data_global # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in Organometallics ; _publ_contact_author ; R. Choukroun, C. Lorber ; _publ_contact_author_address ; Laboratoire de Chimie de Coordination 205 Route de Narbonne 31077 Toulouse Cedex 04 ; _publ_contact_author_email 'lorber@lcc-toulouse.fr' _publ_requested_journal 'Organometallics' #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Vanadocene-Mediated Ionization of Water in the Aqua-Species [H2O.B(C6F5)3]: Structural Characterization of the Hydride [Cp2V(m-H)B(C6F5)3] and the Hydroxide [Cp2V(m-OH)B(C6F5)3] Complexes. ; loop_ _publ_author_name _publ_author_address 'Robert Choukroun, Christian Lorber, Laure Vendier, and Christine Lepetit' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. MULTI SCAN - c.f. r.h. blessing, acta cryst. (1995), a51, 33-38 WINGX - 1.63 Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837. ORTEP3 for Windows, Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565.; ; #**************************************************************************** data_(1) #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H B F15, C10 H10 V' _chemical_formula_sum 'C28 H11 B F15 V' _chemical_formula_weight 694.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.733(2) _cell_length_b 15.9994(17) _cell_length_c 19.453(2) _cell_angle_alpha 90 _cell_angle_beta 95.807(9) _cell_angle_gamma 90 _cell_volume 5800.3(11) _cell_formula_units_Z 8 _cell_measurement_temperature 180 _cell_measurement_reflns_used 2714 _cell_measurement_theta_min 2.7662 _cell_measurement_theta_max 32.0875 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour 'blue grey' _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.59 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9236 _exptl_absorpt_correction_T_max 0.9706 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_unetI/netI 0.2141 _diffrn_reflns_number 29734 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 32.09 _diffrn_reflns_theta_full 32.09 _diffrn_measured_fraction_theta_full 0.931 _diffrn_measured_fraction_theta_max 0.931 _reflns_number_total 9503 _reflns_number_gt 2852 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9503 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1973 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.743 _refine_ls_restrained_S_all 0.743 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.375 _refine_diff_density_min -0.3 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.64040(19) 0.1527(2) 0.35081(18) 0.0436(9) Uani 1 1 d . . . H1 H 0.6472 0.2117 0.3395 0.052 Uiso 1 1 calc R . . C2 C 0.59562(18) 0.0952(2) 0.31154(17) 0.0428(9) Uani 1 1 d . . . H2 H 0.5663 0.1076 0.2681 0.051 Uiso 1 1 calc R . . C3 C 0.59565(19) 0.0198(2) 0.3479(2) 0.0481(10) Uani 1 1 d . . . H3 H 0.5664 -0.0297 0.3348 0.058 Uiso 1 1 calc R . . C4 C 0.6417(2) 0.0307(3) 0.40985(19) 0.0577(12) Uani 1 1 d . . . H4 H 0.6496 -0.0102 0.4472 0.069 Uiso 1 1 calc R . . C5 C 0.6682(2) 0.1128(3) 0.41148(18) 0.0523(11) Uani 1 1 d . . . H5 H 0.698 0.1388 0.45 0.063 Uiso 1 1 calc R . . C6 C 0.81293(18) 0.0054(2) 0.28057(18) 0.0424(9) Uani 1 1 d . . . H6 H 0.8285 0.0214 0.2358 0.051 Uiso 1 1 calc R . . C7 C 0.77410(19) -0.0683(2) 0.29352(17) 0.0424(9) Uani 1 1 d . . . H7 H 0.7587 -0.1122 0.26 0.051 Uiso 1 1 calc R . . C8 C 0.76797(19) -0.0697(2) 0.36532(18) 0.0439(10) Uani 1 1 d . . . H8 H 0.7468 -0.115 0.3904 0.053 Uiso 1 1 calc R . . C9 C 0.80269(19) 0.0024(2) 0.39581(18) 0.0466(10) Uani 1 1 d . . . H9 H 0.8098 0.0151 0.4453 0.056 Uiso 1 1 calc R . . C10 C 0.83051(18) 0.0480(2) 0.34329(18) 0.0446(9) Uani 1 1 d . . . H10 H 0.8603 0.0983 