# Copyright The Royal Society of Chemistry, 1998 data_CRYSTALS_cif _audit_creation_date 98-06-24 _audit_creation_method CRYSTALS_ver_07-07-97 # icl33 #**************************************************************************** # 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_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' linda.doerrer@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ' Graham McCann ' #============================================================================= # 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 # Title of paper _publ_section_title ; Reactions of Oxo- and Peroxo-Molybdenum Complexes with B(C6F5)3: Crystal Structures of cis-[MoO{OB(C6F5)3}(eta-2-O-NEt2)2] and cis-[MoO{OB(C6F5)3}- {eta2-PhN(O)C(O)Ph}2] ; # 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 ' Linda H. Doerrer ' #<--'Last name, first name' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ' Jane R. Galsworthy' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ' Malcolm L.H. Green' ; Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR ; ' Michael A. Leech ' ; Chemical Crystallography 9 Parks Road Oxford OX1 3PD ; ' Matthias Mueller ' ; Chemical Crystallography 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 '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 _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 10.2840(8) _cell_angle_alpha 102.500(5) _cell_length_b 12.4090(8) _cell_angle_beta 98.190(4) _cell_length_c 18.598(2) _cell_angle_gamma 106.397(4) _cell_volume 2169.7 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-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 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 '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' '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' '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' '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' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C46.25 H26 Mo1 F15 O6 N2 B1 ' _chemical_formula_moiety ' C46.25 H26 Mo1 F15 O6 N2 B1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1097.45 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 100 _cell_formula_units_Z 2 _exptl_crystal_description ' square plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.68 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1091.85 _exptl_absorpt_coefficient_mu 0.41 _exptl_absorpt_correction_type none _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 100 _diffrn_reflns_number 4580 _reflns_number_total 4580 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 4580 # Number of reflections without Friedels Law is 0 _reflns_number_observed 4201 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.62 _refine_diff_density_max 0.75 _refine_ls_number_reflns 4201 _refine_ls_number_parameters 646 _refine_ls_R_factor_obs 0.0465 _refine_ls_wR_factor_obs 0.0455 _refine_ls_goodness_of_fit_obs 1.1318 _refine_ls_shift/su_max 0.000835 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 1.30 0.780E-01 0.968 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Mo1 0.52910(3) 0.27979(3) 0.84544(2) 0.0176 1.0000 Uani F12 0.8329(2) 0.7001(2) 0.82839(15) 0.0326 1.0000 Uani F13 1.0968(2) 0.7214(2) 0.83129(17) 0.0431 1.0000 Uani F13 0.6656(2) 0.4773(2) 0.60117(15) 0.0361 1.0000 Uani F14 1.1701(2) 0.5363(3) 0.76274(19) 0.0477 1.0000 Uani F15 0.9686(2) 0.3301(3) 0.68894(17) 0.0418 1.0000 Uani F16 0.7042(2) 0.3060(2) 0.68654(14) 0.0301 1.0000 Uani F22 0.2928(2) 0.3498(2) 0.71911(14) 0.0314 1.0000 Uani F23 0.1261(3) 0.2425(3) 0.58385(18) 0.0514 1.0000 Uani F24 0.2252(3) 0.2518(3) 0.45678(18) 0.0630 1.0000 Uani F25 0.4962(3) 0.3706(3) 0.46833(16) 0.0472 1.0000 Uani F32 0.6186(2) 0.6748(2) 0.69219(15) 0.0323 1.0000 Uani F33 0.5295(3) 0.8568(2) 0.73342(16) 0.0406 1.0000 Uani F34 0.4022(2) 0.8770(2) 0.85118(16) 0.0362 1.0000 Uani F35 0.3742(2) 0.7146(2) 0.93084(15) 0.0341 1.0000 Uani F36 0.4660(2) 0.5366(2) 0.89334(14) 0.0301 1.0000 Uani O1 0.5482(2) 0.3915(2) 0.79830(16) 0.0211 1.0000 Uani O2 0.4974(3) 0.3395(2) 0.92805(16) 0.0241 1.0000 Uani O3 0.7334(2) 0.3183(2) 0.86101(16) 0.0216 1.0000 Uani O4 0.3301(2) 0.1848(2) 0.81494(16) 0.0220 1.0000 Uani O5 0.5736(2) 0.1478(2) 0.88699(17) 0.0234 1.0000 Uani O6 0.5026(2) 0.1542(2) 0.73917(16) 0.0231 1.0000 Uani N3 0.7923(3) 0.2504(3) 0.8965(2) 0.0213 1.0000 Uani N4 0.2827(3) 0.1027(3) 0.7453(2) 0.0245 1.0000 Uani C11 0.7530(4) 0.5019(4) 0.7561(2) 0.0227 1.0000 Uani C12 0.8592(4) 0.6051(4) 0.7918(3) 0.0268 1.0000 Uani C13 0.9991(4) 0.6176(4) 0.7944(3) 0.0286 1.0000 Uani C14 1.0366(4) 0.5266(5) 0.7603(3) 0.0351 1.0000 Uani C15 0.9340(4) 0.4205(4) 0.7232(3) 0.0319 1.0000 Uani C16 0.7977(4) 0.4128(4) 0.7235(3) 0.0267 1.0000 Uani C21 0.4893(4) 0.4169(4) 0.6676(2) 0.0219 1.0000 Uani C22 0.3500(4) 0.3570(4) 0.6584(3) 0.0260 1.0000 Uani C23 0.2602(4) 0.3005(4) 0.5886(3) 0.0351 1.0000 Uani C24 0.3096(5) 0.3051(5) 0.5246(3) 0.0405 1.0000 Uani C25 0.4475(5) 0.3652(4) 0.5308(3) 0.0333 1.0000 Uani C26 0.5325(4) 0.4195(4) 0.6008(3) 0.0293 1.0000 Uani C31 0.5449(4) 0.5939(4) 0.7892(2) 0.0217 1.0000 Uani C32 0.5576(4) 0.6809(4) 0.7518(2) 0.0262 1.0000 Uani C33 0.5137(4) 0.7761(4) 0.7721(3) 0.0264 1.0000 Uani C34 0.4501(4) 0.7871(4) 0.8318(3) 0.0252 1.0000 Uani C35 0.4368(4) 0.7050(4) 0.8720(2) 0.0233 1.0000 Uani C36 0.4832(4) 