89 . N90 . C93 . 109.1(3) yes C91 . N90 . C93 . 108.3(3) yes N90 . C91 . C92 . 110.4(4) yes N90 . C91 . H911 . 109.2(4) no C92 . C91 . H911 . 109.1(4) no N90 . C91 . H912 . 109.1(4) no C92 . C91 . H912 . 109.1(4) no H911 . C91 . H912 . 109.9(4) no N83 . C92 . C91 . 110.2(4) yes N83 . C92 . H921 . 109.4(4) no C91 . C92 . H921 . 109.3(4) no N83 . C92 . H922 . 108.7(4) no C91 . C92 . H922 . 109.2(4) no H921 . C92 . H922 . 109.9(4) no N90 . C93 . H931 . 109.5(4) no N90 . C93 . H932 . 109.4(4) no H931 . C93 . H932 . 109.6(4) no N90 . C93 . H933 . 109.1(4) no H931 . C93 . H933 . 109.6(4) no H932 . C93 . H933 . 109.7(5) no N87 . C94 . H941 . 109.0(4) no N87 . C94 . H942 . 109.5(4) no H941 . C94 . H942 . 109.7(4) no N87 . C94 . H943 . 109.3(4) no H941 . C94 . H943 . 109.4(5) no H942 . C94 . H943 . 109.9(4) no C96 . C95 . N104 . 110.3(4) yes C96 . C95 . H951 . 108.7(4) no N104 . C95 . H951 . 109.9(4) no C96 . C95 . H952 . 108.3(4) no N104 . C95 . H952 . 110.1(4) no H951 . C95 . H952 . 109.4(5) no C95 . C96 . N97 . 110.8(4) yes C95 . C96 . H961 . 109.6(4) no N97 . C96 . H961 . 108.5(4) no C95 . C96 . H962 . 109.8(4) no N97 . C96 . H962 . 108.9(4) no H961 . C96 . H962 . 109.2(4) no W1 . N97 . C96 . 106.7(2) yes W1 . N97 . C98 . 106.7(3) yes C96 . N97 . C98 . 109.9(4) yes W1 . N97 . C99 . 114.2(3) yes C96 . N97 . C99 . 110.8(3) yes C98 . N97 . C99 . 108.5(3) yes N97 . C98 . H981 . 109.3(4) no N97 . C98 . H982 . 109.6(4) no H981 . C98 . H982 . 109.5(4) no N97 . C98 . H983 . 109.4(4) no H981 . C98 . H983 . 109.3(5) no H982 . C98 . H983 . 109.7(5) no N97 . C99 . C100 . 110.6(4) yes N97 . C99 . H991 . 108.4(4) no C100 . C99 . H991 . 109.2(4) no N97 . C99 . H992 . 109.0(4) no C100 . C99 . H992 . 110.0(4) no H991 . C99 . H992 . 109.6(4) no C99 . C100 . N101 . 110.0(3) yes C99 . C100 . H1001 . 109.0(4) no N101 . C100 . H1001 . 109.3(4) no C99 . C100 . H1002 . 109.6(4) no N101 . C100 . H1002 . 108.9(4) no H1001 . C100 . H1002 . 110.1(4) no W1 . N101 . C100 . 106.8(3) yes W1 . N101 . C102 . 114.6(3) yes C100 . N101 . C102 . 110.1(3) yes W1 . N101 . C106 . 107.0(3) yes C100 . N101 . C106 . 108.7(3) yes C102 . N101 . C106 . 109.5(4) yes N101 . C102 . C103 . 111.1(4) yes N101 . C102 . H1021 . 108.6(4) no C103 . C102 . H1021 . 109.1(4) no N101 . C102 . H1022 . 109.2(4) no C103 . C102 . H1022 . 109.1(4) no H1021 . C102 . H1022 . 109.8(4) no C102 . C103 . N104 . 110.8(4) yes C102 . C103 . H1031 . 109.1(4) no N104 . C103 . H1031 . 108.8(4) no C102 . C103 . H1032 . 109.4(4) no N104 . C103 . H1032 . 109.1(4) no H1031 . C103 . H1032 . 109.7(4) no W1 . N104 . C95 . 114.0(3) yes W1 . N104 . C103 . 105.2(3) yes C95 . N104 . C103 . 110.5(3) yes W1 . N104 . C105 . 108.0(3) yes C95 . N104 . C105 . 110.8(3) yes C103 . N104 . C105 . 107.9(3) yes N104 . C105 . H1051 . 109.3(4) no N104 . C105 . H1052 . 109.5(4) no H1051 . C105 . H1052 . 110.1(4) no N104 . C105 . H1053 . 109.0(4) no H1051 . C105 . H1053 . 109.3(4) no H1052 . C105 . H1053 . 109.6(5) no N101 . C106 . H1061 . 109.8(4) no N101 . C106 . H1062 . 109.4(4) no H1061 . C106 . H1062 . 108.9(5) no N101 . C106 . H1063 . 109.5(4) no H1061 . C106 . H1063 . 109.5(4) no H1062 . C106 . H1063 . 109.7(4) no #end