Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Mike Ward' 'Zoe R. Bell' 'Nail M. Shavaleev' _publ_contact_author_name 'Prof Mike Ward' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A simple, general synthesis of mixed d-f complexes containing both {Re(CO)3Cl(diimine)} and lanthanide-tris(beta-diketonate) luminophores linked by bis-diimine bridging ligands ; _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper A simple, general synthesis of mixed d-f complexes... ' by N. M. Shavaleev, et al, submitted to Dalton Trans. for publication. ; data_snoopys _database_code_CSD 191575 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H36 Cl Er F21 N4 O9 Re' _chemical_formula_weight 1516.65 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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 '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 11.756(4) _cell_length_b 12.029(3) _cell_length_c 18.647(5) _cell_angle_alpha 81.475(17) _cell_angle_beta 88.39(2) _cell_angle_gamma 83.33(2) _cell_volume 2589.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour clear _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1462 _exptl_absorpt_coefficient_mu 4.126 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ? _exptl_special_details ; FOD ligands are inherently disordered; no model of disorder proved to be wholly satisfactory, resulting in markedly prolate anisotropic displacement parameters for some atoms. Any attempt to model the disorder which involved increasing the number of parameters made the refinement unstable as the data was weak. The use of ISOR here did not help, so F51-F55 and F51'-F55' were refined with isotropic thermal parameters. ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23986 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.1411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9114 _reflns_number_gt 5556 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9114 _refine_ls_number_parameters 698 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.22534(4) 0.23111(4) 0.76013(3) 0.01682(15) Uani 1 1 d . . . Re1 Re 0.33214(4) 0.37691(4) 0.43272(3) 0.02325(15) Uani 1 1 d . . . Cl1 Cl 0.2966(2) 0.5450(2) 0.49408(18) 0.0318(8) Uani 1 1 d . . . F371 F -0.2014(6) 0.0791(6) 0.8397(4) 0.0362(18) Uani 1 1 d . . . F372 F -0.1952(5) 0.2055(5) 0.7441(4) 0.0304(16) Uani 1 1 d . . . F381 F -0.0060(5) -0.0405(5) 0.7693(4) 0.0314(17) Uani 1 1 d . . . F382 F -0.0630(5) 0.0761(6) 0.6730(3) 0.0319(17) Uani 1 1 d . . . F391 F -0.2097(6) -0.1155(6) 0.7850(4) 0.045(2) Uani 1 1 d . . . F392 F -0.1515(6) -0.1087(6) 0.6748(4) 0.0391(18) Uani 1 1 d . . . F393 F -0.2860(6) 0.0169(6) 0.7035(4) 0.0374(18) Uani 1 1 d . . . F471 F 0.3683(5) -0.1385(5) 0.6099(4) 0.0314(17) Uani 1 1 d . . . F472 F 0.3772(6) 0.0354(6) 0.5629(3) 0.0342(17) Uani 1 1 d . . . F481 F 0.1557(6) 0.0786(6) 0.5499(4) 0.0370(18) Uani 1 1 d . . . F482 F 0.1238(5) -0.0727(6) 0.6218(4) 0.0324(17) Uani 1 1 d . . . F491 F 0.2137(6) -0.2043(6) 0.5267(4) 0.0405(19) Uani 1 1 d . . . F492 F 0.0936(6) -0.0712(6) 0.4760(4) 0.051(2) Uani 1 1 d . . . F493 F 0.2747(7) -0.0625(6) 0.4592(4) 0.044(2) Uani 1 1 d . . . F571 F 0.4828(8) 0.2989(7) 0.9364(5) 0.080(3) Uani 1 1 d . . . F572 F 0.4544(6) 0.4777(7) 0.9287(4) 0.058(3) Uani 1 1 d . . . O34 O 0.1607(6) 0.2381(6) 0.8758(4) 0.0255(19) Uani 1 1 d . . . O36 O 0.0406(6) 0.1961(6) 0.7639(4) 0.0222(18) Uani 1 1 d . . . O44 O 0.3251(7) 0.0743(6) 0.8183(4) 0.027(2) Uani 1 1 d . . . O46 O 0.2396(6) 0.0966(6) 0.6841(4) 0.0175(17) Uiso 1 1 d . . . O54 O 0.1738(6) 0.4191(6) 0.7487(4) 0.0207(18) Uani 1 1 d . . . O56 O 0.3715(6) 0.3019(6) 0.8126(4) 0.0196(17) Uani 1 1 d . . . O61 O 0.5437(7) 0.4535(9) 0.3486(5) 0.052(3) Uani 1 1 d . . . O71 O 0.3765(8) 0.1626(9) 0.3639(6) 0.055(3) Uani 1 1 d . . . O81 O 0.1846(8) 0.4955(10) 0.3043(5) 0.067(4) Uani 1 1 d . . . N11 N 0.3731(8) 0.2698(7) 0.6614(5) 0.020(2) Uani 1 1 d . . . N13 N 0.4131(7) 0.3035(7) 0.5345(5) 0.020(2) Uani 1 1 d . . . N21 N 0.1450(8) 0.3045(7) 0.6324(5) 0.019(2) Uani 1 1 d . . . N23 N 0.1935(7) 0.3325(7) 0.5060(5) 0.016(2) Uani 1 1 d . . . C12 C 0.3435(9) 0.2954(9) 0.5927(6) 0.018(3) Uani 1 1 d . . . C14 C 0.5280(10) 0.2790(9) 0.5474(6) 0.022(3) Uani 1 1 d . . . H14A H 0.5804 0.2818 0.5091 0.026 Uiso 1 1 calc R . . C15 C 0.5649(10) 0.2500(9) 0.6177(6) 0.021(3) Uani 1 1 d . . . H15A H 0.6427 0.2332 0.6272 0.025 Uiso 1 1 calc R . . C16 C 0.4873(9) 0.2461(9) 0.6734(6) 0.021(3) Uani 1 1 d . . . H16A H 0.5132 0.2268 0.7208 0.025 Uiso 1 1 calc R . . C22 C 0.2190(9) 0.3146(8) 0.5759(6) 0.016(3) Uani 1 1 d . . . C24 C 0.0784(9) 0.3469(9) 0.4909(6) 0.020(3) Uani 1 1 d . . . H24A H 0.0556 0.3610 0.4427 0.024 Uiso 1 1 calc R . . C25 C -0.0033(9) 0.3412(9) 0.5443(6) 0.021(3) Uani 1 1 d . . . H25A H -0.0808 0.3500 0.5333 0.025 Uiso 1 1 calc R . . C26 