0.6126(4) 0.8504(2) 0.0235 1.0000 Uani C41 0.9396(3) 0.3005(3) 0.9234(2) 0.0190 1.0000 Uani C42 1.0219(4) 0.3067(4) 0.8709(2) 0.0273 1.0000 Uani C43 1.1632(4) 0.3635(4) 0.8950(3) 0.0315 1.0000 Uani C44 1.2207(4) 0.4124(4) 0.9712(3) 0.0281 1.0000 Uani C45 1.1373(4) 0.4064(4) 1.0232(3) 0.0293 1.0000 Uani C46 0.9945(4) 0.3496(4) 0.9992(3) 0.0249 1.0000 Uani C50 0.7024(4) 0.1575(3) 0.9061(2) 0.0205 1.0000 Uani C51 0.7445(4) 0.0698(4) 0.9356(2) 0.0227 1.0000 Uani C52 0.8386(4) 0.0219(4) 0.9064(3) 0.0285 1.0000 Uani C53 0.8658(4) -0.0691(4) 0.9306(3) 0.0353 1.0000 Uani C54 0.8014(4) -0.1108(4) 0.9841(3) 0.0388 1.0000 Uani C55 0.7093(4) -0.0613(4) 1.0140(3) 0.0370 1.0000 Uani C56 0.6795(4) 0.0284(4) 0.9894(3) 0.0299 1.0000 Uani C71 0.1364(4) 0.0408(4) 0.7297(2) 0.0239 1.0000 Uani C72 0.0919(4) -0.0746(4) 0.7303(3) 0.0342 1.0000 Uani C73 -0.0517(5) -0.1322(4) 0.7126(3) 0.0399 1.0000 Uani C74 -0.1427(4) -0.0745(4) 0.6965(3) 0.0358 1.0000 Uani C75 -0.0965(4) 0.0399(4) 0.6963(3) 0.0339 1.0000 Uani C76 0.0454(4) 0.1005(4) 0.7135(3) 0.0287 1.0000 Uani C80 0.3790(4) 0.0908(4) 0.7065(3) 0.0234 1.0000 Uani C81 0.3482(4) 0.0125(4) 0.6310(3) 0.0283 1.0000 Uani C82 0.2250(5) -0.0141(5) 0.5772(3) 0.0429 1.0000 Uani C83 0.2070(5) -0.0872(6) 0.5069(3) 0.0599 1.0000 Uani C84 0.3083(7) -0.1350(5) 0.4885(4) 0.0627 1.0000 Uani C85 0.4319(6) -0.1059(5) 0.5393(3) 0.0509 1.0000 Uani C86 0.4522(5) -0.0319(4) 0.6105(3) 0.0352 1.0000 Uani C101 0.0000 0.5000 0.5000 0.073(5) 0.5000 Uiso C102 -0.091(2) 0.438(2) 0.4514(17) 0.236(9) 1.0000 Uiso C103 -0.1963(15) 0.3525(14) 0.383(1) 0.156(5) 1.0000 Uiso B1 0.5868 0.4791 0.7536 0.0205 1.0000 Uani H103 -0.1615 0.3033 0.3493 0.0600 1.0000 Uiso H421 0.9785 0.2700 0.8151 0.0256 1.0000 Uiso H431 1.2246 0.3668 0.8569 0.0309 1.0000 Uiso H441 1.3220 0.4522 0.9876 0.0600 1.0000 Uiso H451 1.1805 0.4443 1.0783 0.0298 1.0000 Uiso H461 0.9331 0.3438 1.0366 0.0258 1.0000 Uiso H521 0.8852 0.0519 0.8669 0.0295 1.0000 Uiso H531 0.9340 -0.1039 0.9092 0.0339 1.0000 Uiso H541 0.8205 -0.1798 0.9990 0.0402 1.0000 Uiso H551 0.6662 -0.0885 1.0552 0.0341 1.0000 Uiso H561 0.6088 0.0618 1.0093 0.0280 1.0000 Uiso H721 0.1605 -0.1147 0.7431 0.0340 1.0000 Uiso H731 -0.0874 -0.2173 0.7122 0.0359 1.0000 Uiso H741 -0.2455 -0.1161 0.6855 0.0356 1.0000 Uiso H751 -0.1647 0.0808 0.6836 0.0322 1.0000 Uiso H761 0.0817 0.1846 0.7130 0.0273 1.0000 Uiso H821 0.1495 0.0186 0.5897 0.0411 1.0000 Uiso H831 0.1184 -0.1064 0.4683 0.0528 1.0000 Uiso H841 0.2922 -0.1916 0.4361 0.0580 1.0000 Uiso H851 0.5077 -0.1384 0.5253 0.0550 1.0000 Uiso H861 0.5429 -0.0095 0.6473 0.0365 1.0000 Uiso H1011 0.0076 0.5811 0.4994 0.0600 1.0000 Uiso H1021 -0.0698 0.3620 