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 'Jitendra K. Bera' _publ_contact_author_address ; Department of Chemistry IIT Kanpur 208016 INDIA ; _publ_contact_author_phone ' +91 512 259 7336' _publ_contact_author_fax ' +91 512 259 7436' _publ_contact_author_email jbera@iitk.ac.in _publ_section_title ; Syntheses and Reactivity Studies of Solvated Dirhenium Acetonitrile Complexes ; loop_ _publ_author_name 'Jitendra Bera' 'John Bacsa' 'Kim R. Dunbar' 'Sanjib K. Patra' 'Eric J. Schelter' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 604231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 N10 Re2 4(C32 H12 F24 B) 4(C2 H2 Cl2) (C2 H3 N)' _chemical_formula_sum 'C154 H89 B4 Cl8 F96 N11 Re2' _chemical_formula_weight 4616.60 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' N N 0.0061 0.0033 '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' Re Re -1.0185 7.2310 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 18.2103(9) _cell_length_b 18.9154(9) _cell_length_c 51.481(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.4150(10) _cell_angle_gamma 90.00 _cell_volume 17621.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.154 _cell_measurement_theta_max 21.704 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.135 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9040 _exptl_absorpt_coefficient_mu 1.649 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6463 _exptl_absorpt_correction_T_max 0.7783 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 152223 _diffrn_reflns_av_R_equivalents 0.1184 _diffrn_reflns_av_sigmaI/netI 0.1450 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -63 _diffrn_reflns_limit_l_max 67 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.34 _reflns_number_total 42904 _reflns_number_gt 22507 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0922P)^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 42904 _refine_ls_number_parameters 2482 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.1547 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1975 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.004 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 C8D C -0.0250(6) 0.5072(10) 0.1956(4) 0.048(4) Uani 0.42 1 d PD A -1 F1D F -0.0581(7) 0.5648(7) 0.1855(3) 0.0584(14) Uani 0.42 1 d PD A -1 F2D F -0.0698(6) 0.4917(7) 0.2146(2) 0.0584(14) Uani 0.42 1 d PD A -1 F3D F -0.0291(10) 0.4500(8) 0.1812(3) 0.0584(14) Uani 0.42 1 d PD A -1 C8E C -0.0158(5) 0.5068(8) 0.1884(3) 0.048(4) Uani 0.58 1 d PD A -2 F1E F -0.0365(7) 0.4370(6) 0.1889(2) 0.0584(14) Uani 0.58 1 d PD A -2 F2E F -0.0182(4) 0.5228(5) 0.16330(18) 0.0584(14) Uani 0.58 1 d PD A -2 F3E F -0.0756(5) 0.5405(5) 0.19672(19) 0.0584(14) Uani 0.58 1 d PD A -2 C15C C 0.0958(10) 0.4102(13) 0.4985(4) 0.052(3) Uani 0.50 1 d PD B -3 F7C F 0.0654(7) 0.4640(8) 0.4836(3) 0.0717(16) Uani 0.50 1 d PD B -3 F8C F 0.0606(7) 0.4107(6) 0.5202(2) 0.0717(16) Uani 0.50 1 d PD B -3 F9C F 0.1642(6) 0.4314(6) 0.5058(3) 0.0717(16) Uani 0.50 1 d PD B -3 C15E C 0.0889(10) 0.4087(13) 0.4995(4) 0.052(3) Uani 0.50 1 d PD B -4 F7E F 0.0962(7) 0.4617(8) 0.4827(3) 0.0717(16) Uani 0.50 1 d PD B -4 F8E F 0.0252(6) 0.4228(6) 0.5101(3) 0.0717(16) Uani 0.50 1 d PD B -4 F9E F 0.1412(7) 0.4175(6) 0.5193(2) 0.0717(16) Uani 0.50 1 d PD B -4 C22D C 0.3724(11) 0.6350(7) 0.1681(3) 0.046(2) Uani 0.49 1 d PD C -5 F13D F 0.3627(7) 0.6055(6) 0.1440(2) 0.0676(17) Uani 0.49 1 d PD C -5 F14D F 0.4301(7) 0.6770(7) 0.1683(3) 0.0676(17) Uani 0.49 1 d PD C -5 F15D F 0.3145(6) 0.6744(6) 0.1707(3) 0.0676(17) Uani 0.49 1 d PD C -5 C31A C -0.4853(7) 0.3617(9) 0.3110(3) 0.042(3) Uani 0.50 1 d PD D -7 F19A F -0.5202(7) 0.2998(6) 0.3137(3) 0.0556(14) Uani 0.50 1 d PD D -7 F20A F -0.5355(5) 0.4076(5) 0.3008(2) 0.0556(14) Uani 0.50 1 d PD D -7 F21A F -0.4640(5) 0.3857(6) 0.3356(2) 0.0556(14) Uani 0.50 1 d PD D -7 C31E C -0.4755(8) 0.3600(9) 0.3151(3) 