Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Heinz Berke' _publ_contact_author_address ; Department of Inorganic Chemistry University Winterthurerstrasse 190 Zurich 8057 SWITZERLAND ; _publ_contact_author_email HBERKE@ACI.UNIZH.CH _publ_section_title ; Ligand Controlled Dioxygen Oxidation of Rhenium Nitrosyl Complexes ; loop_ _publ_author_name 'H. Berke' 'Olivier Blacque' 'Christian Frech' 'Helmut W Schmalle' #====END data_3b/4b _database_code_depnum_ccdc_archive 'CCDC 295096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitrosyl-nitrito(nitrato40%)-trans-bis(triisopropylphosphine)- benzylidene-rhenium(-I) tetrakis(2,4-trifluoromethylphenyl)borate ; _chemical_name_common ; Nitrosyl-nitrito(nitrato40%)-trans-bis(triisopropylphosphine)- benzylidene-rhenium(-I) tetrakis(2,4-trifluoromethylphenyl)borate ; _chemical_formula_moiety ? _chemical_formula_sum 'C57 H60 B F24 N2 O3.40 P2 Re' _chemical_formula_weight 1542.42 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 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0867(8) _cell_length_b 17.2051(15) _cell_length_c 18.8175(16) _cell_angle_alpha 90.331(10) _cell_angle_beta 102.566(10) _cell_angle_gamma 95.663(10) _cell_volume 3170.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 30.2 _exptl_crystal_description plate _exptl_crystal_colour 'yellow honeycolor' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 2.082 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.5211 _exptl_absorpt_correction_T_max 0.6931 _exptl_special_details ; The crystal has been oxidized upon standing in air for some days. The material looked like cracked showing a large mosaicity, it had to be cut and cleaned in protecting oil to get a crystalline part for the X-ray experiment. Some intrusions could not be removed. The relatively high R-values (R~int~ and R~\s~) most probably result from the bad crystal quality. The nitrato oxygen atom showed relatively large displacement parameters, thus finally its site occupation factor was set to a 40% level which is in agreement with elemental analysis results. ; _diffrn_ambient_temperature 123(2) _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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 4.0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40977 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 30.21 _reflns_number_total 17041 _reflns_number_gt 12333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17041 _refine_ls_number_parameters 848 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.54826(2) 0.797131(12) 0.681666(10) 0.02509(6) Uani 1 d . . . P1 P 0.37260(15) 0.77066(8) 0.56470(6) 0.0316(3) Uani 1 d . . . P2 P 0.73986(14) 0.84727(7) 0.78782(6) 0.0281(3) Uani 1 d . . . N1 N 0.4236(5) 0.8387(2) 0.7180(2) 0.0318(10) Uani 1 d . . . O1 O 0.3390(4) 0.8702(2) 0.73779(19) 0.0362(8) Uani 1 d . . . N2 N 0.7236(6) 0.8326(3) 0.5954(3) 0.0501(13) Uani 1 d . . . O2 O 0.6976(4) 0.7651(2) 0.6226(2) 0.0408(9) Uani 1 d . . . O3 O 0.6551(5) 0.8844(2) 0.6181(2) 0.0450(10) Uani 1 d . . . O4 O 0.7862(12) 0.8468(7) 0.5517(6) 0.055(3) Uani 0.40 d P . . C1 C 0.5240(6) 0.6941(3) 0.7180(2) 0.0300(10) Uani 1 d . . . H1 H 0.5850 0.6627 0.7022 0.036 Uiso 1 calc R . . C2 C 0.4458(6) 0.6477(3) 0.7608(2) 0.0299(11) Uani 1 d . . . C3 C 0.3536(6) 0.6781(3) 0.7978(3) 0.0400(13) Uani 1 d . . . H3 H 0.3457 0.7326 0.7976 0.048 Uiso 1 calc R . . C4 C 0.2745(7) 0.6296(4) 0.8342(3) 0.0497(15) Uani 1 d . . . H4 H 0.2148 0.6510 0.8599 0.060 Uiso 1 calc R . . C5 C 0.2829(7) 0.5487(4) 0.8329(3) 0.0510(17) Uani 1 d . . . H5 H 0.2262 0.5154 0.8566 0.061 Uiso 1 calc R . . C6 C 0.3719(7) 0.5168(3) 0.7979(3) 0.0464(15) Uani 1 d . . . H6 H 0.3778 0.4620 0.7978 0.056 Uiso 1 calc R . . C7 C 0.4519(6) 0.5651(3) 0.7632(3) 0.0371(12) Uani 1 d . . . H7 H 0.5141 0.5429 0.7397 0.045 Uiso 1 calc R . . C8 C 0.2053(7) 0.7345(4) 0.5880(3) 0.0444(14) Uani 1 d . . . H8 H 0.2076 0.7591 0.6366 0.053 Uiso 1 calc R . . C9 C 0.1936(8) 0.6466(4) 0.5994(3) 0.0515(16) Uani 1 d . . . H9A H 0.1224 0.6326 0.6265 0.077 Uiso 1 calc R . . H9B H 0.2811 0.6318 0.6271 0.077 Uiso 1 calc R . . H9C H 0.1700 0.6188 0.5520 0.077 Uiso 1 calc R . . C10 C 0.0774(8) 0.7577(5) 0.5381(4) 0.068(2) Uani 1 d . . . H10A H 0.0716 0.7372 0.4887 0.101 Uiso 1 calc R . . H10B H 0.0805 0.8148 0.5375 0.101 Uiso 1 calc R . . H10C H -0.0028 0.7361 0.5556 0.101 Uiso 1 calc R . . C11 C 0.4178(8) 0.7051(4) 0.4978(3) 0.0490(16) Uani 1 d . . . H11 H 0.4945 0.7347 0.4804 0.059 Uiso 1 calc R . . C12 C 0.4714(8) 0.6295(4) 0.5271(3) 0.0512(16) Uani 1 d . . . H12A H 0.3976 0.5957 0.5410 0.077 Uiso 1 calc R . . H12B H 0.5461 0.6412 0.5699 0.077 Uiso 1 calc R . . H12C H 0.5051 0.6029 0.4895 0.077 Uiso 1 calc R . . C13 C 0.2987(9) 0.6900(4) 0.4292(3) 0.066(2) Uani 1 d . . . H13A H 0.3316 0.6645 0.3906 0.100 Uiso 1 calc R . . H13B H 0.2660 0.7399 0.4122 0.100 Uiso 1 calc R . . H13C H 0.2238 0.6561 0.4419 0.100 Uiso 1 calc R . . C14 C 0.3346(7) 0.8615(3) 0.5140(3) 0.0443(14) Uani 1 d . . . H14 H 0.2442 0.8492 0.4795 0.053 Uiso 1 calc R . . C15 C 0.4365(8) 0.8908(4) 0.4680(3) 0.0575(18) Uani 1 d . . . H15A H 0.4124 0.9409 0.4470 0.086 Uiso 1 calc R . . H15B H 0.4334 0.8525 0.4288 0.086 Uiso 1 calc R . . H15C H 0.5288 0.8978 0.4989 0.086 Uiso 1 calc R . . C16 C 0.3172(8) 0.9275(4) 0.5660(3) 0.0524(16) Uani 1 d . . . H16A H 0.4048 0.9431 0.5996 0.079 Uiso 1 calc R . . H16B H 0.2493 0.9089 0.5938 0.079 Uiso 1 calc R . . H16C H 0.2866 0.9725 0.5376 0.079 Uiso 1 calc R . . C17 C 0.6933(6) 0.8156(3) 0.8744(2) 0.0356(12) Uani 1 d . . . H17 H 0.6481 0.7611 0.8640 0.043 Uiso 1 calc R . . C18 C 0.5847(7) 0.8627(4) 0.8944(3) 0.0515(17) Uani 1 d . . . H18A H 0.5451 0.8355 0.9317 0.077 Uiso 1 calc R . . H18B H 0.5126 0.8682 0.8510 0.077 Uiso 1 calc R . . H18C H 0.6268 0.9146 0.9133 0.077 Uiso 1 calc R . . C19 C 0.8089(7) 0.8099(4) 0.9403(3) 0.0500(16) Uani 1 d . . . H19A H 0.8558 0.8621 0.9545 0.075 Uiso 1 calc R . . H19B H 0.8737 0.7759 0.9281 0.075 Uiso 1 calc R . . H19C H 0.7718 0.7880 0.9807 0.075 Uiso 1 calc R . . C20 C 0.7807(7) 0.9533(3) 0.7849(3) 0.0480(15) Uani 1 d . . . H20 H 0.8307 0.9603 0.7445 0.058 Uiso 1 calc R . . C21 C 0.8827(8) 0.9882(4) 0.8522(4) 0.0569(18) Uani 1 d . . . H21A H 0.9081 1.0435 0.8447 0.085 Uiso 1 calc R . . H21B H 0.9645 0.9602 0.8606 0.085 Uiso 1 calc R . . H21C H 0.8411 0.9834 0.8947 0.085 Uiso 1 calc R . . C22 C 0.6617(9) 0.9991(4) 0.7628(4) 0.067(2) Uani 1 d . . . H22A H 0.6052 0.9938 0.7991 0.101 Uiso 1 calc R . . H22B H 0.6073 0.9794 0.7153 0.101 Uiso 1 calc R . . H22C H 0.6940 1.0543 0.7594 0.101 Uiso 1 calc R . . C23 C 0.9074(6) 0.8079(4) 0.7926(3) 0.0495(15) Uani 1 d . . . H23 H 0.9650 0.8228 0.8420 0.059 Uiso 1 calc R . . C24 C 0.8851(8) 0.7175(4) 0.7884(4) 0.066(2) Uani 1 d . . . H24A H 0.8351 0.7001 0.7394 0.099 Uiso 1 calc R . . H24B H 0.8324 0.6989 0.8241 0.099 Uiso 1 calc R . . H24C H 0.9738 0.6964 0.7991 0.099 Uiso 1 calc R . . C25 C 0.9869(8) 0.8401(6) 0.7378(4) 0.075(2) Uani 1 d . . . H25A H 1.0831 0.8313 0.7544 0.112 Uiso 1 calc R . . H25B H 0.9791 0.8962 0.7332 0.112 Uiso 1 calc R . . H25C H 0.9498 0.8134 0.6905 0.112 Uiso 1 calc R . . B1 B 1.0452(5) 1.2800(3) 0.8133(2) 0.0205(10) Uani 1 d . . . C26 C 1.1511(5) 1.3230(2) 0.8849(2) 0.0211(9) Uani 1 d . . . C27 C 1.2931(5) 1.3268(2) 0.8914(2) 0.0212(9) Uani 1 d . . . H27 H 1.3267 1.3037 0.8538 0.025 Uiso 1 calc R . . C28 C 1.3868(5) 1.3631(2) 0.9508(2) 0.0231(9) Uani 1 d . . . C281 C 1.5363(6) 1.3619(3) 0.9562(3) 0.0304(11) Uani 1 d . . . F281 F 1.5820(3) 1.29692(18) 0.98704(17) 0.0417(8) Uani 1 d . . . F282 F 1.5692(3) 1.3645(2) 0.89038(17) 0.0421(7) Uani 1 d . . . F283 F 1.6108(3) 1.42224(19) 0.99634(19) 0.0466(8) Uani 1 d . . . C29 C 1.3426(5) 1.3990(3) 1.0063(2) 0.0245(9) Uani 1 d . . . H29 H 1.4059 1.4239 1.0468 0.029 Uiso 1 calc R . . C30 C 1.2027(5) 1.3975(3) 1.0009(2) 0.0272(10) Uani 1 d . . . C301 C 1.1526(6) 1.4379(4) 1.0602(3) 0.0415(13) Uani 1 d . . . F301 F 1.0342(4) 1.4026(2) 1.07058(16) 0.0469(8) Uani 1 d . . . F302 F 1.1348(4) 1.5133(2) 1.0468(2) 0.0573(10) Uani 1 d . . . F303 F 1.2435(4) 1.4387(3) 1.12396(17) 0.0681(12) Uani 1 d . . . C31 C 1.1086(5) 1.3621(3) 0.9410(2) 0.0232(9) Uani 1 d . . . H31 H 1.0138 1.3644 0.9379 0.028 Uiso 1 calc R . . C32 C 0.8960(5) 1.2521(2) 0.8309(2) 0.0193(8) Uani 1 d . . . C33 C 0.8873(5) 1.2174(3) 0.8977(2) 0.0222(9) Uani 1 d . . . H33 H 0.9687 1.2146 0.9338 0.027 Uiso 1 calc R . . C34 C 0.7636(5) 1.1872(3) 0.9123(2) 0.0245(10) Uani 1 d . . . C341 C 0.7656(6) 1.1525(3) 0.9862(3) 0.0331(12) Uani 1 d . . . F341 F 0.8509(4) 1.0962(2) 0.99944(18) 0.0568(11) Uani 1 d . . . F342 F 0.8131(4) 1.2046(2) 1.04072(15) 0.0459(8) Uani 1 d . . . F343 F 0.6427(4) 1.1231(2) 0.99319(17) 0.0546(10) Uani 1 d . . . C35 C 0.6431(5) 1.1900(3) 0.8623(2) 0.0251(10) Uani 1 d . . . H35 H 0.5585 1.1702 0.8730 0.030 Uiso 1 calc R . . C36 C 0.6484(5) 1.2231(3) 0.7949(2) 0.0241(9) Uani 1 d . . . C361 C 0.5204(6) 1.2262(4) 0.7389(3) 0.0426(14) Uani 1 d . . . F361 F 0.4095(4) 1.2175(3) 0.76206(19) 0.0690(13) Uani 1 d . . . F362 F 0.5190(7) 1.1988(8) 0.6783(3) 0.108(5) Uani 0.689(5) d P A 1 F363 F 0.5065(7) 1.3067(4) 0.7210(4) 0.084(3) Uani 0.689(5) d P A 1 F365 F 0.4788(16) 1.1457(17) 0.7041(8) 0.108(5) Uani 0.311(5) d P A 2 F366 F 0.5286(18) 1.2618(12) 0.6805(12) 0.084(3) Uani 0.311(5) d P A 2 C37 C 0.7720(5) 1.2531(2) 0.7800(2) 0.0196(9) Uani 1 d . . . H37 H 0.7726 1.2750 0.7338 0.024 Uiso 1 calc R . . C38 C 1.0367(5) 1.3435(3) 0.7477(2) 0.0205(9) Uani 1 d . . . C39 C 0.9499(5) 