0.4560 0.0600 1.0000 Uiso H1022 -0.0357 0.4570 0.4082 0.0600 1.0000 Uiso H1032 -0.2724 0.3059 0.4026 0.0600 1.0000 Uiso H1033 -0.2383 0.4009 0.3548 0.0600 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01502(17) 0.0175(2) 0.0185(2) 0.00371(13) 0.00167(12) 0.00454(1 F12 0.0297(12) 0.0262(14) 0.0343(15) 0.0020(11) 0.002(1) 0.005(1) F13 0.0252(12) 0.0375(16) 0.054(2) 0.0085(13) -0.0025(11) -0.0015(11 F13 0.0346(13) 0.0467(17) 0.0312(16) 0.0162(12) 0.013(1) 0.0125(11 F14 0.0219(12) 0.059(2) 0.061(2) 0.0146(15) 0.0109(12) 0.0111(12 F15 0.0342(13) 0.0490(18) 0.0488(18) 0.0119(14) 0.0168(12) 0.0209(12 F16 0.0270(11) 0.0243(13) 0.0347(16) 0.0012(11) 0.006(1) 0.007(1) F22 0.0220(11) 0.0387(15) 0.0296(15) 0.0085(11) 0.005(1) 0.005(1) F23 0.0288(13) 0.057(2) 0.0460(19) 0.0056(15) -0.0110(12) -0.0045(12 F24 0.0659(19) 0.070(2) 0.0267(18) -0.0065(15) -0.0170(14) 0.0103(17 F25 0.0668(18) 0.0584(19) 0.0207(16) 0.0107(13) 0.0119(12) 0.0257(15 F32 0.0416(13) 0.0307(14) 0.0300(15) 0.0142(11) 0.0142(11) 0.0125(11 F33 0.0560(16) 0.0335(16) 0.0455(18) 0.0253(13) 0.0169(13) 0.0205(12 F34 0.0417(13) 0.0261(14) 0.0440(17) 0.0090(12) 0.0093(11) 0.0162(11 F35 0.0438(13) 0.0334(15) 0.0358(16) 0.0131(12) 0.0184(11) 0.0210(11 F36 0.0412(13) 0.0284(14) 0.0305(15) 0.0148(11) 0.017(1) 0.0165(11 O1 0.0148(11) 0.0241(15) 0.0224(15) 0.0049(11) 0.002(1) 0.006(1) O2 0.0250(13) 0.0218(15) 0.0227(16) 0.0054(12) 0.0015(11) 0.0054(11 O3 0.0198(12) 0.0212(15) 0.0252(16) 0.0102(12) 0.0038(11) 0.0062(11 O4 0.0208(13) 0.0211(15) 0.0204(15) 0.0017(11) 0.003(1) 0.0048(11 O5 0.0170(13) 0.0212(15) 0.0316(18) 0.0086(12) 0.0051(11) 0.004(1) O6 0.0214(13) 0.0193(15) 0.0248(17) 0.0010(12) 0.0027(11) 0.0054(11 N3 0.0194(15) 0.0208(19) 0.025(2) 0.0086(14) 0.0018(13) 0.0076(13 N4 0.0174(15) 0.026(2) 0.024(2) 0.0008(15) 0.0010(13) 0.0037(13 C11 0.0218(18) 0.026(2) 0.017(2) 0.0062(17) 0.0045(15) 0.0038(16 C12 0.027(2) 0.026(2) 0.024(3) 0.0038(18) 0.0054(17) 0.0065(17 C13 0.0192(19) 0.029(3) 0.030(3) 0.0108(19) -0.0013(16) -0.0029(17 C14 0.020(2) 0.049(3) 0.043(3) 0.022(2) 0.0096(18) 0.013(2) C15 0.029(2) 0.034(3) 0.039(3) 0.013(2) 0.0110(19) 0.0158(19 C16 0.0227(19) 0.030(3) 0.024(2) 0.0064(19) 0.0058(16) 0.0045(17 C21 0.0230(19) 0.018(2) 0.026(2) 0.0050(17) 0.0036(16) 0.0094(16 C22 0.026(2) 0.026(2) 0.026(3) 0.0079(18) 0.0020(17) 0.0098(17 C23 0.027(2) 0.030(3) 0.037(3) 0.002(2) -0.0065(19) 0.0039(18 C24 0.047(3) 0.036(3) 0.026(3) -0.003(2) -0.010(2) 0.012(2) C25 0.051(3) 0.038(3) 0.018(3) 0.0077(19) 0.0064(19) 0.024(2) C26 0.029(2) 0.028(3) 0.033(3) 0.012(2) 0.0062(18) 0.0115(18 C31 0.0193(17) 0.020(2) 0.018(2) 0.0017(16) -0.0023(15) 0.0004(15 C32 0.0247(19) 