0.042(3) Uani 0.50 1 d PD D -8 F19E F -0.5322(7) 0.3147(6) 0.3112(3) 0.0556(14) Uani 0.50 1 d PD D -8 F20E F -0.5021(5) 0.4252(5) 0.3174(2) 0.0556(14) Uani 0.50 1 d PD D -8 F21E F -0.4479(5) 0.3452(6) 0.3404(2) 0.0556(14) Uani 0.50 1 d PD D -8 C31B C 0.6862(13) 0.8816(18) 0.5803(5) 0.048(2) Uani 0.50 1 d PD E -9 F19B F 0.6286(7) 0.9029(6) 0.5925(2) 0.0725(18) Uani 0.50 1 d PD E -9 F20B F 0.6955(8) 0.9333(9) 0.5632(3) 0.0725(18) Uani 0.50 1 d PD E -9 F21B F 0.7441(7) 0.8834(6) 0.5989(2) 0.0725(18) Uani 0.50 1 d PD E -9 C31F C 0.6876(16) 0.883(2) 0.5794(6) 0.048(2) Uani 0.50 1 d P E -10 F19F F 0.6205(8) 0.9257(6) 0.5809(3) 0.0725(18) Uani 0.50 1 d P E -10 F20F F 0.7220(9) 0.9303(9) 0.5676(3) 0.0725(18) Uani 0.50 1 d P E -10 F21F F 0.7074(8) 0.8833(7) 0.6053(3) 0.0725(18) Uani 0.50 1 d P E -10 C31C C 0.1368(4) 0.1895(5) 0.35691(16) 0.047(2) Uani 1 1 d D . . F19C F 0.2089(3) 0.2066(3) 0.35968(11) 0.0627(9) Uani 1 1 d D . . F20C F 0.1330(3) 0.1237(3) 0.36532(11) 0.0627(9) Uani 1 1 d D . . F21C F 0.1180(3) 0.1876(3) 0.33077(11) 0.0627(9) Uani 1 1 d D . . C23A C -0.1543(9) 0.5504(11) 0.3786(3) 0.044(4) Uani 0.50 1 d PD F -14 F13A F -0.1360(15) 0.4842(8) 0.3858(8) 0.0623(13) Uani 0.50 1 d PD F -14 F14A F -0.0904(6) 0.5845(6) 0.3776(2) 0.0623(13) Uani 0.50 1 d PD F -14 F15A F -0.1836(6) 0.5805(6) 0.3991(2) 0.0623(13) Uani 0.50 1 d PD F -14 C23E C -0.1728(10) 0.5449(11) 0.3821(3) 0.044(4) Uani 0.50 1 d PD F -15 F13E F -0.1292(15) 0.4884(8) 0.3866(8) 0.0623(13) Uani 0.50 1 d PD F -15 F14E F -0.2170(6) 0.5424(6) 0.4016(2) 0.0623(13) Uani 0.50 1 d PD F -15 F15E F -0.1305(6) 0.6022(6) 0.3882(2) 0.0623(13) Uani 0.50 1 d PD F -15 Re1 Re 0.286861(15) 0.738593(15) 0.351999(6) 0.02564(8) Uani 1 1 d . . . N1 N 0.3816(3) 0.7996(3) 0.33162(12) 0.0229(13) Uani 1 1 d . . . C1 C 0.4358(5) 0.8239(5) 0.32530(18) 0.044(2) Uani 1 1 d . . . Re2 Re 0.202471(16) 0.680819(15) 0.373187(6) 0.02731(8) Uani 1 1 d . . . N2 N 0.3770(3) 0.7177(3) 0.37870(13) 0.0316(15) Uani 1 1 d . . . C2 C 0.5030(5) 0.8531(5) 0.3167(2) 0.063(3) Uani 1 1 d . . . H2A H 0.5060 0.8397 0.2985 0.095 Uiso 1 1 calc R . . H2B H 0.5460 0.8345 0.3277 0.095 Uiso 1 1 calc R . . H2C H 0.5021 0.9048 0.3181 0.095 Uiso 1 1 calc R . . N3 N 0.2169(3) 0.7761(3) 0.32077(13) 0.0282(14) Uani 1 1 d . . . C3 C 0.4303(4) 0.7110(4) 0.39176(17) 0.0384(19) Uani 1 1 d . . . N4 N 0.2765(3) 0.8351(3) 0.36915(12) 0.0312(14) Uani 1 1 d . . . C4 C 0.5005(5) 0.7011(5) 0.40818(18) 0.053(2) Uani 1 1 d . . . H4A H 0.5019 0.7318 0.4236 0.079 Uiso 1 1 calc R . . H4B H 0.5414 0.7133 0.3982 0.079 Uiso 1 1 calc R . . H4C H 0.5052 0.6516 0.4138 0.079 Uiso 1 1 calc R . . N5 N 0.3195(3) 0.6570(3) 0.32941(12) 0.0275(13) Uani 1 1 d . . . C5 C 0.1825(4) 0.8028(4) 0.30392(16) 0.0288(17) Uani 1 1 d . . . N6 N 0.1178(3) 0.6227(3) 0.39789(13) 0.0298(15) Uani 1 1 d . . . C6 C 0.1386(4) 0.8382(4) 0.28231(16) 0.0365(19) Uani 1 1 d . . . H6A H 0.1510 0.8887 0.2825 0.055 Uiso 1 1 calc R . . H6B H 0.0860 0.8324 0.2841 0.055 Uiso 1 1 calc R . . H6C H 0.1495 0.8174 0.2657 0.055 Uiso 1 1 calc R . . N7 N 0.2629(4) 0.5883(3) 0.37879(12) 0.0335(15) Uani 1 1 d . . . C7 C 0.2762(4) 0.8913(4) 0.37688(16) 0.0355(18) Uani 1 1 d . . . N8 N 0.1252(4) 0.7617(3) 0.37167(13) 0.0342(15) Uani 1 1 d . . . C8 C 0.2752(6) 0.9629(4) 0.38732(17) 0.051(2) Uani 1 1 d . . . H8A H 0.2990 0.9632 0.4054 0.076 Uiso 1 1 calc R . . H8B H 0.2240 0.9790 0.3870 0.076 Uiso 1 1 calc R . . H8C H 0.3021 0.9946 0.3766 0.076 Uiso 1 1 calc R . . N9 N 0.2418(3) 0.7145(3) 0.41001(13) 0.0323(15) Uani 1 1 d . . . C9 C 0.3464(4) 0.6186(4) 0.31680(16) 0.0325(18) Uani 1 1 d . . . N10 N 0.1412(3) 0.6343(3) 0.34184(13) 0.0308(14) Uani 1 1 d . . . C10 C 0.3833(5) 0.5711(4) 0.29954(17) 0.043(2) Uani 1 1 d . . . H10A H 0.4172 0.5986 0.2900 0.065 Uiso 1 1 calc R . . H10B H 0.3461 0.5483 0.2871 0.065 Uiso 1 1 calc R . . H10C H 0.4111 0.5349 0.3101 0.065 Uiso 1 1 calc R . . C11 C 0.0856(6) 