# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1803 data_global _publ_contact_author_name 'Malcolm L.H.Green' _publ_contact_author_address ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; _publ_contact_author_phone '(01865) 272649' _publ_contact_author_fax '(01865) 272690 ' _publ_contact_author_email 'Malcolm.Green@chemistry.ox.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Electrophilic Addition Reactions of the Lewis Acids BR(C6F5)2 [R = C6F5, C6H5, H or Cl] with the Metallocene-hydrides [M(?-C5H5)2H2] (M = Mo or W,) [Re(?-C5H5)2H] and [Ta(?-C5H5)2H3] ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references ; # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # Chebychev Weights # Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 # Denzo # Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # Azimutal absorption correction # North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. # DIFABS # Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. # RC93 # Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #============= Material Relevant to Compound(4)===================== data_1 _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 8.470(4) _cell_angle_alpha 80.26(3) _cell_length_b 10.106(4) _cell_angle_beta 74.88(3) _cell_length_c 13.403(3) _cell_angle_gamma 67.53(2) _cell_volume 1020.4(5) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'W ' -1.4210 6.8720 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C22 H12 B Cl F10 W' _chemical_formula_moiety 'C22 H12 B Cl F10 W' _chemical_compound_source ; ? ; _chemical_formula_weight 696.43 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 125 _cell_formula_units_Z 2 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_max 0.4 _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 657.80 _exptl_absorpt_coefficient_mu 5.90 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 125 _diffrn_reflns_number 5082 _reflns_number_total 3795 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 3795 # Number of reflections without Friedels Law is 0 _reflns_number_gt 3539 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -9 _reflns_limit_h_max 10 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -1.75 _refine_diff_density_max 1.75 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3539 _refine_ls_number_parameters 316 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0296 _refine_ls_goodness_of_fit_ref 1.0594 _refine_ls_shift/su_max 0.002306 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 2.24 -.389 1.78 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type W1 1.728684(16) 0.062346(12) 0.21561(1) 0.0150 1.0000 Uani Cl1 1.18946(11) 0.17543(9) 0.38425(7) 0.0203 1.0000 Uani F21 0.9475(3) 0.5378(2) 0.33851(18) 0.0246 1.0000 Uani F22 0.6795(3) 0.6659(2) 0.2473(2) 0.0314 1.0000 Uani F23 0.6650(3) 0.5615(3) 0.0754(2) 0.0316 1.0000 Uani F24 0.9359(3) 0.3263(3) -0.00324(18) 0.0282 1.0000 Uani F25 1.2103(3) 0.2015(2) 0.08152(18) 0.0266 1.0000 Uani F31 1.3064(3) 0.5405(2) 0.13724(16) 0.0204 1.0000 Uani F32 1.3252(3) 0.7755(2) 0.18933(18) 0.0246 1.0000 Uani F33 1.3309(3) 0.7987(2) 0.38770(19) 0.0269 1.0000 Uani F34 1.3191(3) 0.5773(2) 0.53353(18) 0.0235 1.0000 Uani F35 1.3042(3) 0.3417(2) 0.48573(16) 0.0219 1.0000 Uani C1 1.4403(4) 0.1901(3) 0.1950(3) 0.0167 1.0000 Uani C2 1.4826(5) 0.0397(4) 0.1884(3) 0.0194 1.0000 Uani C3 1.6188(5) -0.0079(4) 0.1015(3) 0.0278 1.0000 Uani C4 1.6678(6) 0.1123(5) 0.0529(3) 0.0322 1.0000 Uani C5 1.5559(5) 0.2332(4) 0.1104(3) 0.0212 1.0000 Uani C6 1.6317(5) 0.0802(4) 0.3908(3) 0.0269 1.0000 Uani C7 1.6831(5) -0.0658(4) 0.3715(3) 0.0262 