# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1188 data_CRYSTALS_cif _audit_creation_date 98-04-12 _audit_creation_method CRYSTALS_ver_07-07-97 # lhd22 #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\REF.CIF # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication as part of a paper for "J. Chem. Soc., Dalton Trans." The remainder of the manuscript and figures have been sent by mail. ; _publ_contact_author_name 'Linda H. Doerrer' _publ_contact_author_address ; Inorganic Chemistry Laboratory South Parks Road OXFORD OX1 3QR ; _publ_contact_author_phone ' 01865 270 675 ' _publ_contact_author_fax ' 01865 272 690 ' _publ_contact_author_email ' linda.doerrer@chem.ox.ac.uk ' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? #choose from: FI FM FO CI CM CO AD# _publ_requested_coeditor_name ' Janet Dean ' #============================================================================= # 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 ; 'Reactions of Transition-metal Nitrido Compounds with B(C6F5)3: Crystal Structure of [Re{NB(C6F5)3}(PMe2Ph)(S2CNMe2)2]' ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Doerrer, Linda H.' #<--'Last name, first name' ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address for author 1 ; 'Graham, Andrew J.' #<--'Last name, first name' ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address for author 1 ; 'Green, Malcolm L. H.' #<--'Last name, first name' ; 'Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK' # Address for author 1 ; #============================================================================== # 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_figure_synopsis #synopsis for materials not shown as diagram ; ? ; _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 # Add your own references - in alphabetic order ; 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 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods in Enzymology, 276,(1997) pp. 307-326; Ed Carter, C.W. & Sweet, R.M., Academic Press. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite # choose from: _diffrn_measurement_device-type ' Enraf-nonius DIP2000 ' _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) ; # end_choice #========================================================================== # 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) ; # choose one of the following two lines _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 8.871(5) _cell_angle_alpha 80.73(4) _cell_length_b 13.233(1) _cell_angle_beta 77.13(5) _cell_length_c 16.7220(13) _cell_angle_gamma 86.05(5) _cell_volume 1887.6 _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 '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' 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' '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 ' C32 H23 Re1 S4 P1 F15 N3 B1 ' _chemical_formula_moiety ' C32 H23 Re1 S4 P1 F15 N3 B1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1090.75 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 0 _cell_formula_units_Z 2 _exptl_crystal_description ' rod ' _exptl_crystal_colour ' purple ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.92 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1058.35 _exptl_absorpt_coefficient_mu 3.62 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.85 _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 6103 _reflns_number_total 6103 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 6103 # Number of reflections without Friedels Law is 0 _reflns_number_observed 5408 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -2.37 _refine_diff_density_max 1.61 _refine_ls_number_reflns 5408 _refine_ls_number_parameters 514 _refine_ls_R_factor_obs 0.0421 _refine_ls_wR_factor_obs 0.0506 _refine_ls_goodness_of_fit_obs 1.0193 _refine_ls_shift/su_max 0.000397 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 2.84 0.362 2.06 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Re1 -0.25156(2) -0.101639(13) -0.25044(1) 0.0142 1.0000 Uani S1 -0.26486(17) -0.1016(1) -0.10690(7) 0.0198 1.0000 Uani S2 -0.51872(17) -0.1318(1) -0.17848(8) 0.0230 1.0000 Uani S3 -0.32732(18) 0.09340(9) -0.26264(8) 0.0231 1.0000 Uani S4 -0.33329(18) -0.0400(1) -0.38165(7) 0.0214 1.0000 Uani P1 0.00223(18) -0.0305(1) -0.29636(8) 0.0199 1.0000 Uani F21 -0.2715(4) -0.5373(2) -0.1554(2) 0.0280 1.0000 Uani F22 -0.5029(5) -0.6386(2) -0.1779(2) 0.0333 1.0000 Uani F23 -0.6632(4) -0.5630(3) -0.2956(2) 0.0326 1.0000 Uani F24 -0.5817(5) -0.3816(3) -0.3960(2) 0.0329 1.0000 Uani F25 -0.3453(4) -0.2802(2) -0.37797(19) 0.0248 1.0000 Uani F31 -0.0288(4) -0.2036(2) -0.43135(19) 0.0279 1.0000 Uani F32 0.1389(5) -0.2710(3) -0.5658(2) 0.0361 1.0000 Uani F33 0.2419(5) -0.4693(3) -0.5608(2) 0.0373 1.0000 Uani F34 0.1687(5) -0.6021(3) -0.4161(2) 0.0337 1.0000 Uani F35 -0.0025(4) -0.5370(2) -0.2797(2) 0.0270 1.0000 Uani F41 -0.3343(4) -0.3515(2) -0.09634(19) 0.0248 1.0000 Uani F42 -0.2377(5) -0.3722(3) 0.04525(19) 0.0315 1.0000 Uani F43 0.0702(5) -0.3890(3) 0.0450(2) 0.0334 1.0000 Uani F44 0.2803(5) -0.3900(3) -0.1018(2) 0.0337 1.0000 Uani F45 0.1861(4) -0.3715(3) -0.2440(2) 0.0276 1.0000 Uani N1 -0.5463(6) -0.1503(4) -0.0120(3) 0.0241 1.0000 Uani N2 -0.4485(7) 0.1531(4) -0.3965(3) 0.0266 1.0000 Uani N3 -0.1898(6) -0.2230(3) -0.2656(2) 