0.3497 0.054 Uiso 1 1 calc R . . C11 C 0.61904(17) 0.1425(2) 0.13635(16) 0.0329(8) Uani 1 1 d . . . C12 C 0.57059(18) 0.1204(2) 0.08093(17) 0.0385(9) Uani 1 1 d . . . C13 C 0.51277(19) 0.1687(3) 0.05596(19) 0.0492(11) Uani 1 1 d . . . C14 C 0.5011(2) 0.2436(3) 0.0869(2) 0.0557(11) Uani 1 1 d . . . C15 C 0.5479(2) 0.2686(3) 0.1409(2) 0.0527(11) Uani 1 1 d . . . C16 C 0.60443(19) 0.2188(2) 0.16389(18) 0.0398(9) Uani 1 1 d . . . C17 C 0.75813(16) 0.1478(2) 0.14316(15) 0.0286(8) Uani 1 1 d . . . C18 C 0.79988(18) 0.2014(2) 0.18670(15) 0.0337(8) Uani 1 1 d . . . C19 C 0.85000(18) 0.2550(2) 0.16526(17) 0.0370(9) Uani 1 1 d . . . C20 C 0.86155(18) 0.2579(2) 0.09660(17) 0.0369(8) Uani 1 1 d . . . C21 C 0.82305(17) 0.2060(2) 0.05118(15) 0.0327(8) Uani 1 1 d . . . C22 C 0.77178(17) 0.1548(2) 0.07433(15) 0.0314(8) Uani 1 1 d . . . C23 C 0.69073(17) -0.0080(2) 0.14239(15) 0.0316(8) Uani 1 1 d . . . C24 C 0.63249(18) -0.0581(2) 0.15251(15) 0.0347(8) Uani 1 1 d . . . C25 C 0.6249(2) -0.1406(2) 0.13485(16) 0.0406(9) Uani 1 1 d . . . C26 C 0.6792(2) -0.1791(2) 0.10493(18) 0.0485(10) Uani 1 1 d . . . C27 C 0.7398(2) -0.1344(2) 0.09432(17) 0.0453(10) Uani 1 1 d . . . C28 C 0.74367(18) -0.0515(2) 0.11318(15) 0.0352(8) Uani 1 1 d . . . F12 F 0.57782(10) 0.04760(14) 0.04602(9) 0.0498(5) Uani 1 1 d . . . F13 F 0.46734(11) 0.14164(15) 0.00172(11) 0.0687(7) Uani 1 1 d . . . F14 F 0.44423(12) 0.29087(16) 0.06282(14) 0.0874(8) Uani 1 1 d . . . F15 F 0.53806(14) 0.34283(16) 0.17211(13) 0.0841(8) Uani 1 1 d . . . F16 F 0.64949(12) 0.24975(12) 0.21687(10) 0.0517(6) Uani 1 1 d . . . F18 F 0.79201(10) 0.20371(12) 0.25573(8) 0.0456(5) Uani 1 1 d . . . F19 F 0.88684(11) 0.30731(13) 0.21049(10) 0.0547(6) Uani 1 1 d . . . F20 F 0.91043(11) 0.31090(13) 0.07498(10) 0.0538(6) Uani 1 1 d . . . F21 F 0.83358(10) 0.20770(12) -0.01661(8) 0.0445(5) Uani 1 1 d . . . F22 F 0.73213(9) 0.10856(12) 0.02602(8) 0.0404(5) Uani 1 1 d . . . F24 F 0.57681(10) -0.02419(12) 0.18188(9) 0.0455(5) Uani 1 1 d . . . F25 F 0.56615(12) -0.18355(13) 0.14548(10) 0.0599(6) Uani 1 1 d . . . F26 F 0.67454(13) -0.25955(14) 0.08576(11) 0.0686(7) Uani 1 1 d . . . F27 F 0.79371(12) -0.17127(13) 0.06506(10) 0.0647(7) Uani 1 1 d . . . F28 F 0.80675(10) -0.01306(12) 0.10209(10) 0.0499(5) Uani 1 1 d . . . V1 V 0.70898(3) 0.04495(4) 0.32100(3) 0.03235(16) Uani 1 1 d . . . B1 B 0.69182(19) 0.0902(3) 0.16421(17) 0.0309(9) Uani 1 1 d . . . H100 H 0.6978(11) 0.0937(14) 0.2332(11) 0.008(6) Uiso 1 1 d . . . 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 C1 0.050(2) 0.047(2) 0.036(2) -0.0058(18) 0.0164(19) 0.007(2) C2 0.033(2) 0.064(3) 0.033(2) 0.0015(19) 0.0116(17) 0.010(2) C3 0.034(2) 0.059(3) 0.055(3) 0.004(2) 0.023(2) -0.0044(19) C4 0.053(3) 0.088(4) 0.035(2) 0.023(2) 0.022(2) 0.016(2) C5 0.060(3) 0.071(3) 0.027(2) -0.005(2) 0.0106(19) 0.003(2) C6 0.036(2) 0.056(3) 0.036(2) 0.0087(18) 0.0075(17) 0.0131(19) C7 0.048(2) 0.044(3) 0.035(2) 0.0016(17) 0.0026(18) 0.0122(19) C8 0.045(2) 0.049(3) 0.036(2) 0.0142(17) 0.0005(18) 0.0061(19) C9 0.045(2) 0.064(3) 0.029(2) 0.0066(19) -0.0028(17) 0.001(2) C10 0.031(2) 0.057(3) 0.045(2) 0.004(2) -0.0028(17) -0.0083(19) C11 0.0308(19) 0.044(2) 0.0244(18) 0.0095(16) 0.0069(15) 0.0021(17) C12 0.034(2) 0.052(3) 0.031(2) 0.0102(18) 0.0098(17) 0.0003(19) C13 0.029(2) 0.082(3) 0.037(2) 0.026(2) 0.0040(18) -0.001(2) C14 0.036(2) 0.069(3) 0.063(3) 0.034(2) 0.009(2) 0.015(2) C15 0.052(3) 0.045(3) 0.064(3) 0.014(2) 0.023(2) 0.010(2) C16 0.035(2) 0.048(3) 0.037(2) 0.0113(18) 0.0084(18) 0.0031(19) C17 0.0284(18) 0.034(2) 0.0244(17) 0.0021(14) 0.0057(15) 0.0060(15) C18 0.043(2) 0.041(2) 0.0180(17) 0.0018(15) 