1.4030(2) 0.7411(2) 0.0214(9) Uani 1 d . . . H39 H 0.8938 1.4066 0.7753 0.026 Uiso 1 calc R . . C40 C 0.9435(5) 1.4571(2) 0.6856(2) 0.0255(10) Uani 1 d . . . C401 C 0.8440(7) 1.5169(3) 0.6787(3) 0.0406(14) Uani 1 d . . . F401 F 0.8814(9) 1.5858(3) 0.6495(4) 0.066(2) Uani 0.689(5) d P A 1 F402 F 0.7242(8) 1.4932(4) 0.6263(5) 0.098(3) Uani 0.689(5) d P A 1 F403 F 0.7898(9) 1.5300(4) 0.7341(4) 0.069(3) Uani 0.689(5) d P A 1 F404 F 0.838(2) 1.5553(7) 0.6304(11) 0.066(2) Uani 0.311(5) d P A 2 F405 F 0.736(2) 1.4909(10) 0.6862(13) 0.098(3) Uani 0.311(5) d P A 2 F406 F 0.8702(19) 1.5548(11) 0.7437(10) 0.069(3) Uani 0.311(5) d P A 2 C41 C 1.0262(6) 1.4554(3) 0.6358(2) 0.0291(11) Uani 1 d . . . H41 H 1.0208 1.4919 0.5978 0.035 Uiso 1 calc R . . C42 C 1.1167(5) 1.3992(3) 0.6428(2) 0.0277(10) Uani 1 d . . . C421 C 1.2119(6) 1.3979(3) 0.5911(3) 0.0382(13) Uani 1 d . . . F421 F 1.2392(5) 1.3263(2) 0.5762(2) 0.0621(11) Uani 1 d . . . F422 F 1.1647(5) 1.4292(3) 0.5282(2) 0.0838(16) Uani 1 d . . . F423 F 1.3328(5) 1.4361(3) 0.6185(2) 0.0837(15) Uani 1 d . . . C43 C 1.1217(5) 1.3441(3) 0.6976(2) 0.0260(10) Uani 1 d . . . H43 H 1.1846 1.3059 0.7009 0.031 Uiso 1 calc R . . C44 C 1.0958(5) 1.1974(2) 0.7898(2) 0.0194(8) Uani 1 d . . . C45 C 1.1760(5) 1.1513(2) 0.8395(2) 0.0204(9) Uani 1 d . . . H45 H 1.2088 1.1701 0.8883 0.025 Uiso 1 calc R . . C46 C 1.2094(5) 1.0788(2) 0.8196(2) 0.0216(9) Uani 1 d . . . C461 C 1.2944(6) 1.0302(3) 0.8742(3) 0.0351(12) Uani 1 d . . . F461 F 1.2521(4) 0.95440(15) 0.86675(15) 0.0381(7) Uani 1 d . . . F462 F 1.4244(4) 1.0331(3) 0.8658(3) 0.0809(15) Uani 1 d . . . F463 F 1.2997(6) 1.0511(2) 0.94193(17) 0.0856(18) Uani 1 d . . . C47 C 1.1663(5) 1.0491(3) 0.7489(2) 0.0290(10) Uani 1 d . . . H47 H 1.1934 1.0010 0.7349 0.035 Uiso 1 calc R . . C48 C 1.0823(6) 1.0920(3) 0.6994(2) 0.0349(12) Uani 1 d . . . C481 C 1.0234(9) 1.0592(4) 0.6226(3) 0.063(2) Uani 1 d . . . F481 F 1.0465(6) 0.9877(3) 0.6125(2) 0.0941(19) Uani 1 d . . . F482 F 0.8856(6) 1.0571(4) 0.6060(3) 0.119(3) Uani 1 d . . . F483 F 1.0605(9) 1.1028(3) 0.5742(2) 0.131(3) Uani 1 d . . . C49 C 1.0475(5) 1.1642(3) 0.7198(2) 0.0289(11) Uani 1 d . . . H49 H 0.9887 1.1919 0.6847 0.035 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02731(11) 0.02611(9) 0.02306(8) -0.00089(6) 0.00815(6) 0.00283(7) P1 0.0339(8) 0.0348(7) 0.0228(5) 0.0004(5) 0.0028(5) -0.0046(6) P2 0.0275(8) 0.0308(6) 0.0263(6) 0.0003(5) 0.0057(5) 0.0042(6) N1 0.041(3) 0.031(2) 0.0247(19) 0.0011(16) 0.0075(18) 0.008(2) O1 0.031(2) 0.044(2) 0.0374(18) -0.0008(15) 0.0113(16) 0.0156(18) N2 0.047(4) 0.059(3) 0.046(3) -0.008(2) 0.018(2) -0.005(3) O2 0.034(2) 0.046(2) 0.044(2) -0.0102(17) 0.0176(18) -0.0025(19) O3 0.045(3) 0.051(2) 0.039(2) 0.0053(17) 0.0133(18) -0.007(2) O4 0.045(7) 0.084(8) 0.044(6) -0.006(5) 0.030(5) -0.004(6) C1 0.032(3) 0.029(2) 0.027(2) -0.0044(18) 0.0033(19) -0.001(2) C2 0.032(3) 0.029(2) 0.024(2) 0.0018(17) -0.0035(19) 0.003(2) C3 0.045(4) 0.044(3) 0.033(3) 0.008(2) 0.011(2) 0.009(3) C4 0.046(4) 0.067(4) 0.037(3) 0.013(3) 0.010(3) 0.007(3) C5 0.052(4) 0.054(4) 0.036(3) 0.020(3) -0.005(3) -0.015(3) C6 0.061(5) 0.036(3) 0.035(3) 0.007(2) -0.001(3) -0.007(3) C7 0.046(4) 0.031(3) 0.030(2) 0.0024(19) -0.003(2) 0.003(2) C8 0.038(4) 0.047(3) 0.043(3) 0.004(2) 0.001(3) -0.002(3) C9 0.059(5) 0.043(3) 0.045(3) 0.007(3) 0.004(3) -0.014(3) C10 0.046(5) 0.073(5) 0.073(5) 0.017(4) -0.006(4) -0.001(4) C11 0.065(5) 0.050(3) 0.029(3) -0.014(2) 0.010(3) -0.009(3) C12 0.064(5) 0.046(3) 0.044(3) -0.020(3) 0.016(3) -0.003(3) C13 0.096(7) 0.063(4) 0.031(3) -0.009(3) 0.002(3) -0.008(4) C14 0.048(4) 0.044(3) 0.033(3) 0.010(2) -0.004(2) -0.004(3) C15 0.082(6) 0.045(3) 0.043(3) 0.008(3) 0.016(3) -0.013(3) C16 0.062(5) 0.042(3) 0.052(3) 0.010(3) 0.006(3) 0.015(3) C17 0.037(3) 0.045(3) 0.022(2) 0.001(2) 0.001(2) 0.003(3) C18 0.047(4) 0.088(5) 0.021(2) -0.003(3) 0.007(2) 0.017(4) C19 0.058(4) 0.057(4) 0.030(3) 0.004(2) -0.004(3) 0.014(3) C20 0.056(5) 0.030(3) 0.054(3) -0.002(2) 0.009(3) -0.008(3) C21 0.065(5) 0.042(3) 0.061(4) -0.017(3) 0.018(3) -0.015(3) C22 0.091(6) 0.028(3) 0.077(5) -0.001(3) 0.009(4) 0.004(4) C23 0.030(4) 0.069(4) 0.047(3) -0.010(3) 0.001(3) 0.010(3) C24 0.052(5) 0.066(4) 0.075(5) -0.012(4) -0.008(4) 0.034(4) C25 0.028(4) 0.116(7) 0.079(5) -0.036(5) 0.019(3) -0.011(4) B1 0.024(3) 0.027(2) 0.0117(18) 0.0025(16) 0.0046(17) 0.008(2) C26 0.025(3) 0.022(2) 0.0169(17) 0.0039(15) 0.0044(16) 0.0070(19) C27 0.027(3) 0.0202(19) 0.0179(18) 0.0014(15) 0.0060(16) 0.0059(18) C28 0.028(3) 0.0169(19) 0.0235(19) 0.0016(15) 0.0023(17) 0.0046(19) C281 0.029(3) 0.025(2) 0.036(2) -0.0065(18) 0.004(2) 0.001(2) F281 0.0316(19) 0.0407(17) 0.0517(18) 0.0014(14) 0.0010(14) 0.0166(15) F282 0.0234(18) 0.059(2) 0.0448(17) -0.0020(15) 0.0115(13) 0.0004(16) F283 0.027(2) 0.0428(18) 0.064(2) -0.0239(15) 0.0019(15) -0.0062(15) C29 0.028(3) 0.023(2) 0.0206(19) 0.0001(16) 0.0015(17) 0.0030(19) C30 0.033(3) 0.029(2) 0.0203(19) -0.0039(16) 0.0050(18) 0.009(2) C301 0.037(4) 0.058(3) 0.030(2) -0.015(2) 0.006(2) 0.007(3) F301 0.051(2) 0.062(2) 0.0331(15) -0.0114(14) 0.0226(15) 0.0035(18) F302 0.048(2) 0.0428(19) 0.085(3) -0.0297(18) 0.0241(19) 0.0061(17) F303 0.052(3) 0.123(4) 0.0280(16) -0.0289(19) 0.0020(15) 0.018(2) C31 0.023(3) 0.029(2) 0.0191(18) 0.0019(16) 0.0058(17) 0.009(2) C32 0.023(2) 0.0190(18) 0.0172(17) 0.0025(14) 0.0069(16) 0.0034(18) C33 0.021(2) 0.029(2) 0.0191(18) 0.0067(16) 0.0077(17) 0.0090(19) C34 0.034(3) 0.026(2) 0.0196(18) 0.0098(16) 0.0162(18) 0.011(2) C341 0.036(3) 0.044(3) 0.028(2) 0.019(2) 0.019(2) 0.018(2) F341 0.074(3) 0.067(2) 0.0494(19) 0.0405(17) 0.0380(19) 0.044(2) F342 0.050(2) 0.069(2) 0.0209(13) 0.0124(14) 0.0088(13) 0.0140(18) F343 0.041(2) 0.089(3) 0.0370(17) 0.0331(17) 0.0174(15) 0.000(2) C35 0.025(3) 0.029(2) 0.026(2) 0.0070(17) 0.0155(19) 0.002(2) C36 0.023(3) 0.029(2) 0.0227(19) 0.0033(17) 0.0093(18) 0.006(2) C361 0.023(3) 0.077(4) 0.029(2) 0.017(3) 0.009(2) 0.004(3) F361 0.022(2) 0.142(4) 0.0448(19) 0.005(2) 0.0099(15) 0.011(2) F362 0.027(4) 0.268(15) 0.027(3) -0.051(5) -0.005(2) 0.031(6) F363 0.055(4) 0.071(5) 0.102(6) 0.041(4) -0.034(4) 0.002(4) F365 0.027(4) 0.268(15) 0.027(3) -0.051(5) -0.005(2) 0.031(6) F366 0.055(4) 0.071(5) 0.102(6) 0.041(4) -0.034(4) 0.002(4) C37 0.018(2) 0.027(2) 0.0166(17) 0.0045(15) 0.0074(16) 0.0045(18) C38 0.020(2) 0.027(2) 0.0148(17) 0.0025(15) 0.0056(16) -0.0006(18) C39 0.027(3) 0.0200(19) 0.0173(18) -0.0024(15) 0.0075(17) -0.0028(18) C40 0.036(3) 0.0157(19) 0.024(2) -0.0001(15) 0.0060(19) -0.0019(19) C401 0.056(4) 0.026(2) 0.046(3) 0.006(2) 0.021(3) 0.011(3) F401 0.110(7) 0.014(3) 0.095(5) 0.029(3) 0.063(5) 0.023(4) F402 0.073(5) 0.063(3) 0.130(6) -0.041(4) -0.051(5) 0.046(4) F403 0.091(7) 0.077(5) 0.068(3) 0.033(4) 0.059(5) 0.058(6) F404 0.110(7) 0.014(3) 0.095(5) 0.029(3) 0.063(5) 0.023(4) F405 0.073(5) 0.063(3) 0.130(6) -0.041(4) -0.051(5) 0.046(4) F406 0.091(7) 0.077(5) 0.068(3) 0.033(4) 0.059(5) 0.058(6) C41 0.043(3) 0.023(2) 0.020(2) -0.0001(16) 0.010(2) -0.007(2) C42 0.032(3) 0.033(2) 0.0195(19) 0.0026(17) 0.0125(19) -0.007(2) C421 0.039(4) 0.048(3) 0.029(2) 0.004(2) 0.017(2) -0.007(3) F421 0.083(3) 0.063(2) 0.057(2) -0.0025(18) 0.052(2) 0.008(2) F422 0.092(4) 0.138(4) 0.043(2) 0.046(2) 0.047(2) 0.045(3) F423 0.063(3) 0.123(4) 0.071(3) -0.031(3) 0.049(2) -0.035(3) C43 0.023(3) 0.038(2) 0.0192(19) 0.0045(17) 0.0075(17) 0.003(2) C44 0.017(2) 0.026(2) 0.0173(17) 0.0019(15) 0.0073(15) 0.0022(18) C45 0.022(3) 0.0197(19) 0.0195(18) 0.0039(15) 0.0060(16) -0.0021(18) C46 0.020(3) 0.023(2) 0.0209(19) 0.0047(15) 0.0044(16) -0.0004(18) C461 0.043(4) 0.027(2) 0.028(2) 0.0070(18) -0.007(2) -0.001(2) F461 0.057(2) 0.0218(13) 0.0320(14) 0.0076(11) 0.0031(14) 0.0030(14) F462 0.032(2) 0.065(3) 0.136(4) 0.056(3) -0.004(2) 0.007(2) F463 0.173(5) 0.045(2) 0.0244(16) -0.0078(14) -0.029(2) 0.052(3) C47 0.033(3) 0.029(2) 0.024(2) -0.0001(17) 0.0027(19) 0.011(2) C48 0.042(3) 0.041(3) 0.022(2) -0.0027(19) 0.002(2) 0.018(3) C481 0.092(6) 0.060(4) 0.033(3) -0.010(3) -0.011(3) 0.045(4) F481 0.142(5) 0.078(3) 0.048(2) -0.035(2) -0.033(2) 0.065(3) F482 0.104(5) 0.144(5) 0.080(3) -0.065(3) -0.059(3) 0.062(4) F483 0.251(9) 0.114(4) 0.0184(18) -0.006(2) 0.023(3) -0.012(5) C49 0.033(3) 0.033(2) 0.021(2) 0.0008(17) 0.0018(18) 0.015(2) _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 Re1 N1 1.762(4) . yes Re1 C1 1.916(5) . yes Re1 O2 2.167(4) . yes Re1 O3 2.260(4) . yes Re1 P1 2.5146(14) . yes Re1 P2 2.5378(14) . yes P1 C11 1.843(6) . yes P1 C14 1.864(5) . yes P1 C8 1.883(7) . yes P2 C20 1.834(6) . yes P2 C17 1.861(5) . yes P2 C23 1.866(6) . yes N1 O1 1.179(5) . yes N2 O4 1.155(10) . yes N2 O2 1.296(7) . yes N2 O3 1.304(7) . yes C1 C2 1.438(7) . yes C1 H1 0.9500 . yes C2 C3 1.413(7) . yes C2 C7 1.428(7) . yes C3 C4 1.383(8) . yes C3 H3 0.9500 . yes C4 C5 1.404(9) . yes C4 H4 0.9500 . yes C5 C6 1.376(10) . yes C5 H5 0.9500 . yes C6 C7 1.369(8) . yes C6 H6 0.9500 . yes C7 H7 0.9500 . yes C8 C10 1.512(9) . yes C8 C9 1.525(8) . yes C8 H8 1.0000 . yes C9 H9A 0.9800 . yes C9 H9B 0.9800 . yes C9 H9C 0.9800 . yes C10 H10A 0.9800 . yes C10 H10B 0.9800 . yes C10 H10C 0.9800 . yes C11 C12 1.518(9) . yes C11 C13 1.561(9) . yes C11 H11 1.0000 . yes C12 H12A 0.9800 . yes C12 H12B 0.9800 . yes C12 H12C 0.9800 . yes C13 H13A 0.9800 . yes C13 H13B 0.9800 . yes C13 H13C 0.9800 . yes C14 C15 1.534(9) . yes C14 C16 1.542(9) . yes C14 H14 1.0000 . yes C15 H15A 0.9800 . yes C15 H15B 0.9800 . yes C15 H15C 0.9800 . yes C16 H16A 0.9800 . yes C16 H16B 0.9800 . yes C16 