# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- compound_2_new.cif' #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 5-Mar-04 _audit_creation_method 'PLATON option' _audit_update_record ; 8-Mar-04 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 9-Mar-04 Updated by the Author E.H. 24-Feb-05 Updated by the Author E.H. 24-Feb-11 Updated by the Author E.H. 24-May-11 Updated by the Author E.H. ; #=================================================================== # 1. SUBMISSION DETAILS #=================================================================== # Name and address of author for X-ray correspondence _publ_contact_author_name 'Dr. Eberhardt Herdtweck' _publ_contact_author_address ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; _publ_contact_author_email eberhardt.herdtweck@ch.tum.de _publ_contact_author_fax ' +49(0)89 289 13473' _publ_contact_author_phone '+49(0)89 289 13143' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission: March 2011 ; #=================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) #=================================================================== #=================================================================== # 3. TITLE AND AUTHOR LIST #=================================================================== _publ_section_title ; Indenyl ring slippage in crown thioether complexes [IndMo(CO)2L]+ and C-S Activation of Trithiacyclononane: Experimental and Theoretical Studies ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address C.A.Gamelas ; Instituto de Tecnologia Quimica e Biologica, Universidade Nova de Lisboa, Av. da Republica, EAN, Apt. 127, P-2781-901 Oeiras, Portugal. ; N.A.G.Bandeira ; Departamento de Quimica e Bioquimica, Universidade de Lisboa, Campo Grande 4, P-1749-016 Lisboa, Portugal. ; C.C.L.Pereira ; Instituto de Tecnologia Quimica e Biologica, Universidade Nova de Lisboa, Av. da Republica, EAN, Apt. 127, P-2781-901 Oeiras, Portugal. ; M.J.Calhorda ; Departamento de Quimica e Bioquimica, Universidade de Lisboa, Campo Grande 4, P-1749-016 Lisboa, Portugal. ; ; E.Herdtweck ; ; Department Chemie, Lehrstuhl f\"ur Anorganische Chemie, Technische Universit\"at M\"unchen, Lichtenbergstrasse 4, D-85747 Garching bei M\"unchen, Germany. ; C.C.Romao ; Instituto de Tecnologia Quimica e Biologica, Universidade Nova de Lisboa, Av. da Republica, EAN, Apt. 127, P-2781-901 Oeiras, Portugal. ; L.F.Veiros ; Centro de Quimica Estrural, DEQB, IST, Av. Rovisco Pais, P-1049-001 Lisboa, Portugal. ; #===================================================================== # 4. TEXT #===================================================================== _publ_section_abstract ; The macrocycle trithiacyclononane (ttcn) reacts with ... ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of G\"ottingen, G\"ottingen, Germany. Spek, A. L. (2010). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; #=================================================================== data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 820539' #TrackingRef '- compound_2_new.cif' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C14 H13 Mo O2 S3, B F4, 0.185(H2 O)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H13.37 B1 F4 Mo1 O2.185 S3' _chemical_formula_weight 495.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 7.5840(1) _cell_length_b 9.8657(2) _cell_length_c 12.4253(2) _cell_angle_alpha 96.8789(8) _cell_angle_beta 102.5955(7) _cell_angle_gamma 98.2379(8) _cell_volume 886.90(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 3174 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.36 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method none _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 40 s per film repetition 1 dx 40 453 films measured in 9 data sets set 1: phi-scan with delta_phi = 2.0 set 2 to 9 omega-scans with delta_omega = 2.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and refined freely. One interstitial water molecule shows a SOF refined to 0.190(6). Hydogen atoms are calculated in dummy positions. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 17320 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.36 _reflns_number_total 3221 _reflns_number_gt 2937 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2010)' _computing_publication_material 'PLATON (Spek, 2010)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0033P)^2^+0.7138P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3221 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0429 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.481 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.057 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Mo Mo Uani 0.10000(2) 0.34437(2) 0.30219(1) 1.000 0.0174(1) . . S1 S Uani 0.39850(7) 0.25248(5) 0.30896(4) 1.000 0.0194(2) . . S2 S Uani 0.04397(7) 0.08600(5) 0.21699(4) 1.000 0.0223(2) . . S3 S Uani 0.23035(7) 0.07147(6) 0.45943(5) 1.000 0.0266(2) . . O1 O Uani -0.1498(2) 0.25245(17) 0.45815(14) 1.000 0.0351(6) . . O2 O Uani 0.3164(2) 0.47374(18) 0.54433(14) 1.000 0.0385(6) . . C1 C Uani -0.0603(3) 0.2815(2) 0.39765(18) 1.000 0.0236(7) . . C2 C Uani 0.2375(3) 0.4275(2) 0.45453(19) 1.000 0.0244(7) . . C3 C Uani 0.2739(3) 0.1172(2) 0.19561(19) 1.000 0.0227(7) . . C4 C Uani 0.0927(3) -0.0191(2) 0.3285(2) 1.000 0.0272(7) . . C5 C Uani 0.4325(3) 0.1462(2) 0.42044(19) 1.000 0.0233(7) . . C11 C Uani 0.1429(4) 0.5625(2) 0.2576(2) 1.000 0.0290(8) . . C12 C Uani -0.0406(4) 0.5288(3) 0.2668(2) 1.000 0.0330(8) . . C13 C Uani -0.1313(3) 0.4155(3) 0.1840(2) 1.000 0.0325(8) . . C13A C Uani -0.0093(3) 0.3851(2) 0.11360(18) 1.000 0.0258(7) . . C14 C Uani -0.0285(4) 0.2892(3) 0.0155(2) 1.000 0.0335(8) . . C15 C Uani 0.1173(4) 0.2872(3) -0.0316(2) 1.000 0.0350(8) . . C16 C Uani 0.2874(4) 0.3747(2) 0.0165(2) 1.000 0.0321(8) . . C17 C Uani 0.3130(3) 0.4671(2) 0.1115(2) 1.000 0.0285(7) . . C17A C Uani 0.1621(3) 0.4766(2) 0.16043(17) 1.000 0.0235(7) . . F1 F Uani 0.4577(2) 0.83051(15) 0.30921(14) 1.000 0.0536(6) . . F2 F Uani 0.6918(2) 0.75463(15) 0.24791(13) 1.000 0.0482(5) . . F3 F Uani 0.66148(18) 0.98054(14) 0.25521(12) 1.000 0.0384(5) . . F4 F Uani 0.4611(2) 0.81590(18) 0.12770(13) 1.000 0.0638(6) . . B B Uani 0.5693(4) 0.8444(3) 0.2347(2) 1.000 0.0289(8) . . O31 O Uiso 0.5767(17) 0.1333(13) 0.0757(10) 0.185(6) 0.075(5) . . H31 H Uiso 0.330(3) 0.036(2) 0.1926(16) 1.000 0.020(5) . . H32 H Uiso 0.269(3) 0.154(2) 0.1297(18) 1.000 0.020(6) . . H41 H Uiso -0.020(3) -0.054(2) 0.3413(18) 1.000 0.029(6) . . H42 H Uiso 0.147(3) -0.091(2) 0.2996(18) 1.000 0.029(6) . . H51 H Uiso 0.499(3) 0.078(2) 0.3983(18) 1.000 0.029(6) . . H52 H Uiso 0.508(3) 0.210(2) 0.4852(18) 1.000 0.023(6) . . H111 H Uiso 0.231(3) 0.632(2) 0.2999(18) 1.000 0.026(6) . . H121 H Uiso -0.091(3) 0.573(3) 0.318(2) 1.000 0.037(7) . . H131 H Uiso -0.246(3) 0.372(2) 0.1700(18) 1.000 0.024(6) . . H141 H Uiso -0.139(3) 0.233(2) -0.0129(19) 1.000 0.028(6) . . H151 H Uiso 0.106(3) 0.226(3) -0.097(2) 1.000 0.043(7) . . H161 H Uiso 0.383(3) 0.363(3) -0.017(2) 1.000 0.040(7) . . H171 H Uiso 0.422(3) 0.527(2) 0.1435(18) 1.000 0.026(6) . . H1 H Uiso 0.53390 0.13380 0.00750 0.185(6) 0.1120 calc . H2 H Uiso 0.62880 0.06400 0.08210 0.185(6) 0.1120 calc . 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 Mo 0.0165(1) 0.0162(1) 0.0227(1) 0.0067(1) 0.0075(1) 0.0056(1) S1 0.0163(3) 0.0192(3) 0.0243(3) 0.0056(2) 0.0065(2) 0.0042(2) S2 0.0192(3) 0.0188(3) 0.0270(3) 0.0047(2) 0.0014(2) 0.0030(2) S3 0.0239(3) 0.0301(3) 0.0297(3) 0.0155(2) 0.0073(2) 0.0068(2) O1 0.0308(9) 0.0368(10) 0.0460(10) 0.0141(8) 0.0231(8) 0.0058(8) O2 0.0352(10) 0.0441(10) 0.0313(10) -0.0092(8) 0.0085(8) 0.0024(8) C1 0.0204(11) 0.0192(11) 0.0319(12) 0.0042(9) 0.0058(10) 0.0059(9) C2 0.0206(11) 0.0216(11) 0.0352(14) 0.0045(10) 0.0141(10) 0.0056(9) C3 0.0241(12) 0.0217(11) 0.0249(12) 0.0042(9) 0.0076(9) 0.0094(10) C4 0.0229(12) 0.0213(12) 0.0389(14) 0.0135(10) 0.0064(11) 0.0027(10) C5 0.0178(11) 0.0257(12) 0.0275(12) 0.0083(10) 0.0036(10) 0.0072(10) C11 0.0432(15) 0.0158(11) 0.0348(13) 0.0111(10) 0.0171(12) 0.0095(11) C12 0.0443(15) 0.0305(13) 0.0392(15) 0.0195(11) 0.0214(12) 0.0260(12) C13 0.0203(13) 0.0416(15) 0.0436(15) 0.0239(12) 0.0086(11) 0.0155(11) C13A 0.0271(12) 0.0286(12) 0.0267(12) 0.0161(10) 0.0057(10) 0.0122(10) C14 0.0334(14) 0.0363(14) 0.0274(13) 0.0136(11) -0.0038(11) 0.0048(12) C15 0.0545(17) 0.0331(14) 0.0197(12) 0.0077(11) 0.0080(12) 0.0140(13) C16 0.0429(15) 0.0328(14) 0.0308(13) 0.0149(11) 0.0212(12) 0.0131(12) C17 0.0328(13) 0.0243(12) 0.0333(13) 0.0134(10) 0.0140(11) 0.0041(11) C17A 0.0338(12) 0.0171(11) 0.0259(12) 0.0138(9) 0.0116(10) 0.0092(10) F1 0.0484(9) 0.0385(9) 0.0811(12) 0.0001(8) 0.0412(9) -0.0011(7) F2 0.0446(9) 0.0465(9) 0.0590(10) 0.0072(7) 0.0116(8) 0.0280(7) F3 0.0294(7) 0.0327(8) 0.0522(9) 0.0061(7) 0.0119(7) -0.0001(6) F4 0.0600(11) 0.0607(11) 0.0519(10) -0.0096(8) -0.0212(8) 0.0179(9) B 0.0224(13) 0.0280(14) 0.0349(15) -0.0016(11) 0.0059(12) 0.0066(11) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo S1 2.5450(6) . . yes Mo S2 2.5779(5) . . yes Mo C1 1.964(2) . . yes Mo C2 1.966(2) . . yes