0.0074(16) -0.0004(18) C19 0.039(2) 0.041(2) 0.0308(19) -0.0024(16) 0.0025(17) -0.0080(18) C20 0.035(2) 0.043(2) 0.033(2) 0.0064(17) 0.0053(17) -0.0080(18) C21 0.0332(19) 0.047(2) 0.0189(17) 0.0033(15) 0.0061(15) -0.0034(17) C22 0.0323(19) 0.039(2) 0.0226(17) -0.0027(15) 0.0015(15) -0.0002(17) C23 0.0291(19) 0.045(2) 0.0204(17) 0.0008(15) -0.0005(14) 0.0001(17) C24 0.036(2) 0.046(2) 0.0212(17) 0.0001(16) 0.0007(15) -0.0026(19) C25 0.046(2) 0.051(3) 0.0226(18) 0.0029(17) -0.0049(17) -0.010(2) C26 0.072(3) 0.038(3) 0.033(2) 0.0015(18) -0.005(2) 0.004(2) C27 0.059(3) 0.046(3) 0.031(2) 0.0007(18) 0.0058(19) 0.018(2) C28 0.035(2) 0.044(2) 0.0271(18) 0.0053(16) 0.0047(15) 0.0009(19) F12 0.0420(12) 0.0779(16) 0.0284(10) 0.0008(11) -0.0025(9) 0.0027(12) F13 0.0397(13) 0.112(2) 0.0520(14) 0.0318(13) -0.0082(11) -0.0034(13) F14 0.0530(15) 0.093(2) 0.115(2) 0.0485(16) 0.0040(15) 0.0252(15) F15 0.092(2) 0.0563(17) 0.106(2) 0.0076(14) 0.0183(16) 0.0298(15) F16 0.0638(15) 0.0431(13) 0.0489(13) -0.0024(10) 0.0089(12) 0.0045(11) F18 0.0615(14) 0.0561(14) 0.0196(10) -0.0021(9) 0.0061(9) -0.0085(11) F19 0.0644(14) 0.0602(15) 0.0388(12) -0.0049(10) 0.0031(11) -0.0235(12) F20 0.0546(14) 0.0617(15) 0.0463(13) 0.0033(10) 0.0115(11) -0.0227(12) F21 0.0505(13) 0.0606(14) 0.0241(10) 0.0046(9) 0.0127(9) -0.0083(11) F22 0.0419(12) 0.0581(13) 0.0214(10) -0.0030(9) 0.0039(9) -0.0102(10) F24 0.0376(12) 0.0606(15) 0.0393(12) -0.0009(10) 0.0093(10) -0.0087(10) F25 0.0649(15) 0.0693(16) 0.0439(13) 0.0015(11) -0.0019(11) -0.0295(13) F26 0.103(2) 0.0453(15) 0.0551(14) -0.0052(11) -0.0017(13) -0.0048(14) F27 0.0778(17) 0.0590(16) 0.0599(15) -0.0050(11) 0.0197(13) 0.0262(13) F28 0.0450(13) 0.0563(14) 0.0513(13) 0.0011(10) 0.0187(10) 0.0047(11) V1 0.0321(3) 0.0426(4) 0.0230(3) 0.0024(3) 0.0058(2) 0.0001(3) B1 0.028(2) 0.049(3) 0.0165(18) 0.0032(17) 0.0041(16) 0.0002(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.397(5) . ? C1 C2 1.414(5) . ? C1 V1 2.260(3) . ? C1 H1 0.98 . ? C2 C3 1.400(5) . ? C2 V1 2.261(3) . ? C2 H2 0.98 . ? C3 C4 1.420(5) . ? C3 V1 2.273(3) . ? C3 H3 0.98 . ? C4 C5 1.402(5) . ? C4 V1 2.252(3) . ? C4 H4 0.98 . ? C5 V1 2.264(3) . ? C5 H5 0.98 . ? C6 C10 1.406(5) . ? C6 C7 1.421(5) . ? C6 V1 2.263(3) . ? C6 H6 0.98 . ? C7 C8 1.413(4) . ? C7 V1 2.278(3) . ? C7 H7 0.98 . ? C8 C9 1.422(5) . ? C8 V1 2.269(3) . ? C8 H8 0.98 . ? C9 C10 1.399(5) . ? C9 V1 2.270(3) . ? C9 H9 0.98 . ? C10 V1 2.274(3) . ? C10 H10 0.98 . ? C11 C16 1.371(5) . ? C11 C12 1.382(4) . ? C11 B1 1.645(5) . ? C12 F12 1.361(4) . ? C12 C13 1.380(5) . ? C13 F13 1.357(4) . ? C13 C14 1.368(6) . ? C14 F14 1.352(4) . ? C14 C15 1.357(6) . ? C15 F15 1.354(4) . ? C15 C16 1.365(5) . ? C16 F16 1.357(4) . ? C17 C18 1.388(4) . ? C17 C22 1.393(4) . ? C17 B1 1.632(5) . ? C18 F18 1.366(3) . ? C18 C19 1.368(4) . ? C19 F19 1.350(4) . ? C19 C20 1.375(4) . ? C20 F20 1.347(3) . ? C20 C21 1.362(4) . ? C21 F21 1.353(3) . ? C21 C22 1.373(4) . ? C22 F22 1.355(3) . ? C23 C28 1.380(4) . ? C23 C24 1.384(4) . ? C23 B1 1.626(5) . ? C24 F24 1.352(3) . ? C24 C25 1.366(5) . ? C25 F25 1.331(4) . ? C25 C26 1.368(5) . ? C26 F26 1.339(4) . ? C26 C27 1.375(5) . ? C27 F27 1.345(4) . ? C27 C28 1.375(5) . ? C28 F28 1.368(4) . ? V1 H100 1.87(2) . ? B1 H100 1.34(2) . ? 