H16C 0.9800 . yes C17 C19 1.517(7) . yes C17 C18 1.534(8) . yes C17 H17 1.0000 . yes C18 H18A 0.9800 . yes C18 H18B 0.9800 . yes C18 H18C 0.9800 . yes C19 H19A 0.9800 . yes C19 H19B 0.9800 . yes C19 H19C 0.9800 . yes C20 C22 1.486(10) . yes C20 C21 1.526(9) . yes C20 H20 1.0000 . yes C21 H21A 0.9800 . yes C21 H21B 0.9800 . yes C21 H21C 0.9800 . yes C22 H22A 0.9800 . yes C22 H22B 0.9800 . yes C22 H22C 0.9800 . yes C23 C25 1.513(10) . yes C23 C24 1.548(10) . yes C23 H23 1.0000 . yes C24 H24A 0.9800 . yes C24 H24B 0.9800 . yes C24 H24C 0.9800 . yes C25 H25A 0.9800 . yes C25 H25B 0.9800 . yes C25 H25C 0.9800 . yes B1 C32 1.637(7) . yes B1 C26 1.646(7) . yes B1 C44 1.646(6) . yes B1 C38 1.649(6) . yes C26 C27 1.405(7) . yes C26 C31 1.413(6) . yes C27 C28 1.396(6) . yes C27 H27 0.9500 . yes C28 C29 1.386(6) . yes C28 C281 1.492(7) . yes C281 F281 1.339(5) . yes C281 F283 1.343(6) . yes C281 F282 1.349(6) . yes C29 C30 1.390(7) . yes C29 H29 0.9500 . yes C30 C31 1.399(7) . yes C30 C301 1.514(6) . yes C301 F301 1.340(7) . yes C301 F303 1.341(6) . yes C301 F302 1.344(7) . yes C31 H31 0.9500 . yes C32 C37 1.401(6) . yes C32 C33 1.412(5) . yes C33 C34 1.388(7) . yes C33 H33 0.9500 . yes C34 C35 1.371(7) . yes C34 C341 1.514(5) . yes C341 F343 1.325(6) . yes C341 F342 1.332(7) . yes C341 F341 1.346(5) . yes C35 C36 1.403(6) . yes C35 H35 0.9500 . yes C36 C37 1.388(6) . yes C36 C361 1.484(7) . yes C361 F362 1.228(8) . yes C361 F366 1.277(19) . yes C361 F361 1.282(6) . yes C361 F363 1.441(9) . yes C361 F365 1.51(3) . yes C37 H37 0.9500 . yes C38 C39 1.400(6) . yes C38 C43 1.405(6) . yes C39 C40 1.398(6) . yes C39 H39 0.9500 . yes C40 C41 1.386(7) . yes C40 C401 1.494(7) . yes C401 F404 1.121(17) . yes C401 F405 1.17(2) . yes C401 F403 1.305(8) . yes C401 F406 1.34(2) . yes C401 F401 1.364(7) . yes C401 F402 1.407(10) . yes C41 C42 1.381(7) . yes C41 H41 0.9500 . yes C42 C43 1.400(6) . yes C42 C421 1.509(7) . yes C421 F422 1.316(6) . yes C421 F423 1.323(7) . yes C421 F421 1.330(7) . yes C43 H43 0.9500 . yes C44 C49 1.398(6) . yes C44 C45 1.402(6) . yes C45 C46 1.394(6) . yes C45 H45 0.9500 . yes C46 C47 1.383(6) . yes C46 C461 1.502(6) . yes C461 F463 1.311(6) . yes C461 F461 1.329(6) . yes C461 F462 1.350(7) . yes C47 C48 1.385(6) . yes C47 H47 0.9500 . yes C48 C49 1.399(6) . yes C48 C481 1.519(8) . yes C481 F483 1.277(9) . yes C481 F481 1.296(7) . yes C481 F482 1.353(10) . yes C49 H49 0.9500 . yes 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 N1 Re1 C1 97.9(2) . . yes N1 Re1 O2 168.71(16) . . yes C1 Re1 O2 92.69(19) . . yes N1 Re1 O3 111.79(17) . . yes C1 Re1 O3 150.27(19) . . yes O2 Re1 O3 57.64(15) . . yes N1 Re1 P1 88.21(14) . . yes C1 Re1 P1 95.48(15) . . yes O2 Re1 P1 87.01(11) . . yes O3 Re1 P1 85.75(11) . . yes N1 Re1 P2 92.95(15) . . yes C1 Re1 P2 95.20(15) . . yes O2 Re1 P2 89.83(11) . . yes O3 Re1 P2 83.65(11) . . yes P1 Re1 P2 168.99(4) . . yes C11 P1 C14 104.4(3) . . yes C11 P1 C8 111.8(3) . . yes C14 P1 C8 103.6(3) . . yes C11 P1 Re1 115.8(2) . . yes C14 P1 Re1 112.4(2) . . yes C8 P1 Re1 108.18(19) . . yes C20 P2 C17 113.1(3) . . yes C20 P2 C23 103.7(3) . . yes C17 P2 C23 103.3(3) . . yes C20 P2 Re1 111.4(2) . . yes C17 P2 Re1 109.01(19) . . yes C23 P2 Re1 116.1(2) . . yes O1 N1 Re1 174.8(4) . . yes O4 N2 O2 127.6(8) . . yes O4 N2 O3 121.5(8) . . yes O2 N2 O3 110.5(4) . . yes N2 O2 Re1 98.2(3) . . yes N2 O3 Re1 93.6(3) . . yes C2 C1 Re1 142.1(4) . . yes C2 C1 H1 109.0 . . yes Re1 C1 H1 109.0 . . yes C3 C2 C7 116.4(5) . . yes C3 C2 C1 123.7(5) . . yes C7 C2 C1 119.8(5) . . yes C4 C3 C2 121.0(5) . . yes C4 C3 H3 119.5 . . yes C2 C3 H3 119.5 . . yes C3 C4 C5 119.8(6) . . yes C3 C4 H4 120.1 . . yes C5 C4 H4 120.1 . . yes C6 C5 C4 121.0(6) . . yes C6 C5 H5 119.5 . . yes C4 C5 H5 119.5 . . yes C7 C6 C5 119.0(5) . . yes C7 C6 H6 120.5 . . yes C5 C6 H6 120.5 . . yes C6 C7 C2 122.8(6) . . yes C6 C7 H7 118.6 . . yes C2 C7 H7 118.6 . . yes C10 C8 C9 110.7(6) . . yes C10 C8 P1 116.7(5) . . yes C9 C8 P1 111.9(5) . . yes C10 C8 H8 105.6 . . yes C9 C8 H8 105.6 . . yes P1 C8 H8 105.6 . . yes C8 C9 H9A 109.5 . . yes C8 C9 H9B 109.5 . . yes H9A C9 H9B 109.5 . . yes C8 C9 H9C 109.5 . . yes H9A C9 H9C 109.5 . . yes H9B C9 H9C 109.5 . . yes C8 C10 H10A 109.5 . . yes C8 C10 H10B 109.5 . . yes H10A C10 H10B 109.5 . . yes C8 C10 H10C 109.5 . . yes H10A C10 H10C 109.5 . . yes H10B C10 H10C 109.5 . . yes C12 C11 C13 111.7(5) . . yes C12 C11 P1 116.0(4) . . yes C13 C11 P1 111.1(5) . . yes C12 C11 H11 105.7 . . yes C13 C11 H11 105.7 . . yes P1 C11 H11 105.7 . . yes C11 C12 H12A 109.5 . . yes C11 C12 H12B 109.5 . . yes H12A C12 H12B 109.5 . . yes C11 C12 H12C 109.5 . . yes H12A C12 H12C 109.5 . . yes H12B C12 H12C 109.5 . . yes C11 C13 H13A 109.5 . . yes C11 C13 H13B 109.5 . . yes H13A C13 H13B 109.5 . . yes C11 C13 H13C 109.5 . . yes H13A C13 H13C 109.5 . . yes H13B C13 H13C 109.5 . . yes C15 C14 C16 110.0(5) . . yes C15 C14 P1 115.5(5) . . yes C16 C14 P1 110.9(4) . . yes C15 C14 H14 106.6 . . yes C16 C14 H14 106.6 . . yes P1 C14 H14 106.6 . . yes C14 C15 H15A 109.5 . . yes C14 C15 H15B 109.5 . . yes H15A C15 H15B 109.5 . . yes C14 C15 H15C 109.5 . . yes H15A C15 H15C 109.5 . . yes H15B C15 H15C 109.5 . . yes C14 C16 H16A 109.5 . . yes C14 C16 H16B 109.5 . . yes H16A C16 H16B 109.5 . . yes C14 C16 H16C 109.5 . . yes H16A C16 H16C 109.5 . . yes H16B C16 H16C 109.5 . . yes C19 C17 C18 110.1(4) . . yes C19 C17 P2 117.5(4) . . yes C18 C17 P2 112.4(4) . . yes C19 C17 H17 105.3 . . yes C18 C17 H17 105.3 . . yes P2 C17 H17 105.3 . . yes C17 C18 H18A 109.5 . . yes C17 C18 H18B 109.5 . . yes H18A C18 H18B 109.5 . . yes C17 C18 H18C 109.5 . . yes H18A C18 H18C 109.5 . . yes H18B C18 H18C 109.5 . . yes C17 C19 H19A 109.5 . . yes C17 C19 H19B 109.5 . . yes H19A C19 H19B 109.5 . . yes C17 C19 H19C 109.5 . . yes H19A C19 H19C 109.5 . . yes H19B C19 H19C 109.5 . . yes C22 C20 C21 112.7(6) . . yes C22 C20 P2 115.6(5) . . yes C21 C20 P2 113.7(4) . . yes C22 C20 H20 104.4 . . yes C21 C20 H20 104.4 . . yes P2 C20 H20 104.4 . . yes C20 C21 H21A 109.5 . . yes C20 C21 H21B 109.5 . . yes H21A C21 H21B 109.5 . . yes C20 C21 H21C 109.5 . . yes H21A C21 H21C 109.5 . . yes H21B C21 H21C 109.5 . . yes C20 C22 H22A 109.5 . . yes C20 C22 H22B 109.5 . . yes H22A C22 H22B 109.5 . . yes C20 C22 H22C 109.5 . . yes H22A C22 H22C 109.5 . . yes H22B C22 H22C 109.5 . . yes C25 C23 C24 111.8(6) . . yes C25 C23 P2 115.3(5) . . yes C24 C23 P2 109.1(5) . . yes C25 C23 H23 106.7 . . yes C24 C23 H23 106.7 . . yes P2 C23 H23 106.7 . . yes C23 C24 H24A 109.5 . . yes C23 C24 H24B 109.5 . . yes H24A C24 H24B 109.5 . . yes C23 C24 H24C 109.5 . . yes H24A C24 H24C 109.5 . . yes H24B C24 H24C 109.5 . . yes C23 C25 H25A 109.5 . . yes C23 C25 H25B 109.5 . . yes H25A C25 H25B 109.5 . . yes C23 C25 H25C 109.5 . . yes H25A C25 H25C 109.5 . . yes H25B C25 H25C 109.5 . . yes C32 B1 C26 111.6(3) . . yes C32 B1 C44 102.9(4) . . yes C26 B1 C44 112.2(3) . . yes C32 B1 C38 112.8(3) . . yes C26 B1 C38 105.9(4) . . yes C44 B1 C38 111.5(3) . . yes C27 C26 C31 115.4(4) . . yes C27 C26 B1 120.8(3) . . yes C31 C26 B1 123.7(4) . . yes C28 C27 C26 122.8(4) . . yes C28 C27 H27 118.6 . . yes C26 C27 H27 118.6 . . yes C29 C28 C27 120.7(4) . . yes C29 C28 C281 119.1(4) . . yes C27 C28 C281 120.2(4) . . yes F281 C281 F283 106.4(4) . . yes F281 C281 F282 106.4(4) . . yes F283 C281 F282 106.7(4) . . yes F281 C281 C28 111.9(4) . . yes F283 C281 C28 112.6(4) . . yes F282 C281 C28 112.4(4) . . yes C28 C29 C30 118.0(4) . . yes C28 C29 H29 121.0 . . yes C30 C29 H29 121.0 . . yes C29 C30 C31 121.5(4) . . yes C29 C30 C301 118.7(4) . . yes C31 C30 C301 119.8(5) . . yes F301 C301 F303 107.3(5) . . yes F301 C301 F302 107.5(5) . . yes F303 C301 F302 105.4(5) . . yes F301 C301 C30 112.1(5) . . yes F303 C301 C30 110.9(5) . . yes F302 C301 C30 113.1(5) . . yes C30 C31 C26 121.5(4) . . yes C30 C31 H31 119.2 . . yes C26 C31 H31 119.2 . . yes C37 C32 C33 115.7(4) . . yes C37 C32 B1 123.8(3) . . yes C33 C32 B1 120.2(4) . . yes C34 C33 C32 122.0(4) . . yes C34 C33 H33 119.0 . . yes C32 C33 H33 119.0 . . yes C35 C34 C33 121.4(4) . . yes C35 C34 C341 120.9(4) . . yes C33 C34 C341 117.7(4) . . yes F343 C341 F342 106.9(4) . . yes F343 C341 F341 108.9(4) . . yes F342 C341 F341 104.3(4) . . yes F343 C341 C34 112.4(4) . . yes F342 C341 C34 112.6(4) . . yes F341 C341 C34 111.3(4) . . yes C34 C35 C36 118.0(4) . . yes C34 C35 H35 121.0 . . yes C36 C35 H35 121.0 . . yes C37 C36 C35 120.8(4) . . yes C37 C36 C361 119.6(4) . . yes C35 C36 C361 119.6(4) . . yes F362 C361 F366 51.0(10) . . yes F362 C361 F361 118.0(7) . . yes F366 C361 F361 122.2(10) . . yes F362 C361 F363 99.7(7) . . yes F366 C361 F363 49.7(11) . . yes F361 C361 F363 93.6(6) . . yes F362 C361 C36 116.3(5) . . yes F366 C361 C36 117.5(9) . . yes F361 C361 C36 115.9(4) . . yes F363 C361 C36 108.2(5) . . yes F362 C361 F365 46.9(8) . . yes F366 C361 F365 96.7(12) . . yes F361 C361 F365 86.6(8) . . yes F363 C361 F365 139.3(9) . . yes C36 C361 F365 108.1(8) . . yes C36 C37 C32 122.1(4) . . yes C36 C37 H37 118.9 . . yes C32 C37 H37 118.9 . . yes C39 C38 C43 115.9(4) . . yes C39 C38 B1 121.9(3) . . yes C43 C38 B1 122.1(4) . . yes C40 C39 C38 121.8(4) . . yes C40 C39 H39 119.1 . . yes C38 C39 H39 119.1 . . yes C41 C40 C39 121.1(4) . . yes C41 C40 C401 119.2(4) . . yes C39 C40 C401 119.7(4) . . yes F404 C401 F405 112.6(16) . . yes F404 C401 F403 124.3(10) . . yes F405 C401 F403 53.7(10) . . yes F404 C401 F406 115.2(11) . . yes F405 C401 F406 91.5(12) . . yes