0.027(2) 0.025(2) 0.0071(18) 0.0050(17) 0.0042(17 C33 0.027(2) 0.020(2) 0.033(3) 0.0141(19) 0.0052(18) 0.0060(17 C34 0.0231(19) 0.014(2) 0.035(3) 0.0009(18) 0.0003(17) 0.0087(16 C35 0.0254(19) 0.019(2) 0.025(2) 0.0060(17) 0.0038(16) 0.0086(16 C36 0.0238(18) 0.022(2) 0.024(2) 0.0090(18) 0.0024(16) 0.0048(16 C41 0.0144(17) 0.013(2) 0.027(2) 0.0034(16) -0.0003(15) 0.0028(14 C42 0.0198(18) 0.037(3) 0.021(2) 0.0033(18) 0.0004(16) 0.0074(17 C43 0.0215(19) 0.039(3) 0.037(3) 0.012(2) 0.0125(18) 0.0097(18 C44 0.0215(19) 0.024(2) 0.036(3) 0.0059(19) 0.0017(17) 0.0065(16 C45 0.033(2) 0.024(2) 0.024(2) 0.0041(18) -0.0005(18) 0.0045(18 C46 0.026(2) 0.025(2) 0.025(2) 0.0082(18) 0.0080(16) 0.0083(17 C50 0.0189(18) 0.018(2) 0.021(2) 0.0025(16) 0.0026(15) 0.0031(15 C51 0.0195(18) 0.017(2) 0.026(2) 0.0024(17) -0.0004(16) 0.0041(15 C52 0.027(2) 0.023(2) 0.033(3) 0.0038(19) 0.0073(18) 0.0086(17 C53 0.028(2) 0.026(3) 0.046(3) 0.002(2) 0.0014(19) 0.0099(18 C54 0.033(2) 0.020(3) 0.061(4) 0.016(2) -0.001(2) 0.0072(18 C55 0.033(2) 0.028(3) 0.048(3) 0.020(2) 0.005(2) 0.0015(19 C56 0.026(2) 0.026(2) 0.035(3) 0.010(2) 0.0042(18) 0.0052(17 C71 0.0194(18) 0.026(2) 0.020(2) 0.0049(18) 0.0002(15) -0.0002(16 C72 0.027(2) 0.030(3) 0.042(3) 0.012(2) 0.0035(18) 0.0034(18 C73 0.040(2) 0.029(3) 0.040(3) 0.011(2) 0.007(2) -0.007(2) C74 0.025(2) 0.039(3) 0.033(3) 0.005(2) 0.0045(18) -0.0015(19 C75 0.024(2) 0.041(3) 0.035(3) 0.009(2) 0.0050(18) 0.0096(19 C76 0.024(2) 0.025(2) 0.032(3) 0.0041(19) 0.0024(17) 0.0046(17 C80 0.024(2) 0.014(2) 0.030(3) 0.0055(17) 0.0045(17) 0.0052(16 C81 0.029(2) 0.021(2) 0.027(3) 0.0034(18) 0.0063(17) -0.0021(17 C82 0.036(2) 0.053(3) 0.027(3) 0.006(2) 0.003(2) 0.001(2) C83 0.046(3) 0.077(4) 0.020(3) -0.011(3) 0.003(2) -0.016(3) C84 0.078(4) 0.044(3) 0.040(4) -0.010(3) 0.024(3) -0.010(3) C85 0.085(4) 0.029(3) 0.043(4) 0.007(2) 0.029(3) 0.020(3) C86 0.057(3) 0.028(3) 0.029(3) 0.011(2) 0.017(2) 0.020(2) B1 0.0215 0.0252 0.0155 0.0069 0.0021 0.0083 _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 Mo1 . O1 . 1.775(3) yes Mo1 . O2 . 1.674(3) yes Mo1 . O3 . 1.982(2) yes Mo1 . O4 . 1.979(2) yes Mo1 . O5 . 2.088(3) yes Mo1 . O6 . 2.164(3) yes F12 . C12 . 1.346(5) yes F13 . C13 . 1.353(5) yes F13 . C26 . 1.352(5) yes F14 . C14 . 1.338(5) yes F15 . C15 . 1.332(6) yes F16 . C16 . 1.360(5) yes F22 . C22 . 1.353(5) yes F23 . C23 . 1.343(5) yes F24 . C24 . 1.336(6) yes F25 . C25 . 1.336(6) yes F32 . C32 . 1.349(5) yes F33 . C33 . 1.342(5) yes F34 . C34 . 1.343(5) yes F35 . C35 . 1.347(5) yes F36 . C36 . 1.352(5) yes O1 . B1 . 1.508(3) yes O3 . N3 . 1.388(4) yes O4 . N4 . 1.386(5) yes O5 . C50 . 1.286(5) yes O6 . C80 . 1.270(4) yes N3 . C41 . 