1.0000 Uani C8 1.8634(5) -0.1170(4) 0.3322(3) 0.0245 1.0000 Uani C9 1.9243(5) -0.0017(4) 0.3231(3) 0.0276 1.0000 Uani C10 1.7803(6) 0.1195(4) 0.3617(3) 0.0306 1.0000 Uani C20 1.0998(4) 0.3653(4) 0.2129(3) 0.0171 1.0000 Uani C21 0.9538(4) 0.4822(4) 0.2524(3) 0.0179 1.0000 Uani C22 0.8109(4) 0.5495(4) 0.2072(3) 0.0217 1.0000 Uani C23 0.8024(4) 0.4987(4) 0.1210(3) 0.0199 1.0000 Uani C24 0.9413(5) 0.3788(4) 0.0797(3) 0.0203 1.0000 Uani C25 1.0833(4) 0.3173(4) 0.1264(3) 0.0176 1.0000 Uani C30 1.3031(4) 0.4255(3) 0.3080(3) 0.0141 1.0000 Uani C31 1.3127(4) 0.5424(3) 0.2362(3) 0.0152 1.0000 Uani C32 1.3202(4) 0.6675(4) 0.2618(3) 0.0179 1.0000 Uani C33 1.3207(4) 0.6799(3) 0.3623(3) 0.0182 1.0000 Uani C34 1.3149(4) 0.5681(4) 0.4358(3) 0.0173 1.0000 Uani C35 1.3083(4) 0.4439(3) 0.4072(3) 0.0155 1.0000 Uani B1 1.2672(5) 0.2943(4) 0.2704(3) 0.0144 1.0000 Uani H202 1.7802 0.1925 0.1931 0.0207 1.0000 Uiso H203 1.8922 0.0743 0.1455 0.0149 1.0000 Uiso H204 1.8515 -0.0572 0.1602 0.0308 1.0000 Uiso H21 1.4239 -0.0224 0.2383 0.0600 1.0000 Uiso H31 1.6717 -0.1074 0.0777 0.0600 1.0000 Uiso H41 1.7628 0.1116 -0.0099 0.0600 1.0000 Uiso H51 1.5589 0.3326 0.0937 0.0600 1.0000 Uiso H61 1.5107 0.1440 0.4202 0.0600 1.0000 Uiso H71 1.6040 -0.1222 0.3839 0.0600 1.0000 Uiso H81 1.9371 -0.2172 0.3135 0.0600 1.0000 Uiso H91 2.0474 -0.0053 0.2945 0.0600 1.0000 Uiso H101 1.7836 0.2158 0.3673 0.0600 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01734(9) 0.01497(9) 0.01092(11) -0.00109(5) -0.00160(6) -0.00465(6) Cl1 0.0289(4) 0.0220(4) 0.0132(4) 0.0009(3) -0.0029(3) -0.0146(3) F21 0.022(1) 0.0288(11) 0.0241(13) -0.0154(9) 0.0005(8) -0.0079(9) F22 0.018(1) 0.0271(11) 0.0454(16) -0.013(1) -0.004(1) -0.0022(9) F23 0.023(1) 0.0415(13) 0.0313(14) 0.005(1) -0.013(1) -0.010(1) F24 0.0319(11) 0.0430(13) 0.0158(12) -0.0035(9) -0.0102(9) -0.016(1) F25 0.027(1) 0.0312(11) 0.0206(13) -0.0156(9) -0.0063(9) -0.0024(9) F31 0.030(1) 0.023(1) 0.0124(11) 0.0020(7) -0.0082(8) -0.0129(8) F32 0.0350(11) 0.019(1) 0.0224(13) 0.0050(8) -0.0094(9) -0.0128(9) F33 0.0374(12) 0.021(1) 0.0297(14) -0.0065(8) -0.008(1) -0.0158(9) F34 0.0324(11) 0.025(1) 0.0161(12) -0.0076(8) -0.0077(9) -0.0099(9) F35 0.0368(12) 0.0180(9) 0.0111(11) -0.0005(7) -0.0059(9) -0.0097(9) C1 0.0195(15) 0.0186(15) 0.0123(18) -0.0001(12) -0.0090(13) -0.0040(12) C2 0.0230(16) 0.0205(16) 0.0173(19) -0.0084(12) -0.0098(14) -0.0040(13) C3 0.033(2) 0.0269(18) 0.020(2) -0.0099(14) -0.0099(16) 0.0002(15) C4 0.033(2) 0.040(2) 0.013(2) -0.0042(15) -0.0034(16) -0.0010(17) C5 0.0219(16) 0.0228(17) 0.0110(19) 0.0035(13) -0.0038(13) -0.0012(13) C6 0.0306(19) 0.0308(19) 0.014(2) -0.0069(14) -0.0069(15) -0.0017(15) C7 0.0318(19) 0.0289(19) 0.017(2) 0.0075(14) -0.0076(15) -0.0118(15) C8 0.0314(19) 0.0175(16) 0.025(2) -0.0005(14) -0.0150(16) -0.0041(14) C9 0.0315(19) 0.0320(19) 0.026(2) -0.0020(15) -0.0152(16) -0.0130(16) C10 0.043(2) 0.0252(18) 0.028(2) -0.0093(15) -0.0155(18) -0.0096(17) C20 0.0207(16) 0.0214(16) 0.0108(18) -0.0034(12) -0.0002(12) -0.0105(13) C21 0.0169(15) 0.0198(15) 0.0193(19) -0.0047(12) -0.0020(13) -0.0090(13) C22 0.0187(16) 0.0207(16) 0.022(2) -0.0044(13) 0.0023(14) -0.0065(13) C23 0.0184(15) 0.0263(17) 0.016(2) 0.0030(13) -0.0055(13) -0.0097(14) C24 0.0224(16) 0.0276(18) 0.0163(19) 0.0010(13) -0.0054(14) -0.0151(14) C25 0.0204(15) 0.0204(15) 0.0112(18) -0.0022(12) -0.0020(13) -0.0071(13) C30 0.0155(14) 0.0156(14) 0.0109(17) -0.0021(11) -0.0027(12) -0.0048(11) C31 0.0147(14) 0.0184(15) 0.0127(18) -0.0019(12) -0.0031(12) -0.0057(12) C32 0.0172(14) 0.0161(15) 0.0193(19) 0.0003(12) -0.0048(13) -0.0048(12) C33 0.0192(15) 0.0142(14) 0.023(2) -0.0046(12) -0.0058(13) -0.0054(12) C34 0.0170(14) 0.0205(15) 0.0146(19) -0.0074(12) -0.0020(12) -0.0054(12) C35 0.0162(14) 0.0158(15) 0.0121(18) -0.0010(11) -0.0021(12) -0.0035(11) B1 0.0221(17) 0.0142(15) 0.0083(19) -0.0022(12) -0.0033(14) -0.0074(13) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 . C1 . 