0.0192 1.0000 Uani C1 -0.3795(7) 0.0790(4) -0.3531(3) 0.0220 1.0000 Uani C2 -0.484(1) 0.1382(5) -0.4749(4) 0.0382 1.0000 Uani C3 -0.5019(9) 0.2496(5) -0.3656(4) 0.0361 1.0000 Uani C4 -0.4593(7) -0.1323(4) -0.0872(3) 0.0208 1.0000 Uani C5 -0.7047(8) -0.1816(5) 0.0033(4) 0.0368 1.0000 Uani C6 -0.4801(8) -0.1469(5) 0.0600(3) 0.0303 1.0000 Uani C7 0.0512(8) 0.0436(5) -0.4004(3) 0.0327 1.0000 Uani C8 0.1604(8) -0.1256(4) -0.2983(4) 0.0276 1.0000 Uani C10 0.0459(7) 0.0537(4) -0.2287(3) 0.0241 1.0000 Uani C11 0.0776(8) 0.0101(4) -0.1525(4) 0.0269 1.0000 Uani C12 0.1092(9) 0.0713(5) -0.0988(4) 0.0333 1.0000 Uani C13 0.1064(9) 0.1762(5) -0.1205(5) 0.0385 1.0000 Uani C14 0.074(1) 0.2213(5) -0.1950(5) 0.0422 1.0000 Uani C15 0.0425(8) 0.1592(5) -0.2497(4) 0.0322 1.0000 Uani C20 -0.2984(7) -0.4005(4) -0.2636(3) 0.0189 1.0000 Uani C21 -0.3452(7) -0.4930(4) -0.2154(3) 0.0202 1.0000 Uani C22 -0.4657(8) -0.5482(4) -0.2253(3) 0.0263 1.0000 Uani C23 -0.5471(7) -0.5107(4) -0.2856(3) 0.0243 1.0000 Uani C24 -0.5068(7) -0.4186(4) -0.3355(3) 0.0224 1.0000 Uani C25 -0.3856(7) -0.3672(4) -0.3236(3) 0.0193 1.0000 Uani C30 -0.0223(6) -0.3666(4) -0.3471(3) 0.0181 1.0000 Uani C31 0.0168(7) -0.3032(4) -0.4231(3) 0.0210 1.0000 Uani C32 0.1040(7) -0.3355(4) -0.4938(3) 0.0230 1.0000 Uani C33 0.1576(8) -0.4368(5) -0.4920(3) 0.0287 1.0000 Uani C34 0.1201(7) -0.5029(4) -0.4196(4) 0.0243 1.0000 Uani C35 0.0328(7) -0.4676(4) -0.3497(3) 0.0229 1.0000 Uani C40 -0.0795(7) -0.3630(4) -0.1783(3) 0.0194 1.0000 Uani C41 -0.1827(7) -0.3623(4) -0.1009(3) 0.0205 1.0000 Uani C42 -0.1336(8) -0.3720(4) -0.0271(3) 0.0258 1.0000 Uani C43 0.0216(8) -0.3806(4) -0.0270(3) 0.0239 1.0000 Uani C44 0.1297(8) -0.3812(4) -0.1007(4) 0.0264 1.0000 Uani C45 0.0738(7) -0.3725(4) -0.1740(3) 0.0208 1.0000 Uani B1 -0.1450(7) -0.3382(4) -0.2646(3) 0.0166 1.0000 Uani H21 -0.5361 0.2019 -0.4988 0.0600 1.0000 Uiso H22 -0.5551 0.0796 -0.4648 0.0600 1.0000 Uiso H23 -0.3866 0.1228 -0.5147 0.0600 1.0000 Uiso H31 -0.5506 0.2952 -0.4074 0.0600 1.0000 Uiso H32 -0.5796 0.2354 -0.3121 0.0600 1.0000 Uiso H33 -0.4119 0.2843 -0.3564 0.0600 1.0000 Uiso H51 -0.7497 -0.1912 0.0643 0.0600 1.0000 Uiso H52 -0.7069 -0.2476 -0.0183 0.0600 1.0000 Uiso H53 -0.7667 -0.1276 -0.0256 0.0600 1.0000 Uiso H61 -0.5616 -0.1623 0.1119 0.0600 1.0000 Uiso H62 -0.3931 -0.1990 0.0608 0.0600 1.0000 Uiso H63 -0.4405 -0.0772 0.0568 0.0600 1.0000 Uiso H71 0.1579 0.0679 -0.4109 0.0600 1.0000 Uiso H72 -0.0220 0.1032 -0.4045 0.0600 1.0000 Uiso H73 0.0442 -0.0002 -0.4420 0.0600 1.0000 Uiso H81 0.2602 -0.0909 -0.3177 0.0600 1.0000 Uiso H82 0.1549 -0.1638 -0.2418 0.0600 1.0000 Uiso H83 0.1521 -0.1738 -0.3366 0.0600 