1.432(4) yes N3 . C50 . 1.323(5) yes N4 . C71 . 1.437(5) yes N4 . C80 . 1.328(6) yes C11 . C12 . 1.382(6) yes C11 . C16 . 1.370(6) yes C11 . B1 . 1.644(4) yes C12 . C13 . 1.395(6) yes C13 . C14 . 1.353(7) yes C14 . C15 . 1.392(7) yes C15 . C16 . 1.378(6) yes C21 . C22 . 1.381(5) yes C21 . C26 . 1.381(7) yes C21 . B1 . 1.652(4) yes C22 . C23 . 1.389(6) yes C23 . C24 . 1.366(8) yes C24 . C25 . 1.378(7) yes C25 . C26 . 1.371(7) yes C31 . C32 . 1.391(6) yes C31 . C36 . 1.389(6) yes C31 . B1 . 1.635(4) yes C32 . C33 . 1.378(7) yes C33 . C34 . 1.367(7) yes C34 . C35 . 1.377(6) yes C35 . C36 . 1.366(6) yes C41 . C42 . 1.381(6) yes C41 . C46 . 1.374(6) yes C42 . C43 . 1.381(5) yes C42 . H421 . 1.016(4) no C43 . C44 . 1.383(7) yes C43 . H431 . 1.013(4) no C44 . C45 . 1.382(7) yes C44 . H441 . 0.988(4) no C45 . C46 . 1.394(6) yes C45 . H451 . 1.005(4) no C46 . H461 . 1.005(4) no C50 . C51 . 1.458(6) yes C51 . C52 . 1.385(6) yes C51 . C56 . 1.389(6) yes C52 . C53 . 1.385(7) yes C52 . H521 . 1.013(4) no C53 . C54 . 1.383(8) yes C53 . H531 . 1.007(5) no C54 . C55 . 1.383(8) yes C54 . H541 . 1.015(5) no C55 . C56 . 1.384(7) yes C55 . H551 . 1.011(5) no C56 . H561 . 1.009(4) no C71 . C72 . 1.378(7) yes C71 . C76 . 1.386(6) yes C72 . C73 . 1.401(6) yes C72 . H721 . 1.002(5) no C73 . C74 . 1.368(8) yes C73 . H731 . 1.013(5) no C74 . C75 . 1.365(7) yes C74 . H741 . 1.005(4) no C75 . C76 . 1.393(6) yes C75 . H751 . 1.005(5) no C76 . H761 . 1.008(4) no C80 . C81 . 1.458(6) yes C81 . C82 . 1.406(7) yes C81 . C86 . 1.396(7) yes C82 . C83 . 1.373(8) yes C82 . H821 . 1.005(6) no C83 . C84 . 1.385(11) yes C83 . H831 . 1.009(6) no C84 . C85 . 1.38(1) yes C84 . H841 . 1.031(6) no C85 . C86 . 1.387(7) yes C85 . H851 . 1.013(6) no C86 . H861 . 1.003(5) no C101 . C102 . 1.16(3) yes C101 . C102 2_566 1.16(3) yes C101 . H1011 . 1. no C101 . H1011 2_566 1. no C102 . C103 . 1.52(3) yes C102 . H1011 2_566 1.28(3) no C102 . H1021 . 1.05(3) no C102 . H1022 . 1.08(3) no C103 . H103 . 0.952(17) no C103 . H1032 . 1.003(15) no C103 . H1033 . 1.016(17) 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 O1 . Mo1 . O2 . 103.68(13) yes O1 . Mo1 . O3 . 86.22(11) yes O2 . Mo1 . O3 . 106.33(12) yes O1 . Mo1 . O4 . 105.95(11) yes O2 . Mo1 . O4 . 87.47(12) yes O3 . Mo1 . O4 . 159.19(12) yes O1 . Mo1 . O5 . 158.72(11) yes O2 . Mo1 . O5 . 91.06(13) yes O3 . Mo1 . O5 . 74.8(1) yes O4 . Mo1 . O5 . 89.73(11) yes O1 . Mo1 . O6 . 89.53(12) yes O2 . Mo1 . O6 . 159.20(11) yes O3 . Mo1 . O6 . 90.3(1) yes O4 . Mo1 . O6 . 73.3(1) yes O5 . Mo1 . O6 . 81.16(11) yes Mo1 . O1 . B1 . 169.07(18) yes Mo1 . O3 . N3 . 116.8(2) yes Mo1 . O4 . N4 . 118.5(2) yes Mo1 . O5 . C50 . 