2.352(3) yes W1 . C2 . 2.307(3) yes W1 . C3 . 2.308(4) yes W1 . C4 . 2.300(4) yes W1 . C5 . 2.331(3) yes W1 . C6 . 2.291(4) yes W1 . C7 . 2.289(4) yes W1 . C8 . 2.328(4) yes W1 . C9 . 2.313(4) yes W1 . C10 . 2.319(4) yes W1 . H202 . 1.49875(12) no W1 . H203 . 1.49236(12) no W1 . H204 . 1.42613(12) no Cl1 . B1 . 1.915(4) yes F21 . C21 . 1.347(4) yes F22 . C22 . 1.346(4) yes F23 . C23 . 1.344(4) yes F24 . C24 . 1.328(4) yes F25 . C25 . 1.352(4) yes F31 . C31 . 1.345(4) yes F32 . C32 . 1.339(4) yes F33 . C33 . 1.341(4) yes F34 . C34 . 1.340(4) yes F35 . C35 . 1.347(4) yes C1 . C2 . 1.435(4) yes C1 . C5 . 1.419(5) yes C1 . B1 . 1.639(5) yes C2 . C3 . 1.408(6) yes C2 . H21 . 1.005(4) no C3 . C4 . 1.431(6) yes C3 . H31 . 1.002(4) no C4 . C5 . 1.427(5) yes C4 . H41 . 1.000(4) no C5 . H51 . 1.001(4) no C6 . C7 . 1.419(6) yes C6 . C10 . 1.402(6) yes C6 . H61 . 0.996(4) no C7 . C8 . 1.395(6) yes C7 . H71 . 1.001(4) no C8 . C9 . 1.421(5) yes C8 . H81 . 0.999(4) no C9 . C10 . 1.413(6) yes C9 . H91 . 1.001(4) no C10 . H101 . 1.000(4) no C20 . C21 . 1.400(5) yes C20 . C25 . 1.388(5) yes C20 . B1 . 1.650(5) yes C21 . C22 . 1.381(5) yes C22 . C23 . 1.371(5) yes C23 . C24 . 1.399(5) yes C24 . C25 . 1.383(5) yes C30 . C31 . 1.406(5) yes C30 . C35 . 1.387(5) yes C30 . B1 . 1.649(4) yes C31 . C32 . 1.393(5) yes C32 . C33 . 1.375(5) yes C33 . C34 . 1.375(5) yes C34 . C35 . 1.398(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . W1 . C2 . 35.88(11) yes C1 . W1 . C3 . 59.87(12) yes C2 . W1 . C3 . 35.54(14) yes C1 . W1 . C4 . 59.89(13) yes C2 . W1 . C4 . 59.59(15) yes C3 . W1 . C4 . 36.19(16) yes C1 . W1 . C5 . 35.28(12) yes C2 . W1 . C5 . 58.90(13) yes C3 . W1 . C5 . 59.54(14) yes C4 . W1 . C5 . 35.89(14) yes C1 . W1 . C6 . 89.10(13) yes C2 . W1 . C6 . 96.08(14) yes C3 . W1 . C6 . 129.60(15) yes C4 . W1 . C6 . 148.98(14) yes C5 . W1 . C6 . 116.61(13) yes C1 . W1 . C7 . 101.50(13) yes C2 . W1 . C7 . 86.69(13) yes C3 . W1 . C7 . 107.88(15) yes C4 . W1 . C7 . 143.56(16) yes C5 . W1 . C7 . 136.71(13) yes C1 . W1 . C8 . 136.26(13) yes C2 . W1 . C8 . 112.98(13) yes C3 . W1 . C8 . 116.35(14) yes C4 . W1 . C8 . 145.08(14) yes C5 . W1 . C8 . 171.27(13) yes C1 . W1 . C9 . 146.79(14) yes C2 . W1 . C9 . 145.90(14) yes C3 . W1 . C9 . 147.93(14) yes C4 . W1 . C9 . 150.92(16) yes C5 . W1 . C9 . 150.72(14) yes C1 . W1 . C10 . 112.24(14) yes C2 . W1 . C10 . 130.49(15) yes C3 . W1 . C10 . 165.00(17) yes C4 . W1 . C10 . 153.88(16) yes C5 . W1 . C10 . 122.60(14) yes C1 . W1 . H202 . 94.28(8) no C2 . W1 . H202 . 128.10(9) no C3 . W1 . H202 . 122.69(11) no C4 . W1 . H202 . 86.60(12) no C5 . W1 . H202 . 70.56(9) no C1 . W1 . H203 . 126.94(9) no C2 . W1 . H203 . 133.75(9) no C3 . W1 . H203 . 100.00(11) no C4 . W1 . H203 . 75.59(11) no C5 . W1 . H203 . 91.66(9) no C1 . W1 . H204 . 125.79(8) no C2 . W1 . H204 . 95.93(8) no C3 . W1 . H204 . 65.95(9) no C4 . W1 . H204 . 75.8(1) no C5 . W1 . H204 . 111.65(9) no C6 . W1 . C7 . 36.11(14) yes C6 . W1 . C8 . 59.03(14) yes C7 . W1 . C8 . 35.17(14) yes C6 . W1 . C9 . 59.15(15) yes C7 . W1 . C9 . 59.38(14) yes C8 . W1 . C9 . 35.65(13) yes C6 . W1 . C10 . 35.40(16) yes C7 . W1 . C10 . 59.57(15) yes C8 . W1 . C10 . 59.09(13) yes C9 . W1 . C10 . 35.53(15) yes C6 . W1 . H202 . 96.1(1) no C7 . W1 . H202 . 128.0(1) no C8 . W1 . H202 . 116.52(9) no C9 . W1 . H202 . 