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_3 _geom_angle_publ_flag C5 C1 C2 107.9(4) . . ? C5 C1 V1 72.1(2) . . ? C2 C1 V1 71.8(2) . . ? C5 C1 H1 125.9 . . ? C2 C1 H1 125.9 . . ? V1 C1 H1 125.9 . . ? C3 C2 C1 108.5(3) . . ? C3 C2 V1 72.5(2) . . ? C1 C2 V1 71.7(2) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? V1 C2 H2 125.6 . . ? C2 C3 C4 107.1(3) . . ? C2 C3 V1 71.56(19) . . ? C4 C3 V1 70.9(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? V1 C3 H3 126.4 . . ? C5 C4 C3 108.4(3) . . ? C5 C4 V1 72.4(2) . . ? C3 C4 V1 72.52(19) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? V1 C4 H4 125.7 . . ? C1 C5 C4 108.1(3) . . ? C1 C5 V1 71.88(19) . . ? C4 C5 V1 71.5(2) . . ? C1 C5 H5 125.9 . . ? C4 C5 H5 125.9 . . ? V1 C5 H5 125.9 . . ? C10 C6 C7 109.0(3) . . ? C10 C6 V1 72.4(2) . . ? C7 C6 V1 72.34(19) . . ? C10 C6 H6 125.4 . . ? C7 C6 H6 125.4 . . ? V1 C6 H6 125.4 . . ? C8 C7 C6 106.5(3) . . ? C8 C7 V1 71.6(2) . . ? C6 C7 V1 71.18(19) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? V1 C7 H7 126.6 . . ? C7 C8 C9 108.5(3) . . ? C7 C8 V1 72.23(19) . . ? C9 C8 V1 71.8(2) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? V1 C8 H8 125.7 . . ? C10 C9 C8 107.9(3) . . ? C10 C9 V1 72.2(2) . . ? C8 C9 V1 71.7(2) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? V1 C9 H9 125.9 . . ? C9 C10 C6 108.0(3) . . ? C9 C10 V1 71.9(2) . . ? C6 C10 V1 71.50(19) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? V1 C10 H10 125.9 . . ? C16 C11 C12 112.9(3) . . ? C16 C11 B1 121.1(3) . . ? C12 C11 B1 125.8(3) . . ? F12 C12 C13 114.8(3) . . ? F12 C12 C11 121.0(3) . . ? C13 C12 C11 124.2(4) . . ? F13 C13 C14 120.3(4) . . ? F13 C13 C12 120.3(4) . . ? C14 C13 C12 119.4(4) . . ? F14 C14 C15 121.9(4) . . ? F14 C14 C13 119.5(4) . . ? C15 C14 C13 118.5(4) . . ? F15 C15 C14 119.8(4) . . ? F15 C15 C16 120.1(4) . . ? C14 C15 C16 120.1(4) . . ? F16 C16 C15 116.0(4) . . ? F16 C16 C11 119.1(3) . . ? C15 C16 C11 124.8(4) . . ? C18 C17 C22 112.9(3) . . ? C18 C17 B1 126.2(3) . . ? C22 C17 B1 120.4(3) . . ? F18 C18 C19 115.4(3) . . ? F18 C18 C17 120.4(3) . . ? C19 C18 C17 124.2(3) . . ? F19 C19 C18 120.7(3) . . ? F19 C19 C20 119.4(3) . . ? C18 C19 C20 119.9(3) . . ? F20 C20 C21 120.8(3) . . ? F20 C20 C19 120.3(3) . . ? C21 C20 C19 118.9(3) . . ? F21 C21 C20 119.9(3) . . ? F21 C21 C22 120.6(3) . . ? C20 C21 C22 119.5(3) . . ? F22 C22 C21 116.7(3) . . ? F22 C22 C17 118.7(3) . . ? C21 C22 C17 124.5(3) . . ? C28 C23 C24 112.1(3) . . ? C28 C23 B1 127.1(3) . . ? C24 C23 B1 120.8(3) . . ? F24 C24 C25 115.3(3) . . ? F24 C24 C23 118.7(3) . . ? C25 C24 C23 125.9(3) . . ? F25 C25 C24 121.7(3) . . ? F25 C25 C26 119.7(4) . . ? C24 C25 C26 118.6(4) . . ? F26 C26 C25 121.3(4) . . ? F26 C26 C27 119.3(4) . . ? C25 C26 C27 119.4(4) . . ? F27 C27 C28 120.9(4) . . ? F27 C27 C26 120.2(4) . . ? C28 C27 C26 118.9(4) . . ? F28 C28 C27 114.5(3) . . ? F28 C28 C23 120.4(3) . . ? C27 C28 C23 125.1(3) . . ? C4 V1 C1 60.28(14) . . ? C4 V1 C2 60.32(13) . . ? C1 V1 C2 36.45(12) . . ? C4 V1 C6 143.75(14) . . ? C1 V1 C6 146.49(14) . . ? C2 V1 C6 154.87(12) . . ? C4 V1 C5 36.18(13) . . ? C1 V1 C5 35.98(12) . . ? C2 V1 C5 60.32(13) . . ? C6 V1 C5 140.71(14) . . ? C4 V1 C8 85.09(14) . . ? C1 V1 C8 141.97(13) . . ? C2 V1 C8 137.45(14) . . ? C6 V1 C8 60.17(13) . . ? C5 V1 C8 106.33(14) . . ? C4 V1 C9 86.20(14) . . ? C1 V1 C9 119.26(14) . . ? C2 V1 C9 144.96(13) . . ? C6 V1 C9 60.10(12) . . ? C5 V1 C9 86.90(14) . . ? C8 V1 C9 36.52(12) . . ? C4 V1 C3 36.57(13) . . ? C1 V1 C3 60.51(14) . . ? C2 V1 C3 35.96(12) . . ? C6 V1 C3 152.50(14) . . ? C5 V1 C3 60.60(14) . . ? C8 V1 C3 101.50(14) . . ? C9 V1 C3 118.60(14) . . ? C4 V1 C10 118.89(14) . . ? C1 V1 C10 121.31(14) . . ? C2 V1 C10 157.21(14) . . ? C6 V1 C10 36.09(12) . . ? C5 V1 C10 104.62(14) . . ? C8 V1 C10 60.28(14) . . ? C9 V1 C10 35.87(12) . . ? C3 V1 C10 154.13(14) . . ? C4 V1 C7 116.96(14) . . ? C1 V1 C7 176.98(14) . . ? C2 V1 C7 141.74(14) . . ? C6 V1 C7 36.48(12) . . ? C5 V1 C7 142.51(13) . . ? C8 V1 C7 36.22(11) . . ? C9 V1 C7 