Mo C11 2.282(2) . . yes Mo C12 2.277(3) . . yes Mo C13 2.281(2) . . yes Mo C13A 2.411(2) . . yes Mo C17A 2.401(2) . . yes S1 C3 1.807(2) . . yes S1 C5 1.832(2) . . yes S2 C3 1.809(2) . . yes S2 C4 1.834(2) . . yes S3 C4 1.783(2) . . yes S3 C5 1.793(2) . . yes F1 B 1.390(3) . . yes F2 B 1.371(3) . . yes F3 B 1.389(3) . . yes F4 B 1.374(3) . . yes O1 C1 1.152(3) . . yes O2 C2 1.149(3) . . yes O31 H2 0.8400 . . no O31 H1 0.8400 . . no C11 C12 1.416(4) . . no C11 C17A 1.437(3) . . no C12 C13 1.406(4) . . no C13 C13A 1.443(3) . . no C13A C14 1.417(3) . . no C13A C17A 1.432(3) . . no C14 C15 1.361(4) . . no C15 C16 1.410(4) . . no C16 C17 1.362(3) . . no C17 C17A 1.417(3) . . no C3 H31 0.96(2) . . no C3 H32 0.93(2) . . no C4 H42 0.94(2) . . no C4 H41 0.93(2) . . no C5 H52 0.97(2) . . no C5 H51 0.95(2) . . no C11 H111 0.91(2) . . no C12 H121 0.91(3) . . no C13 H131 0.88(2) . . no C14 H141 0.91(2) . . no C15 H151 0.93(3) . . no C16 H161 0.93(2) . . no C17 H171 0.92(2) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Mo S2 67.86(2) . . . yes S1 Mo C1 119.68(6) . . . yes S1 Mo C2 79.76(7) . . . yes S1 Mo C11 107.34(8) . . . yes S1 Mo C12 143.51(8) . . . yes S1 Mo C13 142.35(6) . . . yes S1 Mo C13A 106.69(6) . . . yes S1 Mo C17A 89.72(6) . . . yes S2 Mo C1 84.64(6) . . . yes S2 Mo C2 126.42(6) . . . yes S2 Mo C11 142.38(6) . . . yes S2 Mo C12 135.53(7) . . . yes S2 Mo C13 99.66(7) . . . yes S2 Mo C13A 85.78(5) . . . yes S2 Mo C17A 107.26(5) . . . yes C1 Mo C2 75.60(9) . . . yes C1 Mo C11 124.85(9) . . . yes C1 Mo C12 93.38(10) . . . yes C1 Mo C13 92.85(9) . . . yes C1 Mo C13A 124.21(9) . . . yes C1 Mo C17A 150.57(8) . . . yes C2 Mo C11 86.76(8) . . . yes C2 Mo C12 95.48(9) . . . yes C2 Mo C13 130.11(9) . . . yes C2 Mo C13A 145.77(8) . . . yes C2 Mo C17A 114.27(8) . . . yes C11 Mo C12 36.20(11) . . . yes C11 Mo C13 60.30(10) . . . yes C11 Mo C13A 59.08(8) . . . yes C11 Mo C17A 35.62(8) . . . yes C12 Mo C13 35.93(10) . . . yes C12 Mo C13A 58.96(8) . . . yes C12 Mo C17A 59.05(9) . . . yes C13 Mo C13A 35.67(8) . . . yes C13 Mo C17A 59.11(8) . . . yes C13A Mo C17A 34.63(7) . . . yes Mo S1 C3 87.95(8) . . . yes Mo S1 C5 108.73(8) . . . yes C3 S1 C5 98.32(10) . . . yes Mo S2 C3 86.89(7) . . . yes Mo S2 C4 109.74(7) . . . yes C3 S2 C4 96.74(10) . . . yes C4 S3 C5 101.53(11) . . . yes H1 O31 H2 108.00 . . . no Mo C1 O1 175.65(18) . . . yes Mo C2 O2 178.61(19) . . . yes S1 C3 S2 104.51(12) . . . yes S2 C4 S3 115.91(11) . . . yes S1 C5 S3 116.49(13) . . . yes Mo C11 C17A 76.69(12) . . . yes C12 C11 C17A 108.0(2) . . . no Mo C11 C12 71.70(15) . . . yes Mo C12 C13 72.19(16) . . . yes C11 C12 C13 108.6(2) . . . no Mo C12 C11 72.10(15) . . . yes Mo C13 C12 71.88(15) . . . yes C12 C13 C13A 108.4(2) . . . no Mo C13 C13A 77.09(14) . . . yes Mo C13A C13 67.23(13) . . . yes Mo C13A C17A 72.28(12) . . . yes C13 C13A C14 133.6(2) . . . no C13 C13A C17A 107.03(19) . . . no C14 C13A C17A 119.4(2) . . . no Mo C13A C14 125.64(16) . . . yes C13A C14 C15 118.7(3) . . . no C14 C15 C16 121.7(2) . . . no C15 C16 C17 121.6(3) . . . no C16 C17 C17A 118.4(2) . . . no Mo C17A C13A 73.09(12) . . . yes Mo C17A C17 123.09(15) . . . yes Mo C17A C11 67.69(11) . . . yes C11 C17A C17 132.2(2) . . . no C13A C17A C17 120.10(19) . . . no C11 C17A C13A 107.7(2) . . . no S1 C3 H32 107.2(13) . . . no S2 C3 H31 113.8(13) . . . no S2 C3 H32 108.2(14) . . . no H31 C3 H32 109.9(18) . . . no S1 C3 H31 112.9(12) . . . no S2 C4 H41 106.2(13) . . . no S2 C4 H42 105.7(13) . . . no S3 C4 H42 111.7(14) . . . no H41 C4 H42 111.0(18) . . . no S3 C4 H41 106.2(13) . . . no S1 C5 H52 104.4(12) . . . no S3 C5 H51 112.0(13) . . . no S1 C5 H51 106.6(13) . . . no H51 C5 H52 110.0(19) . . . no S3 C5 H52 107.0(13) . . . no Mo C11 H111 122.7(13) . . . no C17A C11 H111 124.6(14) . . . no C12 C11 H111 127.1(15) . . . no Mo C12 H121 121.5(17) . . . no C11 C12 H121 125.6(17) . . . no C13 C12 H121 125.8(16) . . . no Mo C13 H131 121.5(14) . . . no C12 C13 H131 128.8(14) . . . no C13A C13 H131 122.6(14) . . . no C15 C14 H141 123.7(15) . . . no C13A C14 H141 117.6(15) . . . no C14 C15 H151 119.7(15) . . . no C16 C15 H151 118.6(15) . . . no C17 C16 H161 121.3(16) . . . no C15 C16 H161 117.0(16) . . . no C16 C17 H171 123.2(14) . . . no C17A C17 H171 118.4(14) . . . no F1 B F3 108.2(2) . . . yes F1 B F4 108.9(2) . . . yes F1 B F2 110.2(2) . . . yes F2 B F4 109.7(2) . . . yes F3 B F4 109.4(2) . . . yes F2 B F3 110.4(2) . . . yes # End of Crystallographic Information File # End of Crystallographic Information File # Attachment 'compound_5.cif' # CIF-file generated for ROM5 4188-173 # Compound_5 #=================================================================== data_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 820540' #TrackingRef 'compound_5.cif' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C13 H17 Mo O2 S3, B F4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H17 B F4 Mo O2 S3' _chemical_formula_weight 484.