0.5971(6) 0.4140(2) 0.064(3) Uani 1 1 d . . . C12 C 0.0432(9) 0.5628(8) 0.4330(3) 0.115(6) Uani 1 1 d . . . H12A H 0.0469 0.5907 0.4491 0.173 Uiso 1 1 calc R . . H12B H 0.0629 0.5153 0.4368 0.173 Uiso 1 1 calc R . . H12C H -0.0088 0.5593 0.4257 0.173 Uiso 1 1 calc R . . C13 C 0.2976(4) 0.5383(4) 0.38132(15) 0.0330(18) Uani 1 1 d . . . C14 C 0.3432(4) 0.4755(4) 0.38462(16) 0.0386(19) Uani 1 1 d . . . H14A H 0.3799 0.4764 0.3721 0.058 Uiso 1 1 calc R . . H14B H 0.3120 0.4334 0.3815 0.058 Uiso 1 1 calc R . . H14C H 0.3684 0.4742 0.4024 0.058 Uiso 1 1 calc R . . C15 C 0.0801(5) 0.8028(4) 0.37123(16) 0.0364(19) Uani 1 1 d . . . C16 C 0.0233(4) 0.8573(4) 0.37065(18) 0.045(2) Uani 1 1 d . . . H16A H 0.0460 0.9023 0.3765 0.067 Uiso 1 1 calc R . . H16B H -0.0134 0.8437 0.3823 0.067 Uiso 1 1 calc R . . H16C H -0.0010 0.8624 0.3528 0.067 Uiso 1 1 calc R . . C17 C 0.2557(4) 0.7280(4) 0.43167(17) 0.0346(18) Uani 1 1 d . . . C18 C 0.2703(6) 0.7453(5) 0.45900(18) 0.061(3) Uani 1 1 d . . . H18A H 0.2489 0.7915 0.4622 0.091 Uiso 1 1 calc R . . H18B H 0.3238 0.7467 0.4640 0.091 Uiso 1 1 calc R . . H18C H 0.2482 0.7092 0.4694 0.091 Uiso 1 1 calc R . . C19 C 0.1002(4) 0.6071(4) 0.32676(14) 0.0273(16) Uani 1 1 d . . . C20 C 0.0488(5) 0.5725(4) 0.30643(17) 0.045(2) Uani 1 1 d . . . H20A H 0.0271 0.6082 0.2941 0.067 Uiso 1 1 calc R . . H20B H 0.0094 0.5489 0.3146 0.067 Uiso 1 1 calc R . . H20C H 0.0757 0.5376 0.2971 0.067 Uiso 1 1 calc R . . F1A F -0.0640(2) 0.6565(2) 0.25991(9) 0.0392(11) Uani 1 1 d . . . C1A C -0.2270(3) 0.5006(3) 0.26024(13) 0.0200(14) Uani 1 1 d . . . B1A B -0.2326(4) 0.4518(4) 0.28638(15) 0.0197(16) Uani 1 1 d . . . F2A F -0.1059(3) 0.6930(2) 0.22222(9) 0.0505(13) Uani 1 1 d . . . C2A C -0.1818(3) 0.5608(3) 0.26184(14) 0.0226(15) Uani 1 1 d . . . H2A1 H -0.1555 0.5731 0.2782 0.027 Uiso 1 1 calc R . . F3A F -0.1607(2) 0.7205(2) 0.25556(10) 0.0405(12) Uani 1 1 d . . . C3A C -0.1743(3) 0.6026(3) 0.24057(14) 0.0214(14) Uani 1 1 d . . . F4A F -0.2966(3) 0.5587(3) 0.17021(9) 0.0574(15) Uani 1 1 d . . . C4A C -0.2111(4) 0.5881(4) 0.21632(15) 0.0274(16) Uani 1 1 d . . . H4A1 H -0.2060 0.6177 0.2017 0.033 Uiso 1 1 calc R . . F5A F -0.3638(3) 0.4876(4) 0.18933(11) 0.084(2) Uani 1 1 d . . . C5A C -0.2560(4) 0.5287(4) 0.21398(14) 0.0238(15) Uani 1 1 d . . . F6A F -0.2630(4) 0.4529(3) 0.17780(11) 0.0739(18) Uani 1 1 d . . . C6A C -0.2639(3) 0.4862(3) 0.23589(14) 0.0228(15) Uani 1 1 d . . . H6A1 H -0.2958 0.4463 0.2339 0.027 Uiso 1 1 calc R . . F7A F 0.0464(3) 0.4452(2) 0.26567(10) 0.0476(13) Uani 1 1 d . . . C7A C -0.1277(4) 0.6677(4) 0.24418(14) 0.0260(16) Uani 1 1 d . . . F8A F 0.0314(3) 0.3449(3) 0.24713(10) 0.0582(15) Uani 1 1 d . . . C8A C -0.2948(5) 0.5085(4) 0.18802(16) 0.039(2) Uani 1 1 d . . . F9A F 0.0951(2) 0.3533(3) 0.28408(11) 0.0577(15) Uani 1 1 d . . . C9A C -0.1588(3) 0.4010(3) 0.29155(13) 0.0220(14) Uani 1 1 d . . . F10A F -0.0492(2) 0.1853(2) 0.32758(10) 0.0494(13) Uani 1 1 d . . . C10A C -0.0936(3) 0.4118(4) 0.28032(14) 0.0225(15) Uani 1 1 d . . . H10D H -0.0897 0.4528 0.2699 0.027 Uiso 1 1 calc R . . F11A F -0.1653(2) 0.1869(2) 0.31601(10) 0.0452(12) Uani 1 1 d . . . C11A C -0.0333(4) 0.3650(4) 0.28366(14) 0.0247(15) Uani 1 1 d . . . F12A F -0.1210(4) 0.2415(3) 0.35031(10) 0.0653(17) Uani 1 1 d . . . C12A C -0.0383(4) 0.3042(4) 0.29844(14) 0.0254(16) Uani 1 1 d . . . H12D H 0.0013 0.2712 0.3004 0.030 Uiso 1 1 calc R . . C13A C -0.1012(4) 0.2925(4) 0.31025(13) 0.0220(14) Uani 1 1 d . . . C14A C -0.1594(4) 0.3396(4) 0.30668(14) 0.0249(15) Uani 1 1 d . . . H14D H -0.2023 0.3298 0.3150 0.030 Uiso 1 1 calc R . . C15A C 0.0340(4) 0.3772(4) 0.27036(15) 0.0288(17) Uani 1 1 d . . . F16A F -0.3424(3) 0.7200(2) 0.31103(11) 0.0536(14) Uani 1 1 d . . . C16A C -0.1089(4) 0.2267(4) 0.32594(14) 0.0305(17) Uani 1 1 d . . . F17A F -0.3906(3) 0.6837(3) 0.34463(10) 0.0561(14) Uani 1 1 d . . . C17A C -0.2395(4) 0.5069(3) 