117.0(2) yes Mo1 . O6 . C80 . 116.6(3) yes O3 . N3 . C41 . 113.6(3) yes O3 . N3 . C50 . 115.0(3) yes C41 . N3 . C50 . 131.0(4) yes O4 . N4 . C71 . 112.9(3) yes O4 . N4 . C80 . 115.7(3) yes C71 . N4 . C80 . 131.3(4) yes C12 . C11 . C16 . 113.8(4) yes C12 . C11 . B1 . 125.9(4) yes C16 . C11 . B1 . 120.3(3) yes F12 . C12 . C11 . 121.1(4) yes F12 . C12 . C13 . 115.7(4) yes C11 . C12 . C13 . 123.2(4) yes F13 . C13 . C12 . 119.4(4) yes F13 . C13 . C14 . 120.3(4) yes C12 . C13 . C14 . 120.3(4) yes F14 . C14 . C13 . 121.2(4) yes F14 . C14 . C15 . 119.6(5) yes C13 . C14 . C15 . 119.1(4) yes F15 . C15 . C14 . 120.1(4) yes F15 . C15 . C16 . 121.8(4) yes C14 . C15 . C16 . 118.1(5) yes F16 . C16 . C11 . 120.1(3) yes F16 . C16 . C15 . 114.3(4) yes C11 . C16 . C15 . 125.6(4) yes C22 . C21 . C26 . 114.3(4) yes C22 . C21 . B1 . 119.5(3) yes C26 . C21 . B1 . 126.2(3) yes F22 . C22 . C21 . 120.6(3) yes F22 . C22 . C23 . 115.6(4) yes C21 . C22 . C23 . 123.8(4) yes F23 . C23 . C22 . 120.7(4) yes F23 . C23 . C24 . 120.2(4) yes C22 . C23 . C24 . 119.2(4) yes F24 . C24 . C23 . 120.3(4) yes F24 . C24 . C25 . 120.4(5) yes C23 . C24 . C25 . 119.3(4) yes F25 . C25 . C24 . 119.5(4) yes F25 . C25 . C26 . 120.8(4) yes C24 . C25 . C26 . 119.6(4) yes F13 . C26 . C21 . 120.8(4) yes F13 . C26 . C25 . 115.3(4) yes C21 . C26 . C25 . 123.9(4) yes C32 . C31 . C36 . 113.0(4) yes C32 . C31 . B1 . 119.1(3) yes C36 . C31 . B1 . 127.6(3) yes F32 . C32 . C31 . 119.1(4) yes F32 . C32 . C33 . 116.4(4) yes C31 . C32 . C33 . 124.5(4) yes F33 . C33 . C32 . 121.2(4) yes F33 . C33 . C34 . 119.5(4) yes C32 . C33 . C34 . 119.3(4) yes F34 . C34 . C33 . 120.5(4) yes F34 . C34 . C35 . 120.6(4) yes C33 . C34 . C35 . 118.9(4) yes F35 . C35 . C34 . 119.6(4) yes F35 . C35 . C36 . 120.6(4) yes C34 . C35 . C36 . 119.8(4) yes F36 . C36 . C31 . 120.0(4) yes F36 . C36 . C35 . 115.6(4) yes C31 . C36 . C35 . 124.4(4) yes N3 . C41 . C42 . 118.2(4) yes N3 . C41 . C46 . 119.9(4) yes C42 . C41 . C46 . 121.7(3) yes C41 . C42 . C43 . 119.4(4) yes C41 . C42 . H421 . 120.1(3) no C43 . C42 . H421 . 120.5(4) no C42 . C43 . C44 . 119.8(4) yes C42 . C43 . H431 . 119.9(4) no C44 . C43 . H431 . 120.3(4) no C43 . C44 . C45 . 120.4(3) yes C43 . C44 . H441 . 118.9(4) no C45 . C44 . H441 . 120.8(4) no C44 . C45 . C46 . 120.1(4) yes C44 . C45 . H451 . 119.3(4) no C46 . C45 . H451 . 120.6(4) no C41 . C46 . C45 . 118.6(4) yes C41 . C46 . H461 . 120.5(4) no C45 . C46 . H461 . 120.8(4) no O5 . C50 . N3 . 115.7(4) yes O5 . C50 . C51 . 121.3(3) yes N3 . C50 . C51 . 123.0(3) yes C50 . C51 . C52 . 120.9(4) yes C50 . C51 . C56 . 118.4(4) yes C52 . C51 . C56 . 120.5(4) yes C51 . C52 . C53 . 