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 8.0141(1) _cell_length_b 8.5400(1) _cell_length_c 25.5652(3) _cell_angle_alpha 90 _cell_angle_beta 96.1375(3) _cell_angle_gamma 90 _cell_volume 1739.66(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 3414 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.36 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method none _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 3 s per film repetition 1 dx 49.7 972 films measured in 9 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to 9: omega-scans with delta_omega = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and refined freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 27903 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.36 _reflns_number_total 3183 _reflns_number_gt 3008 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0170P)^2^+1.8164P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3183 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.562 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.053 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Mo Mo Uani 0.21225(2) 0.82674(2) 0.17326(1) 1.000 0.0151(1) . . S1 S Uani -0.02106(5) 0.65303(5) 0.13749(2) 1.000 0.0186(1) . . S2 S Uani 0.18385(6) 0.90543(6) 0.07800(2) 1.000 0.0203(1) . . S3 S Uani 0.24100(6) 0.51466(6) 0.02758(2) 1.000 0.0274(2) . . O1 O Uani 0.59602(17) 0.8109(2) 0.16202(6) 1.000 0.0372(5) . . O2 O Uani 0.3303(2) 0.51035(19) 0.22615(6) 1.000 0.0365(5) . . C1 C Uani 0.4538(2) 0.8170(2) 0.16383(7) 1.000 0.0238(6) . . C2 C Uani 0.2865(2) 0.6266(3) 0.20642(8) 1.000 0.0237(6) . . C3 C Uani -0.1252(2) 0.7614(3) 0.08244(8) 1.000 0.0234(6) . . C4 C Uani -0.0110(2) 0.8231(3) 0.04436(8) 1.000 0.0260(6) . . C5 C Uani 0.3409(3) 0.8337(3) 0.03691(8) 1.000 0.0252(6) . . C6 C Uani 0.3990(2) 0.6653(3) 0.04255(9) 1.000 0.0262(6) . . C7 C Uani 0.2069(3) 0.4382(3) 0.09154(9) 1.000 0.0280(6) . . C8 C Uani 0.0350(3) 0.4650(2) 0.10983(9) 1.000 0.0270(6) . . C9 C Uani 0.2627(3) 0.9653(3) 0.24944(8) 1.000 0.0293(6) . . C10 C Uani 0.2558(3) 1.0745(3) 0.20782(9) 1.000 0.0336(7) . . C11 C Uani 0.0900(3) 1.0756(3) 0.18280(9) 1.000 0.0363(7) . . C12 C Uani -0.0046(3) 0.9687(3) 0.20799(9) 1.000 0.0349(7) . . C13 C Uani 0.1013(3) 0.8982(3) 0.24898(9) 1.000 0.0309(7) . . F1 F Uani 0.78291(19) 0.14983(19) 0.09349(7) 1.000 0.0551(6) . . F2 F Uani 0.50106(19) 0.15207(19) 0.08540(8) 1.000 0.0638(6) . . F3 F Uani 0.64255(19) 0.37742(18) 0.09699(8) 1.000 0.0622(6) . . F4 F Uani 0.6470(3) 0.2029(3) 0.16369(6) 1.000 0.0864(9) . . B B Uani 0.6418(3) 0.2215(3) 0.11057(10) 1.000 0.0300(7) . . H31 H Uiso -0.207(3) 0.695(3) 0.0642(10) 1.000 0.036(7) . . H32 H Uiso -0.180(3) 0.845(3) 0.0978(9) 1.000 0.026(6) . . H41 H Uiso -0.062(3) 0.907(3) 0.0244(9) 1.000 0.033(6) . . H42 H Uiso 0.020(3) 0.740(3) 0.0208(9) 1.000 0.033(6) . . H51 H Uiso 0.293(3) 0.856(3) 0.0008(10) 1.000 0.035(6) . . H52 H Uiso 0.432(3) 0.903(3) 0.0450(9) 1.000 0.032(6) . . H61 H Uiso 0.451(3) 0.645(3) 0.0767(9) 1.000 0.024(6) . . H62 H Uiso 0.475(3) 0.651(3) 0.0186(10) 1.000 0.034(6) . . H71 H Uiso 0.222(3) 0.327(3) 0.0892(10) 1.000 0.037(7) . . H72 H Uiso 0.296(3) 0.475(3) 0.1173(9) 1.000 0.035(6) . . H81 H Uiso 0.027(3) 0.397(3) 0.1373(10) 1.000 0.036(7) . . H82 H Uiso -0.054(3) 0.439(3) 0.0836(10) 1.000 0.037(7) . . H91 H Uiso 0.352(3) 0.942(3) 0.2707(9) 1.000 0.032(6) . . H101 H Uiso 0.342(3) 1.135(3) 0.1993(10) 1.000 0.042(7) . . H111 H Uiso 0.053(3) 1.131(3) 0.1551(10) 1.000 0.039(7) . . H121 H Uiso -0.114(3) 0.946(3) 0.1994(10) 1.000 0.043(7) . . H131 H Uiso 0.079(3) 0.824(3) 0.2710(10) 1.000 0.040(7) . . 