60.81(13) . . ? C3 V1 C7 116.61(14) . . ? C10 V1 C7 60.74(14) . . ? C4 V1 H100 136.3(7) . . ? C1 V1 H100 84.3(7) . . ? C2 V1 H100 76.0(7) . . ? C6 V1 H100 79.7(7) . . ? C5 V1 H100 119.6(7) . . ? C8 V1 H100 133.7(7) . . ? C9 V1 H100 136.0(7) . . ? C3 V1 H100 105.3(7) . . ? C10 V1 H100 100.6(7) . . ? C7 V1 H100 97.6(7) . . ? C23 B1 C17 118.0(3) . . ? C23 B1 C11 114.7(3) . . ? C17 B1 C11 104.8(3) . . ? C23 B1 H100 107.3(10) . . ? C17 B1 H100 104.0(10) . . ? C11 B1 H100 107.0(10) . . ? #====END data_(2) #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H11 B F15 O V' _chemical_formula_sum 'C28 H11 B F15 O V' _chemical_formula_weight 710.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9753(9) _cell_length_b 17.2725(13) _cell_length_c 12.4722(9) _cell_angle_alpha 90 _cell_angle_beta 103.225(6) _cell_angle_gamma 90 _cell_volume 2511.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180 _cell_measurement_reflns_used 6500 _cell_measurement_theta_min 3.1707 _cell_measurement_theta_max 32.2212 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.933 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0515 _diffrn_reflns_number 18345 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 26.31 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5126 _reflns_number_gt 3558 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5126 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.254 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1648(2) -0.30889(14) -0.4065(2) 0.0407(6) Uani 1 1 d . . . H1 H -0.0847 -0.2918 -0.3858 0.049 Uiso 1 1 calc R . . C2 C -0.23635(19) -0.31993(12) -0.33577(18) 0.0301(5) Uani 1 1 d . . . H2 H -0.2159 -0.3112 -0.256 0.036 Uiso 1 1 calc R . . C3 C -0.3405(2) -0.35082(12) -0.39535(19) 0.0342(6) Uani 1 1 d . . . H3 H -0.4043 -0.3684 -0.3644 0.041 Uiso 1 1 calc R . . C4 C -0.3318(3) -0.35981(13) -0.5037(2) 0.0478(7) Uani 1 1 d . . . H4 H -0.3884 -0.3849 -0.5627 0.057 Uiso 1 1 calc R . . C5 C -0.2234(3) -0.33373(15) -0.5111(2) 0.0533(8) Uani 1 1 d . . . H5 H -0.1911 -0.3373 -0.5764 0.064 Uiso 1 1 calc R . . C6 C -0.38624(18) -0.21041(13) -0.64711(16) 0.0279(5) Uani 1 1 d . . . H6 H -0.41 -0.2504 -0.7035 0.033 Uiso 1 1 calc R . . C7 C -0.27511(19) -0.17772(13) -0.61449(16) 0.0289(5) Uani 1 1 d . . . H7 H -0.2087 -0.1914 -0.6442 0.035 Uiso 1 1 calc R . . C8 C -0.27979(19) -0.11732(12) -0.54099(16) 0.0279(5) Uani 1 1 d . . . H8 H -0.217 -0.0819 -0.5092 0.033 Uiso 1 1 calc R . . C9 C -0.39310(19) -0.11216(12) -0.52905(16) 0.0264(5) Uani 1 1 d . . . H9 H -0.4225 -0.0729 -0.4859 0.032 Uiso 1 1 calc R . . C10 C -0.45875(19) -0.16962(12) -0.59379(16) 0.0281(5) Uani 1 1 d . . . H10 H -0.5418 -0.1767 -0.6052 0.034 Uiso 1 1 calc R . . C11 C -0.31409(16) -0.16567(11) -0.11788(15) 0.0179(4) Uani 1 1 d . . . C12 C -0.38937(16) -0.21979(11) -0.09218(15) 0.0198(5) Uani 1 1 d . . . C13 C -0.37552(18) -0.25795(12) 0.00683(16) 0.0232(5) Uani 1 1 d . . . C14 C -0.27950(18) -0.24302(12) 0.08739(15) 0.0234(5) Uani 1 1 d . . . C15 C -0.20215(17) -0.18949(12) 0.06829(16) 0.0242(5) Uani 1 1 d . . . C16 C -0.22114(17) -0.15142(11) -0.03106(16) 0.0217(5) Uani 1 1 d . . . C17 C -0.46301(16) -0.07356(11) -0.24224(15) 0.0169(4) Uani 1 1 d . . . C18 C -0.46034(16) -0.01657(11) -0.16298(15) 0.0195(5) Uani 1 1 d . . . C19 C -0.55363(18) 0.02572(12) -0.15146(16) 0.0222(5) Uani 1 1 d . . . C20 C -0.65849(17) 0.01212(12) -0.22145(17) 0.0229(5) Uani 1 1 d . . . C21 C -0.66629(16) -0.04199(12) -0.30313(16) 0.0213(5) Uani 1 1 d . . . C22 C -0.57019(17) -0.08334(11) -0.31100(15) 0.0189(4) Uani 1 1 d . . . C23 C -0.24314(16) -0.07307(11) -0.27107(15) 0.0180(4) Uani 1 1 d . . . C24 