F403 C401 F406 37.9(7) . . yes F404 C401 F401 30.5(11) . . yes F405 C401 F401 129.6(10) . . yes F403 C401 F401 110.2(6) . . yes F406 C401 F401 87.8(9) . . yes F404 C401 F402 70.5(12) . . yes F405 C401 F402 49.9(12) . . yes F403 C401 F402 99.2(7) . . yes F406 C401 F402 134.2(9) . . yes F401 C401 F402 98.9(7) . . yes F404 C401 C40 116.1(10) . . yes F405 C401 C40 112.8(8) . . yes F403 C401 C40 118.5(5) . . yes F406 C401 C40 106.0(8) . . yes F401 C401 C40 115.8(6) . . yes F402 C401 C40 111.2(5) . . yes C42 C41 C40 118.2(4) . . yes C42 C41 H41 120.9 . . yes C40 C41 H41 120.9 . . yes C41 C42 C43 120.7(4) . . yes C41 C42 C421 119.4(4) . . yes C43 C42 C421 119.8(5) . . yes F422 C421 F423 106.7(5) . . yes F422 C421 F421 106.5(5) . . yes F423 C421 F421 104.5(5) . . yes F422 C421 C42 113.1(5) . . yes F423 C421 C42 112.1(4) . . yes F421 C421 C42 113.3(4) . . yes C42 C43 C38 122.1(4) . . yes C42 C43 H43 119.0 . . yes C38 C43 H43 119.0 . . yes C49 C44 C45 115.3(4) . . yes C49 C44 B1 121.3(4) . . yes C45 C44 B1 123.0(4) . . yes C46 C45 C44 122.2(4) . . yes C46 C45 H45 118.9 . . yes C44 C45 H45 118.9 . . yes C47 C46 C45 121.4(4) . . yes C47 C46 C461 117.6(4) . . yes C45 C46 C461 121.0(4) . . yes F463 C461 F461 107.3(4) . . yes F463 C461 F462 107.1(5) . . yes F461 C461 F462 103.1(4) . . yes F463 C461 C46 113.5(4) . . yes F461 C461 C46 113.1(4) . . yes F462 C461 C46 112.0(4) . . yes C46 C47 C48 117.7(4) . . yes C46 C47 H47 121.2 . . yes C48 C47 H47 121.2 . . yes C47 C48 C49 120.7(4) . . yes C47 C48 C481 119.9(4) . . yes C49 C48 C481 119.4(4) . . yes F483 C481 F481 110.4(6) . . yes F483 C481 F482 103.7(6) . . yes F481 C481 F482 104.2(7) . . yes F483 C481 C48 112.4(7) . . yes F481 C481 C48 114.2(5) . . yes F482 C481 C48 111.1(6) . . yes C44 C49 C48 122.6(4) . . yes C44 C49 H49 118.7 . . yes C48 C49 H49 118.7 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Re1 P1 C11 -167.8(3) . . . . yes C1 Re1 P1 C11 -70.0(3) . . . . yes O2 Re1 P1 C11 22.4(3) . . . . yes O3 Re1 P1 C11 80.2(3) . . . . yes P2 Re1 P1 C11 95.9(3) . . . . yes N1 Re1 P1 C14 72.3(3) . . . . yes C1 Re1 P1 C14 170.1(3) . . . . yes O2 Re1 P1 C14 -97.5(3) . . . . yes O3 Re1 P1 C14 -39.7(3) . . . . yes P2 Re1 P1 C14 -23.9(4) . . . . yes N1 Re1 P1 C8 -41.5(2) . . . . yes C1 Re1 P1 C8 56.3(3) . . . . yes O2 Re1 P1 C8 148.7(2) . . . . yes O3 Re1 P1 C8 -153.5(2) . . . . yes P2 Re1 P1 C8 -137.8(3) . . . . yes N1 Re1 P2 C20 -72.1(3) . . . . yes C1 Re1 P2 C20 -170.4(3) . . . . yes O2 Re1 P2 C20 96.9(3) . . . . yes O3 Re1 P2 C20 39.5(3) . . . . yes P1 Re1 P2 C20 23.7(4) . . . . yes N1 Re1 P2 C17 53.4(2) . . . . yes C1 Re1 P2 C17 -44.9(2) . . . . yes O2 Re1 P2 C17 -137.6(2) . . . . yes O3 Re1 P2 C17 165.0(2) . . . . yes P1 Re1 P2 C17 149.2(3) . . . . yes N1 Re1 P2 C23 169.5(3) . . . . yes C1 Re1 P2 C23 71.3(3) . . . . yes O2 Re1 P2 C23 -21.4(3) . . . . yes O3 Re1 P2 C23 -78.9(3) . . . . yes P1 Re1 P2 C23 -94.7(3) . . . . yes C1 Re1 N1 O1 -151(5) . . . . yes O2 Re1 N1 O1 10(5) . . . . yes O3 Re1 N1 O1 29(5) . . . . yes P1 Re1 N1 O1 -55(5) . . . . yes P2 Re1 N1 O1 114(5) . . . . yes O4 N2 O2 Re1 -170.1(10) . . . . yes O3 N2 O2 Re1 2.4(5) . . . . yes N1 Re1 O2 N2 20.2(11) . . . . yes C1 Re1 O2 N2 -179.3(4) . . . . yes O3 Re1 O2 N2 -1.5(3) . . . . yes P1 Re1 O2 N2 85.3(3) . . . . yes P2 Re1 O2 N2 -84.1(3) . . . . yes O4 N2 O3 Re1 170.8(9) . . . . yes O2 N2 O3 Re1 -2.3(5) . . . . yes N1 Re1 O3 N2 -174.0(3) . . . . yes C1 Re1 O3 N2 6.0(5) . . . . yes O2 Re1 O3 N2 1.5(3) . . . . yes P1 Re1 O3 N2 -87.6(3) . . . . yes P2 Re1 O3 N2 95.3(3) . . . . yes N1 Re1 C1 C2 -0.8(6) . . . . yes O2 Re1 C1 C2 -177.0(6) . . . . yes O3 Re1 C1 C2 179.3(5) . . . . yes P1 Re1 C1 C2 -89.7(6) . . . . yes P2 Re1 C1 C2 93.0(6) . . . . yes Re1 C1 C2 C3 -5.5(9) . . . . yes Re1 C1 C2 C7 169.9(5) . . . . yes C7 C2 C3 C4 0.2(8) . . . . yes C1 C2 C3 C4 175.7(5) . . . . yes C2 C3 C4 C5 -1.7(9) . . . . yes C3 C4 C5 C6 2.1(9) . . . . yes C4 C5 C6 C7 -0.8(9) . . . . yes C5 C6 C7 C2 -0.9(9) . . . . yes C3 C2 C7 C6 1.2(8) . . . . yes C1 C2 C7 C6 -174.6(5) . . . . yes C11 P1 C8 C10 -85.4(6) . . . . yes C14 P1 C8 C10 26.5(6) . . . . yes Re1 P1 C8 C10 146.0(5) . . . . yes C11 P1 C8 C9 43.4(5) . . . . yes C14 P1 C8 C9 155.3(4) . . . . yes Re1 P1 C8 C9 -85.2(4) . . . . yes C14 P1 C11 C12 172.6(5) . . . . yes C8 P1 C11 C12 -76.0(6) . . . . yes Re1 P1 C11 C12 48.4(6) . . . . yes C14 P1 C11 C13 -58.5(5) . . . . yes C8 P1 C11 C13 52.9(5) . . . . yes Re1 P1 C11 C13 177.4(4) . . . . yes C11 P1 C14 C15 -44.9(5) . . . . yes C8 P1 C14 C15 -162.1(5) . . . . yes Re1 P1 C14 C15 81.4(5) . . . . yes C11 P1 C14 C16 -170.9(5) . . . . yes C8 P1 C14 C16 72.0(5) . . . . yes Re1 P1 C14 C16 -44.6(5) . . . . yes C20 P2 C17 C19 -79.4(5) . . . . yes C23 P2 C17 C19 32.1(5) . . . . yes Re1 P2 C17 C19 156.1(4) . . . . yes C20 P2 C17 C18 49.9(5) . . . . yes C23 P2 C17 C18 161.4(5) . . . . yes Re1 P2 C17 C18 -74.6(5) . . . . yes C17 P2 C20 C22 -83.1(6) . . . . yes C23 P2 C20 C22 165.6(5) . . . . yes Re1 P2 C20 C22 40.1(6) . . . . yes C17 P2 C20 C21 49.6(6) . . . . yes C23 P2 C20 C21 -61.6(6) . . . . yes Re1 P2 C20 C21 172.8(4) . . . . yes C20 P2 C23 C25 -48.2(6) . . . . yes C17 P2 C23 C25 -166.4(5) . . . . yes Re1 P2 C23 C25 74.3(6) . . . . yes C20 P2 C23 C24 -175.0(5) . . . . yes C17 P2 C23 C24 66.8(5) . . . . yes Re1 P2 C23 C24 -52.4(5) . . . . yes C32 B1 C26 C27 157.5(4) . . . . yes C44 B1 C26 C27 42.6(5) . . . . yes C38 B1 C26 C27 -79.3(4) . . . . yes C32 B1 C26 C31 -26.3(5) . . . . yes C44 B1 C26 C31 -141.2(4) . . . . yes C38 B1 C26 C31 96.9(4) . . . . yes C31 C26 C27 C28 3.1(6) . . . . yes B1 C26 C27 C28 179.6(4) . . . . yes C26 C27 C28 C29 -1.2(6) . . . . yes C26 C27 C28 C281 177.1(4) . . . . yes C29 C28 C281 F281 92.8(5) . . . . yes C27 C28 C281 F281 -85.6(5) . . . . yes C29 C28 C281 F283 -27.0(6) . . . . yes C27 C28 C281 F283 154.6(4) . . . . yes C29 C28 C281 F282 -147.6(4) . . . . yes C27 C28 C281 F282 34.0(6) . . . . yes C27 C28 C29 C30 0.2(6) . . . . yes C281 C28 C29 C30 -178.2(4) . . . . yes C28 C29 C30 C31 -1.1(6) . . . . yes C28 C29 C30 C301 -178.7(4) . . . . yes C29 C30 C301 F301 -148.6(4) . . . . yes C31 C30 C301 F301 33.9(7) . . . . yes C29 C30 C301 F303 -28.5(7) . . . . yes C31 C30 C301 F303 153.9(5) . . . . yes C29 C30 C301 F302 89.7(6) . . . . yes C31 C30 C301 F302 -87.9(6) . . . . yes C29 C30 C31 C26 3.1(7) . . . . yes C301 C30 C31 C26 -179.3(4) . . . . yes C27 C26 C31 C30 -4.0(6) . . . . yes B1 C26 C31 C30 179.7(4) . . . . yes C26 B1 C32 C37 144.9(4) . . . . yes C44 B1 C32 C37 -94.6(4) . . . . yes C38 B1 C32 C37 25.7(6) . . . . yes C26 B1 C32 C33 -41.9(5) . . . . yes C44 B1 C32 C33 78.6(4) . . . . yes C38 B1 C32 C33 -161.1(4) . . . . yes C37 C32 C33 C34 -0.9(6) . . . . yes B1 C32 C33 C34 -174.6(4) . . . . yes C32 C33 C34 C35 -0.3(7) . . . . yes C32 C33 C34 C341 -179.0(4) . . . . yes C35 C34 C341 F343 3.5(6) . . . . yes C33 C34 C341 F343 -177.9(4) . . . . yes C35 C34 C341 F342 -117.3(5) . . . . yes C33 C34 C341 F342 61.3(5) . . . . yes C35 C34 C341 F341 125.9(5) . . . . yes C33 C34 C341 F341 -55.4(6) . . . . yes C33 C34 C35 C36 1.3(7) . . . . yes C341 C34 C35 C36 179.9(4) . . . . yes C34 C35 C36 C37 -1.1(7) . . . . yes C34 C35 C36 C361 179.1(5) . . . . yes C37 C36 C361 F362 52.8(10) . . . . yes C35 C36 C361 F362 -127.4(9) . . . . yes C37 C36 C361 F366 -4.9(15) . . . . yes C35 C36 C361 F366 174.9(14) . . . . yes C37 C36 C361 F361 -161.9(5) . . . . yes C35 C36 C361 F361 18.0(8) . . . . yes C37 C36 C361 F363 -58.3(7) . . . . yes C35 C36 C361 F363 121.5(6) . . . . yes C37 C36 C361 F365 103.0(9) . . . . yes C35 C36 C361 F365 -77.1(9) . . . . yes C35 C36 C37 C32 -0.2(7) . . . . yes C361 C36 C37 C32 179.7(5) . . . . yes C33 C32 C37 C36 1.1(6) . . . . yes B1 C32 C37 C36 174.6(4) . . . . yes C32 B1 C38 C39 39.2(6) . . . . yes C26 B1 C38 C39 -83.2(5) . . . . yes C44 B1 C38 C39 154.5(4) . . . . yes C32 B1 C38 C43 -144.5(4) . . . . yes C26 B1 C38 C43 93.1(5) . . . . yes C44 B1 C38 C43 -29.3(6) . . . . yes C43 C38 C39 C40 3.2(7) . . . . yes B1 C38 C39 C40 179.6(4) . . . . yes C38 C39 C40 C41 -1.9(7) . . . . yes C38 C39 C40 C401 176.9(5) . . . . yes C41 C40 C401 F404 3.7(14) . . . . yes C39 C40 C401 F404 -175.1(13) . . . . yes C41 C40 C401 F405 135.7(13) . . . . yes C39 C40 C401 F405 -43.1(15) . . . . yes C41 C40 C401 F403 -164.5(7) . . . . yes C39 C40 C401 F403 16.7(10) . . . . yes C41 C40 C401 F406 -125.7(9) . . . . yes C39 C40 C401 F406 55.5(10) . . . . yes C41 C40 C401 F401 -30.3(8) . . . . yes C39 C40 C401 F401 150.9(6) . . . . yes C41 C40 C401 F402 81.6(8) . . . . yes C39 C40 C401 F402 -97.2(7) . . . . yes C39 C40 C41 C42 -0.7(7) . . . . yes C401 C40 C41 C42 -179.5(5) . . . . yes C40 C41 C42 C43 1.8(8) . . . . yes C40 C41 C42 C421 -177.6(5) . . . . yes C41 C42 C421 F422 -25.6(8) . . . . yes C43 C42 C421 F422 155.0(5) . . . . yes C41 C42 C421 F423 95.0(6) . . . . yes C43 C42 C421 F423 -84.4(6) . . . . yes C41 C42 C421 F421 -147.0(5) . . . . yes C43 C42 C421 F421 33.6(7) . . . . yes C41 C42 C43 C38 -0.4(8) . . . . yes C421 C42 C43 C38 179.1(5) . . . . yes C39 C38 C43 C42 -2.1(7) . . . . yes B1 C38 C43 C42 -178.5(4) . . . . yes C32 B1 C44 C49 80.0(5) . . . . yes C26 B1 C44 C49 -159.9(4) . . . . yes C38 B1 C44 C49 -41.2(6) . . . . yes C32 B1 C44 C45 -92.4(5) . . . . yes C26 B1 C44 C45 27.7(6) . . . . yes C38 B1 C44 C45 146.4(4) . . . . yes C49 C44 C45 C46 2.3(7) . . . . yes B1 C44 C45 C46 175.1(4) . . . . yes C44 C45 C46 C47 1.0(7) . . . . yes C44 C45 C46 C461 -179.4(5) . . . . yes C47 C46 C461 F463 -162.5(5) . . . . yes