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 Mo 0.0135(1) 0.0167(1) 0.0157(1) -0.0009(1) 0.0036(1) -0.0001(1) S1 0.0168(2) 0.0194(2) 0.0203(2) -0.0006(2) 0.0052(2) -0.0024(2) S2 0.0207(2) 0.0212(2) 0.0198(2) 0.0028(2) 0.0054(2) -0.0004(2) S3 0.0276(3) 0.0314(3) 0.0238(2) -0.0088(2) 0.0053(2) -0.0050(2) O1 0.0153(7) 0.0574(11) 0.0396(9) -0.0072(8) 0.0062(6) -0.0007(7) O2 0.0375(8) 0.0346(9) 0.0378(9) 0.0151(7) 0.0054(7) 0.0125(7) C1 0.0244(10) 0.0285(11) 0.0184(9) -0.0030(8) 0.0025(8) -0.0016(8) C2 0.0182(9) 0.0320(11) 0.0212(9) 0.0001(9) 0.0040(7) -0.0001(8) C3 0.0161(9) 0.0278(11) 0.0257(10) -0.0006(9) -0.0006(8) 0.0010(8) C4 0.0201(9) 0.0359(12) 0.0214(10) 0.0039(9) -0.0012(8) 0.0016(9) C5 0.0231(10) 0.0320(12) 0.0220(10) -0.0011(9) 0.0098(8) -0.0061(9) C6 0.0185(9) 0.0346(12) 0.0264(11) -0.0081(9) 0.0069(8) -0.0018(8) C7 0.0325(11) 0.0211(11) 0.0313(11) -0.0024(9) 0.0081(9) 0.0045(9) C8 0.0320(11) 0.0178(10) 0.0323(12) -0.0026(9) 0.0092(9) -0.0036(8) C9 0.0287(11) 0.0351(12) 0.0235(10) -0.0124(9) -0.0004(9) 0.0006(9) C10 0.0405(13) 0.0221(11) 0.0408(13) -0.0110(10) 0.0163(10) -0.0084(10) C11 0.0518(14) 0.0250(12) 0.0324(12) -0.0056(10) 0.0052(10) 0.0177(11) C12 0.0214(10) 0.0402(13) 0.0438(13) -0.0256(11) 0.0061(9) 0.0068(10) C13 0.0411(12) 0.0278(11) 0.0275(11) -0.0088(10) 0.0207(10) -0.0038(10) F1 0.0458(9) 0.0569(10) 0.0617(10) 0.0000(8) 0.0019(7) 0.0165(7) F2 0.0418(9) 0.0525(10) 0.0939(13) -0.0202(9) -0.0081(8) -0.0141(7) F3 0.0400(8) 0.0329(8) 0.1124(14) 0.0182(9) 0.0024(9) -0.0008(7) F4 0.1389(19) 0.0899(15) 0.0310(9) -0.0064(9) 0.0123(10) -0.0060(13) B 0.0311(12) 0.0276(13) 0.0311(12) -0.0013(10) 0.0026(10) -0.0044(10) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo S1 2.4834(4) . . yes Mo S2 2.5133(5) . . yes Mo C1 1.9779(16) . . yes Mo C2 1.971(2) . . yes Mo C9 2.278(2) . . yes Mo C10 2.305(3) . . yes Mo C11 2.364(3) . . yes Mo C12 2.368(2) . . yes Mo C13 2.297(2) . . yes S1 C3 1.812(2) . . yes S1 C8 1.8299(19) . . yes S2 C4 1.8399(19) . . yes S2 C5 1.829(2) . . yes S3 C6 1.817(2) . . yes S3 C7 1.808(2) . . yes F1 B 1.396(3) . . yes F2 B 1.372(3) . . yes F3 B 1.376(3) . . yes F4 B 1.363(3) . . yes O1 C1 1.147(2) . . yes O2 C2 1.151(3) . . yes C3 C4 1.501(3) . . no C5 C6 1.514(4) . . no C7 C8 1.519(3) . . no C9 C10 1.411(3) . . no C9 C13 1.414(3) . . no C10 C11 1.412(3) . . no C11 C12 1.388(3) . . no C12 C13 1.411(3) . . no C3 H31 0.95(2) . . no C3 H32 0.95(2) . . no C4 H41 0.95(2) . . no C4 H42 0.98(2) . . no C5 H52 0.95(3) . . no C5 H51 0.98(3) . . no C6 H62 0.92(2) . . no C6 H61 0.94(2) . . no C7 H71 0.96(3) . . no C7 H72 0.97(2) . . no C8 H81 0.92(3) . . no C8 H82 0.95(2) . . no C9 H91 0.87(2) . . no C10 H101 0.91(3) . . no C11 H111 0.88(3) . . no C12 H121 0.90(2) . . no C13 H131 0.88(3) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Mo S2 79.41(2) . . . yes S1 Mo C1 129.65(5) . . . yes S1 Mo C2 79.70(6) . . . yes S1 Mo C9 133.08(6) . . . yes S1 Mo C10 140.05(6) . . . yes S1 Mo C11 105.72(6) . . . yes S1 Mo C12 83.69(6) . . . yes S1 Mo C13 97.18(6) . . . yes S2 Mo C1 83.19(5) . . . yes S2 Mo C2 129.82(6) . . . yes S2 Mo C9 132.77(6) . . . yes S2 Mo C10 96.91(6) . . . yes S2 Mo C11 82.18(6) . . . yes S2 Mo C12 103.43(6) . . . yes S2 Mo C13 137.93(6) . . . yes C1 Mo C2 76.21(7) . . . yes C1 Mo C9 92.27(8) . . . yes C1 Mo C10 88.58(8) . . . yes C1 Mo C11 118.18(8) . . . yes C1 Mo C12 146.54(8) . . . yes C1 Mo C13 125.87(8) . . . yes C2 Mo C9 93.72(9) . . . yes C2 Mo C10 127.21(9) . . . yes C2 Mo C11 147.63(8) . . . yes C2 Mo C12 118.85(8) . . . yes C2 Mo C13 89.67(9) . . . yes C9 Mo C10 35.87(8) . . . yes C9 Mo C11 58.82(8) . . . yes C9 Mo C12 58.92(8) . . . yes C9 Mo C13 35.99(9) . . . yes C10 Mo C11 35.17(8) . . . yes C10 Mo C12 58.23(9) . . . yes C10 Mo C13 59.31(9) . . . yes C11 Mo C12 34.12(8) . . . yes C11 Mo C13 58.14(8) . . . yes C12 Mo C13 35.16(8) . . . yes Mo S1 C3 104.30(7) . . . yes Mo S1 C8 117.40(8) . . . yes C3 S1 C8 105.06(11) . . . yes Mo S2 C4 109.58(7) . . . yes Mo S2 C5 118.06(7) . . . yes C4 S2 C5 101.85(10) . . . yes C6 S3 C7 103.56(11) . . . yes Mo C1 O1 175.33(16) . . . yes Mo C2 O2 179.45(18) . . . yes S1 C3 C4 114.89(12) . . . yes S2 C4 C3 112.14(14) . . . yes S2 C5 C6 119.15(16) . . . yes S3 C6 C5 116.89(14) . . . yes S3 C7 C8 116.98(17) . . . yes S1 C8 C7 121.30(16) . . . yes Mo C9 C10 73.12(13) . . . yes Mo C9 C13 72.76(13) . . . yes C10 C9 C13 107.4(2) . . . no Mo C10 C9 71.01(14) . . . yes Mo C10 C11 74.68(15) . . . yes C9 C10 C11 107.8(2) . . . no Mo C11 C10 70.14(14) . . . yes Mo C11 C12 73.11(15) . . . yes C10 C11 C12 108.6(2) . . . no Mo C12 C11 72.77(14) . . . yes Mo C12 C13 69.68(14) . . . yes C11 C12 C13 108.1(2) . . . no Mo C13 C9 71.24(13) . . . yes Mo C13 C12 75.16(14) . . . yes C9 C13 C12 108.1(2) . . . no S1 C3 H31 108.2(16) . . . no S1 C3 H32 105.0(14) . . . no C4 C3 H31 109.1(15) . . . no C4 C3 H32 110.3(15) . . . no H31 C3 H32 109(2) . . . no S2 C4 H41 105.0(15) . . . no S2 C4 H42 107.8(14) . . . no C3 C4 H41 110.9(15) . . . no C3 C4 H42 110.9(15) . . . no H41 C4 H42 110(2) . . . no S2 C5 H51 104.6(15) . . . no S2 C5 H52 103.1(14) . . . no