0.31066(13) 0.0213(14) Uani 1 1 d . . . F18A F -0.4243(3) 0.6385(3) 0.30718(11) 0.0559(15) Uani 1 1 d . . . C18A C -0.1973(4) 0.5043(4) 0.33469(14) 0.0259(16) Uani 1 1 d . F . H18D H -0.1595 0.4697 0.3377 0.031 Uiso 1 1 calc R . . C19A C -0.2092(4) 0.5521(4) 0.35470(15) 0.0361(19) Uani 1 1 d D . . C20A C -0.2627(4) 0.6044(4) 0.35124(16) 0.0344(18) Uani 1 1 d . F . H20D H -0.2696 0.6369 0.3648 0.041 Uiso 1 1 calc R . . C21A C -0.3056(4) 0.6076(3) 0.32737(14) 0.0252(15) Uani 1 1 d . . . F22A F -0.4332(2) 0.2282(3) 0.22937(10) 0.0550(14) Uani 1 1 d . . . C22A C -0.2942(4) 0.5599(3) 0.30733(14) 0.0232(15) Uani 1 1 d . F . H22A H -0.3242 0.5635 0.2911 0.028 Uiso 1 1 calc R . . F23A F -0.3499(3) 0.1730(2) 0.25423(10) 0.0520(13) Uani 1 1 d . . . F24A F -0.3189(2) 0.2448(2) 0.22525(8) 0.0356(10) Uani 1 1 d . . . C24A C -0.3653(4) 0.6606(4) 0.32252(16) 0.0326(18) Uani 1 1 d . F . C25A C -0.3035(3) 0.3983(3) 0.28352(13) 0.0221(14) Uani 1 1 d . . . C26A C -0.3624(3) 0.4019(4) 0.29829(14) 0.0259(15) Uani 1 1 d . D . H26A H -0.3633 0.4390 0.3107 0.031 Uiso 1 1 calc R . . C27A C -0.4205(4) 0.3537(4) 0.29572(15) 0.0283(16) Uani 1 1 d D . . C28A C -0.4221(4) 0.2995(4) 0.27822(14) 0.0263(16) Uani 1 1 d . D . H28A H -0.4613 0.2661 0.2768 0.032 Uiso 1 1 calc R . . C29A C -0.3649(4) 0.2943(4) 0.26245(14) 0.0244(15) Uani 1 1 d . . . C30A C -0.3075(4) 0.3425(3) 0.26540(14) 0.0246(15) Uani 1 1 d . D . H30A H -0.2687 0.3377 0.2546 0.030 Uiso 1 1 calc R . . C32A C -0.3669(4) 0.2363(4) 0.24302(16) 0.0322(17) Uani 1 1 d . D . F1B F 0.6829(3) 0.9514(2) 0.47410(12) 0.0611(15) Uani 1 1 d . . . C1B C 0.5739(4) 0.7571(4) 0.48526(13) 0.0229(14) Uani 1 1 d . . . B1B B 0.5303(4) 0.7396(4) 0.51101(16) 0.0230(16) Uani 1 1 d . . . F2B F 0.5829(3) 0.9564(3) 0.45022(12) 0.0628(16) Uani 1 1 d . . . C2B C 0.5880(4) 0.8267(4) 0.47835(14) 0.0282(16) Uani 1 1 d . . . H2B1 H 0.5660 0.8641 0.4871 0.034 Uiso 1 1 calc R . . F3B F 0.6828(4) 0.9304(3) 0.43400(13) 0.097(3) Uani 1 1 d . . . C3B C 0.6326(4) 0.8431(4) 0.45933(14) 0.0264(16) Uani 1 1 d . . . F4B F 0.7665(2) 0.6848(2) 0.43641(10) 0.0441(12) Uani 1 1 d . . . C4B C 0.6693(4) 0.7908(4) 0.44712(14) 0.0275(16) Uani 1 1 d . . . H4B1 H 0.7012 0.8022 0.4343 0.033 Uiso 1 1 calc R . . F5B F 0.6622(2) 0.6421(2) 0.41871(9) 0.0393(11) Uani 1 1 d . . . C5B C 0.6580(4) 0.7210(3) 0.45424(14) 0.0240(15) Uani 1 1 d . . . F6B F 0.7093(2) 0.6061(2) 0.45657(9) 0.0385(11) Uani 1 1 d . . . C6B C 0.6112(4) 0.7049(4) 0.47256(14) 0.0243(15) Uani 1 1 d . . . H6B1 H 0.6040 0.6566 0.4768 0.029 Uiso 1 1 calc R . . F7B F 0.3798(3) 0.5941(2) 0.43878(9) 0.0429(12) Uani 1 1 d . . . C7B C 0.6450(5) 0.9191(4) 0.45398(17) 0.0373(19) Uani 1 1 d . . . F8B F 0.3702(3) 0.4886(2) 0.45368(9) 0.0399(11) Uani 1 1 d . . . C8B C 0.6989(4) 0.6641(4) 0.44168(15) 0.0290(17) Uani 1 1 d . . . F9B F 0.2898(2) 0.5680(3) 0.46097(10) 0.0498(13) Uani 1 1 d . . . C9B C 0.4898(4) 0.6624(3) 0.50879(14) 0.0226(15) Uani 1 1 d . . . F10B F 0.4507(2) 0.4447(2) 0.55017(8) 0.0339(10) Uani 1 1 d . . . C10B C 0.4499(3) 0.6397(3) 0.48557(14) 0.0231(15) Uani 1 1 d . . . H10E H 0.4507 0.6671 0.4702 0.028 Uiso 1 1 calc R . . F11B F 0.3766(2) 0.5213(2) 0.56340(9) 0.0432(12) Uani 1 1 d . . . C11B C 0.4087(4) 0.5772(3) 0.48460(14) 0.0218(14) Uani 1 1 d . . . F12B F 0.4927(3) 0.5317(2) 0.57366(9) 0.0436(12) Uani 1 1 d . . . C12B C 0.4067(4) 0.5353(3) 0.50643(14) 0.0242(15) Uani 1 1 d . . . H12E H 0.3786 0.4928 0.5055 0.029 Uiso 1 1 calc R . . F13B F 0.3600(14) 0.7895(10) 0.5826(5) 0.0619(17) Uani 0.50 1 d PD G -17 C13B C 0.4462(3) 0.5562(3) 0.52963(14) 0.0214(15) Uani 1 1 d . . . F14B F 0.3474(7) 0.9107(6) 0.5779(2) 0.0619(17) Uani 0.50 1 d PD G -17 C14B C 0.4867(4) 0.6192(3) 0.53069(13) 0.0229(15) Uani 1 1 d . . . H14E H 0.5129 0.6331 0.5469 0.027 Uiso 1 1 calc R . . F15B F 0.2684(8) 0.8309(6) 0.5652(3) 0.0619(17) Uani 0.50 1 d PD G -17 C15B C 0.3632(4) 0.5574(4) 0.46008(15) 0.0296(17) Uani 