80.9(1) no C10 . W1 . H202 . 68.59(11) no C6 . W1 . H203 . 130.0(1) no C7 . W1 . H203 . 131.5(1) no C8 . W1 . H203 . 96.8(1) no C9 . W1 . H203 . 75.87(11) no C10 . W1 . H203 . 94.84(12) no C6 . W1 . H204 . 129.4(1) no C7 . W1 . H204 . 96.13(11) no C8 . W1 . H204 . 71.0(1) no C9 . W1 . H204 . 85.33(11) no C10 . W1 . H204 . 120.9(1) no H202 . W1 . H203 . 53.460(4) no H202 . W1 . H204 . 113.722(8) no H203 . W1 . H204 . 60.282(5) no W1 . C1 . C2 . 70.37(18) yes W1 . C1 . C5 . 71.55(19) yes C2 . C1 . C5 . 106.0(3) yes W1 . C1 . B1 . 132.2(2) yes C2 . C1 . B1 . 125.5(3) yes C5 . C1 . B1 . 127.3(3) yes W1 . C2 . C1 . 73.75(18) yes W1 . C2 . C3 . 72.3(2) yes C1 . C2 . C3 . 109.7(3) yes W1 . C2 . H21 . 120.4(2) no C1 . C2 . H21 . 125.1(3) no C3 . C2 . H21 . 125.2(3) no W1 . C3 . C2 . 72.2(2) yes W1 . C3 . C4 . 71.6(2) yes C2 . C3 . C4 . 107.5(3) yes W1 . C3 . H31 . 121.8(3) no C2 . C3 . H31 . 126.4(4) no C4 . C3 . H31 . 126.1(4) no W1 . C4 . C3 . 72.2(2) yes W1 . C4 . C5 . 73.2(2) yes C3 . C4 . C5 . 107.4(4) yes W1 . C4 . H41 . 120.3(3) no C3 . C4 . H41 . 126.2(4) no C5 . C4 . H41 . 126.4(4) no W1 . C5 . C1 . 73.17(19) yes W1 . C5 . C4 . 70.9(2) yes C1 . C5 . C4 . 109.4(3) yes W1 . C5 . H51 . 122.1(3) no C1 . C5 . H51 . 125.5(3) no C4 . C5 . H51 . 125.2(4) no W1 . C6 . C7 . 71.9(2) yes W1 . C6 . C10 . 73.4(2) yes C7 . C6 . C10 . 108.4(3) yes W1 . C6 . H61 . 120.7(3) no C7 . C6 . H61 . 125.8(4) no C10 . C6 . H61 . 125.8(4) no W1 . C7 . C6 . 72.0(2) yes W1 . C7 . C8 . 74.0(2) yes C6 . C7 . C8 . 107.9(3) yes W1 . C7 . H71 . 119.9(3) no C6 . C7 . H71 . 126.1(4) no C8 . C7 . H71 . 126.0(4) no W1 . C8 . C7 . 70.9(2) yes W1 . C8 . C9 . 71.6(2) yes C7 . C8 . C9 . 108.1(3) yes W1 . C8 . H81 . 123.1(3) no C7 . C8 . H81 . 126.1(4) no C9 . C8 . H81 . 125.9(4) no W1 . C9 . C8 . 72.8(2) yes W1 . C9 . C10 . 72.5(2) yes C8 . C9 . C10 . 107.9(4) yes W1 . C9 . H91 . 120.6(3) no C8 . C9 . H91 . 126.1(4) no C10 . C9 . H91 . 125.9(4) no W1 . C10 . C6 . 71.2(2) yes W1 . C10 . C9 . 72.0(2) yes C6 . C10 . C9 . 107.6(3) yes W1 . C10 . H101 . 122.4(3) no C6 . C10 . H101 . 126.1(4) no C9 . C10 . H101 . 126.2(4) no C21 . C20 . C25 . 113.3(3) yes C21 . C20 . B1 . 120.6(3) yes C25 . C20 . B1 . 126.1(3) yes F21 . C21 . C20 . 120.3(3) yes F21 . C21 . C22 . 115.7(3) yes C20 . C21 . C22 . 124.0(3) yes F22 . C22 . C21 . 120.2(3) yes F22 . C22 . C23 . 119.6(3) yes C21 . C22 . C23 . 120.2(3) yes F23 . C23 . C22 . 121.6(3) yes F23 . C23 . C24 . 119.7(3) yes C22 . C23 . C24 . 118.7(3) yes F24 . C24 . C23 . 120.0(3) yes F24 . C24 . C25 . 121.1(3) yes C23 . C24 . C25 . 118.9(3) yes F25 . C25 . C20 . 120.5(3) yes F25 . C25 . C24 . 114.6(3) yes C20 . C25 . C24 . 124.9(3) yes C31 . C30 . C35 . 113.5(3) yes C31 . C30 . B1 . 118.4(3) yes C35 . C30 . B1 . 127.7(3) yes F31 . C31 . C30 . 120.1(3) yes F31 . C31 . C32 . 116.0(3) yes C30 . C31 . C32 . 123.8(3) yes F32 . C32 . C31 . 120.2(3) yes F32 . C32 . C33 . 120.2(3) yes C31 . C32 . C33 . 119.6(3) yes F33 . C33 . C32 . 120.2(3) yes F33 . C33 . C34 . 120.4(3) yes C32 . C33 . C34 . 119.4(3) yes F34 . C34 . C33 . 120.1(3) yes F34 . C34 . C35 . 120.4(3) yes C33 . C34 . C35 . 119.5(3) yes F35 . C35 . C30 . 121.9(3) yes F35 . C35 . C34 . 114.0(3) yes C30 . C35 . C34 . 124.1(3) yes Cl1 . B1 . C1 . 107.8(2) yes Cl1 . B1 . C20 . 103.2(2) yes C1 . B1 . C20 . 111.5(3) yes Cl1 . B1 . C30 . 112.8(2) yes C1 . B1 . C30 . 112.7(3) yes C20 . B1 . C30 . 