C6 C5 H51 111.1(15) . . . no C6 C5 H52 110.6(15) . . . no H51 C5 H52 107(2) . . . no S3 C6 H61 107.1(15) . . . no S3 C6 H62 105.2(16) . . . no C5 C6 H61 111.3(16) . . . no C5 C6 H62 106.4(16) . . . no H61 C6 H62 110(2) . . . no S3 C7 H71 105.6(15) . . . no S3 C7 H72 109.0(14) . . . no C8 C7 H71 107.0(15) . . . no C8 C7 H72 111.6(14) . . . no H71 C7 H72 106(2) . . . no S1 C8 H81 102.7(16) . . . no S1 C8 H82 106.3(15) . . . no C7 C8 H81 106.2(15) . . . no C7 C8 H82 112.6(15) . . . no H81 C8 H82 106(2) . . . no Mo C9 H91 118.2(16) . . . no C10 C9 H91 125.6(16) . . . no C13 C9 H91 126.9(16) . . . no Mo C10 H101 121.2(16) . . . no C9 C10 H101 126.0(16) . . . no C11 C10 H101 126.2(16) . . . no Mo C11 H111 120.7(17) . . . no C10 C11 H111 126.2(16) . . . no C12 C11 H111 125.1(16) . . . no Mo C12 H121 122.1(16) . . . no C11 C12 H121 126.4(16) . . . no C13 C12 H121 125.5(16) . . . no Mo C13 H131 118.2(17) . . . no C9 C13 H131 122.4(16) . . . no C12 C13 H131 129.5(16) . . . no F1 B F2 108.5(2) . . . yes F1 B F3 108.64(19) . . . yes F1 B F4 108.7(2) . . . yes F2 B F3 109.0(2) . . . yes F2 B F4 110.7(2) . . . yes F3 B F4 111.3(2) . . . yes # End of Crystallographic Information File # Attachment 'compound_6.cif' # CIF-file generated for ROMH 3017-293 # compound_6 #=================================================================== data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 820541' #TrackingRef 'compound_6.cif' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C14 H15 Mo O S3, B F4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H15 B F4 Mo O S3' _chemical_formula_weight 478.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.542(2) _cell_length_b 17.268(2) _cell_length_c 10.837(2) _cell_angle_alpha 90 _cell_angle_beta 94.07(1) _cell_angle_gamma 90 _cell_volume 1781.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(1) _cell_measurement_reflns_used 1804 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.76 _exptl_crystal_description fragment _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method none _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.521 _exptl_absorpt_correction_T_max 1.414 _exptl_absorpt_process_details ; decay correction and absorption correction with the program INTEGRATE source: 'IPDS (STOE, 1997) ; _exptl_special_details ; Diffractometer operator E. Herdtweck exposure_time 180 s per image exposure_phi_range 0-230 exposure_delta_phi 1.0 exposure_sum_images 230 exposure_sum_images_used 1-230 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; straight forward after integration with the program INTEGRATE; source: 'IPDS (STOE, 1995)' Hydrogen atoms could not be located in the difference Fourier maps. Included with riding model. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 293(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'one-circle diffractometer' _diffrn_measurement_device_type 'IPDS (STOE&CIE)' _diffrn_measurement_method 'phi-rotation ' _diffrn_detector 'imaging plate' _diffrn_detector_area_resol_mean 67 _diffrn_standards_decay_% 3 # number of measured reflections (redundant set) _diffrn_reflns_number 12002 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.76 _reflns_number_total 2984 _reflns_number_gt 2528 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement 'IPDS (STOE, 1997)' _computing_data_reduction 'IPDS (STOE, 1997)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0713P)^2^+0.9586P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2984 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.76 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.560 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.071 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Mo Mo Uani 0.36342(4) 0.23925(2) 0.16211(3) 1.000 0.0533(1) . . S1 S Uani 0.33256(14) 0.24933(7) 0.36941(11) 1.000 0.0677(4) . . S4 S Uani 0.33851(13) 0.09901(6) 0.20240(11) 1.000 0.0659(4) . . S7 S Uani 0.15359(13) 0.22225(8) 0.04308(12) 1.000 0.0742(4) . . O O Uani 0.2365(5) 0.4065(2) 0.1681(5) 1.000 0.122(2) . . C C Uani 0.2858(6) 0.3476(3) 0.1653(5) 1.000 0.0800(19) . . C2 C Uani 0.3403(6) 0.1527(3) 0.4344(5) 1.000 0.0839(19) . . C3 C Uani 0.2602(8) 0.0968(3) 0.3513(5) 1.000 0.102(3) . . C5 C Uani 0.1929(7) 0.0683(3) 0.0959(7) 1.000 0.103(3) . . C6 C Uani 0.0928(8) 0.1239(4) 0.0597(7) 1.000 0.112(3) . . C21 C Uani 0.5111(5) 0.3178(3) 0.0558(5) 1.000 0.0689(16) . . C22 C Uani 0.5811(5) 0.2959(3) 0.1693(4) 1.000 0.0694(17) . . C23 C Uani 0.5998(5) 0.2158(3) 0.1693(4) 1.000 0.0651(16) . . C23A C Uani 0.5532(4) 0.1876(3) 