C -0.13388(16) -0.10296(11) -0.25985(15) 0.0192(5) Uani 1 1 d . . . C25 C -0.04385(17) -0.06461(12) -0.28762(17) 0.0243(5) Uani 1 1 d . . . C26 C -0.06009(17) 0.00833(13) -0.33099(16) 0.0260(5) Uani 1 1 d . . . C27 C -0.16679(18) 0.04135(12) -0.34482(16) 0.0229(5) Uani 1 1 d . . . C28 C -0.25417(16) 0.00102(12) -0.31539(15) 0.0206(5) Uani 1 1 d . . . F12 F -0.48608(9) -0.23820(7) -0.16961(9) 0.0286(3) Uani 1 1 d . . . F13 F -0.45409(10) -0.30909(7) 0.02395(9) 0.0344(3) Uani 1 1 d . . . F14 F -0.26099(10) -0.28041(7) 0.18446(9) 0.0342(3) Uani 1 1 d . . . F15 F -0.10811(10) -0.17399(7) 0.14823(9) 0.0367(3) Uani 1 1 d . . . F16 F -0.14260(9) -0.09658(7) -0.03907(9) 0.0310(3) Uani 1 1 d . . . F18 F -0.35912(9) -0.00041(6) -0.09271(9) 0.0270(3) Uani 1 1 d . . . F19 F -0.54432(10) 0.08026(7) -0.07275(9) 0.0322(3) Uani 1 1 d . . . F20 F -0.75089(10) 0.05228(7) -0.21039(10) 0.0350(3) Uani 1 1 d . . . F21 F -0.76678(9) -0.05373(7) -0.37557(9) 0.0305(3) Uani 1 1 d . . . F22 F -0.58701(9) -0.13632(7) -0.39417(9) 0.0272(3) Uani 1 1 d . . . F24 F -0.11008(9) -0.17537(6) -0.21819(9) 0.0268(3) Uani 1 1 d . . . F25 F 0.05993(9) -0.09853(7) -0.27173(10) 0.0344(3) Uani 1 1 d . . . F26 F 0.02499(10) 0.04710(8) -0.36003(10) 0.0410(3) Uani 1 1 d . . . F27 F -0.18553(10) 0.11305(7) -0.38671(10) 0.0344(3) Uani 1 1 d . . . F28 F -0.35649(9) 0.03797(6) -0.33710(9) 0.0290(3) Uani 1 1 d . . . V1 V -0.32125(3) -0.23127(2) -0.46510(3) 0.01990(9) Uani 1 1 d . . . O1 O -0.37094(13) -0.18838(8) -0.32656(11) 0.0205(3) Uani 1 1 d . . . B1 B -0.34661(19) -0.12422(13) -0.24117(18) 0.0184(5) Uani 1 1 d . . . HO1 H -0.4218(19) -0.2122(13) -0.3223(18) 0.037(8) Uiso 1 1 d . . . 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 C1 0.0303(14) 0.0338(15) 0.0599(17) 0.0143(13) 0.0143(13) 0.0181(11) C2 0.0358(14) 0.0221(13) 0.0285(12) 0.0067(10) -0.0006(11) 0.0110(10) C3 0.0352(14) 0.0208(13) 0.0453(15) 0.0088(11) 0.0061(12) 0.0007(10) C4 0.073(2) 0.0193(14) 0.0408(16) -0.0083(12) -0.0095(15) 0.0098(13) C5 0.090(2) 0.0344(16) 0.0458(17) 0.0077(13) 0.0369(17) 0.0350(16) C6 0.0356(14) 0.0315(13) 0.0145(10) 0.0001(9) 0.0017(10) -0.0017(10) C7 0.0359(14) 0.0339(14) 0.0192(11) 0.0036(10) 0.0109(10) -0.0011(11) C8 0.0374(14) 0.0254(13) 0.0203(11) 0.0027(10) 0.0055(10) -0.0047(10) C9 0.0376(14) 0.0218(12) 0.0184(11) 0.0064(9) 0.0040(10) 0.0082(10) C10 0.0259(12) 0.0314(13) 0.0243(12) 0.0049(10) -0.0001(10) 0.0042(10) C11 0.0184(11) 0.0174(11) 0.0193(10) -0.0010(9) 0.0070(9) 0.0036(8) C12 0.0184(11) 0.0226(12) 0.0172(10) -0.0034(9) 0.0014(9) 0.0024(9) C13 0.0292(13) 0.0174(12) 0.0267(12) -0.0002(9) 0.0139(10) 0.0017(9) C14 0.0329(13) 0.0248(12) 0.0143(10) 0.0040(9) 0.0092(10) 0.0106(10) C15 0.0224(12) 0.0293(13) 0.0186(11) -0.0028(10) 0.0001(9) 0.0067(9) C16 0.0200(11) 0.0226(12) 0.0234(11) 0.0009(9) 0.0066(9) 0.0007(9) C17 0.0182(11) 0.0167(11) 0.0164(10) 0.0028(9) 0.0053(9) -0.0007(8) C18 0.0165(11) 0.0228(12) 0.0182(10) 0.0028(9) 0.0021(9) -0.0015(9) C19 0.0286(13) 0.0197(12) 0.0198(11) -0.0024(9) 0.0087(10) -0.0005(9) C20 0.0192(12) 0.0218(12) 0.0309(12) 0.0041(10) 0.0125(10) 0.0063(9) C21 0.0154(11) 0.0252(12) 0.0229(11) 0.0044(10) 0.0037(9) -0.0020(9) C22 0.0231(12) 0.0177(11) 0.0174(10) 0.0004(9) 0.0081(9) -0.0011(9) C23 0.0192(11) 0.0201(11) 0.0148(10) -0.0021(9) 0.0039(9) 0.0008(8) C24 0.0217(12) 0.0188(11) 0.0164(10) 0.0013(9) 0.0026(9) 0.0003(9) C25 0.0169(12) 0.0309(13) 0.0250(11) -0.0008(10) 0.0049(9) 0.0029(9) C26 0.0218(12) 0.0306(13) 0.0271(12) 0.0006(10) 0.0091(10) -0.0093(10) C27 0.0309(13) 0.0163(11) 0.0219(11) 0.0004(9) 0.0070(10) -0.0030(9) C28 0.0176(11) 0.0230(12) 0.0206(11) 