1 1 d . . . F16B F 0.3401(3) 0.9022(3) 0.45314(11) 0.0728(18) Uani 1 1 d . . . C16B C 0.4418(4) 0.5147(4) 0.55387(15) 0.0259(16) Uani 1 1 d . . . F17B F 0.3865(4) 0.9890(3) 0.47621(14) 0.087(2) Uani 1 1 d . . . C17B C 0.4628(4) 0.7943(3) 0.51449(15) 0.0264(16) Uani 1 1 d . . . F18B F 0.2752(3) 0.9559(3) 0.47870(11) 0.0670(16) Uani 1 1 d . . . C18B C 0.4326(4) 0.7976(4) 0.53827(15) 0.0291(17) Uani 1 1 d . . . H18E H 0.4529 0.7686 0.5523 0.035 Uiso 1 1 calc R . . C19B C 0.3734(4) 0.8422(4) 0.54205(16) 0.0333(18) Uani 1 1 d D . . C20B C 0.3416(4) 0.8851(4) 0.52176(18) 0.040(2) Uani 1 1 d . . . H20E H 0.3013 0.9153 0.5242 0.047 Uiso 1 1 calc R . . C21B C 0.3704(4) 0.8824(4) 0.49826(17) 0.0338(18) Uani 1 1 d . . . C22B C 0.4287(4) 0.8367(4) 0.49447(16) 0.0314(17) Uani 1 1 d . . . H22B H 0.4457 0.8346 0.4777 0.038 Uiso 1 1 calc R . . C23B C 0.3417(11) 0.8449(10) 0.5676(3) 0.048(3) Uani 0.50 1 d PD G -17 C24B C 0.3419(5) 0.9318(5) 0.4767(2) 0.050(2) Uani 1 1 d . G . C25B C 0.5961(4) 0.7439(4) 0.53506(14) 0.0269(16) Uani 1 1 d . . . C26B C 0.6106(4) 0.8060(4) 0.54910(14) 0.0303(17) Uani 1 1 d . E . H26B H 0.5770 0.8444 0.5462 0.036 Uiso 1 1 calc R . . C27B C 0.6734(4) 0.8140(4) 0.56751(15) 0.0342(18) Uani 1 1 d . . . C28B C 0.7244(4) 0.7592(4) 0.57213(16) 0.0385(19) Uani 1 1 d . E . H28B H 0.7667 0.7641 0.5845 0.046 Uiso 1 1 calc R . . C29B C 0.7111(4) 0.6973(4) 0.55798(15) 0.0309(17) Uani 1 1 d . . . C30B C 0.6485(4) 0.6904(4) 0.53996(15) 0.0291(16) Uani 1 1 d . E . H30B H 0.6412 0.6473 0.5306 0.035 Uiso 1 1 calc R . . C32B C 0.7641(4) 0.6395(4) 0.56279(18) 0.041(2) Uani 1 1 d . E . F24B F 0.7685(3) 0.5970(3) 0.54094(12) 0.0590(15) Uani 1 1 d . . . F23B F 0.7491(3) 0.5937(3) 0.58079(13) 0.0755(19) Uani 1 1 d . . . F22B F 0.8337(2) 0.6612(3) 0.56938(11) 0.0519(13) Uani 1 1 d . . . F1C F -0.2777(4) 0.2833(4) 0.36708(14) 0.103(3) Uani 1 1 d . . . C1C C -0.1119(3) 0.2887(4) 0.42916(14) 0.0225(15) Uani 1 1 d . . . B1C B -0.0334(4) 0.2458(4) 0.42809(16) 0.0218(16) Uani 1 1 d . . . F2C F -0.2702(3) 0.3952(3) 0.37046(12) 0.078(2) Uani 1 1 d . . . C2C C -0.1605(4) 0.3002(3) 0.40705(14) 0.0225(15) Uani 1 1 d . . . H2C1 H -0.1455 0.2884 0.3905 0.027 Uiso 1 1 calc R . . F3C F -0.3527(3) 0.3382(3) 0.38728(11) 0.0601(15) Uani 1 1 d . . . C3C C -0.2307(4) 0.3284(4) 0.40805(15) 0.0283(16) Uani 1 1 d . . . F4C F -0.2453(3) 0.4356(3) 0.47878(13) 0.082(2) Uani 1 1 d . . . C4C C -0.2534(4) 0.3485(5) 0.43116(17) 0.042(2) Uani 1 1 d . . . H4C1 H -0.3013 0.3679 0.4317 0.051 Uiso 1 1 calc R . . F5C F -0.2924(3) 0.3327(3) 0.48424(11) 0.0653(16) Uani 1 1 d . . . C5C C -0.2062(4) 0.3405(5) 0.45360(17) 0.039(2) Uani 1 1 d . . . F6C F -0.1809(3) 0.3540(4) 0.49951(12) 0.092(2) Uani 1 1 d . . . C6C C -0.1364(4) 0.3093(4) 0.45262(15) 0.0330(18) Uani 1 1 d . . . H6C1 H -0.1052 0.3021 0.4684 0.040 Uiso 1 1 calc R . . C7C C -0.2807(4) 0.3368(5) 0.38313(19) 0.043(2) Uani 1 1 d . . . C8C C -0.2295(5) 0.3648(6) 0.4792(2) 0.058(3) Uani 1 1 d . . . C9C C 0.0267(4) 0.2602(4) 0.45284(14) 0.0261(15) Uani 1 1 d . . . F10C F 0.1876(2) 0.1539(2) 0.51738(9) 0.0407(11) Uani 1 1 d . . . C10C C 0.0346(4) 0.3272(4) 0.46553(15) 0.0295(16) Uani 1 1 d . B . H10F H 0.0014 0.3642 0.4598 0.035 Uiso 1 1 calc R . . F11C F 0.2588(2) 0.1850(3) 0.48911(10) 0.0468(13) Uani 1 1 d . . . C11C C 0.0896(4) 0.3399(4) 0.48600(16) 0.0341(18) Uani 1 1 d . . . F12C F 0.1765(3) 0.1046(2) 0.47956(10) 0.0475(12) Uani 1 1 d . . . C12C C 0.1401(4) 0.2880(4) 0.49436(16) 0.0354(18) Uani 1 1 d . B . H12F H 0.1780 0.2972 0.5082 0.043 Uiso 1 1 calc R . . F13C F -0.0801(4) 0.0564(4) 0.49613(13) 0.096(2) Uani 1 1 d . . . C13C C 0.1348(4) 0.2225(4) 0.48230(14) 0.0255(16) Uani 1 1 d . . . F14C F -0.0743(3) -0.0415(3) 0.47628(14) 0.093(2) Uani 1 1 d . . . C14C C 0.0802(4) 0.2099(4) 0.46197(14) 0.0245(15) Uani 1 1 d . B . H14F H 0.0787 0.1649 0.4537 0.029 Uiso 1 1 calc R . . F15C F -0.1779(3) 0.0067(3) 