1.0000 Uiso H111 0.0775 -0.0661 -0.1364 0.0600 1.0000 Uiso H121 0.1338 0.0394 -0.0446 0.0600 1.0000 Uiso H131 0.1283 0.2202 -0.0814 0.0600 1.0000 Uiso H141 0.0735 0.2976 -0.2103 0.0600 1.0000 Uiso H151 0.0175 0.1913 -0.3038 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 0.01692(15) 0.01501(12) 0.01175(12) -0.00458(7) -0.00468(8) 0.00292(8 S1 0.0215(8) 0.0245(6) 0.0145(5) -0.0060(4) -0.0047(5) 0.0008(5) S2 0.0189(8) 0.0293(6) 0.0218(6) -0.0074(5) -0.0046(5) 0.0011(5) S3 0.0346(9) 0.0190(6) 0.0182(6) -0.0074(4) -0.0099(5) 0.0077(5) S4 0.0283(8) 0.0212(6) 0.0177(6) -0.0061(4) -0.0103(5) 0.0039(5) P1 0.0216(8) 0.0224(6) 0.0162(6) -0.0051(5) -0.0039(5) 0.0001(5) F21 0.035(2) 0.0246(16) 0.0259(16) 0.0015(12) -0.0131(14) -0.0016(14 F22 0.040(2) 0.0214(16) 0.0361(18) -0.0007(13) -0.0053(16) -0.0050(14 F23 0.023(2) 0.0297(17) 0.051(2) -0.0120(15) -0.0138(16) -0.0027(14 F24 0.037(2) 0.0330(18) 0.0347(18) -0.0051(14) -0.0201(16) -0.0005(15 F25 0.029(2) 0.0238(15) 0.0230(15) -0.0003(12) -0.0114(13) -0.0023(13 F31 0.038(2) 0.0229(15) 0.0199(14) -0.0036(12) -0.0018(14) 0.0023(13 F32 0.048(3) 0.0346(18) 0.0196(15) -0.0036(13) 0.0037(15) -0.0007(16 F33 0.036(2) 0.046(2) 0.0304(18) -0.0226(15) 0.0014(16) 0.0087(16 F34 0.038(2) 0.0260(17) 0.0417(19) -0.0191(14) -0.0116(16) 0.0132(15 F35 0.031(2) 0.0209(15) 0.0278(16) -0.0040(12) -0.0063(14) 0.0048(13 F41 0.025(2) 0.0263(15) 0.0227(15) -0.0044(12) -0.0033(13) 0.0017(12 F42 0.041(2) 0.0362(18) 0.0165(14) -0.0068(13) -0.0022(14) -0.0040(15 F43 0.050(3) 0.0340(18) 0.0248(16) -0.0074(13) -0.0255(16) 0.0008(16 F44 0.024(2) 0.043(2) 0.0395(19) -0.0114(15) -0.0184(16) 0.0069(15 F45 0.021(2) 0.0356(17) 0.0269(16) -0.0119(13) -0.0041(13) 0.0051(13 N1 0.022(3) 0.026(2) 0.023(2) -0.0043(17) -0.0022(19) 0.0017(18 N2 0.032(3) 0.023(2) 0.028(2) -0.0050(18) -0.015(2) 0.0045(19 N3 0.020(3) 0.025(2) 0.0128(18) -0.0045(15) -0.0021(16) 0.0006(17 C1 0.024(3) 0.024(2) 0.018(2) -0.0024(19) -0.007(2) 0.002(2) C2 0.058(5) 0.032(3) 0.030(3) -0.001(2) -0.027(3) 0.007(3) C3 0.039(4) 0.027(3) 0.043(3) -0.007(2) -0.013(3) 0.012(3) C4 0.020(3) 0.023(2) 0.018(2) -0.0041(18) -0.001(2) 0.0047(19 C5 0.024(4) 0.042(3) 0.042(3) -0.008(3) 0.000(3) -0.004(3) C6 0.031(4) 0.039(3) 0.018(2) -0.006(2) 0.000(2) 0.002(2) C7 0.036(4) 0.041(3) 0.019(3) -0.002(2) -0.003(2) -0.005(3) C8 0.029(4) 0.027(3) 0.030(3) -0.012(2) -0.008(2) 0.005(2) C10 0.023(3) 0.028(3) 0.023(2) -0.006(2) -0.005(2) -0.003(2) C11 0.030(4) 0.025(3) 0.028(3) -0.005(2) -0.010(2) -0.003(2) C12 0.036(4) 0.034(3) 0.034(3) -0.014(2) -0.012(3) 0.005(3) C13 0.034(4) 0.036(3) 0.054(4) -0.027(3) -0.014(3) -0.000(3) C14 0.044(5) 0.023(3) 