0.0003(9) 0.0033(9) 0.0043(9) F12 0.0276(7) 0.0319(7) 0.0253(6) 0.0003(6) 0.0036(5) -0.0092(5) F13 0.0420(8) 0.0317(8) 0.0339(7) 0.0053(6) 0.0176(6) -0.0076(6) F14 0.0491(8) 0.0365(8) 0.0189(6) 0.0083(6) 0.0118(6) 0.0108(6) F15 0.0301(7) 0.0517(9) 0.0234(7) 0.0019(6) -0.0038(6) 0.0034(6) F16 0.0264(7) 0.0370(8) 0.0269(7) 0.0010(6) 0.0005(6) -0.0096(6) F18 0.0223(7) 0.0278(7) 0.0284(7) -0.0068(5) 0.0009(5) -0.0012(5) F19 0.0358(8) 0.0285(7) 0.0342(7) -0.0105(6) 0.0123(6) 0.0025(6) F20 0.0255(7) 0.0384(8) 0.0437(8) -0.0022(6) 0.0129(6) 0.0119(6) F21 0.0153(6) 0.0392(8) 0.0350(7) 0.0002(6) 0.0017(6) 0.0015(5) F22 0.0216(6) 0.0322(7) 0.0265(6) -0.0091(6) 0.0032(5) -0.0003(5) F24 0.0235(7) 0.0225(7) 0.0346(7) 0.0061(6) 0.0074(5) 0.0061(5) F25 0.0175(7) 0.0450(8) 0.0421(8) 0.0074(6) 0.0099(6) 0.0050(6) F26 0.0285(7) 0.0445(9) 0.0532(9) 0.0117(7) 0.0158(7) -0.0089(6) F27 0.0417(8) 0.0210(7) 0.0431(8) 0.0094(6) 0.0152(6) -0.0014(6) F28 0.0250(7) 0.0232(7) 0.0402(7) 0.0088(6) 0.0104(6) 0.0071(5) V1 0.0225(2) 0.01896(19) 0.01816(18) 0.00014(16) 0.00437(15) 0.00347(15) O1 0.0206(9) 0.0210(9) 0.0209(8) -0.0025(6) 0.0067(7) -0.0022(7) B1 0.0195(13) 0.0176(13) 0.0183(12) -0.0020(10) 0.0048(10) 0.0014(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.376(3) . ? C1 C5 1.400(3) . ? C1 V1 2.284(2) . ? C1 H1 0.98 . ? C2 C3 1.403(3) . ? C2 V1 2.288(2) . ? C2 H2 0.98 . ? C3 C4 1.388(3) . ? C3 V1 2.273(2) . ? C3 H3 0.98 . ? C4 C5 1.396(4) . ? C4 V1 2.269(2) . ? C4 H4 0.98 . ? C5 V1 2.267(2) . ? C5 H5 0.98 . ? C6 C10 1.399(3) . ? C6 C7 1.417(3) . ? C6 V1 2.254(2) . ? C6 H6 0.98 . ? C7 C8 1.398(3) . ? C7 V1 2.260(2) . ? C7 H7 0.98 . ? C8 C9 1.401(3) . ? C8 V1 2.288(2) . ? C8 H8 0.98 . ? C9 C10 1.401(3) . ? C9 V1 2.302(2) . ? C9 H9 0.98 . ? C10 V1 2.284(2) . ? C10 H10 0.98 . ? C11 C16 1.386(3) . ? C11 C12 1.386(3) . ? C11 B1 1.660(3) . ? C12 F12 1.365(2) . ? C12 C13 1.376(3) . ? C13 F13 1.343(2) . ? C13 C14 1.367(3) . ? C14 F14 1.346(2) . ? C14 C15 1.368(3) . ? C15 F15 1.349(2) . ? C15 C16 1.375(3) . ? C16 F16 1.354(2) . ? C17 C22 1.381(3) . ? C17 C18 1.390(3) . ? C17 B1 1.643(3) . ? C18 F18 1.352(2) . ? C18 C19 1.370(3) . ? C19 F19 1.346(2) . ? C19 C20 1.376(3) . ? C20 F20 1.340(2) . ? C20 C21 1.369(3) . ? C21 F21 1.345(2) . ? C21 C22 1.377(3) . ? C22 F22 1.363(2) . ? C23 C24 1.384(3) . ? C23 C28 1.389(3) . ? C23 B1 1.633(3) . ? C24 F24 1.360(2) . ? C24 C25 1.375(3) . ? C25 F25 1.347(2) . ? C25 C26 1.368(3) . ? C26 F26 1.337(2) . ? C26 C27 1.374(3) . ? C27 F27 1.343(2) . ? C27 C28 1.375(3) . ? C28 F28 1.353(2) . ? V1 O1 2.0875(14) . ? O1 B1 1.518(3) . ? O1 HO1 0.75(2) . ? 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_3 _geom_angle_publ_flag C2 C1 C5 107.6(2) . . ? C2 C1 V1 72.63(12) . . ? C5 C1 V1 71.42(13) . . ? C2 C1 H1 126.1 . . ? C5 C1 H1 126.1 . . ? V1 C1 H1 126.1 . . ? C1 C2 C3 108.8(2) . . ? C1 C2 V1 72.34(13) . . ? C3 C2 V1 71.52(12) . . ? C1 C2 H2 125.5 . . ? C3 C2 H2 125.5 . . ? V1 C2 H2 125.5 . . ? C4 C3 C2 107.6(2) . . ? C4 C3 V1 72.03(14) . . ? C2 C3 V1 72.66(12) . . ? C4 C3 H3 126 . . ? C2 C3 H3 126 . . ? V1 C3 H3 126 . . ? C3 C4 C5 107.8(2) . . ? C3 C4 V1 72.39(13) . . ? C5 C4 V1 72.01(14) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? V1 C4 H4 125.9 . . ? C4 C5 C1 108.2(2) . . ? C4 C5 V1 72.14(14) . . ? C1 C5 V1 72.75(13) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? V1 C5 H5 125.8 . . ? C10 C6 C7 107.9(2) . . ? C10 C6 V1 73.20(12) . . ? C7 C6 V1 71.91(11) . . ? C10 C6 H6 125.9 . . ? C7 C6 H6 125.9 . . ? V1 C6 H6 125.9 . . ? C8 C7 C6 108.02(19) . . ? C8 C7 V1 73.20(12) . . ? C6 C7 V1 71.51(12) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? V1 