0.47782(12) 0.0729(19) Uani 1 1 d . . . F16C F -0.1077(3) -0.0366(3) 0.37500(12) 0.0765(19) Uani 1 1 d . . . C16C C 0.1896(4) 0.1663(4) 0.49198(16) 0.0313(17) Uani 1 1 d . B . F17C F -0.2140(3) 0.0054(3) 0.37683(13) 0.081(2) Uani 1 1 d . . . C17C C -0.0612(3) 0.1630(4) 0.42696(14) 0.0248(15) Uani 1 1 d . . . F18C F -0.1393(4) 0.0637(3) 0.35700(13) 0.088(2) Uani 1 1 d . . . C18C C -0.0703(4) 0.1258(4) 0.44976(15) 0.0299(17) Uani 1 1 d . . . H18F H -0.0554 0.1477 0.4661 0.036 Uiso 1 1 calc R . . C19C C -0.1002(4) 0.0582(4) 0.44980(18) 0.039(2) Uani 1 1 d . . . C20C C -0.1239(5) 0.0249(4) 0.42631(17) 0.041(2) Uani 1 1 d . . . H20F H -0.1446 -0.0212 0.4260 0.050 Uiso 1 1 calc R . . C21C C -0.1164(4) 0.0606(4) 0.40340(17) 0.0350(18) Uani 1 1 d . . . F22C F -0.0155(4) 0.4459(3) 0.34629(13) 0.0746(18) Uani 1 1 d . . . C22C C -0.0854(4) 0.1278(4) 0.40354(15) 0.0281(16) Uani 1 1 d . . . H22C H -0.0805 0.1505 0.3874 0.034 Uiso 1 1 calc R . . F23C F 0.1014(4) 0.4551(3) 0.35461(18) 0.121(3) Uani 1 1 d . . . C23C C -0.1084(5) 0.0215(5) 0.4745(2) 0.053(3) Uani 1 1 d . . . F24C F 0.0299(4) 0.4792(3) 0.38251(13) 0.087(2) Uani 1 1 d . . . C24C C -0.1420(6) 0.0250(5) 0.3779(2) 0.053(2) Uani 1 1 d . . . C25C C 0.0072(4) 0.2676(4) 0.40254(14) 0.0238(15) Uani 1 1 d . . . C26C C 0.0519(4) 0.2204(4) 0.39042(14) 0.0257(16) Uani 1 1 d . . . H26C H 0.0558 0.1729 0.3964 0.031 Uiso 1 1 calc R . . C27C C 0.0905(4) 0.2412(4) 0.36989(15) 0.0311(17) Uani 1 1 d . . . C28C C 0.0882(4) 0.3094(5) 0.36127(16) 0.039(2) Uani 1 1 d . . . H28C H 0.1149 0.3233 0.3473 0.047 Uiso 1 1 calc R . . C29C C 0.0461(4) 0.3579(4) 0.37326(15) 0.0316(18) Uani 1 1 d . . . C30C C 0.0057(4) 0.3370(4) 0.39302(15) 0.0304(17) Uani 1 1 d . . . H30C H -0.0243 0.3709 0.4005 0.036 Uiso 1 1 calc R . . C32C C 0.0431(5) 0.4314(5) 0.36345(19) 0.049(2) Uani 1 1 d . . . C1D C 0.1820(4) 0.4868(3) 0.21615(13) 0.0221(15) Uani 1 1 d . . . B1D B 0.2513(4) 0.4322(4) 0.21435(15) 0.0211(16) Uani 1 1 d . . . C2D C 0.1909(4) 0.5472(3) 0.23156(14) 0.0243(15) Uani 1 1 d . . . H2D H 0.2386 0.5582 0.2400 0.029 Uiso 1 1 calc R . . C3D C 0.1318(4) 0.5924(4) 0.23497(14) 0.0260(16) Uani 1 1 d . . . F4D F 0.1870(3) 0.6392(2) 0.27524(9) 0.0457(12) Uani 1 1 d . . . C4D C 0.0626(4) 0.5804(4) 0.22255(16) 0.0337(19) Uani 1 1 d . A . H4D H 0.0222 0.6103 0.2252 0.040 Uiso 1 1 calc R . . F5D F 0.0853(2) 0.6864(2) 0.25884(11) 0.0526(14) Uani 1 1 d . . . C5D C 0.0536(4) 0.5226(4) 0.20585(15) 0.0303(17) Uani 1 1 d D . . F6D F 0.1847(2) 0.7068(2) 0.24182(9) 0.0379(11) Uani 1 1 d . . . C6D C 0.1119(4) 0.4771(4) 0.20314(15) 0.0287(16) Uani 1 1 d . A . H6D H 0.1033 0.4375 0.1919 0.034 Uiso 1 1 calc R . . C7D C 0.1464(4) 0.6555(4) 0.25260(17) 0.0346(19) Uani 1 1 d . . . C9D C 0.2309(3) 0.3765(3) 0.19069(14) 0.0219(14) Uani 1 1 d . . . C10D C 0.1750(4) 0.3250(3) 0.19236(14) 0.0249(15) Uani 1 1 d . . . H10G H 0.1523 0.3214 0.2081 0.030 Uiso 1 1 calc R . . C11D C 0.1521(4) 0.2795(4) 0.17177(15) 0.0287(17) Uani 1 1 d . . . C12D C 0.1853(4) 0.2820(4) 0.14891(16) 0.0337(18) Uani 1 1 d . . . H12G H 0.1699 0.2506 0.1349 0.040 Uiso 1 1 calc R . . C13D C 0.2406(4) 0.3300(4) 0.14657(16) 0.0347(18) Uani 1 1 d . . . C14D C 0.2635(4) 0.3768(4) 0.16703(14) 0.0270(16) Uani 1 1 d . . . H14G H 0.3019 0.4096 0.1649 0.032 Uiso 1 1 calc R . . C15D C 0.0924(4) 0.2280(4) 0.17441(16) 0.0346(18) Uani 1 1 d . . . C16D C 0.2762(5) 0.3327(5) 0.12209(18) 0.047(2) Uani 1 1 d . . . C17D C 0.3247(3) 0.4804(3) 0.21051(13) 0.0202(14) Uani 1 1 d . . . C18D C 0.3208(4) 0.5339(3) 0.19138(15) 0.0281(17) Uani 1 1 d . C . H18G H 0.2758 0.5404 0.1804 0.034 Uiso 1 1 calc R . . C19D C 0.3800(4) 0.5775(4) 0.18795(15) 0.0288(17) Uani 1 1 d D . . C20D C 0.4462(4) 0.5703(4) 0.20372(15) 0.0309(17) Uani 1 1 d . C . H20G H 0.4869 0.6002 0.2015 0.037 Uiso 1 1 calc R . . C21D C 0.4515(3) 0.5184(3) 0.22286(14) 0.0231(15) Uani 1 1 d . . . C23D C 0.3926(4) 0.4743(4) 0.22614(14) 