C 0.0327(10) 0.3219(9) 0.6155(6) 0.024(3) Uani 1 1 d . . . H26A H -0.0217 0.3209 0.6527 0.029 Uiso 1 1 calc R . . C30 C 0.0806(10) 0.2309(11) 0.9929(6) 0.028(3) Uani 1 1 d . . . C31 C 0.1917(14) 0.1740(14) 1.0215(9) 0.068(5) Uiso 1 1 d . . . H31A H 0.2516 0.1930 0.9874 0.102 Uiso 1 1 calc R . . H31B H 0.1896 0.0935 1.0289 0.102 Uiso 1 1 calc R . . H31C H 0.2061 0.1983 1.0668 0.102 Uiso 1 1 calc R . . C32 C 0.0761(14) 0.3569(12) 0.9929(8) 0.060(5) Uani 1 1 d . . . H32A H 0.1339 0.3863 0.9605 0.089 Uiso 1 1 calc R . . H32B H 0.0894 0.3714 1.0411 0.089 Uiso 1 1 calc R . . H32C H 0.0020 0.3930 0.9772 0.089 Uiso 1 1 calc R . . C33 C -0.0169(11) 0.1852(12) 1.0411(7) 0.045(4) Uani 1 1 d . . . H33A H -0.0265 0.1105 1.0317 0.068 Uiso 1 1 calc R . . H33B H -0.0867 0.2341 1.0303 0.068 Uiso 1 1 calc R . . H33C H 0.0016 0.1824 1.0912 0.068 Uiso 1 1 calc R . . C34 C 0.0750(10) 0.2111(9) 0.9149(7) 0.025(3) Uani 1 1 d . . . C35 C -0.0173(10) 0.1664(9) 0.8875(6) 0.023(3) Uani 1 1 d . . . H35A H -0.0724 0.1374 0.9194 0.028 Uiso 1 1 calc R . . C36 C -0.0273(9) 0.1649(9) 0.8160(6) 0.018(3) Uani 1 1 d . . . C37 C -0.1317(10) 0.1206(9) 0.7866(6) 0.025(3) Uani 1 1 d . . . C38 C -0.0965(10) 0.0283(10) 0.7386(6) 0.029(3) Uani 1 1 d . . . C39 C -0.1880(10) -0.0464(10) 0.7264(7) 0.028(3) Uani 1 1 d . . . C40 C 0.4410(11) -0.0903(9) 0.8720(7) 0.030(3) Uani 1 1 d . . . C41 C 0.3494(11) -0.1140(11) 0.9295(7) 0.043(4) Uani 1 1 d . . . H41A H 0.3024 -0.0448 0.9348 0.064 Uiso 1 1 calc R . . H41B H 0.3852 -0.1449 0.9749 0.064 Uiso 1 1 calc R . . H41C H 0.3028 -0.1673 0.9153 0.064 Uiso 1 1 calc R . . C42 C 0.5252(11) -0.0200(11) 0.8981(7) 0.038(3) Uani 1 1 d . . . H42A H 0.4855 0.0503 0.9084 0.057 Uiso 1 1 calc R . . H42B H 0.5823 -0.0052 0.8612 0.057 Uiso 1 1 calc R . . H42C H 0.5613 -0.0604 0.9414 0.057 Uiso 1 1 calc R . . C43 C 0.5021(11) -0.2011(10) 0.8529(8) 0.043(4) Uani 1 1 d . . . H43A H 0.5455 -0.2402 0.8938 0.064 Uiso 1 1 calc R . . H43B H 0.5527 -0.1854 0.8123 0.064 Uiso 1 1 calc R . . H43C H 0.4465 -0.2475 0.8406 0.064 Uiso 1 1 calc R . . C44 C 0.3768(9) -0.0179(10) 0.8067(6) 0.024(3) Uani 1 1 d . . . C45 C 0.3750(9) -0.0541(10) 0.7377(6) 0.027(3) Uani 1 1 d . . . H45A H 0.4212 -0.1195 0.7298 0.033 Uiso 1 1 calc R . . C46 C 0.3087(9) 0.0028(9) 0.6829(6) 0.021(3) Uani 1 1 d . . . C47 C 0.3154(10) -0.0330(9) 0.6090(7) 0.025(3) Uani 1 1 d . . . C48 C 0.1957(11) -0.0295(10) 0.5730(6) 0.029(3) Uani 1 1 d . . . C49 C 0.1938(11) -0.0929(11) 0.5080(7) 0.034(3) Uani 1 1 d . . . C50 C 0.1281(10) 0.6137(9) 0.7561(6) 0.028(3) Uani 1 1 d . . . C51 C 0.0207(11) 0.6064(12) 0.8036(8) 0.050(4) Uani 1 1 d . . . H51A H 0.0423 0.5826 0.8533 0.075 Uiso 1 1 calc R . . H51B H -0.0243 0.5527 0.7883 0.075 Uiso 1 1 calc R . . H51C H -0.0234 0.6794 0.7991 0.075 Uiso 1 1 calc R . . C52 C 0.0964(11) 0.6273(11) 0.6756(6) 0.039(3) Uani 1 1 d . . . H52A H 0.0554 0.7008 0.6615 0.058 Uiso 1 1 calc R . . H52B H 0.0489 0.5702 0.6684 0.058 Uiso 1 1 calc R . . H52C H 0.1649 0.6194 0.6467 0.058 Uiso 1 1 calc R . . C53 C 0.1894(12) 0.7149(10) 0.7705(8) 0.044(4) Uani 1 1 d . . . H53A H 0.2057 0.7077 0.8213 0.066 Uiso 1 1 calc R . . H53B H 0.1410 0.7841 0.7561 0.066 Uiso 1 1 calc R . . H53C H 0.2597 0.7158 0.7431 0.066 Uiso 1 1 calc R . . C54 C 0.2042(9) 0.5002(9) 0.7761(5) 0.015(2) Uani 1 1 d . . . C55 C 0.2962(9) 0.4912(9) 0.8226(6) 0.023(3) Uani 1 1 d . . . H55A H 0.3078 0.5537 0.8444 0.028 Uiso 1 1 calc R . . C56 C 0.3720(9) 0.3928(10) 0.8381(6) 0.023(3) Uani 1 1 d . . . C57 C 0.4718(10) 0.3940(10) 0.8887(6) 0.025(3) Uani 1 1 d . A . C58 C 0.5877(12) 0.4043(13) 0.8515(6) 0.045(4) Uani 1 1 d . . . C59 C 0.6881(13) 0.4229(13) 0.8954(8) 0.047(4) Uani 1 1 d . A . C61 C 0.4626(12) 0.4264(11) 0.3807(6) 0.035(3) Uani 1 1 d . . . C71 C 0.3561(9) 0.2455(13) 0.3911(7) 0.035(3) Uani 1 1 d . . . C81 C 0.2437(10) 0.4483(12) 0.3513(7) 0.041(4) Uani 1 1 d . . . F51 F 0.6140(14) 0.3560(15) 0.7967(9) 0.060(6) Uiso 0.525(13) 1 d P A 1 F52 F 0.5659(13) 0.5220(14) 0.8109(8) 0.052(5) Uiso 0.525(13) 1 d P A 1 F53 F 0.7802(15) 0.4489(17) 0.8562(9) 0.056(5) Uiso 0.525(13) 1 d P A 1 F54 F 0.6893(11) 0.3744(11) 0.9627(7) 0.027(4) Uiso 0.525(13) 1 d P A 1 F55 F 0.6720(18) 0.4960(19) 0.9381(13) 0.090(7) Uiso 0.525(13) 1 d P A 1 F51' F 0.6188(11) 0.2772(12) 0.8432(7) 0.028(4) Uiso 0.475(13) 1 d P A 2 F52' F 0.5820(13) 0.4487(14) 0.7876(9) 0.038(5) Uiso 0.475(13) 1 d P A 2 F53' F 0.7864(13) 0.3868(15) 0.8618(8) 0.036(4) Uiso 0.475(13) 1 d P A 2 F54' F 0.723(2) 0.322(3) 0.9293(16) 0.117(10) Uiso 0.475(13) 1 d P A 2 F55' F 0.6758(13) 0.5342(14) 0.8913(10) 0.041(5) Uiso 0.475(13) 1 d P A 2 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 Er1 0.0129(3) 0.0180(3) 0.0184(3) -0.0016(2) -0.0028(2) 0.0025(2) Re1 0.0153(3) 0.0349(3) 0.0183(3) 0.0017(2) -0.0032(2) -0.0041(2) Cl1 0.0229(16) 0.0189(16) 