108.5(3) yes #==END #============= Material Relevant to Compound(8)===================== data_2 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 15.427(3) _cell_angle_alpha 90 _cell_length_b 15.619(4) _cell_angle_beta 90 _cell_length_c 19.877(2) _cell_angle_gamma 90 _cell_volume 4789.4(5) _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P b c a ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,z' 'x+1/2,-y+1/2,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 'x+1/2,y,-z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C28 H9 B F15 Re' _chemical_formula_moiety 'C28 H9 B F15 Re' _chemical_compound_source ; ? ; _chemical_formula_weight 827.36 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 125 _cell_formula_units_Z 8 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' brown ' _exptl_crystal_size_min 0.2 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_max 0.4 _exptl_crystal_density_diffrn 2.29 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3125.24 _exptl_absorpt_coefficient_mu 5.21 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 1.00 # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 125 _diffrn_reflns_number 4766 _reflns_number_total 3940 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 3940 # Number of reflections without Friedels Law is 0 _reflns_number_gt 3940 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -0.57 _refine_diff_density_max 1.06 _reflns_threshold_expression >0.00\s(I) _refine_ls_number_reflns 3940 _refine_ls_number_parameters 407 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0247 _refine_ls_goodness_of_fit_ref 1.0402 _refine_ls_shift/su_max 0.003635 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 2.39 0.108 2.21 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.669731(5) 0.082103(5) 0.799297(4) 0.0214 1.0000 Uani F31 0.53508(8) 0.11433(8) 0.66888(6) 0.0296 1.0000 Uani F32 0.5624(1) 0.14014(9) 0.53880(7) 0.0405 1.0000 Uani F33 0.71857(13) 0.10494(12) 0.48234(8) 0.0547 1.0000 Uani F34 0.8508(1) 0.04818(11) 0.56166(9) 0.0491 1.0000 Uani F35 0.82883(8) 0.02892(12) 0.69329(8) 0.0393 1.0000 Uani F41 0.74258(8) 0.33283(8) 0.68453(8) 0.0366 1.0000 Uani F42 0.71257(11) 0.3778(1) 0.55760(8) 0.0491 1.0000 Uani F43 0.55118(12) 0.36409(13) 0.50417(8) 0.0585 1.0000 Uani F44 0.4192(1) 0.30279(11) 0.58015(8) 0.0481 1.0000 Uani F45 0.44652(8) 0.25889(9) 0.70777(7) 0.0337 1.0000 Uani F51 0.62557(9) 0.41803(8) 0.83581(8) 0.0355 1.0000 Uani F52 0.52674(9) 0.48858(8) 0.93047(7) 0.0357 1.0000 Uani F53 0.3843(1) 0.40416(9) 0.97749(7) 0.0393 1.0000 Uani F54 0.34423(9) 0.2467(1) 0.92727(9) 0.0384 1.0000 Uani F55 0.44184(8) 0.17580(8) 0.83209(7) 0.0339 1.0000 Uani C1 0.69276(17) 0.22288(15) 0.80763(12) 0.0273 1.0000 Uani C2 0.76661(14) 0.18418(14) 0.77502(13) 0.0300 1.0000 Uani C3 0.80753(15) 0.12573(17) 0.81867(14) 0.0365 1.0000 Uani C4 0.76148(16) 0.12583(17) 0.87894(12) 0.0372 1.0000 Uani C5 0.69107(15) 0.18462(15) 0.87328(13) 0.0317 1.0000 Uani C6 0.66681(15) -0.0612(2) 0.81277(18) 0.0382 1.0000 Uani C7 0.64230(17) -0.01965(17) 0.87295(13) 0.0392 1.0000 Uani C8 0.56411(15) 0.02714(15) 0.86171(12) 0.0342 1.0000 Uani C9 0.53981(14) 0.01323(15) 0.79387(12) 0.0312 1.0000 Uani C10 0.60274(15) -0.04155(14) 0.76480(11) 0.0315 1.0000 Uani C30 0.68322(17) 0.07828(13) 0.69047(13) 0.0256 1.0000 Uani C31 0.61694(14) 0.10123(13) 0.64544(11) 0.0272 1.0000 Uani C32 0.62829(16) 0.11230(14) 0.57786(11) 0.0318 1.0000 Uani C33 0.70670(18) 0.09519(16) 0.54841(14) 0.0382 1.0000 Uani C34 0.77370(16) 0.06621(15) 0.58911(13) 0.0352 1.0000 Uani C35 0.75969(15) 0.05768(14) 0.65693(12) 0.0312 1.0000 Uani C40 0.59609(15) 0.29039(14) 0.7024(1) 0.0264 1.0000 Uani C41 0.66158(14) 0.32316(14) 0.66119(13) 0.0292 1.0000 Uani C42 0.64702(18) 0.34775(15) 0.59504(13) 0.0363 1.0000 Uani C43 0.56560(17) 0.34188(15) 0.56814(12) 0.0366 1.0000 Uani C44 