0.0241(15) Uani 1 1 d . C . H23D H 0.3983 0.4390 0.2393 0.029 Uiso 1 1 calc R . . F10D F 0.3325(4) 0.3734(4) 0.12242(13) 0.105(3) Uani 1 1 d . . . F11D F 0.2290(4) 0.3529(3) 0.10148(11) 0.079(2) Uani 1 1 d . . . C24D C 0.5204(4) 0.5092(4) 0.24107(16) 0.0323(18) Uani 1 1 d . C . F12D F 0.2984(4) 0.2686(3) 0.11478(11) 0.0732(18) Uani 1 1 d . . . C25D C 0.2677(4) 0.3875(3) 0.24171(14) 0.0231(15) Uani 1 1 d . . . C26D C 0.3041(3) 0.3214(3) 0.24220(13) 0.0204(14) Uani 1 1 d . . . H26D H 0.3166 0.3020 0.2263 0.025 Uiso 1 1 calc R . . F9D F 0.0541(3) 0.2105(3) 0.15149(10) 0.0536(13) Uani 1 1 d . . . C27D C 0.3221(3) 0.2838(3) 0.26531(14) 0.0240(15) Uani 1 1 d . . . F7D F 0.1168(2) 0.1669(2) 0.18554(9) 0.0419(11) Uani 1 1 d . . . C28D C 0.3057(4) 0.3098(4) 0.28875(15) 0.0277(16) Uani 1 1 d . . . H28D H 0.3184 0.2842 0.3045 0.033 Uiso 1 1 calc R . . F8D F 0.0417(2) 0.2514(2) 0.18926(11) 0.0506(13) Uani 1 1 d . . . C29D C 0.2696(4) 0.3755(4) 0.28899(14) 0.0241(15) Uani 1 1 d . . . C30D C 0.2518(4) 0.4121(4) 0.26612(13) 0.0232(15) Uani 1 1 d . . . H30D H 0.2275 0.4564 0.2669 0.028 Uiso 1 1 calc R . . C31D C 0.3608(4) 0.2141(4) 0.26373(15) 0.0297(17) Uani 1 1 d . . . C32D C 0.2561(4) 0.4059(5) 0.31441(16) 0.039(2) Uani 1 1 d . . . F21D F 0.3211(2) 0.1692(2) 0.24750(9) 0.0330(10) Uani 1 1 d . . . F20D F 0.3744(3) 0.1821(2) 0.28646(10) 0.0508(13) Uani 1 1 d . . . F19D F 0.4260(2) 0.2213(2) 0.25370(10) 0.0449(13) Uani 1 1 d . . . F23D F 0.2349(3) 0.3594(3) 0.33152(10) 0.0540(14) Uani 1 1 d . . . F22D F 0.3175(3) 0.4349(4) 0.32707(11) 0.088(2) Uani 1 1 d . . . F24D F 0.2065(4) 0.4567(3) 0.31280(11) 0.083(2) Uani 1 1 d . . . F17D F 0.5498(2) 0.4445(2) 0.23891(10) 0.0426(12) Uani 1 1 d . . . F18D F 0.5093(3) 0.5149(3) 0.26643(10) 0.0595(15) Uani 1 1 d . . . F16D F 0.5735(2) 0.5549(2) 0.23718(11) 0.0538(14) Uani 1 1 d . . . Cl1S Cl 0.38607(19) 0.2251(2) 0.35993(7) 0.1141(15) Uani 1 1 d D . . N1S N 0.5263(5) 0.4273(5) 0.63833(19) 0.068(3) Uani 1 1 d . . . C1S C 0.4728(5) 0.4575(5) 0.63359(17) 0.044(2) Uani 1 1 d . . . Cl2S Cl 0.46579(17) 0.32236(14) 0.39662(5) 0.0705(8) Uani 1 1 d D . . C2S C 0.4058(5) 0.4983(5) 0.62727(17) 0.046(2) Uani 1 1 d . . . H2S1 H 0.3808 0.5043 0.6430 0.070 Uiso 1 1 calc R . . H2S2 H 0.3730 0.4734 0.6139 0.070 Uiso 1 1 calc R . . H2S3 H 0.4184 0.5448 0.6206 0.070 Uiso 1 1 calc R . . Cl3S Cl 0.4740(2) 0.89087(18) 0.39543(9) 0.1166(14) Uani 1 1 d D . . C3S C 0.4678(5) 0.2441(5) 0.3790(2) 0.061(3) Uani 1 1 d D . . H3S1 H 0.5080 0.2471 0.3676 0.073 Uiso 1 1 calc R . . H3S2 H 0.4796 0.2047 0.3915 0.073 Uiso 1 1 calc R . . Cl4S Cl 0.4717(2) 1.0167(3) 0.36433(7) 0.1235(15) Uani 1 1 d D . . C4S C 0.5136(6) 0.9741(5) 0.3919(2) 0.077(3) Uani 1 1 d D . . H4S1 H 0.5081 1.0032 0.4076 0.092 Uiso 1 1 calc R . . H4S2 H 0.5671 0.9686 0.3904 0.092 Uiso 1 1 calc R . . Cl5S Cl 0.0458(3) 0.2518(3) 0.57727(12) 0.170(2) Uani 1 1 d D . . C5S C 0.1188(7) 0.9716(5) 0.44178(19) 0.075(3) Uani 1 1 d D . . H5S1 H 0.0821 0.9687 0.4545 0.090 Uiso 1 1 calc R . . H5S2 H 0.1638 0.9947 0.4505 0.090 Uiso 1 1 calc R . . Cl6S Cl -0.0502(3) 0.2516(3) 0.52821(10) 0.160(2) Uani 1 1 d D . . Cl7S Cl 0.0839(2) 1.02012(16) 0.41551(8) 0.1105(14) Uani 1 1 d D . . Cl8S Cl 0.1409(2) 0.88510(15) 0.43152(8) 0.1122(15) Uani 1 1 d D . . C6S C 0.0298(6) 0.2095(9) 0.54564(16) 0.238(16) Uani 1 1 d D . . H6S1 H 0.0205 0.1583 0.5477 0.286 Uiso 1 1 calc R . . H6S2 H 0.0733 0.2153 0.5359 0.286 Uiso 1 1 calc R . . C22E C 0.3719(9) 0.6328(9) 0.1678(3) 0.046(2) Uani 0.51 1 d PD C -6 F15F F 0.3420(6) 0.6960(5) 0.1786(2) 0.0676(17) Uani 0.51 1 d PD C -6 F14F F 0.4337(6) 0.6582(7) 0.1612(3) 0.0676(17) Uani 0.51 1 d PD C -6 F13F F 0.3233(6) 0.6224(6) 0.1479(2) 0.0676(17) Uani 0.51 1 d PD C -6 C23F C 0.3499(11) 0.8491(12) 0.5688(3) 0.048(3) Uani 0.50 1 d PD G -18 F13G F 0.3724(14) 0.7986(10) 0.5854(5) 0.0619(17) Uani 0.50 1 d PD G -18 F14G F 0.3876(7) 0.8993(6) 0.5833(2) 