0.050(2) 0.0059(15) -0.0079(15) 0.0006(13) F371 0.029(4) 0.055(5) 0.029(4) -0.009(4) 0.013(3) -0.022(4) F372 0.018(4) 0.037(4) 0.037(4) -0.010(3) -0.006(3) 0.004(3) F381 0.015(4) 0.033(4) 0.045(4) -0.008(3) -0.015(3) 0.007(3) F382 0.027(4) 0.046(4) 0.025(4) -0.013(3) 0.007(3) -0.005(3) F391 0.050(5) 0.042(5) 0.040(5) 0.011(4) -0.006(4) -0.016(4) F392 0.040(5) 0.041(4) 0.040(4) -0.020(4) -0.008(4) -0.001(4) F393 0.023(4) 0.038(4) 0.050(5) -0.007(4) -0.009(3) 0.004(3) F471 0.024(4) 0.028(4) 0.042(4) -0.014(3) -0.013(3) 0.012(3) F472 0.039(4) 0.038(4) 0.027(4) -0.001(3) 0.006(3) -0.015(3) F481 0.036(4) 0.036(4) 0.037(4) -0.008(3) -0.018(3) 0.014(3) F482 0.016(4) 0.039(4) 0.043(4) -0.008(4) 0.003(3) -0.002(3) F491 0.039(5) 0.034(4) 0.050(5) -0.013(4) -0.012(4) 0.004(3) F492 0.047(5) 0.058(5) 0.050(5) -0.024(4) -0.029(4) 0.016(4) F493 0.061(5) 0.044(5) 0.026(4) -0.013(4) 0.007(4) 0.001(4) F571 0.083(7) 0.065(6) 0.086(7) 0.050(5) -0.068(6) -0.043(5) F572 0.027(5) 0.093(7) 0.062(6) -0.053(5) -0.023(4) 0.025(4) O34 0.021(5) 0.026(5) 0.031(5) -0.008(4) 0.008(4) -0.004(4) O36 0.020(4) 0.030(5) 0.016(4) -0.003(4) 0.006(3) 0.000(4) O44 0.039(5) 0.018(4) 0.023(5) -0.005(4) -0.007(4) 0.004(4) O54 0.012(4) 0.021(4) 0.030(5) -0.002(4) -0.009(3) -0.004(3) O56 0.015(4) 0.021(4) 0.023(4) -0.002(4) 0.000(3) 0.001(3) O61 0.020(5) 0.099(8) 0.032(5) 0.018(5) 0.000(4) -0.019(5) O71 0.026(6) 0.092(8) 0.062(7) -0.056(7) 0.002(5) -0.009(5) O81 0.029(6) 0.124(10) 0.037(6) 0.027(6) -0.018(5) -0.013(6) N11 0.025(6) 0.012(5) 0.022(6) -0.004(4) -0.007(4) 0.001(4) N13 0.015(5) 0.020(5) 0.024(5) 0.001(4) -0.006(4) -0.005(4) N21 0.019(6) 0.016(5) 0.018(5) -0.001(4) -0.007(4) 0.010(4) N23 0.009(5) 0.021(5) 0.017(5) -0.001(4) -0.010(4) 0.001(4) C12 0.021(6) 0.017(6) 0.013(6) 0.009(5) -0.005(5) -0.005(5) C14 0.021(7) 0.013(6) 0.032(7) -0.006(5) 0.002(5) 0.000(5) C15 0.021(6) 0.023(6) 0.021(6) -0.010(5) -0.009(5) -0.005(5) C16 0.019(7) 0.021(6) 0.020(6) 0.003(5) -0.008(5) 0.006(5) C22 0.014(6) 0.010(6) 0.023(7) -0.003(5) 0.005(5) 0.008(5) C24 0.021(7) 0.016(6) 0.021(6) 0.006(5) -0.007(5) -0.006(5) C25 0.012(6) 0.027(7) 0.022(6) -0.002(5) -0.008(5) 0.008(5) C26 0.024(7) 0.020(6) 0.025(7) 0.001(5) 0.011(6) 0.000(5) C30 0.019(7) 0.049(8) 0.017(6) -0.013(6) -0.003(5) 0.007(6) C32 0.088(13) 0.056(11) 0.041(9) -0.023(8) 0.006(9) -0.015(9) C33 0.038(9) 0.069(11) 0.028(8) -0.014(7) -0.006(7) 0.005(7) C34 0.016(7) 0.018(6) 0.036(7) 0.001(6) -0.009(6) 0.013(5) C35 0.021(7) 0.026(7) 0.019(6) 0.004(5) 0.002(5) 0.001(5) C36 0.014(6) 0.009(6) 0.027(7) 0.003(5) -0.003(5) 0.002(5) C37 0.020(7) 0.026(7) 0.028(7) -0.006(6) -0.004(5) 0.007(5) C38 0.023(7) 0.040(8) 0.023(7) 0.000(6) -0.004(5) -0.003(6) C39 0.024(7) 0.029(7) 0.031(7) -0.006(6) 0.006(6) -0.003(6) C40 0.034(8) 0.020(7) 0.035(7) -0.001(6) 0.000(6) 0.007(6) C41 0.043(9) 0.048(9) 0.029(8) 0.008(7) -0.008(7) 0.012(7) C42 0.037(8) 0.049(9) 0.027(7) -0.004(6) -0.021(6) -0.003(7) C43 0.040(9) 0.028(8) 0.055(10) -0.005(7) -0.013(7) 0.018(6) C44 0.009(6) 0.036(8) 0.025(7) 0.005(6) -0.001(5) -0.010(5) C45 0.017(6) 0.025(7) 0.037(8) 0.000(6) -0.005(6) 0.003(5) C46 0.019(6) 0.027(7) 0.019(6) -0.012(5) 0.003(5) 0.000(5) C47 0.019(6) 0.020(7) 0.037(7) -0.006(6) 0.000(6) -0.001(5) C48 0.043(8) 0.023(7) 0.020(7) -0.002(5) -0.002(6) 0.002(6) C49 0.034(8) 0.036(8) 0.031(8) -0.006(6) -0.003(6) 0.007(6) C50 0.030(7) 0.018(6) 0.032(7) 0.006(6) -0.009(6) 0.001(5) C51 0.028(8) 0.059(10) 0.055(10) 0.006(8) 0.007(7) 0.006(7) C52 0.050(9) 0.034(8) 0.031(8) 0.002(6) -0.014(7) 0.000(7) C53 0.049(9) 0.021(7) 0.064(10) -0.012(7) -0.025(8) 0.003(6) C54 0.017(6) 0.013(6) 0.013(6) 0.001(5) -0.005(5) 0.004(5) C55 0.020(6) 0.025(7) 0.027(7) -0.017(5) -0.007(5) 0.002(5) C56 0.019(6) 0.025(7) 0.022(6) 0.005(5) 0.001(5) -0.003(5) C57 0.022(7) 0.031(7) 0.020(6) 0.000(6) -0.004(5) 0.002(5) C58 0.041(9) 0.085(12) 0.010(6) -0.026(7) 0.003(6) 0.007(8) C59 0.048(10) 0.049(10) 0.043(9) -0.007(8) -0.014(8) 0.001(8) C61 0.041(9) 0.047(9) 0.013(6) 0.007(6) -0.009(6) -0.005(7) C71 0.008(6) 0.081(11) 0.028(7) -0.032(8) 0.009(5) -0.021(6) C81 0.011(7) 0.074(11) 0.032(8) 0.002(7) 0.003(6) 0.006(7) _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 Er1 O44 2.250(7) . ? Er1 O54 2.251(7) . ? Er1 O36 2.257(7) . ? Er1 O34 2.276(7) . ? Er1 O46 2.294(7) . ? Er1 O56 2.306(7) . ? Er1 N11 2.526(9) . ? Er1 N21 2.579(8) . ? Re1 C71 1.852(14) . ? Re1 C61 1.898(14) . ? Re1 C81 1.902(13) . ? Re1 N23 2.161(9) . ? Re1 N13 2.166(9) . ? Re1 Cl1 2.456(3) . ? F371 C37 1.343(13) . ? F372 C37 1.358(12) . ? F381 C38 1.355(13) . ? F382 C38 1.342(13) . ? F391 C39 1.309(13) . ? F392 C39 1.338(13) . ? F393 C39 1.348(13) . ? F471 C47 1.346(12) . ? F472 C47 1.356(12) . ? F481 C48 1.342(12) . ? F482 C48 1.315(13) . ? F491 C49 1.329(14) . ? F492 C49 1.318(14) . ? F493 C49 