0.0481(4) 1.000 0.0606(12) . . C24 C Uani 0.5561(5) 0.1124(3) -0.0063(5) 1.000 0.0743(17) . . C25 C Uani 0.5046(6) 0.1049(3) -0.1238(5) 1.000 0.083(2) . . C26 C Uani 0.4474(6) 0.1676(4) -0.1930(5) 1.000 0.084(2) . . C27 C Uani 0.4422(5) 0.2402(3) -0.1455(5) 1.000 0.0726(17) . . C27A C Uani 0.4988(5) 0.2515(2) -0.0222(4) 1.000 0.0603(14) . . F1 F Uani 0.7629(9) -0.0329(4) 0.3612(8) 1.000 0.227(5) . . F2 F Uani 0.8649(18) 0.0842(6) 0.3292(14) 0.500 0.166(6) . . F3 F Uani 0.801(3) 0.0595(17) 0.213(2) 0.500 0.277(14) . . F4 F Uani 0.9409(15) -0.0231(6) 0.2554(18) 0.500 0.182(7) . . F5 F Uani 0.9262(18) 0.0197(13) 0.3766(17) 0.500 0.243(10) . . F6 F Uani 0.723(3) 0.064(2) 0.335(3) 0.500 0.39(2) . . F7 F Uani 0.787(3) -0.0017(14) 0.1943(13) 0.500 0.242(10) . . B B Uani 0.8263(9) 0.0172(4) 0.2984(7) 1.000 0.095(3) . . H21 H Uiso 0.43750 0.13630 0.44620 1.000 0.1090 calc R H22 H Uiso 0.30110 0.15320 0.51460 1.000 0.1090 calc R H31 H Uiso 0.16200 0.11170 0.34110 1.000 0.1320 calc R H32 H Uiso 0.26630 0.04510 0.38610 1.000 0.1320 calc R H51 H Uiso 0.23160 0.04810 0.02210 1.000 0.1330 calc R H52 H Uiso 0.14540 0.02580 0.13400 1.000 0.1330 calc R H61 H Uiso 0.02200 0.12400 0.11970 1.000 0.1460 calc R H62 H Uiso 0.04700 0.10780 -0.01890 1.000 0.1460 calc R H211 H Uiso 0.47840 0.36730 0.03540 1.000 0.0900 calc R H221 H Uiso 0.61000 0.32920 0.23350 1.000 0.0900 calc R H231 H Uiso 0.63590 0.18590 0.23560 1.000 0.0850 calc R H241 H Uiso 0.59260 0.07000 0.03830 1.000 0.0960 calc R H251 H Uiso 0.50670 0.05650 -0.16110 1.000 0.1080 calc R H261 H Uiso 0.41200 0.15910 -0.27400 1.000 0.1090 calc R H271 H Uiso 0.40290 0.28100 -0.19210 1.000 0.0950 calc R 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 Mo 0.0517(2) 0.0499(2) 0.0580(3) -0.0013(1) 0.0025(2) 0.0004(1) S1 0.0677(7) 0.0743(7) 0.0611(7) -0.0114(5) 0.0052(5) -0.0038(5) S4 0.0767(8) 0.0526(6) 0.0687(6) 0.0013(5) 0.0067(5) 0.0005(5) S7 0.0634(7) 0.0807(8) 0.0764(8) 0.0063(6) -0.0095(6) -0.0015(6) O 0.124(4) 0.062(2) 0.187(5) 0.016(3) 0.064(3) 0.025(2) C 0.079(3) 0.058(3) 0.106(4) 0.006(2) 0.027(3) 0.006(2) C2 0.098(4) 0.086(3) 0.067(3) 0.006(2) 0.002(3) -0.005(3) C3 0.139(6) 0.081(4) 0.088(4) 0.007(3) 0.029(4) -0.015(4) C5 0.112(5) 0.067(3) 0.127(5) -0.011(3) -0.011(4) -0.023(3) C6 0.114(5) 0.090(4) 0.125(5) 0.005(4) -0.037(4) -0.025(4) C21 0.063(3) 0.056(2) 0.089(3) 0.004(2) 0.015(2) -0.006(2) C22 0.060(3) 0.077(3) 0.071(3) -0.010(2) 0.004(2) -0.015(2) C23 0.051(2) 0.078(3) 0.066(3) 0.003(2) 0.0010(19) 0.001(2) C23A 0.050(2) 0.063(2) 0.069(2) -0.0006(19) 0.0058(18) 0.0024(18) C24 0.073(3) 0.065(3) 0.087(3) -0.005(2) 0.020(2) 0.008(2) C25 0.084(4) 0.075(3) 0.093(4) -0.022(3) 0.025(3) -0.007(3) C26 0.075(3) 0.115(5) 0.063(3) -0.017(3) 0.010(2) -0.011(3) C27 0.061(3) 0.089(3) 0.068(3) 0.010(2) 0.005(2) 0.004(2) C27A 0.053(2) 0.064(2) 0.065(3) 0.0020(19) 0.011(2) -0.0006(18) F1 0.287(10) 0.147(5) 0.258(8) 0.051(5) 0.097(7) -0.042(6) F2 0.239(15) 0.071(5) 0.182(11) -0.024(7) -0.021(11) -0.065(8) F3 0.27(2) 0.32(3) 0.25(2) 0.20(2) 0.091(18) 0.16(2) F4 0.170(10) 0.099(6) 0.287(16) 0.047(8) 0.091(11) 0.036(7) F5 0.207(15) 0.233(19) 0.266(18) -0.027(16) -0.140(14) 0.002(14) F6 0.34(3) 0.37(4) 0.48(5) 0.19(3) 0.12(3) 0.23(3) F7 0.30(2) 0.31(2) 0.109(9) -0.084(13) -0.044(11) -0.10(2) B 0.106(5) 0.064(4) 0.110(5) 0.019(4) -0.025(4) -0.015(4) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo S1 2.2930(13) . . yes Mo S4 2.4751(12) . . yes Mo S7 2.3221(14) . . yes Mo C 2.013(5) . . yes Mo C21 2.320(5) . . yes Mo C22 2.292(5) . . yes Mo C23 2.287(5) . . yes Mo C23A 2.433(4) . . yes Mo C27A 2.464(5) . . yes S1 C2 1.811(5) . . yes S4 C3 1.826(6) . . yes S4 C5 1.821(7) . . yes S7 C6 1.808(7) . . yes F1 B 1.279(11) . . yes F2 B 1.252(14) . . yes F2 F5 1.34(2) . . yes F2 F6 1.40(3) . . yes F2 F3 1.42(3) . . yes F3 F6 1.56(4) . . yes F3 F7 1.08(4) . . yes F3 B 1.19(3) . . yes F4 F5 1.52(3) . . yes F4 F7 1.61(3) . . yes F4 B 1.403(16) . . yes F5 B 1.23(2) . . yes F6 B 1.36(3) . . yes F7 B 1.208(18) . . yes O C 1.122(6) . . yes C2 C3 1.493(8) . . no C5 C6 1.391(10) . . no C21 C22 1.409(7) . . no C21 C27A 1.423(6) . . no C22 C23 1.395(7) . . no C23 C23A 1.441(6) . . no C23A C27A 1.418(6) . . no C23A C24 1.427(7) . . no C24 C25 1.338(8) . . no C25 C26 1.405(8) . . no C26 C27 1.357(8) . . no C27 C27A 1.419(7) . . no C2 H21 0.9695 . . no C2 H22 0.9703 . . no C3 H31 0.9704 . . no C3 H32 0.9693 . . no C5 H52 0.9701 . . no C5 H51 0.9693 . . no C6 H61 0.9703 . . no C6 H62 0.9700 . . no C21 H211 0.9312 . . no C22 H221 0.9293 . . no C23 H231 0.9308 . . no C24 