C45 C46 C461 F463 17.8(7) . . . . yes C47 C46 C461 F461 -40.0(7) . . . . yes C45 C46 C461 F461 140.4(5) . . . . yes C47 C46 C461 F462 76.0(6) . . . . yes C45 C46 C461 F462 -103.6(6) . . . . yes C45 C46 C47 C48 -3.5(8) . . . . yes C461 C46 C47 C48 176.8(5) . . . . yes C46 C47 C48 C49 2.6(8) . . . . yes C46 C47 C48 C481 -175.4(6) . . . . yes C47 C48 C481 F483 -119.5(7) . . . . yes C49 C48 C481 F483 62.4(9) . . . . yes C47 C48 C481 F481 7.2(11) . . . . yes C49 C48 C481 F481 -170.8(7) . . . . yes C47 C48 C481 F482 124.8(6) . . . . yes C49 C48 C481 F482 -53.3(9) . . . . yes C45 C44 C49 C48 -3.3(7) . . . . yes B1 C44 C49 C48 -176.2(5) . . . . yes C47 C48 C49 C44 0.8(9) . . . . yes C481 C48 C49 C44 178.9(6) . . . . yes _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 30.21 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 4.546 _refine_diff_density_min -1.527 _refine_diff_density_rms 0.156 #===END data_of2b _database_code_depnum_ccdc_archive 'CCDC 295097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dinitrosyl-trans-bis(triisopropylphosphine)benzylidene-rhenium(-I) tetrakis(3,5-bis(trifluoromethyl)phenyl)-borate ; _chemical_name_common ; Dinitrosyl-trans-bis(triisopropylphosphine)benzylidene- rhenium(-I) tetrakis(3,5-bis(trifluoromethyl)phenyl)-borate ; _chemical_formula_moiety ? _chemical_formula_sum 'C57 H60 B F24 N2 O2 P2 Re' _chemical_formula_weight 1520.02 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 0.0000 0.0000 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8544(7) _cell_length_b 17.4738(12) _cell_length_c 18.3549(14) _cell_angle_alpha 91.674(9) _cell_angle_beta 100.282(9) _cell_angle_gamma 95.462(8) _cell_volume 3092.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 30.25 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 2.132 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Coppens et al. 1965' _exptl_absorpt_correction_T_min 0.5867 _exptl_absorpt_correction_T_max 0.7267 _exptl_special_details ; see text ; _diffrn_ambient_temperature 123(2) _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 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 to 200' _diffrn_standards_interval_count ' image' _diffrn_standards_interval_time 4.0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 43789 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 30.27 _reflns_number_total 16823 _reflns_number_gt 13940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'XRED (Stoe & Cie, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, PLUTON (Spek, 1990, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16823 _refine_ls_number_parameters 815 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.553603(14) 0.780749(7) 0.680034(6) 0.01394(4) Uani 1 d . . . P1 P 0.38401(9) 0.75462(5) 0.56310(4) 0.01701(16) Uani 1 d . . . P2 P 0.73147(9) 0.84202(5) 0.78359(4) 0.01675(15) Uani 1 d . . . N1 N 0.4239(3) 0.83501(15) 0.71300(14) 0.0157(5) Uani 1 d . . . O1 O 0.3384(3) 0.87019(16) 0.73090(15) 0.0315(6) Uani 1 d . . . N2 N 0.6840(3) 0.76988(18) 0.62119(15) 0.0242(6) Uani 1 d . . . O2 O 0.7597(3) 0.7613(2) 0.57975(16) 0.0430(8) Uani 1 d . . . C1 C 0.5360(3) 0.67884(17) 0.72091(16) 0.0169(6) Uani 1 d . . . H1 H 0.6025 0.6474 0.7081 0.020 Uiso 1 calc R . . C2 C 0.4473(4) 0.63909(19) 0.76576(17) 0.0211(7) Uani 1 d . . . C3 C 0.3532(4) 0.6749(2) 0.80060(19) 0.0266(7) Uani 1 d . . . H3 H 0.3502 0.7290 0.7983 0.032 Uiso 1 calc R . . C4 C 0.2644(5) 0.6324(3) 0.8385(2) 0.0338(9) Uani 1 d . . . H4 H 0.2016 0.6574 0.8623 0.041 Uiso 1 calc R . . C5 C 0.2672(4) 0.5532(3) 0.8416(2) 0.0361(10) Uani 1 d . . . H5 H 0.2051 0.5241 0.8667 0.043 Uiso 1 calc R . . C6 C 0.3601(5) 0.5168(2) 0.8083(2) 0.0353(10) Uani 1 d . . . H6 H 0.3618 0.4626 0.8106 0.042 Uiso 1 calc R . . C7 C 0.4511(4) 0.5593(2) 0.77148(19) 0.0258(7) Uani 1 d . . . H7 H 0.5166 0.5341 0.7499 0.031 Uiso 1 calc R . . C8 C 0.2040(4) 0.7316(2) 0.57870(19) 0.0236(7) Uani 1 d . . . H8 H 0.1931 0.7669 0.6207 0.028 Uiso 1 calc R . . C9 C 0.1807(4) 0.6492(2) 0.6049(2) 0.0288(8) Uani 1 d . . . H9A H 0.0917 0.6424 0.6219 0.043 Uiso 1 calc R . . H9B H 0.2557 0.6407 0.6458 0.043 Uiso 1 calc R . . H9C H 0.1798 0.6121 0.5637 0.043 Uiso 1 calc R . . C10 C 0.0890(4) 0.7453(3) 0.5140(2) 0.0372(10) Uani 1 d . . . H10A H 0.0871 0.7072 0.4735 0.056 Uiso 1 calc R . . H10B H 0.1067 0.7971 0.4965 0.056 Uiso 1 calc R . . H10C H -0.0005 0.7404 0.5306 0.056 Uiso 1 calc R . . C11 C 0.3803(4) 0.8429(2) 0.50988(19) 0.0302(9) Uani 1 d . . . H11 H 0.3149 0.8304 0.4618 0.036 Uiso 1 calc R . . C12 C 0.5225(5) 0.8709(2) 0.4917(2) 0.0400(11) Uani 1 d . . . H12A H 0.5136 0.9154 0.4606 0.060 Uiso 1 calc R . . H12B H 0.5566 0.8294 0.4652 0.060 Uiso 1 calc R . . H12C H 0.5880 0.8857 0.5379 0.060 Uiso 1 calc R . . C13 C 0.3253(5) 0.9080(2) 0.5506(2) 0.0379(10) Uani 1 d . . . H13A H 0.3936 0.9263 0.5947 0.057 Uiso 1 calc R . . H13B H 0.2381 0.8888 0.5655 0.057 Uiso 1 calc R . . H13C H 0.3092 0.9506 0.5175 0.057 Uiso 1 calc R . . C14 C 0.4324(4) 0.6815(2) 0.50020(17) 0.0243(7) Uani 1 d . . . H14 H 0.5129 0.7067 0.4805 0.029 Uiso 1 calc R . . C15 C 0.3188(5) 0.6582(3) 0.4321(2) 0.0377(10) Uani 1 d . . . H15A H 0.3584 0.6309 0.3948 0.057 Uiso 1 calc R . . H15B H 0.2811 0.7043 0.4112 0.057 Uiso 1 calc R . . H15C H 0.2443 0.6243 0.4470 0.057 Uiso 1 calc R . . C16 C 0.4834(5) 0.6104(2) 0.5381(2) 0.0314(9) Uani 1 d . . . H16A H 0.4107 0.5854 0.5621 0.047 Uiso 1 calc R . . H16B H 0.5665 0.6257 0.5756 0.047 Uiso 1 calc R . . H16C H 0.5058 0.5744 0.5012 0.047 Uiso 1 calc R . . C17 C 0.6968(4) 0.8050(2) 0.87318(18) 0.0266(8) Uani 1 d . . . H17 H 0.6656 0.7489 0.8633 0.032 Uiso 1 calc R . . C18 C 0.5774(5) 0.8407(3) 0.8985(2) 0.0367(9) Uani 1 d . . . H18A H 0.5484 0.8115 0.9389 0.055 Uiso 1 calc R . . H18B H 0.4994 0.8393 0.8569 0.055 Uiso 1 calc R . . H18C H 0.6074 0.8942 0.9160 0.055 Uiso 1 calc R . . C19 C 0.8221(5) 0.8103(3) 0.9370(2) 0.0371(10) Uani 1 d . . . H19A H 0.8554 0.8644 0.9499 0.056 Uiso 1 calc R . . H19B H 0.8963 0.7838 0.9215 0.056 Uiso 1 calc R . . H19C H 0.7945 0.7859 0.9803 0.056 Uiso 1 calc R . . C20 C 0.7258(4) 0.94722(19) 0.7881(2) 0.0265(7) Uani 1 d . . . H20 H 0.6406 0.9563 0.8083 0.032 Uiso 1 calc R . . C21 C 0.7089(5) 0.9824(2) 0.7122(2) 0.0394(10) Uani 1 d . . . H21A H 0.7009 1.0376 0.7180 0.059 Uiso 1 calc R . . H21B H 0.6251 0.9574 0.6802 0.059 Uiso 1 calc R . . H21C H 0.7899 0.9747 0.6897 0.059 Uiso 1 calc R . . C22 C 0.8481(5) 0.9901(2) 0.8424(3) 0.0425(11) Uani 1 d . . . H22A H 0.9354 0.9798 0.8273 0.064 Uiso 1 calc R . . H22B H 0.8473 0.9724 0.8925 0.064 Uiso 1 calc R . . H22C H 0.8397 1.0455 0.8420 0.064 Uiso 1 calc R . . C23 C 0.9110(4) 0.8230(2) 0.7796(2) 0.0278(8) Uani 1 d . . . H23 H 0.9692 0.8426 0.8281 0.033 Uiso 1 calc R . . C24 C 0.9732(4) 0.8641(3) 0.7190(3) 0.0387(10) Uani 1 d . . . H24A H 1.0664 0.8490 0.7190 0.058 Uiso 1 calc R . . H24B H 0.9786 0.9199 0.7285 0.058 Uiso 1 calc R . . H24C H 0.9144 0.8499 0.6707 0.058 Uiso 1 calc R . . C25 C 0.9215(5) 0.7363(2) 0.7737(3) 0.0389(10) Uani 1 d . . . H25A H 0.8736 0.7156 0.7247 0.058 Uiso 1 calc R . . H25B H 0.8783 0.7111 0.8120 0.058 Uiso 1 calc R . . H25C H 1.0193 0.7268 0.7806 0.058 Uiso 1 calc R . . B1 B 0.9449(4) -0.27239(19) 0.18689(17) 0.0139(6) Uani 1 d . . . C26 C 0.9513(3) -0.33640(16) 0.25085(15) 0.0137(5) Uani 1 d . . . C27 C 0.8595(3) -0.34014(17) 0.30121(16) 0.0168(6) Uani 1 d . . . H27 H 0.7942 -0.3033 0.2997 0.020 Uiso 1 calc R . . C28 C 0.8619(4) -0.39672(18) 0.35368(16) 0.0188(6) Uani 1 d . . . C281 C 0.7598(4) -0.3975(2) 0.40537(19) 0.0270(8) Uani 1 d . . . F281 F 0.7411(3) -0.32790(14) 0.42959(15) 0.0465(7) Uani 1 d . . . F282 F 0.6352(3) -0.4299(2) 0.37447(17) 0.0660(11) Uani 1 d . . . F283 F 0.7990(4) -0.4361(2) 0.46600(16) 0.0698(11) Uani 1 d . . . C29 C 0.9532(4) -0.45182(17) 0.35712(16) 0.0188(6) Uani 1 d . . . H29 H 0.9552 -0.4898 0.3932 0.023 Uiso 1 calc R . . C30 C 1.0427(4) -0.45044(17) 0.30651(16) 0.0172(6) Uani 1 d . . . C301 C 1.1381(4) -0.51157(19) 0.3062(2) 0.0263(7) Uani 1 d . . . F301 F 1.2589(3) -0.48633(14) 0.28856(16) 0.0440(6) Uani 1 d . . . F302 F 1.1662(4) -0.54417(19) 0.37097(16) 0.0630(10) Uani 1 d . . . F303 F 1.0845(4) -0.56842(15) 0.25649(19) 0.0604(9) Uani 1 d . . . C31 C 1.0413(3) -0.39399(16) 0.25451(15) 0.0148(6) Uani 1 d . . . H31 H 1.1033 -0.3946 0.2204 0.018 Uiso 1 calc R . . C32 C 0.8419(3) -0.31505(16) 0.11452(15) 0.0139(6) Uani 1 d . . . C33 C 0.8889(4) -0.35339(17) 0.05703(16) 0.0174(6) Uani 1 d . . . H33 H 0.9857 -0.3541 0.0589 0.021 Uiso 1 calc R . . C34 C 0.7961(4) -0.39059(18) -0.00313(17) 0.0207(6) Uani 1 d . . . C341 C 0.8516(4) -0.4283(2) -0.0648(2) 0.0318(9) Uani 1 d . . . F341 F 0.9730(3) -0.39385(15) -0.07428(13) 0.0410(6) Uani 1 d . . . F342 F 0.8689(4) -0.50152(16) -0.0547(2) 0.0640(10) Uani 1 d . . . F343 F 0.7657(3) -0.4262(3) -0.12958(15) 0.0785(13) Uani 1 d . . . C35 C 0.6548(4) -0.39369(18) -0.00722(17) 0.0216(7) Uani 1 d . . . H35 H 0.5927 -0.4189 -0.0483 0.026 Uiso 1 calc R . . C36 C 0.6055(3) -0.35875(17) 0.05075(17) 0.0178(6) Uani 1 d . . . C361 C 0.4532(4) -0.3620(2) 0.04900(19) 0.0250(7) Uani 1 d . . . F361 F 0.3842(2) -0.42536(14) 0.01283(14) 0.0383(6) Uani 1 d . . . F362 F 0.4203(2) -0.35962(16) 0.11653(13) 0.0381(6) Uani 1 d . . . F363 F 0.3983(3) -0.30228(14) 0.01388(14) 0.0389(6) Uani 1 d . . . C37 C 0.6981(3) -0.31972(17) 0.10975(16) 0.0160(6) Uani 1 d . . . H37 H 0.6619 -0.2954 0.1481 0.019 Uiso 1 calc R . . C38 C 1.0983(3) -0.24359(16) 0.16926(15) 0.0131(5) Uani 1 d . . . C39 C 1.1127(3) -0.21111(17) 