1.342(14) . ? F571 C57 1.338(13) . ? F572 C57 1.335(13) . ? O34 C34 1.272(13) . ? O36 C36 1.282(12) . ? O44 C44 1.246(13) . ? O46 C46 1.313(12) . ? O54 C54 1.257(12) . ? O56 C56 1.256(13) . ? O61 C61 1.165(14) . ? O71 C71 1.181(15) . ? O81 C81 1.170(14) . ? N11 C12 1.318(13) . ? N11 C16 1.358(14) . ? N13 C12 1.341(13) . ? N13 C14 1.369(14) . ? N21 C22 1.349(13) . ? N21 C26 1.351(14) . ? N23 C22 1.325(13) . ? N23 C24 1.376(13) . ? C12 C22 1.490(14) . ? C14 C15 1.374(15) . ? C15 C16 1.362(15) . ? C24 C25 1.365(14) . ? C25 C26 1.382(15) . ? C30 C31 1.477(18) . ? C30 C32 1.511(18) . ? C30 C34 1.513(16) . ? C30 C33 1.538(17) . ? C34 C35 1.406(16) . ? C35 C36 1.344(15) . ? C36 C37 1.539(15) . ? C37 C38 1.540(16) . ? C38 C39 1.521(16) . ? C40 C42 1.509(16) . ? C40 C41 1.519(16) . ? C40 C43 1.524(15) . ? C40 C44 1.547(16) . ? C44 C45 1.419(16) . ? C45 C46 1.354(15) . ? C46 C47 1.501(16) . ? C47 C48 1.570(16) . ? C48 C49 1.525(17) . ? C50 C51 1.524(16) . ? C50 C52 1.537(16) . ? C50 C54 1.545(14) . ? C50 C53 1.545(16) . ? C54 C55 1.390(14) . ? C55 C56 1.395(15) . ? C56 C57 1.529(15) . ? C57 C58 1.521(17) . ? C58 F52' 1.233(19) . ? C58 F51 1.262(19) . ? C58 F52 1.50(2) . ? C58 C59 1.511(19) . ? C58 F51' 1.56(2) . ? C59 F55 1.27(2) . ? C59 F54 1.304(18) . ? C59 F54' 1.31(3) . ? C59 F55' 1.32(2) . ? C59 F53 1.33(2) . ? C59 F53' 1.36(2) . ? F54 F55 1.46(3) . ? F53' F54' 1.59(3) . ? 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 O44 Er1 O54 149.6(3) . . ? O44 Er1 O36 106.1(3) . . ? O54 Er1 O36 91.6(3) . . ? O44 Er1 O34 79.6(3) . . ? O54 Er1 O34 82.5(3) . . ? O36 Er1 O34 72.9(3) . . ? O44 Er1 O46 72.5(3) . . ? O54 Er1 O46 135.8(3) . . ? O36 Er1 O46 81.4(3) . . ? O34 Er1 O46 134.7(3) . . ? O44 Er1 O56 77.1(3) . . ? O54 Er1 O56 75.0(2) . . ? O36 Er1 O56 148.4(3) . . ? O34 Er1 O56 77.0(3) . . ? O46 Er1 O56 128.1(3) . . ? O44 Er1 N11 95.8(3) . . ? O54 Er1 N11 87.9(3) . . ? O36 Er1 N11 135.5(3) . . ? O34 Er1 N11 150.5(3) . . ? O46 Er1 N11 68.8(3) . . ? O56 Er1 N11 73.7(3) . . ? O44 Er1 N21 138.2(3) . . ? O54 Er1 N21 70.0(3) . . ? O36 Er1 N21 73.6(3) . . ? O34 Er1 N21 135.5(3) . . ? O46 Er1 N21 66.1(3) . . ? O56 Er1 N21 125.2(3) . . ? N11 Er1 N21 64.4(3) . . ? C71 Re1 C61 88.4(5) . . ? C71 Re1 C81 89.8(6) . . ? C61 Re1 C81 87.2(5) . . ? C71 Re1 N23 98.7(4) . . ? C61 Re1 N23 170.8(4) . . ? C81 Re1 N23 98.6(4) . . ? C71 Re1 N13 95.2(5) . . ? C61 Re1 N13 99.1(4) . . ? C81 Re1 N13 172.1(4) . . ? N23 Re1 N13 74.6(3) . . ? C71 Re1 Cl1 176.8(4) . . ? C61 Re1 Cl1 94.3(4) . . ? C81 Re1 Cl1 92.2(5) . . ? N23 Re1 Cl1 78.5(2) . . ? N13 Re1 Cl1 82.6(3) . . ? C34 O34 Er1 138.2(8) . . ? C36 O36 Er1 132.9(7) . . ? C44 O44 Er1 141.0(8) . . ? C46 O46 Er1 132.3(7) . . ? C54 O54 Er1 136.0(6) . . ? C56 O56 Er1 130.1(7) . . ? C12 N11 C16 115.5(10) . . ? C12 N11 Er1 121.2(7) . . ? C16 N11 Er1 122.4(7) . . ? C12 N13 C14 116.4(9) . . ? C12 N13 Re1 115.7(7) . . ? C14 N13 Re1 127.3(8) . . ? C22 N21 C26 115.8(9) . . ? C22 N21 Er1 118.5(7) . . ? C26 N21 Er1 125.2(7) . . ? C22 N23 C24 115.4(9) . . ? C22 N23 Re1 115.5(7) . . ? C24 N23 Re1 127.1(7) . . ? N11 C12 N13 127.5(10) . . ? N11 C12 C22 117.9(10) . . ? N13 C12 C22 114.6(9) . . ? N13 C14 C15 119.3(11) . . ? C16 C15 C14 119.9(11) . . ? N11 C16 C15 121.5(10) . . ? N23 C22 N21 127.0(10) . . ? N23 C22 C12 115.7(9) . . ? N21 C22 C12 117.2(10) . . ? C25 C24 N23 122.0(10) . . ? C24 C25 C26 117.9(10) . . ? N21 C26 C25 121.7(10) . . ? C31 C30 C32 109.8(12) . . ? C31 C30 C34 107.1(10) . . ? C32 C30 C34 107.6(10) . . ? C31 C30 C33 109.4(11) . . ? C32 C30 C33 109.4(11) . . ? C34 C30 C33 113.6(10) . . ? O34 C34 C35 122.4(11) . . ? O34 C34 C30 114.7(10) . . ? C35 C34 C30 123.0(11) . . ? C36 C35 C34 121.2(11) . . ? O36 C36 C35 129.3(11) . . ? O36 C36 C37 110.2(10) . . ? C35 C36 C37 120.5(10) . . ? F371 C37 F372 106.9(9) . . ? F371 C37 C36 112.5(9) . . ? F372 C37 C36 110.3(9) . . ? F371 C37 C38 108.4(9) . . ? F372 C37 C38 106.3(9) . . ? C36 C37 C38 112.2(9) . . ? F382 C38 F381 107.8(9) . . ? F382 C38 C39 107.0(10) . . ? F381 C38 C39 107.3(10) . . ? F382 C38 C37 109.7(10) . . ? F381 C38 C37 108.6(9) . . ? C39 C38 C37 116.2(10) . . ? F391 C39 F392 108.0(10) . . ? F391 C39 F393 109.0(10) . . ? F392 C39 F393 107.8(10) . . ? F391 C39 C38 112.3(10) . . ? F392 C39 C38 108.9(10) . . ? F393 C39 C38 110.8(10) . . ? C42 C40 C41 110.2(11) . . ? C42 C40 C43 110.7(11) . . ? C41 C40 C43 110.1(10) . . ? C42 C40 C44 107.8(9) . . ? C41 C40 C44 105.4(9) . . ? C43 C40 C44 112.5(11) . . ? O44 C44 C45 121.5(11) . . ? O44 C44 C40 116.0(11) . . ? C45 C44 C40 122.5(11) . . ? C46 C45 C44 122.6(11) . . ? O46 C46 C45 127.0(11) . . ? O46 C46 C47 111.7(10) . . ? C45 C46 C47 121.1(10) . . ? F471 C47 F472 106.0(9) . . ? F471 C47 C46 112.3(10) . . ? F472 C47 C46 110.6(9) . . ? F471 C47 C48 106.9(9) . . ? F472 C47 C48 106.6(9) . . ? C46 C47 C48 