0.49833(16) 0.31156(15) 0.60690(13) 0.0357 1.0000 Uani C45 0.51465(14) 0.28849(13) 0.67235(12) 0.0280 1.0000 Uani C50 0.53982(13) 0.29305(13) 0.83074(11) 0.0256 1.0000 Uani C51 0.55557(13) 0.37308(14) 0.85770(11) 0.0263 1.0000 Uani C52 0.50517(14) 0.41166(13) 0.90589(12) 0.0275 1.0000 Uani C53 0.43356(14) 0.36942(15) 0.92923(11) 0.0283 1.0000 Uani C54 0.41362(13) 0.28946(14) 0.90462(12) 0.0274 1.0000 Uani C55 0.46605(13) 0.25363(14) 0.85561(11) 0.0267 1.0000 Uani B1 0.60963(15) 0.25916(14) 0.77731(13) 0.0257 1.0000 Uani H21 0.7860 0.1970 0.7280 0.0600 1.0000 Uiso H31 0.8602 0.0903 0.8083 0.0600 1.0000 Uiso H41 0.7752 0.0906 0.9196 0.0448 1.0000 Uiso H51 0.6474 0.1972 0.9094 0.0600 1.0000 Uiso H61 0.7194 -0.0976 0.8054 0.0600 1.0000 Uiso H71 0.6746 -0.0225 0.9164 0.0463 1.0000 Uiso H81 0.5321 0.0629 0.8953 0.0600 1.0000 Uiso H91 0.4880 0.0380 0.7704 0.0600 1.0000 Uiso H101 0.6015 -0.0630 0.7175 0.0600 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02117(8) 0.02155(8) 0.02140(9) 0.00064(3) -0.00267(3) -0.00062(3) F31 0.0288(6) 0.0288(6) 0.0311(7) -0.0033(5) -0.0016(5) 0.0022(5) F32 0.0569(9) 0.0379(7) 0.0266(7) 0.0001(6) -0.0109(6) 0.0006(7) F33 0.0771(12) 0.062(1) 0.0254(9) -0.0017(7) 0.0126(7) -0.0015(9) F34 0.0446(8) 0.0460(9) 0.057(1) -0.0091(8) 0.0226(8) -0.0002(7) F35 0.0278(8) 0.0405(9) 0.050(1) -0.0009(7) 0.0015(5) 0.0049(5) F41 0.0330(7) 0.0380(8) 0.0388(8) 0.0003(6) 0.0061(6) -0.0080(6) F42 0.055(1) 0.0444(8) 0.048(1) 0.0143(7) 0.0199(7) 0.0030(7) F43 0.0749(11) 0.0703(12) 0.0303(8) 0.0125(8) 0.0012(8) 0.0168(9) F44 0.0470(8) 0.056(1) 0.0411(9) -0.0024(7) -0.0125(6) 0.0082(7) F45 0.0283(7) 0.0383(8) 0.0346(8) -0.0025(6) 0.0017(5) -0.0015(6) F51 0.0371(7) 0.0310(7) 0.0383(9) -0.0036(5) 0.0078(6) -0.0102(5) F52 0.0438(8) 0.0259(6) 0.0372(8) -0.0100(5) -0.0002(6) -0.0031(6) F53 0.0398(8) 0.0441(8) 0.0342(8) -0.0146(6) 0.0095(6) 0.0007(6) F54 0.0325(6) 0.0362(7) 0.0465(9) -0.0025(6) 0.0123(6) -0.0059(6) F55 0.0344(7) 0.0228(6) 0.0444(9) -0.0081(5) 0.0053(6) -0.0054(5) C1 0.030(1) 0.022(1) 0.0299(12) -0.0038(8) -0.0014(9) -0.0046(9) C2 0.025(1) 0.028(1) 0.0372(13) -0.0026(9) -0.0021(9) -0.0085(8) C3 0.026(1) 0.0376(13) 0.0461(14) -0.0037(11) -0.0090(11) -0.001(1) C4 0.0366(12) 0.0382(12) 0.0369(13) -0.001(1) -0.017(1) -0.007(1) C5 0.035(1) 0.0331(11) 0.0268(13) -0.0052(9) -0.0063(9) -0.0034(9) C6 0.0357(15) 0.0250(11) 0.0540(17) 0.0016(13) -0.001(1) 0.0002(9) C7 0.0430(13) 0.0400(13) 0.0346(13) 0.0153(11) -0.0086(11) -0.0123(11) C8 0.0384(11) 0.0318(11) 0.0323(13) 0.004(1) 0.0068(9) -0.0060(9) C9 0.025(1) 0.0293(11) 0.0391(14) 0.0037(9) -0.0012(8) -0.0079(9) C10 0.0373(11) 0.0275(11) 0.0298(12) -0.0015(9) -0.0012(9) -0.0090(9) C30 0.0314(11) 0.0232(12) 0.0224(12) -0.0044(8) 0.0005(9) 0.0009(8) C31 0.0329(11) 0.0185(9) 0.0300(12) -0.0029(8) -0.0009(9) -0.0003(8) C32 0.0472(14) 0.022(1) 0.0268(12) -0.0027(9) -0.0043(9) -0.0042(9) C33 0.0536(16) 0.0318(11) 0.0292(13) -0.005(1) 0.0085(11) -0.0061(11) C34 0.0390(12) 0.031(1) 0.0356(15) -0.0076(9) 0.015(1) -0.0031(9) C35 0.0335(11) 0.0239(9) 0.0361(13) -0.0024(9) -0.0009(9) 0.0018(9) C40 0.0325(11) 0.020(1) 0.0261(12) -0.0064(8) 0.0038(8) -0.0019(8) C41 0.0337(11) 0.022(1) 0.0315(13) -0.0028(9) 0.0047(9) -0.0015(8) C42 0.0470(13) 0.0292(11) 0.0328(13) 0.005(1) 0.0121(11) 0.002(1) C43 0.0517(15) 0.0331(12) 0.0249(13) 0.0012(9) 0.000(1) 0.010(1) C44 0.0403(12) 0.0315(11) 0.0353(14) -0.005(1) -0.003(1) 0.0081(9) C45 0.0318(11) 0.025(1) 0.0275(12) -0.0031(8) 0.0023(8) 0.0015(8) C50 0.027(1) 0.024(1) 0.0265(12) -0.0008(8) -0.0002(8) 0.0002(8) C51 0.028(1) 0.026(1) 0.0248(11) 0.0018(8) -0.0001(8) -0.0031(8) C52 0.0333(11) 0.0240(9) 0.0252(12) -0.0030(8) -0.0043(9) 0.0014(8) C53 0.029(1) 0.0339(11) 0.0226(11) -0.0046(8) 0.0018(8) 0.0035(9) C54 0.026(1) 0.029(1) 0.0276(12) 0.0032(9) 0.0025(8) -0.0005(8) C55 0.0284(9) 0.0233(9) 0.0283(11) -0.0024(8) 0.0011(8) -0.0013(8) B1 0.0285(11) 0.020(1) 0.0287(12) -0.0043(9) 0.0021(9) -0.0025(9) _refine_ls_extinction_coef 335.0(166) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . C1 . 