119.3(4) yes C51 . C52 . H521 . 120.2(4) no C53 . C52 . H521 . 120.5(4) no C52 . C53 . C54 . 120.5(4) yes C52 . C53 . H531 . 119.1(5) no C54 . C53 . H531 . 120.4(5) no C53 . C54 . C55 . 120.0(5) yes C53 . C54 . H541 . 118.5(5) no C55 . C54 . H541 . 121.5(5) no C54 . C55 . C56 . 120.1(4) yes C54 . C55 . H551 . 120.2(5) no C56 . C55 . H551 . 119.7(5) no C51 . C56 . C55 . 119.7(4) yes C51 . C56 . H561 . 120.3(4) no C55 . C56 . H561 . 120.0(4) no N4 . C71 . C72 . 119.4(4) yes N4 . C71 . C76 . 117.9(4) yes C72 . C71 . C76 . 122.7(4) yes C71 . C72 . C73 . 117.3(4) yes C71 . C72 . H721 . 120.6(4) no C73 . C72 . H721 . 122.1(4) no C72 . C73 . C74 . 120.6(4) yes C72 . C73 . H731 . 119.1(5) no C74 . C73 . H731 . 120.3(4) no C73 . C74 . C75 . 121.1(4) yes C73 . C74 . H741 . 119.8(5) no C75 . C74 . H741 . 119.1(5) no C74 . C75 . C76 . 120.1(4) yes C74 . C75 . H751 . 120.1(4) no C76 . C75 . H751 . 119.7(4) no C71 . C76 . C75 . 118.1(4) yes C71 . C76 . H761 . 120.5(4) no C75 . C76 . H761 . 121.4(4) no O6 . C80 . N4 . 115.4(4) yes O6 . C80 . C81 . 121.0(4) yes N4 . C80 . C81 . 123.6(3) yes C80 . C81 . C82 . 123.8(4) yes C80 . C81 . C86 . 117.0(4) yes C82 . C81 . C86 . 119.0(5) yes C81 . C82 . C83 . 119.4(5) yes C81 . C82 . H821 . 120.9(5) no C83 . C82 . H821 . 119.7(5) no C82 . C83 . C84 . 120.9(5) yes C82 . C83 . H831 . 119.4(6) no C84 . C83 . H831 . 119.7(6) no C83 . C84 . C85 . 120.4(5) yes C83 . C84 . H841 . 120.1(7) no C85 . C84 . H841 . 119.5(7) no C84 . C85 . C86 . 119.4(5) yes C84 . C85 . H851 . 120.5(6) no C86 . C85 . H851 . 120.0(6) no C81 . C86 . C85 . 120.7(5) yes C81 . C86 . H861 . 119.7(5) no C85 . C86 . H861 . 119.5(5) no C102 . C101 . C102 2_566 180. yes C102 . C101 . H1011 . 107.6(12) no C102 2_566 C101 . H1011 . 72.4(12) no C102 . C101 . H1011 2_566 72.4(12) no C102 2_566 C101 . H1011 2_566 107.6(12) no H1011 . C101 . H1011 2_566 180. no C101 . C102 . C103 . 172.2(25) yes C101 . C102 . H1011 2_566 47.7(10) no C103 . C102 . H1011 2_566 129.0(21) no C101 . C102 . H1021 . 94.9(19) no C103 . C102 . H1021 . 81.1(18) no H1011 2_566 C102 . H1021 . 48.0(10) no C101 . C102 . H1022 . 93.4(16) no C103 . C102 . H1022 . 80.7(20) no H1011 2_566 C102 . H1022 . 106.0(18) no H1021 . C102 . H1022 . 98.9(23) no C102 . C103 . H103 . 116.1(17) no C102 . C103 . H1032 . 105.7(18) no H103 . C103 . H1032 . 111.5(16) no C102 . C103 . H1033 . 106.2(16) no H103 . C103 . H1033 . 110.4(17) no H1032 . C103 . H1033 . 106.4(14) no O1 . B1 . C11 . 104.73(17) yes O1 . B1 . C21 . 106.21(17) yes C11 . B1 . C21 . 112.81(19) yes O1 . B1 . C31 . 109.22(18) yes C11 . B1 . C31 . 115.78(19) yes C21 . B1 . C31 . 107.61(19) yes C101 . H1011 . C102 2_566 59.9(11) no