113.9(9) . . ? F482 C48 F481 108.6(10) . . ? F482 C48 C49 107.2(10) . . ? F481 C48 C49 106.7(9) . . ? F482 C48 C47 109.1(9) . . ? F481 C48 C47 108.9(10) . . ? C49 C48 C47 116.1(10) . . ? F492 C49 F491 107.4(11) . . ? F492 C49 F493 108.3(10) . . ? F491 C49 F493 106.9(10) . . ? F492 C49 C48 110.9(10) . . ? F491 C49 C48 112.4(10) . . ? F493 C49 C48 110.7(11) . . ? C51 C50 C52 110.2(11) . . ? C51 C50 C54 106.4(9) . . ? C52 C50 C54 108.9(10) . . ? C51 C50 C53 109.9(11) . . ? C52 C50 C53 109.9(10) . . ? C54 C50 C53 111.6(10) . . ? O54 C54 C55 124.3(9) . . ? O54 C54 C50 114.7(9) . . ? C55 C54 C50 121.0(10) . . ? C54 C55 C56 122.9(10) . . ? O56 C56 C55 127.5(11) . . ? O56 C56 C57 114.3(10) . . ? C55 C56 C57 118.2(10) . . ? F572 C57 F571 105.2(10) . . ? F572 C57 C58 106.3(10) . . ? F571 C57 C58 107.0(10) . . ? F572 C57 C56 112.5(9) . . ? F571 C57 C56 109.9(9) . . ? C58 C57 C56 115.4(10) . . ? F52' C58 F51 53.5(10) . . ? F52' C58 F52 43.2(10) . . ? F51 C58 F52 96.3(12) . . ? F52' C58 C59 118.2(15) . . ? F51 C58 C59 115.0(14) . . ? F52 C58 C59 97.6(12) . . ? F52' C58 C57 114.0(13) . . ? F51 C58 C57 120.1(14) . . ? F52 C58 C57 99.8(11) . . ? C59 C58 C57 119.3(11) . . ? F52' C58 F51' 101.3(13) . . ? F51 C58 F51' 48.2(10) . . ? F52 C58 F51' 144.4(12) . . ? C59 C58 F51' 100.4(11) . . ? C57 C58 F51' 97.8(11) . . ? F55 C59 F54 69.2(15) . . ? F55 C59 F54' 112(2) . . ? F54 C59 F54' 44.6(13) . . ? F55 C59 F55' 41.9(11) . . ? F54 C59 F55' 111.0(15) . . ? F54' C59 F55' 151(2) . . ? F55 C59 F53 105.1(17) . . ? F54 C59 F53 125.2(15) . . ? F54' C59 F53 102.2(18) . . ? F55' C59 F53 79.1(14) . . ? F55 C59 F53' 128.8(18) . . ? F54 C59 F53' 109.3(14) . . ? F54' C59 F53' 73.5(17) . . ? F55' C59 F53' 110.7(15) . . ? F53 C59 F53' 31.7(9) . . ? F55 C59 C58 117.9(16) . . ? F54 C59 C58 115.4(13) . . ? F54' C59 C58 103.9(17) . . ? F55' C59 C58 101.6(13) . . ? F53 C59 C58 114.5(14) . . ? F53' C59 C58 108.6(13) . . ? O61 C61 Re1 178.1(13) . . ? O71 C71 Re1 177.0(10) . . ? O81 C81 Re1 175.7(12) . . ? C59 F54 F55 54.2(11) . . ? C59 F55 F54 56.6(13) . . ? C59 F53' F54' 51.8(13) . . ? C59 F54' F53' 54.7(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.274 _refine_diff_density_min -1.713 _refine_diff_density_rms 0.199 #=END data_mares _database_code_CSD 191576 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H22 Cl F9 N4 Nd O9 Re S3' _chemical_formula_weight 1347.70 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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.800(3) _cell_length_b 38.712(8) _cell_length_c 13.527(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.45(2) _cell_angle_gamma 90.00 _cell_volume 4532(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2596 _exptl_absorpt_coefficient_mu 4.095 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23681 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7988 _reflns_number_gt 5067 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7988 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd -0.32636(6) 0.167842(12) -0.23897(3) 0.02478(14) Uani 1 1 d . . . Re1 Re -0.15971(5) 0.041080(9) 0.18282(3) 0.02538(11) Uani 1 1 d . . . Cl1 Cl -0.3596(3) 0.07238(6) 0.25286(17) 0.0404(6) Uani 1 1 d . . . S46 S -0.7840(4) 0.08924(7) -0.3533(2) 0.0568(8) Uani 1 1 d . . . S56 S -0.3212(4) 0.03509(7) -0.2918(2) 0.0625(10) Uani 1 1 d . . . F421 F -0.8388(8) 0.26128(14) -0.3631(5) 0.078(2) Uani 1 1 d . . . F422 F -0.6447(8) 0.26437(14) -0.4400(5) 0.0636(19) Uani 1 1 d . . . F423 F -0.6186(7) 0.27949(14) -0.2847(5) 0.066(2) Uani 1 1 d . . . F521 F -0.5266(9) 0.19363(15) -0.5871(4) 0.073(2) Uani 1 1 d . . . F522 F -0.2952(8) 0.18675(17) -0.6074(4) 0.074(2) Uani 1 1 d . . . F523 F -0.4671(7) 0.14971(13) -0.6667(4) 0.0457(15) Uani 1 1 d . . . F621 F -0.0090(10) 0.26853(16) -0.0642(6) 0.087(3) Uani 1 1 d . . . F622 F 0.1935(8) 0.26079(15) -0.1319(5) 0.075(2) Uani 1 1 d . . . F623 F -0.0195(8) 0.27822(15) -0.2207(6) 0.085(2) Uani 1 1 d . . . O41 O -0.4958(8) 0.21642(15) -0.2730(4) 0.0349(16) Uani 1 1 d . . . O44 O -0.5856(8) 0.14706(15) -0.2767(5) 0.0366(16) Uani 1 1 d . . . O51 O -0.3399(8) 0.17196(14) -0.4132(4) 0.0341(16) Uani 1 1 d . . . O54 O -0.3182(8) 0.11006(14) -0.3091(4) 0.0345(16) Uani 1 1 d . . . O61 O -0.1441(8) 0.21546(15) -0.2235(5) 0.0366(17) Uani 1 1 d . . . O64 O -0.0755(7) 0.14593(14) -0.1674(4) 0.0302(15) Uani 1 1 d . . . O71 O -0.0682(8) 0.00457(17) 0.3863(5) 0.0485(19) Uani 1 1 d . . . O81 O -0.3776(9) -0.01955(18) 0.1106(6) 0.063(2) Uani 1 1 d . . . O91 O 0.1035(9) 0.00615(18) 0.1017(5) 0.054(2) Uani 1 1 d . . . N11 N -0.2970(9) 0.19202(17) -0.0554(5) 0.0265(18) Uani 1 1 d . . . N21 N -0.3558(8) 0.12451(17) -0.0852(5) 0.0240(17) Uani 1 1 d . . . N24 N -0.2326(8) 0.07540(16) 0.0552(5) 0.0234(17) Uani 1 1 d . . . N31 N -0.0275(9) 0.08839(17) 0.2185(5) 0.0247(17) Uani 1 1 d . . . C12 