2.233(2) yes Re1 . C2 . 2.238(2) yes Re1 . C3 . 2.265(2) yes Re1 . C4 . 2.231(2) yes Re1 . C5 . 2.199(2) yes Re1 . C6 . 2.254(3) yes Re1 . C7 . 2.202(2) yes Re1 . C8 . 2.221(2) yes Re1 . C9 . 2.277(2) yes Re1 . C10 . 2.295(2) yes Re1 . C30 . 2.174(3) yes F31 . C31 . 1.361(2) yes F32 . C32 . 1.351(3) yes F33 . C33 . 1.335(3) yes F34 . C34 . 1.338(3) yes F35 . C35 . 1.364(3) yes F41 . C41 . 1.341(3) yes F42 . C42 . 1.341(3) yes F43 . C43 . 1.337(3) yes F44 . C44 . 1.339(3) yes F45 . C45 . 1.347(3) yes F51 . C51 . 1.360(2) yes F52 . C52 . 1.339(2) yes F53 . C53 . 1.339(2) yes F54 . C54 . 1.340(2) yes F55 . C55 . 1.355(2) yes C1 . C2 . 1.443(3) yes C1 . C5 . 1.436(4) yes C1 . B1 . 1.526(3) yes C2 . C3 . 1.409(4) yes C2 . H21 . 1.001(3) no C3 . C4 . 1.393(4) yes C3 . H31 . 1.004(3) no C4 . C5 . 1.427(4) yes C4 . H41 . 1.001(2) no C5 . H51 . 1.005(3) no C6 . C7 . 1.412(4) yes C6 . C10 . 1.407(4) yes C6 . H61 . 1.001(3) no C7 . C8 . 1.428(4) yes C7 . H71 . 0.999(2) no C8 . C9 . 1.416(3) yes C8 . H81 . 1.000(2) no C9 . C10 . 1.417(3) yes C9 . H91 . 1.002(2) no C10 . H101 . 0.998(2) no C30 . C31 . 1.405(3) yes C30 . C35 . 1.393(4) yes C31 . C32 . 1.366(3) yes C32 . C33 . 1.370(4) yes C33 . C34 . 1.389(4) yes C34 . C35 . 1.372(4) yes C40 . C41 . 1.398(3) yes C40 . C45 . 1.392(3) yes C40 . B1 . 1.581(3) yes C41 . C42 . 1.388(4) yes C42 . C43 . 1.368(4) yes C43 . C44 . 1.376(4) yes C44 . C45 . 1.373(3) yes C50 . C51 . 1.382(3) yes C50 . C55 . 1.385(3) yes C50 . B1 . 1.602(3) yes C51 . C52 . 1.373(3) yes C52 . C53 . 1.368(3) yes C53 . C54 . 1.376(3) yes C54 . C55 . 1.384(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Re1 . C2 . 37.67(9) yes C1 . Re1 . C3 . 62.7(1) yes C2 . Re1 . C3 . 36.46(9) yes C1 . Re1 . C4 . 62.94(9) yes C2 . Re1 . C4 . 60.74(9) yes C3 . Re1 . C4 . 36.1(1) yes C1 . Re1 . C5 . 37.79(9) yes C2 . Re1 . C5 . 61.67(9) yes C3 . Re1 . C5 . 61.76(9) yes C4 . Re1 . C5 . 37.57(9) yes C1 . Re1 . C6 . 166.33(11) yes C2 . Re1 . C6 . 138.26(8) yes C3 . Re1 . C6 . 107.29(9) yes C4 . Re1 . C6 . 103.4(1) yes C5 . Re1 . C6 . 130.27(11) yes C1 . Re1 . C7 . 133.78(9) yes C2 . Re1 . C7 . 141.81(9) yes C3 . Re1 . C7 . 106.5(1) yes C4 . Re1 . C7 . 82.59(9) yes C5 . Re1 . C7 . 96.3(1) yes C1 . Re1 . C8 . 117.12(9) yes C2 . Re1 . C8 . 152.36(9) yes C3 . Re1 . C8 . 135.2(1) yes C4 . Re1 . C8 . 100.81(9) yes C5 . Re1 . C8 . 91.02(9) yes C1 . Re1 . C9 . 127.48(9) yes C2 . Re1 . C9 . 156.07(9) yes C3 . Re1 . C9 . 167.44(9) yes C4 . Re1 . C9 . 137.45(9) yes C5 . Re1 . C9 . 120.49(9) yes C1 . Re1 . C10 . 157.24(9) yes C2 . Re1 . C10 . 146.69(9) yes C3 . Re1 . C10 . 136.59(9) yes C4 . Re1 . C10 . 139.06(9) yes C5 . Re1 . C10 . 151.64(9) yes C1 . Re1 . C30 . 94.91(8) yes C2 . Re1 . C30 . 74.99(9) yes C3 . Re1 . C30 . 95.0(1) yes C4 . Re1 . C30 . 130.83(9) yes C5 . Re1 . C30 . 132.16(9) yes C6 . Re1 . C7 . 36.93(11) yes C6 . Re1 . C8 . 62.30(9) yes C7 . Re1 . C8 . 37.67(9) yes C6 . Re1 . C9 . 61.26(8) yes C7 . Re1 . C9 . 61.41(8) yes C8 . Re1 . C9 . 36.68(9) yes C6 . Re1 . C10 . 36.02(9) yes C7 . Re1 . C10 . 60.32(9) yes C8 . Re1 . C10 . 60.74(8) yes C9 . Re1 . C10 . 36.11(9) yes C6 . Re1 . C30 . 95.3(1) yes C7 . Re1 . C30 . 131.31(9) yes C8 . Re1 . C30 . 