C7 H7 125.8 . . ? C7 C8 C9 107.60(19) . . ? C7 C8 V1 71.00(12) . . ? C9 C8 V1 72.77(12) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? V1 C8 H8 126.1 . . ? C10 C9 C8 108.84(19) . . ? C10 C9 V1 71.50(12) . . ? C8 C9 V1 71.67(12) . . ? C10 C9 H9 125.5 . . ? C8 C9 H9 125.5 . . ? V1 C9 H9 125.5 . . ? C6 C10 C9 107.6(2) . . ? C6 C10 V1 70.90(12) . . ? C9 C10 V1 72.91(11) . . ? C6 C10 H10 126.1 . . ? C9 C10 H10 126.1 . . ? V1 C10 H10 126.1 . . ? C16 C11 C12 112.78(17) . . ? C16 C11 B1 128.58(18) . . ? C12 C11 B1 118.57(17) . . ? F12 C12 C13 115.60(17) . . ? F12 C12 C11 118.98(17) . . ? C13 C12 C11 125.42(18) . . ? F13 C13 C14 120.60(18) . . ? F13 C13 C12 120.87(18) . . ? C14 C13 C12 118.53(19) . . ? F14 C14 C13 120.57(19) . . ? F14 C14 C15 120.20(18) . . ? C13 C14 C15 119.23(18) . . ? F15 C15 C14 119.28(18) . . ? F15 C15 C16 120.61(19) . . ? C14 C15 C16 120.11(19) . . ? F16 C16 C15 115.26(17) . . ? F16 C16 C11 120.88(17) . . ? C15 C16 C11 123.85(19) . . ? C22 C17 C18 113.24(17) . . ? C22 C17 B1 127.32(17) . . ? C18 C17 B1 119.33(16) . . ? F18 C18 C19 116.99(17) . . ? F18 C18 C17 118.55(17) . . ? C19 C18 C17 124.45(18) . . ? F19 C19 C18 121.07(18) . . ? F19 C19 C20 119.54(18) . . ? C18 C19 C20 119.38(18) . . ? F20 C20 C21 120.83(18) . . ? F20 C20 C19 120.14(18) . . ? C21 C20 C19 119.02(18) . . ? F21 C21 C20 120.03(18) . . ? F21 C21 C22 120.56(18) . . ? C20 C21 C22 119.41(18) . . ? F22 C22 C21 114.96(17) . . ? F22 C22 C17 120.58(17) . . ? C21 C22 C17 124.46(18) . . ? C24 C23 C28 112.71(17) . . ? C24 C23 B1 121.61(18) . . ? C28 C23 B1 125.57(17) . . ? F24 C24 C25 115.56(17) . . ? F24 C24 C23 119.53(17) . . ? C25 C24 C23 124.91(19) . . ? F25 C25 C26 120.15(18) . . ? F25 C25 C24 120.21(19) . . ? C26 C25 C24 119.64(19) . . ? F26 C26 C25 121.37(19) . . ? F26 C26 C27 120.17(19) . . ? C25 C26 C27 118.46(18) . . ? F27 C27 C26 119.99(18) . . ? F27 C27 C28 120.10(18) . . ? C26 C27 C28 119.91(19) . . ? F28 C28 C27 114.65(18) . . ? F28 C28 C23 120.93(17) . . ? C27 C28 C23 124.37(18) . . ? O1 V1 C6 132.73(7) . . ? O1 V1 C7 135.00(7) . . ? C6 V1 C7 36.58(7) . . ? O1 V1 C5 138.39(8) . . ? C6 V1 C5 87.12(9) . . ? C7 V1 C5 82.72(9) . . ? O1 V1 C4 120.66(8) . . ? C6 V1 C4 87.35(9) . . ? C7 V1 C4 103.78(9) . . ? C5 V1 C4 35.85(9) . . ? O1 V1 C3 86.11(7) . . ? C6 V1 C3 119.31(8) . . ? C7 V1 C3 138.88(8) . . ? C5 V1 C3 59.41(9) . . ? C4 V1 C3 35.58(8) . . ? O1 V1 C10 96.90(7) . . ? C6 V1 C10 35.90(7) . . ? C7 V1 C10 60.14(8) . . ? C5 V1 C10 121.18(9) . . ? C4 V1 C10 108.15(9) . . ? C3 V1 C10 124.98(8) . . ? O1 V1 C1 108.14(8) . . ? C6 V1 C1 119.06(9) . . ? C7 V1 C1 99.64(9) . . ? C5 V1 C1 35.83(9) . . ? C4 V1 C1 59.67(9) . . ? C3 V1 C1 59.42(8) . . ? C10 V1 C1 154.95(9) . . ? O1 V1 C8 99.64(7) . . ? C6 V1 C8 60.18(8) . . ? C7 V1 C8 35.80(7) . . ? C5 V1 C8 113.17(9) . . ? C4 V1 C8 139.55(9) . . ? C3 V1 C8 172.25(8) . . ? C10 V1 C8 59.81(8) . . ? C1 V1 C8 113.47(9) . . ? O1 V1 C2 79.55(7) . . ? C6 V1 C2 144.39(8) . . ? C7 V1 C2 134.66(8) . . ? C5 V1 C2 58.91(8) . . ? C4 V1 C2 59.23(8) . . ? C3 V1 C2 35.81(7) . . ? C10 V1 C2 160.22(8) . . ? C1 V1 C2 35.03(8) . . ? C8 V1 C2 139.88(8) . . ? O1 V1 C9 79.35(7) . . ? C6 V1 C9 59.46(8) . . ? C7 V1 C9 59.36(8) . . ? C5 V1 C9 141.63(9) . . ? C4 V1 C9 143.42(8) . . ? C3 V1 C9 151.94(8) . . ? C10 V1 C9 35.58(7) . . ? C1 V1 C9 148.24(9) . . ? C8 V1 C9 35.55(7) . . ? C2 V1 C9 156.05(8) . . ? B1 O1 V1 142.57(13) . . ? B1 O1 HO1 112.4(18) . . ? V1 O1 HO1 104.7(18) . . ? O1 B1 C23 105.57(15) . . ? O1 B1 C17 110.89(16) . . ? C23 B1 C17 113.36(16) . . ? O1 B1 C11 107.55(16) . . ? C23 B1 C11 114.57(16) . . ? C17 B1 C11 104.85(15) . . ? #====END