C -0.2799(10) 0.1716(2) 0.0277(6) 0.022(2) Uani 1 1 d . . . C13 C -0.2866(11) 0.1833(2) 0.1220(7) 0.030(2) Uani 1 1 d . . . H13A H -0.2810 0.1678 0.1769 0.036 Uiso 1 1 calc R . . C14 C -0.3020(11) 0.2189(2) 0.1355(7) 0.035(2) Uani 1 1 d . . . H14A H -0.3062 0.2282 0.2000 0.041 Uiso 1 1 calc R . . C15 C -0.3107(13) 0.2402(2) 0.0537(7) 0.045(3) Uani 1 1 d . . . H15A H -0.3154 0.2646 0.0614 0.055 Uiso 1 1 calc R . . C16 C -0.3127(12) 0.2261(2) -0.0384(7) 0.043(3) Uani 1 1 d . . . H16A H -0.3259 0.2413 -0.0946 0.052 Uiso 1 1 calc R . . C22 C -0.3826(10) 0.0908(2) -0.1019(6) 0.024(2) Uani 1 1 d . . . H22A H -0.4402 0.0836 -0.1648 0.029 Uiso 1 1 calc R . . C23 C -0.3282(10) 0.0662(2) -0.0293(6) 0.025(2) Uani 1 1 d . . . H23A H -0.3588 0.0427 -0.0397 0.030 Uiso 1 1 calc R . . C25 C -0.1951(10) 0.10950(19) 0.0722(5) 0.019(2) Uani 1 1 d . . . C26 C -0.2731(10) 0.1336(2) 0.0050(6) 0.020(2) Uani 1 1 d . . . C32 C -0.0633(10) 0.1151(2) 0.1571(6) 0.019(2) Uani 1 1 d . . . C33 C 0.0251(10) 0.1449(2) 0.1672(6) 0.028(2) Uani 1 1 d . . . H33A H 0.0008 0.1634 0.1210 0.033 Uiso 1 1 calc R . . C34 C 0.1504(11) 0.1473(2) 0.2464(7) 0.034(2) Uani 1 1 d . . . H34A H 0.2124 0.1675 0.2547 0.041 Uiso 1 1 calc R . . C35 C 0.1834(11) 0.1204(3) 0.3120(8) 0.045(3) Uani 1 1 d . . . H35A H 0.2655 0.1218 0.3681 0.054 Uiso 1 1 calc R . . C36 C 0.0926(11) 0.0907(2) 0.2938(7) 0.031(2) Uani 1 1 d . . . H36A H 0.1176 0.0714 0.3369 0.037 Uiso 1 1 calc R . . C41 C -0.6330(12) 0.2189(2) -0.3205(7) 0.034(2) Uani 1 1 d . . . C42 C -0.6831(13) 0.2566(3) -0.3509(8) 0.049(3) Uani 1 1 d . . . C43 C -0.7379(12) 0.1935(2) -0.3532(7) 0.038(3) Uani 1 1 d . . . H43A H -0.8351 0.2000 -0.3914 0.045 Uiso 1 1 calc R . . C44 C -0.7091(13) 0.1577(3) -0.3329(7) 0.039(3) Uani 1 1 d . . . C45 C -0.8186(12) 0.1322(2) -0.3799(7) 0.038(3) Uani 1 1 d . . . C47 C -0.9424(13) 0.0769(3) -0.4402(8) 0.050(3) Uani 1 1 d . . . H47 H -0.9737 0.0536 -0.4539 0.060 Uiso 1 1 calc R . . C48 C -1.0163(12) 0.1046(3) -0.4864(8) 0.046(3) Uani 1 1 d . . . H48A H -1.1065 0.1027 -0.5367 0.056 Uiso 1 1 calc R . . C49 C -0.9496(12) 0.1362(3) -0.4543(7) 0.042(3) Uani 1 1 d . . . H49A H -0.9887 0.1580 -0.4801 0.050 Uiso 1 1 calc R . . C51 C -0.3794(11) 0.1517(2) -0.4873(6) 0.028(2) Uani 1 1 d . . . C52 C -0.4162(12) 0.1694(3) -0.5878(7) 0.037(2) Uani 1 1 d . . . C53 C -0.3907(10) 0.1158(2) -0.4856(6) 0.023(2) Uani 1 1 d . . . H53A H -0.4277 0.1036 -0.5462 0.028 Uiso 1 1 calc R . . C54 C -0.3479(11) 0.0972(2) -0.3948(7) 0.029(2) Uani 1 1 d . . . C55 C -0.3375(11) 0.0591(2) -0.4010(6) 0.030(2) Uani 1 1 d . . . C57 C -0.3143(12) -0.0025(2) -0.3554(7) 0.042(3) Uani 1 1 d . . . H57 H -0.3077 -0.0246 -0.3245 0.050 Uiso 1 1 calc R . . C58 C -0.3192(11) 0.0024(2) -0.4532(7) 0.034(2) Uani 1 1 d . . . H58A H -0.3136 -0.0156 -0.4999 0.040 Uiso 1 1 calc R . . C59 C -0.3337(11) 0.0375(2) -0.4789(7) 0.036(2) Uani 1 1 d . . . H59A H -0.3403 0.0454 -0.5460 0.043 Uiso 1 1 calc R . . C61 C -0.0131(13) 0.2191(3) -0.1690(8) 0.041(3) Uani 1 1 d . . . C62 C 0.0365(15) 0.2573(3) -0.1481(11) 0.063(4) Uani 1 1 d . . . C63 C 0.0862(11) 0.1941(3) -0.1201(7) 0.039(3) Uani 1 1 d . . . H63A H 0.1844 0.2014 -0.0850 0.047 Uiso 1 1 calc R . . C64 C 0.0512(12) 0.1587(2) -0.1192(7) 0.032(2) Uani 1 1 d . C . C65 C 0.1578(11) 0.1352(2) -0.0598(7) 0.033(2) Uani 1 1 d . . . C67 C 0.2760(13) 0.0842(3) 0.0332(8) 0.049(3) Uani 1 1 d . . . H67 H 0.3028 0.0619 0.0601 0.059 Uiso 1 1 calc R A 1 C68 C 0.3575(13) 0.1126(3) 0.0618(9) 0.056(3) Uani 1 1 d . C . H68A H 0.4476 0.1122 0.1125 0.068 Uiso 1 1 calc R B 1 C71 C -0.1013(11) 0.0182(2) 0.3096(7) 0.029(2) Uani 1 1 d . . . C81 C -0.2950(12) 0.0033(2) 0.1398(7) 0.037(2) Uani 1 1 d . . . C91 C 0.0065(12) 0.0195(2) 0.1304(7) 0.031(2) Uani 1 1 d . . . C69 C 0.3013(9) 0.1438(2) 0.0118(6) 0.050(3) Uani 0.845(10) 1 d P C 1 H69 H 0.3475 0.1660 0.0224 0.061 Uiso 0.845(10) 1 calc PR C 1 S66 S 0.1187(4) 0.09240(7) -0.0567(2) 0.0441(11) Uani 0.845(10) 1 d P C 1 S66' S 0.3013(9) 0.1438(2) 0.0118(6) 0.050(3) Uani 0.155(10) 1 d P C 2 C69' C 0.1187(4) 0.09240(7) -0.0567(2) 0.0441(11) Uani 0.155(10) 1 d P C 2 H69' H 0.0387 0.0783 -0.0922 0.053 Uiso 0.155(10) 1 calc PR C 2 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 Nd1 0.0342(3) 0.0214(3) 0.0162(3) 0.0015(2) -0.0021(2) 0.0009(2) Re1 0.0332(2) 0.01916(19) 0.0214(2) 0.00319(17) -0.00158(15) 0.00070(19) Cl1 0.0453(17) 0.0466(15) 0.0292(14) 0.0084(12) 0.0069(12) 0.0139(13) S46 0.058(2) 0.0376(17) 0.070(2) 0.0108(15) -0.0026(17) -0.0046(15) S56 0.127(3) 0.0294(16) 0.0323(15) 0.0078(12) 0.0172(17) 0.0258(17) F421 0.047(5) 0.042(4) 0.129(6) -0.015(4) -0.024(4) 0.026(3) F422 0.080(5) 0.042(4) 0.058(4) 0.011(3) -0.017(4) 0.014(3) F423 0.068(5) 0.032(3) 0.088(5) -0.031(3) -0.016(4) 0.011(3) F521 0.115(6) 0.061(4) 0.038(4) 0.008(3) -0.001(4) 0.050(4) F522 