127.99(9) yes C9 . Re1 . C30 . 91.39(9) yes C10 . Re1 . C30 . 73.90(8) yes Re1 . C1 . C2 . 71.34(13) yes Re1 . C1 . C5 . 69.80(13) yes C2 . C1 . C5 . 104.4(2) yes Re1 . C1 . B1 . 101.69(15) yes C2 . C1 . B1 . 129.9(2) yes C5 . C1 . B1 . 119.9(2) yes Re1 . C2 . C1 . 71.00(13) yes Re1 . C2 . C3 . 72.83(13) yes C1 . C2 . C3 . 110.4(2) yes Re1 . C2 . H21 . 122.88(17) no C1 . C2 . H21 . 124.9(2) no C3 . C2 . H21 . 124.8(2) no Re1 . C3 . C2 . 70.72(12) yes Re1 . C3 . C4 . 70.61(13) yes C2 . C3 . C4 . 107.5(2) yes Re1 . C3 . H31 . 123.97(19) no C2 . C3 . H31 . 126.4(3) no C4 . C3 . H31 . 126.1(3) no Re1 . C4 . C3 . 73.32(14) yes Re1 . C4 . C5 . 70.00(12) yes C3 . C4 . C5 . 108.7(2) yes Re1 . C4 . H41 . 122.66(18) no C3 . C4 . H41 . 125.9(3) no C5 . C4 . H41 . 125.4(3) no Re1 . C5 . C1 . 72.41(13) yes Re1 . C5 . C4 . 72.43(13) yes C1 . C5 . C4 . 109.0(2) yes Re1 . C5 . H51 . 121.37(17) no C1 . C5 . H51 . 125.5(2) no C4 . C5 . H51 . 125.5(2) no Re1 . C6 . C7 . 69.51(16) yes Re1 . C6 . C10 . 73.58(15) yes C7 . C6 . C10 . 106.6(2) yes Re1 . C6 . H61 . 122.0(2) no C7 . C6 . H61 . 127.0(3) no C10 . C6 . H61 . 126.4(3) no Re1 . C7 . C6 . 73.56(16) yes Re1 . C7 . C8 . 71.88(13) yes C6 . C7 . C8 . 109.2(2) yes Re1 . C7 . H71 . 120.82(18) no C6 . C7 . H71 . 125.4(3) no C8 . C7 . H71 . 125.4(3) no Re1 . C8 . C7 . 70.45(13) yes Re1 . C8 . C9 . 73.84(13) yes C7 . C8 . C9 . 107.1(2) yes Re1 . C8 . H81 . 121.26(17) no C7 . C8 . H81 . 126.7(2) no C9 . C8 . H81 . 126.2(2) no Re1 . C9 . C8 . 69.48(12) yes Re1 . C9 . C10 . 72.64(12) yes C8 . C9 . C10 . 107.4(2) yes Re1 . C9 . H91 . 122.78(16) no C8 . C9 . H91 . 126.5(2) no C10 . C9 . H91 . 126.1(2) no Re1 . C10 . C6 . 70.40(15) yes Re1 . C10 . C9 . 71.25(12) yes C6 . C10 . C9 . 109.6(2) yes Re1 . C10 . H101 . 124.95(16) no C6 . C10 . H101 . 125.3(2) no C9 . C10 . H101 . 125.0(2) no Re1 . C30 . C31 . 123.85(19) yes Re1 . C30 . C35 . 124.32(18) yes C31 . C30 . C35 . 111.7(2) yes F31 . C31 . C30 . 119.7(2) yes F31 . C31 . C32 . 115.9(2) yes C30 . C31 . C32 . 124.4(2) yes F32 . C32 . C31 . 120.6(2) yes F32 . C32 . C33 . 118.8(2) yes C31 . C32 . C33 . 120.6(2) yes F33 . C33 . C32 . 121.3(3) yes F33 . C33 . C34 . 120.6(2) yes C32 . C33 . C34 . 118.2(2) yes F34 . C34 . C33 . 119.5(2) yes F34 . C34 . C35 . 121.3(2) yes C33 . C34 . C35 . 119.1(2) yes F35 . C35 . C30 . 119.0(2) yes F35 . C35 . C34 . 115.4(2) yes C30 . C35 . C34 . 125.6(2) yes C41 . C40 . C45 . 114.1(2) yes C41 . C40 . B1 . 124.7(2) yes C45 . C40 . B1 . 121.13(19) yes F41 . C41 . C40 . 120.8(2) yes F41 . C41 . C42 . 116.6(2) yes C40 . C41 . C42 . 122.6(2) yes F42 . C42 . C41 . 120.0(2) yes F42 . C42 . C43 . 119.9(2) yes C41 . C42 . C43 . 120.0(2) yes F43 . C43 . C42 . 120.5(2) yes F43 . C43 . C44 . 119.8(2) yes C42 . C43 . C44 . 119.8(2) yes F44 . C44 . C43 . 120.0(2) yes F44 . C44 . C45 . 121.1(2) yes C43 . C44 . C45 . 118.8(2) yes F45 . C45 . C40 . 119.2(2) yes F45 . C45 . C44 . 116.2(2) yes C40 . C45 . C44 . 124.5(2) yes C51 . C50 . C55 . 114.09(19) yes C51 . C50 . B1 . 115.96(18) yes C55 . C50 . B1 . 129.93(19) yes F51 . C51 . C50 . 118.87(19) yes F51 . C51 . C52 . 116.51(18) yes C50 . C51 . C52 . 124.62(19) yes F52 . C52 . C51 . 120.51(19) yes F52 . C52 . C53 . 120.7(2) yes C51 . C52 . C53 . 118.83(19) yes F53 . C53 . C52 . 120.4(2) yes F53 . C53 . C54 . 119.7(2) yes C52 . C53 . C54 . 119.9(2) yes F54 . C54 . C53 . 120.8(2) yes F54 . C54 . C55 . 120.1(2) yes C53 . C54 . C55 . 119.1(2) yes F55 . C55 . C50 . 120.14(18) yes F55 . C55 . C54 . 116.39(18) yes C50 . C55 . C54 . 123.5(2) yes C1 . B1 . C40 . 126.7(2) yes C1 . B1 . C50 . 115.2(2) yes C40 . B1 . C50 . 115.70(18) yes #==END