0.10205(16) 0.0158(6) Uani 1 d . . . H39 H 1.0331 -0.2114 0.0642 0.019 Uiso 1 calc R . . C40 C 1.2396(3) -0.17837(17) 0.08867(16) 0.0163(6) Uani 1 d . . . C401 C 1.2434(4) -0.1440(2) 0.01484(18) 0.0227(7) Uani 1 d . . . F401 F 1.2039(3) -0.19609(14) -0.04194(11) 0.0375(6) Uani 1 d . . . F402 F 1.1541(3) -0.09028(14) 0.00123(12) 0.0380(6) Uani 1 d . . . F403 F 1.3682(3) -0.11206(17) 0.00877(13) 0.0443(7) Uani 1 d . . . C41 C 1.3580(3) -0.17559(19) 0.14219(17) 0.0198(6) Uani 1 d . . . H41 H 1.4447 -0.1532 0.1331 0.024 Uiso 1 calc R . . C42 C 1.3461(3) -0.20669(19) 0.21003(16) 0.0194(6) Uani 1 d . . . C421 C 1.4707(4) -0.2025(3) 0.26995(19) 0.0326(9) Uani 1 d . . . F421 F 1.5835(3) -0.2145(3) 0.24810(17) 0.0813(13) Uani 1 d . . . F422 F 1.4545(5) -0.2367(3) 0.3301(2) 0.0552(9) Uani 0.672(4) d P A 1 F423 F 1.5153(5) -0.1262(3) 0.2954(2) 0.0552(9) Uani 0.672(4) d P A 1 F424 F 1.4926(9) -0.2865(6) 0.2839(5) 0.0552(9) Uani 0.328(4) d P A 2 F425 F 1.4443(10) -0.1902(7) 0.3344(5) 0.0552(9) Uani 0.328(4) d P A 2 C43 C 1.2191(3) -0.23952(18) 0.22307(16) 0.0164(6) Uani 1 d . . . H43 H 1.2141 -0.2599 0.2701 0.020 Uiso 1 calc R . . C44 C 0.8914(3) -0.19227(16) 0.21424(15) 0.0136(6) Uani 1 d . . . C45 C 0.8185(3) -0.14451(16) 0.16514(15) 0.0141(6) Uani 1 d . . . H45 H 0.7932 -0.1606 0.1142 0.017 Uiso 1 calc R . . C46 C 0.7817(3) -0.07353(16) 0.18863(15) 0.0139(5) Uani 1 d . . . C461 C 0.7038(4) -0.02324(18) 0.13532(18) 0.0214(7) Uani 1 d . . . F461 F 0.7676(2) 0.04868(11) 0.13929(11) 0.0271(5) Uani 1 d . . . F462 F 0.5766(3) -0.01466(14) 0.14992(15) 0.0387(6) Uani 1 d . . . F463 F 0.6859(3) -0.04903(13) 0.06534(11) 0.0413(7) Uani 1 d . . . C47 C 0.8176(4) -0.04773(17) 0.26227(16) 0.0176(6) Uani 1 d . . . H47 H 0.7911 -0.0002 0.2786 0.021 Uiso 1 calc R . . C48 C 0.8932(4) -0.09316(17) 0.31119(16) 0.0184(6) Uani 1 d . . . C481 C 0.9359(5) -0.0672(2) 0.39161(18) 0.0289(8) Uani 1 d . . . F481 F 1.0678(3) -0.07828(18) 0.41820(14) 0.0571(8) Uani 1 d . . . F482 F 0.9317(4) 0.00731(16) 0.40362(14) 0.0690(11) Uani 1 d . . . F483 F 0.8639(4) -0.1051(2) 0.43459(15) 0.0839(14) Uani 1 d . . . C49 C 0.9307(3) -0.16349(17) 0.28782(15) 0.0149(6) Uani 1 d . . . H49 H 0.9845 -0.1927 0.3228 0.018 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01308(6) 0.01502(5) 0.01299(5) -0.00054(3) 0.00142(4) -0.00003(4) P1 0.0185(4) 0.0164(3) 0.0138(3) 0.0009(3) -0.0007(3) -0.0039(3) P2 0.0155(4) 0.0151(3) 0.0181(3) -0.0034(3) -0.0016(3) 0.0031(3) N1 0.0076(12) 0.0208(12) 0.0185(11) -0.0063(9) -0.0008(9) 0.0092(10) O1 0.0293(16) 0.0332(14) 0.0314(13) -0.0050(11) 0.0005(11) 0.0113(12) N2 0.0188(15) 0.0334(15) 0.0201(13) -0.0065(11) 0.0076(11) -0.0049(13) O2 0.0288(16) 0.068(2) 0.0331(15) -0.0137(14) 0.0159(12) -0.0060(15) C1 0.0163(16) 0.0170(13) 0.0167(13) 0.0006(10) 0.0018(11) 0.0011(12) C2 0.0219(18) 0.0217(15) 0.0180(14) 0.0025(11) -0.0001(12) -0.0003(13) C3 0.028(2) 0.0291(17) 0.0234(16) 0.0059(13) 0.0054(13) 0.0013(15) C4 0.032(2) 0.045(2) 0.0256(17) 0.0085(15) 0.0100(15) 0.0006(18) C5 0.031(2) 0.046(2) 0.0275(18) 0.0137(16) 0.0010(15) -0.0117(19) C6 0.044(3) 0.0263(17) 0.0301(18) 0.0110(14) -0.0012(16) -0.0109(18) C7 0.027(2) 0.0231(16) 0.0254(16) 0.0037(12) 0.0008(13) 0.0010(15) C8 0.0145(17) 0.0280(17) 0.0257(16) -0.0010(13) -0.0002(12) -0.0025(14) C9 0.0185(18) 0.0336(18) 0.0318(18) 0.0042(14) 0.0037(13) -0.0096(15) C10 0.020(2) 0.039(2) 0.047(2) 0.0064(18) -0.0072(16) 0.0003(18) C11 0.038(2) 0.0246(16) 0.0216(15) 0.0083(13) -0.0079(14) -0.0061(16) C12 0.057(3) 0.033(2) 0.0259(18) 0.0076(15) 0.0064(17) -0.017(2) C13 0.042(3) 0.0214(17) 0.044(2) 0.0085(15) -0.0101(18) 0.0022(17) C14 0.0281(19) 0.0257(16) 0.0175(14) -0.0043(12) 0.0062(12) -0.0081(14) C15 0.042(2) 0.047(2) 0.0201(16) -0.0102(15) 0.0042(15) -0.012(2) C16 0.041(2) 0.0261(17) 0.0288(17) -0.0070(14) 0.0129(16) 0.0011(16) C17 0.032(2) 0.0291(17) 0.0158(14) 0.0014(12) -0.0049(13) 0.0031(15) C18 0.037(2) 0.055(3) 0.0177(16) 0.0008(16) 0.0038(15) 0.005(2) C19 0.041(3) 0.043(2) 0.0220(17) -0.0033(15) -0.0099(15) 0.010(2) C20 0.027(2) 0.0173(14) 0.0351(18) -0.0075(13) 0.0034(14) 0.0061(14) C21 0.050(3) 0.0201(17) 0.046(2) 0.0054(16) 0.004(2) 0.0018(18) C22 0.042(3) 0.0245(18) 0.054(3) -0.0193(17) -0.007(2) 0.0012(18) C23 0.0146(18) 0.0273(17) 0.039(2) -0.0096(14) -0.0010(14) 0.0036(15) C24 0.019(2) 0.038(2) 0.057(3) -0.0149(19) 0.0105(17) -0.0084(17) C25 0.035(3) 0.0309(19) 0.049(2) -0.0083(17) -0.0015(18) 0.0123(18) B1 0.0157(17) 0.0149(14) 0.0102(13) 0.0009(10) 0.0012(11) -0.0007(13) C26 0.0138(14) 0.0144(12) 0.0117(11) 0.0005(9) 0.0006(10) -0.0009(11) C27 0.0202(16) 0.0159(13) 0.0141(12) 0.0012(10) 0.0049(11) -0.0018(12) C28 0.0238(17) 0.0183(13) 0.0143(13) 0.0008(10) 0.0065(11) -0.0043(13) C281 0.033(2) 0.0262(16) 0.0241(16) 0.0036(13) 0.0148(14) -0.0024(15) F281 0.0619(19) 0.0359(13) 0.0514(15) -0.0082(11) 0.0418(14) -0.0025(13) F282 0.0441(17) 0.096(2) 0.0565(17) -0.0317(17) 0.0329(14) -0.0364(17) F283 0.086(3) 0.099(3) 0.0468(16) 0.0483(17) 0.0486(17) 0.046(2) C29 0.0269(18) 0.0138(13) 0.0161(13) 0.0037(10) 0.0054(12) -0.0005(12) C30 0.0206(17) 0.0135(13) 0.0166(13) 0.0010(10) 0.0008(11) 0.0014(12) C301 0.035(2) 0.0180(14) 0.0281(17) 0.0059(12) 0.0084(15) 0.0079(15) F301 0.0382(16) 0.0323(12) 0.0695(18) 0.0111(12) 0.0228(13) 0.0176(12) F302 0.085(3) 0.073(2) 0.0488(16) 0.0408(15) 0.0291(16) 0.0574(19) F303 0.069(2) 0.0248(12) 0.083(2) -0.0242(13) 0.0017(17) 0.0144(13) C31 0.0183(16) 0.0136(12) 0.0127(12) -0.0006(9) 0.0035(10) 0.0009(11) C32 0.0164(15) 0.0122(12) 0.0132(12) 0.0022(9) 0.0025(10) 0.0021(11) C33 0.0168(16) 0.0183(13) 0.0172(13) -0.0007(10) 0.0026(11) 0.0034(12) C34 0.0252(18) 0.0196(14) 0.0164(13) -0.0033(11) 0.0025(12) 0.0014(13) C341 0.028(2) 0.037(2) 0.0277(17) -0.0131(15) 0.0051(15) -0.0008(17) F341 0.0387(15) 0.0515(15) 0.0350(12) -0.0145(11) 0.0220(11) -0.0080(12) F342 0.074(2) 0.0324(13) 0.098(2) -0.0243(15) 0.054(2) -0.0014(14) F343 0.0456(19) 0.161(4) 0.0262(13) -0.0395(18) -0.0025(12) 0.026(2) C35 0.0262(18) 0.0185(14) 0.0177(14) -0.0037(11) 0.0000(12) -0.0009(13) C36 0.0183(16) 0.0137(12) 0.0197(14) 0.0005(10) -0.0002(11) -0.0002(12) C361 0.0203(18) 0.0259(16) 0.0260(16) -0.0053(13) 0.0001(13) -0.0023(14) F361 0.0212(12) 0.0361(12) 0.0522(14) -0.0176(11) 0.0019(10) -0.0099(10) F362 0.0211(12) 0.0590(16) 0.0337(12) -0.0053(11) 0.0098(9) -0.0052(11) F363 0.0266(13) 0.0399(13) 0.0502(14) 0.0041(11) 0.0010(10) 0.0138(11) C37 0.0167(16) 0.0134(12) 0.0176(13) 0.0000(10) 0.0032(11) 0.0002(12) C38 0.0152(15) 0.0134(12) 0.0113(12) 0.0011(9) 0.0038(10) 0.0026(11) C39 0.0161(15) 0.0177(13) 0.0132(12) 0.0027(10) 0.0018(10) 0.0012(12) C40 0.0202(16) 0.0177(13) 0.0129(12) 0.0037(10) 0.0069(11) 0.0027(12) C401 0.0236(18) 0.0285(16) 0.0197(14) 0.0107(12) 0.0099(12) 0.0067(14) F401 0.0586(17) 0.0408(13) 0.0143(9) 0.0049(8) 0.0082(10) 0.0075(12) F402 0.0522(17) 0.0415(13) 0.0305(11) 0.0224(10) 0.0212(11) 0.0251(12) F403 0.0320(14) 0.0700(18) 0.0305(12) 0.0253(12) 0.0095(10) -0.0108(13) C41 0.0161(16) 0.0258(15) 0.0187(14) 0.0038(11) 0.0071(11) 0.0004(13) C42 0.0163(16) 0.0283(16) 0.0133(13) 0.0045(11) 0.0031(11) -0.0004(13) C421 0.0173(18) 0.062(3) 0.0180(15) 0.0083(15) 0.0035(12) -0.0018(18) F421 0.0228(15) 0.177(4) 0.0440(17) -0.006(2) -0.0007(12) 0.025(2) F422 0.0383(15) 0.072(2) 0.0423(14) 0.0085(14) -0.0211(11) -0.0085(17) F423 0.0383(15) 0.072(2) 0.0423(14) 0.0085(14) -0.0211(11) -0.0085(17) F424 0.0383(15) 0.072(2) 0.0423(14) 0.0085(14) -0.0211(11) -0.0085(17) F425 0.0383(15) 0.072(2) 0.0423(14) 0.0085(14) -0.0211(11) -0.0085(17) C43 0.0134(15) 0.0227(14) 0.0136(12) 0.0045(10) 0.0037(10) 0.0014(12) C44 0.0143(15) 0.0128(12) 0.0132(12) 0.0019(9) 0.0028(10) -0.0025(11) C45 0.0135(15) 0.0146(12) 0.0137(12) 0.0026(10) 0.0022(10) -0.0011(11) C46 0.0126(14) 0.0136(12) 0.0149(12) 0.0035(10) 0.0013(10) -0.0005(11) C461 0.0259(19) 0.0150(13) 0.0206(14) 0.0032(11) -0.0030(12) 0.0009(13) F461 0.0393(13) 0.0139(8) 0.0257(10) 0.0085(7) 0.0009(9) -0.0015(9) F462 0.0247(13) 0.0353(12) 0.0561(15) 0.0171(11) 0.0014(10) 0.0103(11) F463 0.074(2) 0.0267(11) 0.0176(10) -0.0004(8) -0.0149(10) 0.0183(12) C47 0.0228(17) 0.0132(12) 0.0163(13) -0.0005(10) 0.0027(11) 0.0009(12) C48 0.0259(18) 0.0164(13) 0.0119(12) -0.0007(10) 0.0014(11) 0.0009(13) C481 0.042(2) 0.0252(16) 0.0173(15) -0.0029(12) -0.0013(14) 0.0088(16) F481 0.061(2) 0.0683(19) 0.0318(13) -0.0180(12) -0.0239(12) 0.0208(16) F482 0.132(3) 0.0383(14) 0.0290(13) -0.0178(11) -0.0213(16) 0.0414(17) F483 0.106(3) 0.117(3) 0.0214(13) -0.0095(15) 0.0249(16) -0.044(3) C49 0.0116(15) 0.0178(13) 0.0142(12) 0.0029(10) -0.0017(10) 0.0024(11) _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 Re1 N1 1.837(3) . yes Re1 N2 1.840(3) . yes Re1 C1 1.957(3) . yes Re1 P1 2.4750(8) . yes Re1 P2 2.4831(8) . yes P1 C14 1.849(4) . yes P1 C11 1.849(3) . yes P1 C8 1.855(4) . yes P2 C20 1.844(3) . yes P2 C23 1.845(4) . yes P2 C17 1.860(4) . yes N1 O1 1.175(4) . yes N2 O2 1.173(4) . yes C1 C2 1.449(4) . yes C1 H1 0.9500 . yes C2 C3 1.399(5) . yes C2 C7 1.405(5) . yes C3 C4 1.388(5) . yes C3 H3 0.9500 . yes C4 C5 1.389(6) . yes C4 H4 0.9500 . yes C5 C6 1.380(7) . yes C5 H5 0.9500 . yes C6 C7 1.390(5) . yes C6 H6 0.9500 . yes C7 H7 0.9500 . yes C8 C10 1.530(5) . yes C8 C9 1.541(5) . yes C8 H8 1.0000 . yes C9 H9A 0.9800 . yes C9 H9B 0.9800 . yes C9 H9C 0.9800 . yes C10 H10A 0.9800 . yes C10 H10B 0.9800 . yes C10 H10C 0.9800 . yes C11 C12 1.536(6) . yes C11 C13 1.537(6) . yes C11 H11 1.0000 . yes C12 H12A 0.9800 . yes C12 H12B 