0.093(6) 0.091(5) 0.035(4) 0.019(3) 0.001(4) -0.058(4) F523 0.073(5) 0.041(3) 0.017(3) 0.003(3) -0.007(3) -0.003(3) F621 0.114(7) 0.045(4) 0.100(6) -0.019(4) 0.011(5) -0.023(4) F622 0.053(5) 0.056(4) 0.105(6) 0.030(4) -0.018(4) -0.020(3) F623 0.072(5) 0.038(4) 0.124(6) 0.040(4) -0.033(4) -0.015(4) O41 0.035(4) 0.034(4) 0.032(4) 0.001(3) -0.003(3) 0.006(3) O44 0.034(4) 0.034(4) 0.037(4) 0.009(3) -0.008(3) -0.005(3) O51 0.050(5) 0.024(3) 0.027(4) -0.002(3) 0.004(3) -0.002(3) O54 0.058(5) 0.023(3) 0.019(3) 0.004(3) -0.001(3) 0.010(3) O61 0.035(5) 0.033(4) 0.038(4) 0.013(3) -0.003(3) -0.005(3) O64 0.032(4) 0.025(3) 0.030(4) 0.003(3) -0.004(3) 0.006(3) O71 0.053(5) 0.054(5) 0.036(4) 0.022(4) 0.004(4) 0.014(4) O81 0.066(6) 0.035(4) 0.078(6) -0.004(4) -0.012(5) -0.013(4) O91 0.055(6) 0.061(5) 0.043(5) 0.008(4) 0.002(4) 0.026(4) N11 0.037(5) 0.016(4) 0.024(4) 0.005(3) 0.000(4) -0.005(3) N21 0.028(5) 0.033(5) 0.009(4) -0.003(3) 0.000(3) 0.001(4) N24 0.025(5) 0.018(4) 0.026(4) -0.003(3) 0.001(3) -0.001(3) N31 0.033(5) 0.020(4) 0.020(4) 0.007(3) 0.003(3) 0.002(3) C12 0.027(5) 0.023(5) 0.010(4) -0.001(4) -0.010(4) 0.000(4) C13 0.040(6) 0.018(5) 0.028(6) 0.002(4) -0.003(5) 0.002(4) C14 0.050(7) 0.029(5) 0.024(5) -0.003(4) 0.005(5) 0.010(5) C15 0.075(9) 0.020(5) 0.039(6) -0.017(5) 0.003(6) -0.001(5) C16 0.066(8) 0.022(5) 0.039(6) 0.003(5) 0.001(6) -0.007(5) C22 0.032(6) 0.022(5) 0.017(5) -0.009(4) -0.001(4) -0.004(4) C23 0.034(6) 0.020(5) 0.020(5) -0.002(4) 0.000(4) 0.002(4) C25 0.031(6) 0.016(5) 0.006(4) 0.002(3) -0.004(4) 0.001(4) C26 0.024(5) 0.018(5) 0.017(5) -0.005(4) 0.001(4) -0.003(4) C32 0.025(5) 0.019(5) 0.015(4) -0.005(4) 0.006(4) 0.002(4) C33 0.031(6) 0.032(5) 0.020(5) 0.003(4) 0.002(4) -0.004(5) C34 0.030(6) 0.024(5) 0.047(6) 0.004(5) 0.003(5) -0.007(4) C35 0.023(6) 0.051(7) 0.055(7) -0.005(6) -0.010(5) -0.008(5) C36 0.033(6) 0.030(6) 0.028(5) 0.008(4) -0.001(4) 0.007(5) C41 0.034(7) 0.032(6) 0.033(6) -0.002(5) -0.004(5) 0.003(5) C42 0.052(8) 0.037(7) 0.050(7) -0.011(6) -0.012(6) 0.017(6) C43 0.036(7) 0.032(6) 0.039(6) 0.004(5) -0.010(5) 0.008(5) C44 0.057(8) 0.038(6) 0.023(6) 0.001(5) 0.004(5) 0.004(5) C45 0.042(7) 0.033(6) 0.041(6) -0.008(5) 0.016(5) -0.006(5) C47 0.049(8) 0.040(7) 0.063(8) -0.016(6) 0.014(6) -0.025(6) C48 0.036(7) 0.042(7) 0.058(7) -0.007(6) 0.000(6) 0.006(5) C49 0.028(6) 0.050(7) 0.046(7) -0.004(5) 0.001(5) -0.001(5) C51 0.032(6) 0.035(6) 0.017(5) 0.004(4) 0.003(4) 0.004(5) C52 0.049(7) 0.038(6) 0.018(5) 0.001(5) -0.006(5) -0.001(6) C53 0.038(6) 0.019(5) 0.010(4) 0.005(4) -0.001(4) -0.012(4) C54 0.035(6) 0.026(5) 0.024(5) -0.005(4) -0.001(4) -0.004(4) C55 0.045(7) 0.018(5) 0.024(5) 0.003(4) -0.005(5) -0.004(4) C57 0.059(8) 0.019(5) 0.044(7) 0.003(5) 0.002(6) 0.010(5) C58 0.035(6) 0.027(6) 0.036(6) -0.011(5) -0.002(5) 0.002(5) C59 0.042(6) 0.039(6) 0.027(5) -0.011(5) 0.009(5) -0.002(5) C61 0.041(7) 0.046(7) 0.037(6) 0.012(5) 0.009(5) -0.004(6) C62 0.049(9) 0.046(8) 0.086(10) 0.038(8) -0.010(7) -0.019(6) C63 0.024(6) 0.058(7) 0.031(6) 0.012(5) -0.006(5) 0.000(5) C64 0.033(6) 0.037(6) 0.027(5) 0.007(5) 0.005(5) 0.012(5) C65 0.029(6) 0.038(6) 0.034(6) 0.012(5) 0.013(5) 0.005(5) C67 0.051(8) 0.046(7) 0.055(7) 0.020(6) 0.021(6) 0.025(6) C68 0.021(7) 0.089(10) 0.060(8) 0.019(7) 0.010(6) 0.020(7) C71 0.041(7) 0.017(5) 0.028(6) 0.003(4) 0.001(5) 0.007(4) C81 0.036(7) 0.033(6) 0.040(6) -0.001(5) 0.005(5) -0.001(5) C91 0.030(6) 0.038(6) 0.022(5) 0.000(4) -0.008(4) 0.008(5) C69 0.032(5) 0.066(6) 0.053(5) 0.019(4) 0.008(4) 0.010(4) S66 0.046(2) 0.038(2) 0.048(2) 0.0074(15) 0.0088(16) 0.0111(15) S66' 0.032(5) 0.066(6) 0.053(5) 0.019(4) 0.008(4) 0.010(4) C69' 0.046(2) 0.038(2) 0.048(2) 0.0074(15) 0.0088(16) 0.0111(15) _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 Nd1 O51 2.343(6) . ? Nd1 O44 2.386(6) . ? Nd1 O41 2.392(6) . ? Nd1 O64 2.399(6) . ? Nd1 O61 2.427(6) . ? Nd1 O54 2.436(6) . ? Nd1 N11 2.622(7) . ? Nd1 N21 2.721(6) . ? Re1 C81 1.908(10) . ? Re1 C71 1.916(9) . ? Re1 C91 1.928(10) . ? Re1 N31 2.177(7) . ? Re1 N24 2.181(7) . ? Re1 Cl1 2.462(2) . ? S46 C45 1.719(10) . ? S46 C47 1.721(11) . ? S56 C57 1.696(9) . ? S56 C55 1.729(8) . ? F421 C42 1.362(12) . ? F422 C42 1.343(12) . ? F423 C42 1.312(11) . ? F521 C52 1.353(11) . ? F522 C52 1.326(11) . ? F523 C52 1.321(10) . ? F621 C62 1.342(14) . ? F622 C62 1.366(13) . ? F623 C62 1.299(12) . ? O41 C41 1.264(11) . ? O44 C44 1.277(11) . ? O51 C51 1.272(10) . ? O54 C54 1.245(9) . ? O61 C61 1.259(11) . ? O64 C64 1.283(11) . ? O71 C71 1.153(9) . ? O81 C81 1.168(10) . ? O91 C91 1.125(10) . ? N11 C16 1.352(10) . ? N11 C12 1.360(9) . ? N21 C22 1.336(9) . ? N21 C26 1.349(10) . ? N24 C23 1.339(10) . ? N24 C25 1.370(9) . ? N31 C32 1.328(10) . ? N31 C36 1.331(11) . ? C12 C13 1.366(11) . ? C12 C26 1.503(11) . ? C13 C14 1.402(11) . ? C14 C15 1.369(12) . ? C15 C16 1.357(12) . ? C22 C23 1.392(11) . ? C25 C26 1.395(11) . ? C25 C32 1.492(11) . ? C32 C33 1.385(11) . ? C33 C34 1.394(12) . ? C34 C35 1.364(12) . ? C35 C36 1.395(12) . ? C41 C43 1.365(13) . ? C41 C42 1.560(13) . ? C43 C44 1.426(12) . ? C44 C45 1.443(13) . ? C45 C49 1.395(13) . ? C47 C48 1.349(13) . ? C48 C49 1.392(13) . ? C51 C53 1.394(11) . ? C51 C52 1.505(12) . ? C53 C54 1.415(11) . ? C54 C55 1.478(11) . ? C55 C59 1.352(11) . ? C57 C58 1.329(12) . ? C58 C59 1.400(12) . ? C61 C63 1.390(13) . ? C61 C62 1.552(15) . ? C63 C64 1.405(13) . ? C64 C65 1.443(12) . ? C65 C69 1.483(12) . ? C65 S66 1.694(9) . ? C67 C68 1.333(14) . ? C67 S66 1.699(11) . ? C68 C69 1.425(12) . ? 