0.067(5) -0.015(3) -0.026(4) 0.003(3) C15 0.035(4) 0.025(3) 0.039(3) -0.005(2) -0.013(3) 0.003(2) C20 0.014(3) 0.026(3) 0.019(2) -0.0085(18) -0.006(2) 0.0033(19 C21 0.020(3) 0.021(2) 0.019(2) -0.0063(18) -0.003(2) 0.0064(19 C22 0.030(3) 0.020(2) 0.027(3) -0.006(2) 0.002(2) 0.001(2) C23 0.021(3) 0.023(3) 0.032(3) -0.013(2) -0.006(2) -0.001(2) C24 0.024(3) 0.023(3) 0.024(2) -0.0097(19) -0.010(2) 0.001(2) C25 0.024(3) 0.018(2) 0.016(2) -0.0013(17) -0.0051(19) 0.0018(19 C30 0.014(3) 0.022(2) 0.020(2) -0.0074(18) -0.0054(19) 0.0010(18 C31 0.019(3) 0.023(2) 0.022(2) -0.0061(19) -0.006(2) 0.002(2) C32 0.020(3) 0.029(3) 0.019(2) -0.006(2) -0.002(2) -0.002(2) C33 0.026(3) 0.039(3) 0.022(3) -0.018(2) -0.001(2) 0.000(2) C34 0.015(3) 0.027(3) 0.035(3) -0.016(2) -0.010(2) 0.006(2) C35 0.024(3) 0.025(3) 0.021(2) -0.0096(19) -0.007(2) 0.006(2) C40 0.021(3) 0.020(2) 0.018(2) -0.0057(17) -0.006(2) 0.0025(19 C41 0.021(3) 0.021(2) 0.021(2) -0.0038(18) -0.007(2) 0.0043(19 C42 0.040(4) 0.023(3) 0.015(2) -0.0076(18) -0.006(2) -0.001(2) C43 0.033(4) 0.024(3) 0.020(2) -0.0016(19) -0.019(2) 0.001(2) C44 0.036(4) 0.018(2) 0.031(3) -0.005(2) -0.020(2) 0.005(2) C45 0.018(3) 0.022(2) 0.024(2) -0.0066(19) -0.006(2) 0.0042(19 B1 0.016(3) 0.018(2) 0.018(2) -0.0041(19) -0.006(2) 0.000(2) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . S1 . 2.3769(12) yes Re1 . S2 . 2.4350(15) yes Re1 . S3 . 2.6090(12) yes Re1 . S4 . 2.4608(13) yes Re1 . P1 . 2.4154(15) yes Re1 . N3 . 1.700(4) yes S1 . C4 . 1.746(6) yes S2 . C4 . 1.721(6) yes S3 . C1 . 1.719(6) yes S4 . C1 . 1.715(5) yes P1 . C7 . 1.830(6) yes P1 . C8 . 1.817(6) yes P1 . C10 . 1.825(6) yes F21 . C21 . 1.351(6) yes F22 . C22 . 1.342(6) yes F23 . C23 . 1.334(7) yes F24 . C24 . 1.341(7) yes F25 . C25 . 1.362(6) yes F31 . C31 . 1.345(6) yes F32 . C32 . 1.347(6) yes F33 . C33 . 1.341(6) yes F34 . C34 . 1.350(6) yes F35 . C35 . 1.357(6) yes F41 . C41 . 1.329(7) yes F42 . C42 . 1.348(6) yes F43 . C43 . 1.351(6) yes F44 . C44 . 1.330(8) yes F45 . C45 . 1.357(6) yes N1 . C4 . 1.315(7) yes N1 . C5 . 1.448(9) yes N1 . C6 . 1.461(8) yes N2 . C1 . 1.323(7) yes N2 . C2 . 1.462(8) yes N2 . C3 . 1.463(7) yes N3 . B1 . 1.548(7) yes C2 . H21 . 1.000(6) no C2 . H22 . 1.000(8) no C2 . H23 . 1.000(8) no C3 . H31 . 1.000(7) no C3 . H32 . 1.000(7) no C3 . H33 . 1.000(8) no C5 . H51 . 1.000(7) no C5 . H52 . 1.000(7) no C5 . H53 . 1.000(7) no C6 . H61 . 1.000(6) no C6 . H62 . 1.000(6) no C6 . H63 . 1.000(7) no C7 . H71 . 0.990(7) no C7 . H72 . 0.990(7) no C7 . H73 . 0.990(6) no C8 . H81 . 0.990(7) no C8 . H82 . 0.990(6) no C8 . H83 . 0.990(6) no C10 . C11 . 1.392(8) yes C10 . C15 . 1.383(8) yes C11 . C12 . 