0.9800 . yes C12 H12C 0.9800 . yes C13 H13A 0.9800 . yes C13 H13B 0.9800 . yes C13 H13C 0.9800 . yes C14 C16 1.525(6) . yes C14 C15 1.538(5) . yes C14 H14 1.0000 . yes C15 H15A 0.9800 . yes C15 H15B 0.9800 . yes C15 H15C 0.9800 . yes C16 H16A 0.9800 . yes C16 H16B 0.9800 . yes C16 H16C 0.9800 . yes C17 C18 1.519(6) . yes C17 C19 1.537(5) . yes C17 H17 1.0000 . yes C18 H18A 0.9800 . yes C18 H18B 0.9800 . yes C18 H18C 0.9800 . yes C19 H19A 0.9800 . yes C19 H19B 0.9800 . yes C19 H19C 0.9800 . yes C20 C21 1.528(6) . yes C20 C22 1.537(5) . yes C20 H20 1.0000 . yes C21 H21A 0.9800 . yes C21 H21B 0.9800 . yes C21 H21C 0.9800 . yes C22 H22A 0.9800 . yes C22 H22B 0.9800 . yes C22 H22C 0.9800 . yes C23 C24 1.528(6) . yes C23 C25 1.529(5) . yes C23 H23 1.0000 . yes C24 H24A 0.9800 . yes C24 H24B 0.9800 . yes C24 H24C 0.9800 . yes C25 H25A 0.9800 . yes C25 H25B 0.9800 . yes C25 H25C 0.9800 . yes B1 C32 1.633(4) . yes B1 C38 1.638(4) . yes B1 C44 1.638(5) . yes B1 C26 1.642(4) . yes C26 C31 1.398(5) . yes C26 C27 1.403(4) . yes C27 C28 1.399(4) . yes C27 H27 0.9500 . yes C28 C29 1.375(5) . yes C28 C281 1.500(5) . yes C281 F281 1.323(4) . yes C281 F282 1.324(5) . yes C281 F283 1.335(5) . yes C29 C30 1.389(4) . yes C29 H29 0.9500 . yes C30 C31 1.392(4) . yes C30 C301 1.489(5) . yes C301 F301 1.328(5) . yes C301 F302 1.329(4) . yes C301 F303 1.332(4) . yes C31 H31 0.9500 . yes C32 C37 1.398(4) . yes C32 C33 1.403(4) . yes C33 C34 1.401(4) . yes C33 H33 0.9500 . yes C34 C35 1.376(5) . yes C34 C341 1.504(5) . yes C341 F342 1.321(5) . yes C341 F341 1.329(4) . yes C341 F343 1.335(5) . yes C35 C36 1.394(5) . yes C35 H35 0.9500 . yes C36 C37 1.398(4) . yes C36 C361 1.491(5) . yes C361 F361 1.335(4) . yes C361 F362 1.337(4) . yes C361 F363 1.349(5) . yes C37 H37 0.9500 . yes C38 C39 1.397(4) . yes C38 C43 1.399(4) . yes C39 C40 1.390(4) . yes C39 H39 0.9500 . yes C40 C41 1.380(5) . yes C40 C401 1.503(4) . yes C401 F403 1.326(4) . yes C401 F401 1.341(4) . yes C401 F402 1.345(4) . yes C41 C42 1.393(4) . yes C41 H41 0.9500 . yes C42 C43 1.389(4) . yes C42 C421 1.490(5) . yes C421 F425 1.273(11) . yes C421 F421 1.281(5) . yes C421 F422 1.298(6) . yes C421 F423 1.404(6) . yes C421 F424 1.525(11) . yes F421 F424 1.692(10) . yes C43 H43 0.9500 . yes C44 C45 1.397(4) . yes C44 C49 1.401(4) . yes C45 C46 1.402(4) . yes C45 H45 0.9500 . yes C46 C47 1.385(4) . yes C46 C461 1.493(4) . yes C461 F463 1.324(4) . yes C461 F461 1.344(3) . yes C461 F462 1.349(5) . yes C47 C48 1.381(5) . yes C47 H47 0.9500 . yes C48 C49 1.394(4) . yes C48 C481 1.505(4) . yes C481 F483 1.306(5) . yes C481 F482 1.320(4) . yes C481 F481 1.338(5) . yes C49 H49 0.9500 . yes 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 N1 Re1 N2 151.45(14) . . yes N1 Re1 C1 106.37(13) . . yes N2 Re1 C1 101.83(14) . . yes N1 Re1 P1 86.74(8) . . yes N2 Re1 P1 84.62(9) . . yes C1 Re1 P1 98.82(9) . . yes N1 Re1 P2 89.13(8) . . yes N2 Re1 P2 91.97(9) . . yes C1 Re1 P2 96.74(9) . . yes P1 Re1 P2 164.44(3) . . yes C14 P1 C11 104.27(17) . . yes C14 P1 C8 111.42(16) . . yes C11 P1 C8 105.35(19) . . yes C14 P1 Re1 113.50(13) . . yes C11 P1 Re1 108.82(11) . . yes C8 P1 Re1 112.76(11) . . yes C20 P2 C23 107.96(17) . . yes C20 P2 C17 107.68(17) . . yes C23 P2 C17 105.56(19) . . yes C20 P2 Re1 110.67(13) . . yes C23 P2 Re1 114.85(12) . . yes C17 P2 Re1 109.78(12) . . yes O1 N1 Re1 177.1(2) . . yes O2 N2 Re1 175.4(3) . . yes C2 C1 Re1 136.2(3) . . yes C2 C1 H1 111.9 . . yes Re1 C1 H1 111.9 . . yes C3 C2 C7 118.2(3) . . yes C3 C2 C1 123.8(3) . . yes C7 C2 C1 118.0(3) . . yes C4 C3 C2 120.8(4) . . yes C4 C3 H3 119.6 . . yes C2 C3 H3 119.6 . . yes C3 C4 C5 120.0(4) . . yes C3 C4 H4 120.0 . . yes C5 C4 H4 120.0 . . yes C6 C5 C4 120.2(3) . . yes C6 C5 H5 119.9 . . yes C4 C5 H5 119.9 . . yes C5 C6 C7 120.0(4) . . yes C5 C6 H6 120.0 . . yes C7 C6 H6 120.0 . . yes C6 C7 C2 120.8(4) . . yes C6 C7 H7 119.6 . . yes C2 C7 H7 119.6 . . yes C10 C8 C9 110.1(3) . . yes C10 C8 P1 115.9(3) . . yes C9 C8 P1 111.7(3) . . yes C10 C8 H8 106.2 . . yes C9 C8 H8 106.2 . . yes P1 C8 H8 106.2 . . yes C8 C9 H9A 109.5 . . yes C8 C9 H9B 109.5 . . yes H9A C9 H9B 109.5 . . yes C8 C9 H9C 109.5 . . yes H9A C9 H9C 109.5 . . yes H9B C9 H9C 109.5 . . yes C8 C10 H10A 109.5 . . yes C8 C10 H10B 109.5 . . yes H10A C10 H10B 109.5 . . yes C8 C10 H10C 109.5 . . yes H10A C10 H10C 109.5 . . yes H10B C10 H10C 109.5 . . yes C12 C11 C13 109.7(3) . . yes C12 C11 P1 112.7(3) . . yes C13 C11 P1 111.4(3) . . yes C12 C11 H11 107.6 . . yes C13 C11 H11 107.6 . . yes P1 C11 H11 107.6 . . yes C11 C12 H12A 109.5 . . yes C11 C12 H12B 109.5 . . yes H12A C12 H12B 109.5 . . yes C11 C12 H12C 109.5 . . yes H12A C12 H12C 109.5 . . yes H12B C12 H12C 109.5 . . yes C11 C13 H13A 109.5 . . yes C11 C13 H13B 109.5 . . yes H13A C13 H13B 109.5 . . yes C11 C13 H13C 109.5 . . yes H13A C13 H13C 109.5 . . yes H13B C13 H13C 109.5 . . yes C16 C14 C15 110.6(3) . . yes C16 C14 P1 114.5(2) . . yes C15 C14 P1 113.4(3) . . yes C16 C14 H14 105.9 . . yes C15 C14 H14 105.9 . . yes P1 C14 H14 105.9 . . yes C14 C15 H15A 109.5 . . yes C14 C15 H15B 109.5 . . yes H15A C15 H15B 109.5 . . yes C14 C15 H15C 109.5 . . yes H15A C15 H15C 109.5 . . yes H15B C15 H15C 109.5 . . yes C14 C16 H16A 109.5 . . yes C14 C16 H16B 109.5 . . yes H16A C16 H16B 109.5 . . yes C14 C16 H16C 109.5 . . yes H16A C16 H16C 109.5 . . yes H16B C16 H16C 109.5 . . yes C18 C17 C19 109.9(3) . . yes C18 C17 P2 112.1(3) . . yes C19 C17 P2 115.9(3) . . yes C18 C17 H17 106.1 . . yes C19 C17 H17 106.1 . . yes P2 C17 H17 106.1 . . yes C17 C18 H18A 109.5 . . yes C17 C18 H18B 109.5 . . yes H18A C18 H18B 109.5 . . yes C17 C18 H18C 109.5 . . yes H18A C18 H18C 109.5 . . yes H18B C18 H18C 109.5 . . yes C17 C19 H19A 109.5 . . yes C17 C19 H19B 109.5 . . yes H19A C19 H19B 109.5 . . yes C17 C19 H19C 109.5 . . yes H19A C19 H19C 109.5 . . yes H19B C19 H19C 109.5 . . yes C21 C20 C22 111.1(3) . . yes C21 C20 P2 113.3(3) . . yes C22 C20 P2 113.4(3) . . yes C21 C20 H20 106.1 . . yes C22 C20 H20 106.1 . . yes P2 C20 H20 106.1 . . yes C20 C21 H21A 109.5 . . yes C20 C21 H21B 109.5 . . yes H21A C21 H21B 109.5 . . yes C20 C21 H21C 109.5 . . yes H21A C21 H21C 109.5 . . yes H21B C21 H21C 109.5 . . yes C20 C22 H22A 109.5 . . yes C20 C22 H22B 109.5 . . yes H22A C22 H22B 109.5 . . yes C20 C22 H22C 109.5 . . yes H22A C22 H22C 109.5 . . yes H22B C22 H22C 109.5 . . yes C24 C23 C25 111.0(3) . . yes C24 C23 P2 114.6(3) . . yes C25 C23 P2 110.4(3) . . yes C24 C23 H23 106.8 . . yes C25 C23 H23 106.8 . . yes P2 C23 H23 106.8 . . yes C23 C24 H24A 109.5 . . yes C23 C24 H24B 109.5 . . yes H24A C24 H24B 109.5 . . yes C23 C24 H24C 109.5 . . yes H24A C24 H24C 109.5 . . yes H24B C24 H24C 109.5 . . yes C23 C25 H25A 109.5 . . yes C23 C25 H25B 109.5 . . yes H25A C25 H25B 109.5 . . yes C23 C25 H25C 109.5 . . yes H25A C25 H25C 109.5 . . yes H25B C25 H25C 109.5 . . yes C32 B1 C38 112.2(2) . . yes C32 B1 C44 113.0(3) . . yes C38 B1 C44 102.7(2) . . yes C32 B1 C26 104.8(2) . . yes C38 B1 C26 112.5(3) . . yes C44 B1 C26 111.9(2) . . yes C31 C26 C27 116.1(3) . . yes C31 C26 B1 121.8(3) . . yes C27 C26 B1 121.9(3) . . yes C28 C27 C26 121.6(3) . . yes C28 C27 H27 119.2 . . yes C26 C27 H27 119.2 . . yes C29 C28 C27 121.1(3) . . yes C29 C28 C281 120.2(3) . . yes C27 C28 C281 118.6(3) . . yes F281 C281 F282 105.8(4) . . yes F281 C281 F283 105.7(3) . . yes F282 C281 F283 106.1(3) . . yes F281 C281 C28 113.3(3) . . yes F282 C281 C28 112.8(3) . . yes F283 C281 C28 112.5(4) . . yes C28 C29 C30 118.2(3) . . yes C28 C29 H29 120.9 . . yes C30 C29 H29 120.9 . . yes C29 C30 C31 120.8(3) . . yes C29 C30 C301 119.7(3) . . yes C31 C30 C301 119.5(3) . . yes F301 C301 F302 106.8(4) . . yes F301 C301 F303 105.4(3) . . yes F302 C301 F303 106.1(3) . . yes F301 C301 C30 113.1(3) . . yes F302 C301 C30 113.2(3) . . yes F303 C301 C30 111.6(3) . . yes C30 C31 C26 122.0(3) . . yes C30 C31 H31 119.0 . . yes C26 C31 H31 119.0 . . yes C37 C32 C33 116.0(3) . . yes C37 C32 B1 120.2(3) . . yes C33 C32 B1 123.6(3) . . yes C34 C33 C32 121.4(3) . . yes C34 C33 H33 119.3 . . yes C32 C33 H33 119.3 . . yes C35 C34 C33 121.6(3) . . yes C35 C34 C341 119.0(3) . . yes C33 C34 C341 119.4(3) . . yes F342 C341 F341 106.8(4) . . yes F342 C341 F343 106.3(4) . . yes F341 C341 F343 106.1(3) . . yes F342 C341 C34 113.1(3) . . yes F341 C341 C34 112.8(3) . . yes F343 C341 C34 111.2(4) . . yes C34 C35 C36 118.0(3) . . yes C34 C35 H35 121.0 . . yes C36 C35 H35 121.0 . . yes C35 C36 C37 120.3(3) . . yes C35 C36 C361 119.7(3) . . yes C37 C36 C361 120.0(3) . . yes F361 C361 F362 107.2(3) . . yes F361 C361 F363 105.8(3) . . yes F362 C361 F363 106.1(3) . . yes F361 C361 C36 112.4(3) . . yes F362 C361 C36 113.1(3) . . yes F363 C361 C36 111.7(3) . . yes C36 C37 C32 122.5(3) . . yes C36 C37 H37 118.7 . . yes C32 C37 H37 118.7 . . yes C39 C38 C43 115.8(3) . . yes C39 C38 B1 120.9(3) . . yes C43 C38 B1 122.6(2) . . yes C40 C39 C38 122.2(3) . . yes C40 C39 H39 118.9 . . yes C38 C39 H39 118.9 . . yes C41 C40 C39 121.1(3) . . yes C41 C40 C401 120.9(3) . . yes C39 C40 C401 118.0(3) . . yes F403 C401 F401 106.6(3) . . yes F403 C401 F402 107.9(3) . . yes F401 C401 F402 104.5(3) . . yes F403 C401 C40 113.1(3) . . yes F401 C401 C40 112.5(3) . . yes F402 C401 C40 111.7(3) . . yes C40 C41 C42 117.8(3) . . yes C40 C41 H41 121.1 . . yes C42 C41 H41 121.1 . . yes C43 C42 C41 120.9(3) . . yes C43 C42 C421 119.8(3) . . yes C41 C42 C421 119.3(3) . . yes F425 C421 F421 131.5(5) . . yes F425 C421 F422 37.7(5) . . yes F421 C421 F422 113.6(4) . . yes F425 C421 F423 69.3(6) . . yes F421 C421 F423 94.9(4) . . yes F422 C421 F423 103.1(4) . . yes F425 C421 C42 113.5(5) . . yes F421 C421 C42 114.9(3) . . yes F422 C421 C42 116.1(3) . . yes F423 C421 C42 111.3(4) . . yes F425 C421 F424 92.8(7) . . yes F421 C421 F424 73.6(5) . . yes F422 C421 F424 55.2(5) . . yes F423 C421 F424 144.2(4) . . yes C42 C421 F424 104.2(4) . . yes C421 F421 F424 59.9(5) . . yes C421 F424 F421 46.6(3) . . yes C42 C43 C38 122.1(3) . . yes C42 C43 H43 118.9 . . yes C38 C43 H43 118.9 . . yes C45 C44 C49 116.0(3) . . yes C45 C44 B1 122.7(2) . . yes C49 C44 B1 120.9(3) . . yes C44 C45 C46 122.1(3) . . yes C44 C45 H45 119.0 . . yes C46 C45 H45 119.0 . . yes C47 C46 C45 120.7(3) . . yes C47 C46 C461 118.0(3) . . yes C45 C46 C461 121.3(3) . . yes F463 C461 F461 107.3(3) . . yes F463 C461 F462 106.6(3) . . yes F461 C461 F462 104.8(3) . . yes F463 C461 C46 113.6(3) . . yes F461 C461 C46 111.8(3) . . yes F462 C461 C46 112.2(3) . . yes C48 C47 C46 118.0(3) . . yes C48 C47 H47 121.0 . . yes C46 C47 H47 121.0 . . yes C47 C48 C49 121.3(3) . . yes C47 C48 C481 119.9(3) . . yes C49 C48 C481 118.7(3) . . yes F483 C481 F482 109.2(4) . . yes F483 C481 F481 104.8(4) . . yes F482 C481 F481 104.0(3) . . yes F483 C481 C48 113.0(3) . . yes F482 C481 C48 113.2(3) . . yes F481 C481 C48 112.0(3) . . yes C48 C49 C44 121.8(3) . . yes C48 C49 H49 119.1 . . yes C44 C49 H49 119.1 . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Re1 P1 C14 -169.33(14) . . . . yes N2 Re1 P1 C14 37.91(15) . . . . yes C1 Re1 P1 C14 -63.26(15) . . . . yes P2 Re1 P1 C14 115.82(15) . . . . yes N1 Re1 P1 C11 75.06(18) . . . . yes N2 Re1 P1 C11 -77.69(19) . . . . yes C1 Re1 P1 C11 -178.87(18) . . . . yes P2 Re1 P1 C11 0.2(2) . . . . yes N1 Re1 P1 C8 -41.43(16) . . . . yes N2 Re1 P1 C8 165.81(16) . . . . yes C1 Re1 P1 C8 64.64(16) . . . . yes P2 Re1 P1 C8 -116.28(16) . . . . yes N1 Re1 P2 C20 -49.33(16) . . . . yes N2 Re1 P2 C20 102.13(17) . . . . yes C1 Re1 P2 C20 -155.71(17) . . . . yes P1 Re1 P2 C20 25.20(19) . . . . yes N1 Re1 P2 C23 -171.88(17) . . . . yes N2 Re1 P2 C23 -20.42(18) . . . . yes C1 Re1 P2 C23 81.74(17) . . . . yes P1 Re1 P2 C23 -97.35(18) . . . . yes N1 Re1 P2 C17 69.39(16) . . . . yes N2 Re1 P2 C17 -139.15(17) . . . . yes C1 Re1 P2 C17 -36.98(17) . . . . yes P1 Re1 P2 C17 143.92(16) . . . . yes N2 Re1 N1 O1 48(5) . . . . yes C1 Re1 N1 O1 -122(5) . . . . yes P1 Re1 N1 O1 -24(5) . . . . yes P2 Re1 N1 O1 141(5) . . . . yes N1 Re1 N2 O2 -81(4) . . . . yes C1 Re1 N2 O2 90(4) . . . . yes P1 Re1 N2 O2 -8(4) . . . . yes P2 Re1 N2 O2 -173(4) . . . . yes N1 Re1 C1 C2 2.4(3) . . . . yes N2 Re1 C1 C2 -173.1(3) . . . . yes P1 Re1 C1 C2 -86.8(3) . . . . yes P2 Re1 C1 C2 93.5(3) . . . . yes Re1 C1 C2 C3 -9.0(5) . . . . yes Re1 C1 C2 C7 167.7(3) . . . . yes C7 C2 C3 C4 -1.2(5) . . . . yes C1 C2 C3 C4 175.5(3) . . . . yes C2 C3 C4 C5 -0.6(6) . . . . yes C3 C4 C5 C6 1.3(6) . . . . yes C4 C5 C6 C7 -0.1(6) . . . . yes C5 C6 C7 C2 -1.8(6) . . . . yes C3 C2 C7 C6 2.4(5) . . . . yes C1 C2 C7 C6 -174.4(3) . . . . yes C14 P1 C8 C10 -73.9(3) . . . . yes C11 P1 C8 C10 38.6(3) . . . . yes Re1 P1 C8 C10 157.1(3) . . . . yes C14 P1 C8 C9 53.2(3) . . . . yes C11 P1 C8 C9 165.7(2) . . . . yes Re1 P1 C8 C9 -75.8(2) . . . . yes C14 P1 C11 C12 -62.7(3) . . . . yes C8 P1 C11 C12 179.9(3) . . . . yes Re1 P1 C11 C12 58.8(3) . . . . yes C14 P1 C11 C13 173.5(3) . . . . yes C8 P1 C11 C13 56.1(3) . . . . yes Re1 P1 C11 C13 -65.1(3) . . . . yes C11 P1 C14 C16 163.1(3) . . . . yes C8 P1 C14 C16 -83.8(3) . . . . yes Re1 P1 C14 C16 44.8(3) . . . . yes C11 P1 C14 C15 -68.8(3) . . . . yes C8 P1 C14 C15 44.3(3) . . . . yes Re1 P1 C14 C15 172.9(2) . . . . yes C20 P2 C17 C18 44.1(3) . . . . yes C23 P2 C17 C18 159.3(3) . . . . yes Re1 P2 C17 C18 -76.4(3) . . . . yes C20 P2 C17 C19 -83.2(3) . . . . yes C23 P2 C17 C19 32.0(3) . . . . yes Re1 P2 C17 C19 156.3(3) . . . . yes C23 P2 C20 C21 83.9(3) . . . . yes C17 P2 C20 C21 -162.6(3) . . . . yes Re1 P2 C20 C21 -42.6(3) . . . . yes C23 P2 C20 C22 -44.0(4) . . . . yes C17 P2 C20 C22 69.5(3) . . . . yes Re1 P2 C20 C22 -170.5(3) . . . . yes C20 P2 C23 C24 -52.3(3) . . . . yes C17 P2 C23 C24 -167.2(3) . . . . yes Re1 P2 C23 C24 71.7(3) . . . . yes C20 P2 C23 C25 -178.5(3) . . . . yes C17 P2 C23 C25 66.5(3) . . . . yes Re1 P2 C23 C25 -54.5(3) . . . . yes C32 B1 C26 C31 83.3(3) . . . . yes C38 B1 C26 C31 -38.9(4) . . . . yes C44 B1 C26 C31 -153.9(3) . . . . yes C32 B1 C26 C27 -91.6(3) . . . . yes C38 B1 C26 C27 146.2(3) . . . . yes C44 B1 C26 C27 31.2(4) . . . . yes C31 C26 C27 C28 2.2(4) . . . . yes B1 C26 C27 C28 177.4(3) . . . . yes C26 C27 C28 C29 -1.0(5) . . . . yes C26 C27 C28 C281 -179.6(3) . . . . yes C29 C28 C281 F281 141.3(3) . . . . yes C27 C28 C281 F281 -40.1(5) . . . . yes C29 C28 C281 F282 -98.5(4) . . . . yes C27 C28 C281 F282 80.0(4) . . . . yes C29 C28 C281 F283 21.5(5) . . . . yes C27 C28 C281 F283 -160.0(3) . . . . yes C27 C28 C29 C30 -0.7(5) . . . . yes C281 C28 C29 C30 177.8(3) . . . . yes C28 C29 C30 C31 1.0(4) . . . . yes C28 C29 C30 C301 -177.0(3) . . . . yes C29 C30 C301 F301 -146.1(3) . . . . yes C31 C30 C301 F301 35.9(4) . . . . yes C29 C30 C301 F302 -24.4(5) . . . . yes C31 C30 C301 F302 157.6(3) . . . . yes C29 C30 C301 F303 95.2(4) . . . . yes C31 C30 C301 F303 -82.8(4) . . . . yes C29 C30 C31 C26 0.3(4) . . . . yes C301 C30 C31 C26 178.3(3) . . . . yes C27 C26 C31 C30 -1.9(4) . . . . yes B1 C26 C31 C30 -177.0(3) . . . . yes C38 B1 C32 C37 -157.9(3) . . . . yes C44 B1 C32 C37 -42.3(3) . . . . yes C26 B1 C32 C37 79.8(3) . . . . yes C38 B1 C32 C33 26.9(4) . . . . yes C44 B1 C32 C33 142.5(3) . . . . yes C26 B1 C32 C33 -95.5(3) . . . . yes C37 C32 C33 C34 3.1(4) . . . . yes B1 C32 C33 C34 178.6(3) . . . . yes C32 C33 C34 C35 -2.5(5) . . . . yes C32 C33 C34 C341 177.7(3) . . . . yes C35 C34 C341 F342 -88.3(5) . . . . yes C33 C34 C341 F342 91.5(4) . . . . yes C35 C34 C341 F341 150.3(3) . . . . yes C33 C34 C341 F341 -29.8(5) . . . . yes C35 C34 C341 F343 31.3(5) . . . . yes C33 C34 C341 F343 -148.9(4) . . . . yes C33 C34 C35 C36 -0.2(5) . . . . yes C341 C34 C35 C36 179.6(3) . . . . yes C34 C35 C36 C37 2.1(5) . . . . yes C34 C35 C36 C361 -179.0(3) . . . . yes C35 C36 C361 F361 29.8(4) . . . . yes C37 C36 C361 F361 -151.3(3) . . . . yes C35 C36 C361 F362 151.3(3) . . . . yes C37 C36 C361 F362 -29.7(4) . . . . yes C35 C36 C361 F363 -89.1(4) . . . . yes C37 C36 C361 F363 89.9(4) . . . . yes C35 C36 C37 C32 -1.3(5) . . . . yes C361 C36 C37 C32 179.7(3) . . . . yes C33 C32 C37 C36 -1.3(4) . . . . yes B1 C32 C37 C36 -176.9(3) . . . . yes C32 B1 C38 C39 40.2(4) . . . . yes C44 B1 C38 C39 -81.5(3) . . . . yes C26 B1 C38 C39 158.0(3) . . . . yes C32 B1 C38 C43 -149.2(3) . . . . yes C44 B1 C38 C43 89.1(3) . . . . yes C26 B1 C38 C43 -31.4(4) . . . . yes C43 C38 C39 C40 1.5(5) . . . . yes B1 C38 C39 C40 172.7(3) . . . . yes C38 C39 C40 C41 -0.9(5) . . . . yes C38 C39 C40 C401 -179.2(3) . . . . yes C41 C40 C401 F403 -0.5(5) . . . . yes C39 C40 C401 F403 177.8(3) . . . . yes C41 C40 C401 F401 120.4(4) . . . . yes C39 C40 C401 F401 -61.3(4) . . . . yes C41 C40 C401 F402 -122.4(3) . . . . yes C39 C40 C401 F402 55.9(4) . . . . yes C39 C40 C41 C42 0.0(5) . . . . yes C401 C40 C41 C42 178.3(3) . . . . yes C40 C41 C42 C43 0.2(5) . . . . yes C40 C41 C42 C421 -178.1(3) . . . . yes C43 C42 C421 F425 -35.8(8) . . . . yes C41 C42 C421 F425 142.4(7) . . . . yes C43 C42 C421 F421 141.9(4) . . . . yes C41 C42 C421 F421 -39.9(6) . . . . yes C43 C42 C421 F422 5.8(6) . . . . yes C41 C42 C421 F422 -175.9(5) . . . . yes C43 C42 C421 F423 -111.7(4) . . . . yes C41 C42 C421 F423 66.5(5) . . . . yes C43 C42 C421 F424 63.7(6) . . . . yes C41 C42 C421 F424 -118.1(5) . . . . yes F425 C421 F421 F424 78.9(9) . . . . yes F422 C421 F421 F424 38.8(4) . . . . yes F423 C421 F421 F424 145.4(4) . . . . yes C42 C421 F421 F424 -98.3(5) . . . . yes F425 C421 F424 F421 -132.7(5) . . . . yes F422 C421 F424 F421 -135.6(4) . . . . yes F423 C421 F424 F421 -75.1(8) . . . . yes C42 C421 F424 F421 112.2(3) . . . . yes C41 C42 C43 C38 0.5(5) . . . . yes C421 C42 C43 C38 178.8(3) . . . . yes C39 C38 C43 C42 -1.3(5) . . . . yes B1 C38 C43 C42 -172.3(3) . . . . yes C32 B1 C44 C45 -32.3(4) . . . . yes C38 B1 C44 C45 88.9(3) . . . . yes C26 B1 C44 C45 -150.2(3) . . . . yes C32 B1 C44 C49 155.3(3) . . . . yes C38 B1 C44 C49 -83.6(3) . . . . yes C26 B1 C44 C49 37.3(4) . . . . yes C49 C44 C45 C46 -2.7(4) . . . . yes B1 C44 C45 C46 -175.5(3) . . . . yes C44 C45 C46 C47 0.5(4) . . . . yes C44 C45 C46 C461 180.0(3) . . . . yes C47 C46 C461 F463 173.8(3) . . . . yes C45 C46 C461 F463 -5.7(4) . . . . yes C47 C46 C461 F461 52.3(4) . . . . yes C45 C46 C461 F461 -127.3(3) . . . . yes C47 C46 C461 F462 -65.1(4) . . . . yes C45 C46 C461 F462 115.3(3) . . . . yes C45 C46 C47 C48 1.4(4) . . . . yes C461 C46 C47 C48 -178.1(3) . . . . yes C46 C47 C48 C49 -1.0(5) . . . . yes C46 C47 C48 C481 179.4(3) . . . . yes C47 C48 C481 F483 105.8(4) . . . . yes C49 C48 C481 F483 -73.9(5) . . . . yes C47 C48 C481 F482 -18.9(5) . . . . yes C49 C48 C481 F482 161.4(4) . . . . yes C47 C48 C481 F481 -136.1(3) . . . . yes C49 C48 C481 F481 44.2(4) . . . . yes C47 C48 C49 C44 -1.4(5) . . . . yes C481 C48 C49 C44 178.3(3) . . . . yes C45 C44 C49 C48 3.2(4) . . . . yes B1 C44 C49 C48 176.1(3) . . . . yes _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 30.27 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 2.632 _refine_diff_density_min -2.866 _refine_diff_density_rms 0.145