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 O51 Nd1 O44 86.3(2) . . ? O51 Nd1 O41 80.6(2) . . ? O44 Nd1 O41 71.7(2) . . ? O51 Nd1 O64 107.8(2) . . ? O44 Nd1 O64 137.9(2) . . ? O41 Nd1 O64 148.4(2) . . ? O51 Nd1 O61 87.0(2) . . ? O44 Nd1 O61 150.0(2) . . ? O41 Nd1 O61 78.4(2) . . ? O64 Nd1 O61 71.9(2) . . ? O51 Nd1 O54 70.76(19) . . ? O44 Nd1 O54 72.6(2) . . ? O41 Nd1 O54 135.1(2) . . ? O64 Nd1 O54 75.1(2) . . ? O61 Nd1 O54 131.7(2) . . ? O51 Nd1 N11 155.0(2) . . ? O44 Nd1 N11 104.4(2) . . ? O41 Nd1 N11 81.5(2) . . ? O64 Nd1 N11 79.5(2) . . ? O61 Nd1 N11 72.4(2) . . ? O54 Nd1 N11 133.78(19) . . ? O51 Nd1 N21 144.72(19) . . ? O44 Nd1 N21 74.7(2) . . ? O41 Nd1 N21 119.3(2) . . ? O64 Nd1 N21 71.4(2) . . ? O61 Nd1 N21 123.7(2) . . ? O54 Nd1 N21 75.26(19) . . ? N11 Nd1 N21 60.2(2) . . ? C81 Re1 C71 88.3(4) . . ? C81 Re1 C91 91.6(4) . . ? C71 Re1 C91 91.8(4) . . ? C81 Re1 N31 172.3(3) . . ? C71 Re1 N31 98.3(3) . . ? C91 Re1 N31 92.0(3) . . ? C81 Re1 N24 98.5(3) . . ? C71 Re1 N24 169.4(3) . . ? C91 Re1 N24 96.1(3) . . ? N31 Re1 N24 74.4(2) . . ? C81 Re1 Cl1 92.6(3) . . ? C71 Re1 Cl1 88.7(3) . . ? C91 Re1 Cl1 175.8(3) . . ? N31 Re1 Cl1 83.7(2) . . ? N24 Re1 Cl1 82.92(18) . . ? C45 S46 C47 92.0(5) . . ? C57 S56 C55 91.9(5) . . ? C41 O41 Nd1 131.4(6) . . ? C44 O44 Nd1 134.1(6) . . ? C51 O51 Nd1 135.0(5) . . ? C54 O54 Nd1 135.7(5) . . ? C61 O61 Nd1 131.0(6) . . ? C64 O64 Nd1 136.0(6) . . ? C16 N11 C12 115.3(7) . . ? C16 N11 Nd1 120.9(6) . . ? C12 N11 Nd1 123.5(5) . . ? C22 N21 C26 117.3(7) . . ? C22 N21 Nd1 120.7(5) . . ? C26 N21 Nd1 114.8(5) . . ? C23 N24 C25 119.7(7) . . ? C23 N24 Re1 124.2(5) . . ? C25 N24 Re1 115.2(5) . . ? C32 N31 C36 119.4(7) . . ? C32 N31 Re1 117.4(6) . . ? C36 N31 Re1 123.1(6) . . ? N11 C12 C13 124.2(8) . . ? N11 C12 C26 113.7(7) . . ? C13 C12 C26 121.7(7) . . ? C12 C13 C14 118.0(8) . . ? C15 C14 C13 118.7(8) . . ? C16 C15 C14 119.4(9) . . ? N11 C16 C15 124.3(9) . . ? N21 C22 C23 121.5(8) . . ? N24 C23 C22 120.1(8) . . ? N24 C25 C26 117.4(7) . . ? N24 C25 C32 113.5(7) . . ? C26 C25 C32 128.8(7) . . ? N21 C26 C25 122.3(7) . . ? N21 C26 C12 113.9(7) . . ? C25 C26 C12 123.7(7) . . ? N31 C32 C33 121.4(8) . . ? N31 C32 C25 115.6(7) . . ? C33 C32 C25 122.8(7) . . ? C32 C33 C34 118.9(8) . . ? C35 C34 C33 119.6(9) . . ? C34 C35 C36 117.8(9) . . ? N31 C36 C35 122.8(8) . . ? O41 C41 C43 129.6(9) . . ? O41 C41 C42 113.7(8) . . ? C43 C41 C42 116.5(9) . . ? F423 C42 F422 108.3(10) . . ? F423 C42 F421 107.1(8) . . ? F422 C42 F421 105.8(9) . . ? F423 C42 C41 112.7(8) . . ? F422 C42 C41 109.9(8) . . ? F421 C42 C41 112.7(9) . . ? C41 C43 C44 123.4(9) . . ? O44 C44 C43 122.1(9) . . ? O44 C44 C45 118.0(9) . . ? C43 C44 C45 119.9(9) . . ? C49 C45 C44 129.8(9) . . ? C49 C45 S46 110.5(7) . . ? C44 C45 S46 119.4(8) . . ? C48 C47 S46 110.9(8) . . ? C47 C48 C49 114.6(10) . . ? C48 C49 C45 111.9(10) . . ? O51 C51 C53 127.8(8) . . ? O51 C51 C52 114.4(8) . . ? C53 C51 C52 117.7(8) . . ? F523 C52 F522 107.3(8) . . ? F523 C52 F521 105.5(8) . . ? F522 C52 F521 104.7(8) . . ? F523 C52 C51 116.9(8) . . ? F522 C52 C51 111.3(8) . . ? F521 C52 C51 110.3(8) . . ? C51 C53 C54 120.9(8) . . ? O54 C54 C53 125.5(8) . . ? O54 C54 C55 116.6(8) . . ? C53 C54 C55 117.8(7) . . ? C59 C55 C54 132.3(8) . . ? C59 C55 S56 108.8(7) . . ? C54 C55 S56 118.9(6) . . ? C58 C57 S56 112.6(7) . . ? C57 C58 C59 111.8(8) . . ? C55 C59 C58 114.9(8) . . ? O61 C61 C63 129.1(10) . . ? O61 C61 C62 114.3(9) . . ? C63 C61 C62 116.5(10) . . ? F623 C62 F621 107.9(11) . . ? F623 C62 F622 107.1(9) . . ? F621 C62 F622 106.3(11) . . ? F623 C62 C61 113.6(10) . . ? F621 C62 C61 110.2(9) . . ? F622 C62 C61 111.4(10) . . ? C61 C63 C64 124.4(10) . . ? O64 C64 C63 122.9(8) . . ? O64 C64 C65 117.2(9) . . ? C63 C64 C65 119.8(9) . . ? C64 C65 C69 127.9(9) . . ? C64 C65 S66 121.0(8) . . ? C69 C65 S66 110.8(6) . . ? C68 C67 S66 112.2(8) . . ? C67 C68 C69 116.1(10) . . ? O71 C71 Re1 179.0(9) . . ? O81 C81 Re1 178.1(9) . . ? O91 C91 Re1 178.0(9) . . ? C68 C69 C65 107.5(8) . . ? C65 S66 C67 93.3(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.818 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.173 #=END