1.385(9) yes C11 . H111 . 1.000(6) no C12 . C13 . 1.377(9) yes C12 . H121 . 1.000(7) no C13 . C14 . 1.372(11) yes C13 . H131 . 1.000(6) no C14 . C15 . 1.408(9) yes C14 . H141 . 1.000(6) no C15 . H151 . 1.000(7) no C20 . C21 . 1.388(7) yes C20 . C25 . 1.398(7) yes C20 . B1 . 1.635(8) yes C21 . C22 . 1.389(9) yes C22 . C23 . 1.377(9) yes C23 . C24 . 1.382(8) yes C24 . C25 . 1.378(8) yes C30 . C31 . 1.392(7) yes C30 . C35 . 1.394(7) yes C30 . B1 . 1.635(7) yes C31 . C32 . 1.375(7) yes C32 . C33 . 1.389(8) yes C33 . C34 . 1.365(9) yes C34 . C35 . 1.381(7) yes C40 . C41 . 1.410(7) yes C40 . C45 . 1.373(9) yes C40 . B1 . 1.650(8) yes C41 . C42 . 1.383(8) yes C42 . C43 . 1.37(1) yes C43 . C44 . 1.384(9) yes C44 . C45 . 1.406(8) 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 S1 . Re1 . S2 . 72.74(5) yes S1 . Re1 . S3 . 88.02(4) yes S2 . Re1 . S3 . 86.81(5) yes S1 . Re1 . S4 . 152.79(4) yes S2 . Re1 . S4 . 90.94(5) yes S3 . Re1 . S4 . 69.04(4) yes S1 . Re1 . P1 . 95.28(5) yes S2 . Re1 . P1 . 162.55(5) yes S3 . Re1 . P1 . 80.01(5) yes S4 . Re1 . P1 . 94.91(5) yes S1 . Re1 . N3 . 104.07(14) yes S2 . Re1 . N3 . 100.14(16) yes S3 . Re1 . N3 . 167.36(14) yes S4 . Re1 . N3 . 100.08(15) yes P1 . Re1 . N3 . 95.01(16) yes Re1 . S1 . C4 . 88.75(18) yes Re1 . S2 . C4 . 87.4(2) yes Re1 . S3 . C1 . 85.92(18) yes Re1 . S4 . C1 . 90.84(18) yes Re1 . P1 . C7 . 118.2(2) yes Re1 . P1 . C8 . 114.0(2) yes C7 . P1 . C8 . 102.3(3) yes Re1 . P1 . C10 . 113.88(19) yes C7 . P1 . C10 . 104.2(3) yes C8 . P1 . C10 . 102.3(3) yes C4 . N1 . C5 . 122.3(5) yes C4 . N1 . C6 . 119.9(5) yes C5 . N1 . C6 . 117.6(5) yes C1 . N2 . C2 . 120.7(5) yes C1 . N2 . C3 . 121.8(5) yes C2 . N2 . C3 . 117.4(5) yes Re1 . N3 . B1 . 170.9(3) yes S3 . C1 . S4 . 113.7(3) yes S3 . C1 . N2 . 122.9(4) yes S4 . C1 . N2 . 123.3(4) yes N2 . C2 . H21 . 109.5(6) no N2 . C2 . H22 . 109.5(5) no H21 . C2 . H22 . 109.5(8) no N2 . C2 . H23 . 109.4(7) no H21 . C2 . H23 . 109.5(6) no H22 . C2 . H23 . 109.5(6) no N2 . C3 . H31 . 109.5(6) no N2 . C3 . H32 . 109.5(6) no H31 . C3 . H32 . 109.5(7) no N2 . C3 . H33 . 109.5(6) no H31 . C3 . H33 . 109.5(6) no H32 . C3 . H33 . 109.5(7) no S1 . C4 . S2 . 110.8(3) yes S1 . C4 . N1 . 123.2(5) yes S2 . C4 . N1 . 126.0(5) yes N1 . C5 . H51 . 109.4(7) no N1 . C5 . H52 . 109.4(6) no H51 . C5 . H52 . 109.5(6) no N1 . C5 . H53 . 109.5(6) no H51 . C5 . H53 . 109.5(6) no H52 . C5 . H53 . 109.5(7) no N1 . C6 . H61 . 109.4(6) no N1 . C6 . H62 . 109.4(5) no H61 . C6 . H62 . 109.5(6) no N1 . C6 . H63 . 109.5(5) no H61 . C6 . H63 . 109.5(5) no H62 . C6 . H63 . 109.5(7) no P1 . C7 . H71 . 109.5(5) no P1 . C7 . H72 . 109.5(4) no H71 . C7 . H72 . 109.5(6) no P1 . C7 . H73 . 