H241 0.9312 . . no C25 H251 0.9292 . . no C26 H261 0.9296 . . no C27 H271 0.9301 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Mo S4 83.16(4) . . . yes S1 Mo S7 112.84(5) . . . yes S1 Mo C 80.77(16) . . . yes S1 Mo C21 124.53(14) . . . yes S1 Mo C22 96.51(11) . . . yes S1 Mo C23 100.08(11) . . . yes S1 Mo C23A 132.64(11) . . . yes S1 Mo C27A 154.03(11) . . . yes S4 Mo S7 83.37(5) . . . yes S4 Mo C 150.01(16) . . . yes S4 Mo C21 136.79(13) . . . yes S4 Mo C22 120.64(13) . . . yes S4 Mo C23 85.85(13) . . . yes S4 Mo C23A 79.35(12) . . . yes S4 Mo C27A 106.83(9) . . . yes S7 Mo C 79.82(16) . . . yes S7 Mo C21 109.16(13) . . . yes S7 Mo C22 144.72(12) . . . yes S7 Mo C23 143.68(12) . . . yes S7 Mo C23A 108.36(11) . . . yes S7 Mo C27A 92.38(11) . . . yes C Mo C21 72.7(2) . . . yes C Mo C22 86.4(2) . . . yes C Mo C23 121.8(2) . . . yes C Mo C23A 129.6(2) . . . yes C Mo C27A 98.56(18) . . . yes C21 Mo C22 35.57(17) . . . yes C21 Mo C23 59.22(17) . . . yes C21 Mo C23A 57.45(17) . . . yes C21 Mo C27A 34.44(16) . . . yes C22 Mo C23 35.46(18) . . . yes C22 Mo C23A 57.88(16) . . . yes C22 Mo C27A 57.65(15) . . . yes C23 Mo C23A 35.38(15) . . . yes C23 Mo C27A 58.02(15) . . . yes C23A Mo C27A 33.66(15) . . . yes Mo S1 C2 107.86(18) . . . yes Mo S4 C3 103.11(17) . . . yes Mo S4 C5 104.57(18) . . . yes C3 S4 C5 102.3(3) . . . yes Mo S7 C6 109.5(2) . . . yes F5 F2 F6 99.9(18) . . . yes F5 F2 B 56.5(10) . . . yes F6 F2 B 61.1(16) . . . yes F3 F2 B 52.3(13) . . . yes F3 F2 F5 103.7(16) . . . yes F3 F2 F6 67.1(19) . . . yes F2 F3 F6 55.8(15) . . . yes F7 F3 B 64.0(17) . . . yes F2 F3 F7 120(2) . . . yes F2 F3 B 56.4(11) . . . yes F6 F3 F7 98(2) . . . yes F6 F3 B 57.0(16) . . . yes F5 F4 B 49.5(9) . . . yes F7 F4 B 46.6(8) . . . yes F5 F4 F7 96.1(12) . . . yes F4 F5 B 60.2(10) . . . yes F2 F5 F4 97.9(14) . . . yes F2 F5 B 58.0(11) . . . yes F2 F6 F3 57.1(16) . . . yes F2 F6 B 53.9(13) . . . yes F3 F6 B 47.4(15) . . . yes F3 F7 F4 93(2) . . . yes F3 F7 B 62.3(16) . . . yes F4 F7 B 57.6(12) . . . yes Mo C O 176.7(5) . . . yes S1 C2 C3 110.9(4) . . . yes S4 C3 C2 107.2(4) . . . yes S4 C5 C6 117.1(5) . . . yes S7 C6 C5 117.2(5) . . . yes Mo C21 C27A 78.3(3) . . . yes Mo C21 C22 71.1(3) . . . yes C22 C21 C27A 108.5(4) . . . no C21 C22 C23 108.6(4) . . . no Mo C22 C21 73.3(3) . . . yes Mo C22 C23 72.1(3) . . . yes Mo C23 C22 72.5(3) . . . yes Mo C23 C23A 77.8(3) . . . yes C22 C23 C23A 107.7(4) . . . no Mo C23A C23 66.8(2) . . . yes Mo C23A C24 125.5(3) . . . yes Mo C23A C27A 74.4(3) . . . yes C23 C23A C24 132.1(5) . . . no C23 C23A C27A 107.7(4) . . . no C24 C23A C27A 120.2(4) . . . no C23A C24 C25 117.7(5) . . . no C24 C25 C26 122.4(5) . . . no C25 C26 C27 122.2(5) . . . no C26 C27 C27A 117.5(5) . . . no C21 C27A C27 132.8(4) . . . no Mo C27A C21 67.3(3) . . . yes Mo C27A C23A 72.0(2) . . . yes C23A C27A C27 120.0(4) . . . no C21 C27A C23A 107.2(4) . . . no Mo C27A C27 124.4(3) . . . yes S1 C2 H22 109.42 . . . no C3 C2 H21 109.55 . . . no H21 C2 H22 108.09 . . . no C3 C2 H22 109.43 . . . no S1 C2 H21 109.43 . . . no S4 C3 H31 110.25 . . . no S4 C3 H32 110.24 . . . no C2 C3 H31 110.25 . . . no C2 C3 H32 110.29 . . . no H31 C3 H32 108.62 . . . no S4 C5 H51 108.03 . . . no S4 C5 H52 108.00 . . . no C6 C5 H51 108.05 . . . no H51 C5 H52 107.21 . . . no C6 C5 H52 108.06 . . . no S7 C6 H62 108.03 . . . no C5 C6 H61 108.00 . . . no S7 C6 H61 107.98 . . . no H61 C6 H62 107.29 . . . no C5 C6 H62 107.90 . . . no Mo C21 H211 116.71 . . . no C22 C21 H211 125.71 . . . no C27A C21 H211 125.83 . . . no Mo C22 H221 120.63 . . . no C21 C22 H221 125.77 . . . no C23 C22 H221 125.63 . . . no Mo C23 H231 115.75 . . . no C22 C23 H231 126.19 . . . no C23A C23 H231 126.12 . . . no C23A C24 H241 121.23 . . . no C25 C24 H241 121.09 . . . no C26 C25 H251 118.71 . . . no C24 C25 H251 118.89 . . . no C25 C26 H261 118.92 . . . no C27 C26 H261 118.90 . . . no C27A C27 H271 121.27 . . . no C26 C27 H271 121.19 . . . no F1 B F2 128.6(10) . . . yes F1 B F3 138.7(16) . . . yes F1 B F4 104.5(8) . . . yes F1 B F5 91.7(11) . . . yes F1 B F6 82.3(15) . . . yes F1 B F7 100.8(13) . . . yes F2 B F3 71.3(15) . . . yes F2 B F4 109.0(11) . . . yes F2 B F5 65.5(13) . . . yes F2 B F6 65.0(16) . . . yes F2 B F7 124.4(14) . . . yes F3 B F4 99.6(16) . . . yes F3 B F5 128.2(18) . . . yes F3 B F6 76(2) . . . yes F3 B F7 53.7(17) . . . yes F4 B F5 70.3(12) . . . yes F4 B F6 173.1(16) . . . yes F4 B F7 75.7(16) . . . yes F5 B F6 108.7(17) . . . yes F5 B F7 145.7(17) . . . yes F6 B F7 104(2) . . . yes # End of Crystallographic Information File