109.4(5) no H71 . C7 . H73 . 109.5(6) no H72 . C7 . H73 . 109.5(6) no P1 . C8 . H81 . 109.5(4) no P1 . C8 . H82 . 109.5(4) no H81 . C8 . H82 . 109.5(6) no P1 . C8 . H83 . 109.5(5) no H81 . C8 . H83 . 109.5(5) no H82 . C8 . H83 . 109.5(5) no P1 . C10 . C11 . 118.6(4) yes P1 . C10 . C15 . 121.9(5) yes C11 . C10 . C15 . 119.4(5) yes C10 . C11 . C12 . 120.5(5) yes C10 . C11 . H111 . 119.7(5) no C12 . C11 . H111 . 119.7(6) no C11 . C12 . C13 . 119.6(6) yes C11 . C12 . H121 . 120.2(6) no C13 . C12 . H121 . 120.2(6) no C12 . C13 . C14 . 121.1(6) yes C12 . C13 . H131 . 119.4(7) no C14 . C13 . H131 . 119.5(7) no C13 . C14 . C15 . 119.4(6) yes C13 . C14 . H141 . 120.3(7) no C15 . C14 . H141 . 120.3(7) no C10 . C15 . C14 . 120.0(6) yes C10 . C15 . H151 . 120.0(6) no C14 . C15 . H151 . 120.0(6) no C21 . C20 . C25 . 113.2(5) yes C21 . C20 . B1 . 127.1(5) yes C25 . C20 . B1 . 119.1(5) yes F21 . C21 . C20 . 121.0(5) yes F21 . C21 . C22 . 115.0(5) yes C20 . C21 . C22 . 124.0(5) yes F22 . C22 . C21 . 121.0(6) yes F22 . C22 . C23 . 119.2(6) yes C21 . C22 . C23 . 119.7(5) yes F23 . C23 . C22 . 120.2(5) yes F23 . C23 . C24 . 120.5(5) yes C22 . C23 . C24 . 119.2(6) yes F24 . C24 . C23 . 120.4(5) yes F24 . C24 . C25 . 120.8(5) yes C23 . C24 . C25 . 118.8(5) yes F25 . C25 . C20 . 118.8(5) yes F25 . C25 . C24 . 116.0(5) yes C20 . C25 . C24 . 125.0(5) yes C31 . C30 . C35 . 113.6(5) yes C31 . C30 . B1 . 126.2(5) yes C35 . C30 . B1 . 119.4(4) yes F31 . C31 . C30 . 121.0(5) yes F31 . C31 . C32 . 115.3(5) yes C30 . C31 . C32 . 123.7(5) yes F32 . C32 . C31 . 121.4(5) yes F32 . C32 . C33 . 118.5(5) yes C31 . C32 . C33 . 120.0(5) yes F33 . C33 . C32 . 120.5(5) yes F33 . C33 . C34 . 120.8(5) yes C32 . C33 . C34 . 118.8(5) yes F34 . C34 . C33 . 120.2(5) yes F34 . C34 . C35 . 120.2(5) yes C33 . C34 . C35 . 119.6(5) yes F35 . C35 . C30 . 118.7(4) yes F35 . C35 . C34 . 117.0(5) yes C30 . C35 . C34 . 124.3(5) yes C41 . C40 . C45 . 114.2(5) yes C41 . C40 . B1 . 119.9(5) yes C45 . C40 . B1 . 125.4(5) yes F41 . C41 . C40 . 120.5(5) yes F41 . C41 . C42 . 116.8(5) yes C40 . C41 . C42 . 122.7(6) yes F42 . C42 . C41 . 120.2(6) yes F42 . C42 . C43 . 119.5(5) yes C41 . C42 . C43 . 120.3(5) yes F43 . C43 . C42 . 120.5(5) yes F43 . C43 . C44 . 119.4(6) yes C42 . C43 . C44 . 120.2(5) yes F44 . C44 . C43 . 121.0(5) yes F44 . C44 . C45 . 121.6(5) yes C43 . C44 . C45 . 117.4(6) yes F45 . C45 . C40 . 120.6(5) yes F45 . C45 . C44 . 114.2(5) yes C40 . C45 . C44 . 125.2(5) yes N3 . B1 . C20 . 109.0(4) yes N3 . B1 . C30 . 115.2(4) yes C20 . B1 . C30 . 103.3(4) yes N3 . B1 . C40 . 100.4(4) yes C20 . B1 . C40 . 114.7(4) yes C30 . B1 . C40 . 114.5(4) yes