0.0619(17) Uani 0.50 1 d PD G -18 F15G F 0.2774(8) 0.8643(6) 0.5684(3) 0.0619(17) Uani 0.50 1 d PD G -18 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 C8D 0.018(5) 0.043(5) 0.088(12) -0.027(7) 0.024(6) 0.006(4) F1D 0.033(2) 0.080(4) 0.058(4) 0.001(3) -0.010(2) -0.007(2) F2D 0.033(2) 0.080(4) 0.058(4) 0.001(3) -0.010(2) -0.007(2) F3D 0.033(2) 0.080(4) 0.058(4) 0.001(3) -0.010(2) -0.007(2) C8E 0.018(5) 0.043(5) 0.088(12) -0.027(7) 0.024(6) 0.006(4) F1E 0.033(2) 0.080(4) 0.058(4) 0.001(3) -0.010(2) -0.007(2) F2E 0.033(2) 0.080(4) 0.058(4) 0.001(3) -0.010(2) -0.007(2) F3E 0.033(2) 0.080(4) 0.058(4) 0.001(3) -0.010(2) -0.007(2) C15C 0.062(7) 0.062(6) 0.029(6) -0.011(5) -0.005(5) 0.012(5) F7C 0.087(5) 0.053(3) 0.073(4) -0.020(3) -0.002(3) 0.009(3) F8C 0.087(5) 0.053(3) 0.073(4) -0.020(3) -0.002(3) 0.009(3) F9C 0.087(5) 0.053(3) 0.073(4) -0.020(3) -0.002(3) 0.009(3) C15E 0.062(7) 0.062(6) 0.029(6) -0.011(5) -0.005(5) 0.012(5) F7E 0.087(5) 0.053(3) 0.073(4) -0.020(3) -0.002(3) 0.009(3) F8E 0.087(5) 0.053(3) 0.073(4) -0.020(3) -0.002(3) 0.009(3) F9E 0.087(5) 0.053(3) 0.073(4) -0.020(3) -0.002(3) 0.009(3) C22D 0.039(5) 0.047(5) 0.052(6) 0.017(5) 0.006(4) -0.010(4) F13D 0.072(3) 0.060(4) 0.068(4) 0.038(3) -0.005(3) -0.017(3) F14D 0.072(3) 0.060(4) 0.068(4) 0.038(3) -0.005(3) -0.017(3) F15D 0.072(3) 0.060(4) 0.068(4) 0.038(3) -0.005(3) -0.017(3) C31A 0.035(5) 0.063(6) 0.029(7) -0.017(5) 0.004(5) -0.015(5) F19A 0.042(3) 0.054(3) 0.077(4) -0.002(3) 0.036(2) 0.001(2) F20A 0.042(3) 0.054(3) 0.077(4) -0.002(3) 0.036(2) 0.001(2) F21A 0.042(3) 0.054(3) 0.077(4) -0.002(3) 0.036(2) 0.001(2) C31E 0.035(5) 0.063(6) 0.029(7) -0.017(5) 0.004(5) -0.015(5) F19E 0.042(3) 0.054(3) 0.077(4) -0.002(3) 0.036(2) 0.001(2) F20E 0.042(3) 0.054(3) 0.077(4) -0.002(3) 0.036(2) 0.001(2) F21E 0.042(3) 0.054(3) 0.077(4) -0.002(3) 0.036(2) 0.001(2) C31B 0.054(6) 0.054(6) 0.033(6) 0.000(5) -0.012(4) -0.013(5) F19B 0.116(6) 0.045(3) 0.055(4) -0.013(2) -0.002(3) -0.021(4) F20B 0.116(6) 0.045(3) 0.055(4) -0.013(2) -0.002(3) -0.021(4) F21B 0.116(6) 0.045(3) 0.055(4) -0.013(2) -0.002(3) -0.021(4) C31F 0.054(6) 0.054(6) 0.033(6) 0.000(5) -0.012(4) -0.013(5) F19F 0.116(6) 0.045(3) 0.055(4) -0.013(2) -0.002(3) -0.021(4) F20F 0.116(6) 0.045(3) 0.055(4) -0.013(2) -0.002(3) -0.021(4) F21F 0.116(6) 0.045(3) 0.055(4) -0.013(2) -0.002(3) -0.021(4) C31C 0.026(4) 0.087(7) 0.026(5) 0.003(5) 0.002(3) 0.003(4) F19C 0.0514(19) 0.082(2) 0.057(2) -0.0088(18) 0.0172(16) 0.0142(17) F20C 0.0514(19) 0.082(2) 0.057(2) -0.0088(18) 0.0172(16) 0.0142(17) F21C 0.0514(19) 0.082(2) 0.057(2) -0.0088(18) 0.0172(16) 0.0142(17) C23A 0.052(10) 0.053(7) 0.026(6) -0.019(5) 0.006(6) 0.015(7) F13A 0.068(3) 0.071(3) 0.042(3) -0.001(2) -0.016(2) 0.007(2) F14A 0.068(3) 0.071(3) 0.042(3) -0.001(2) -0.016(2) 0.007(2) F15A 0.068(3) 0.071(3) 0.042(3) -0.001(2) -0.016(2) 0.007(2) C23E 0.052(10) 0.053(7) 0.026(6) -0.019(5) 0.006(6) 0.015(7) F13E 0.068(3) 0.071(3) 0.042(3) -0.001(2) -0.016(2) 0.007(2) F14E 0.068(3) 0.071(3) 0.042(3) -0.001(2) -0.016(2) 0.007(2) F15E 0.068(3) 0.071(3) 0.042(3) -0.001(2) -0.016(2) 0.007(2) Re1 0.02669(15) 0.02518(15) 0.02402(16) 0.00149(13) -0.00169(11) -0.00113(12) N1 0.025(3) 0.014(3) 0.029(4) 0.003(2) 0.003(3) -0.003(2) C1 0.045(5) 0.046(5) 0.041(5) 0.004(4) -0.003(4) 0.001(4) Re2 0.03022(15) 0.02688(15) 0.02385(17) 0.00073(13) -0.00134(12) -0.00398(12) N2 0.027(3) 0.029(3) 0.037(4) 0.008(3) -0.002(3) -0.003(3) C2 0.050(6) 0.064(6) 0.079(8) 0.021(6) 0.025(5) -0.010(5) N3 0.030(3) 0.024(3) 0.032(4) 0.002(3) 0.007(3) 0.001(3) C3 0.036(4) 0.038(4) 0.039(5) 0.011(4) -0.008(4) -0.008(4) N4 0.035(3) 0.040(4) 0.017(3) -0.002(3) -0.006(3) -0.003(3) C4 0.048(5) 0.067(6) 0.039(6) 0.010(5) -0.017(4) -0.004(5) N5 0.024(3) 0.027(3) 0.032(4) 0.000(3) 0.000(3) -0.003(3) C5 0.028(4) 0.022(4) 0.037(5) -0.002(3) 0.007(3) -0.002(3) N6 0.037(3) 0.017(3) 0.038(4) 0.003(3) 0.016(3) -0.013(3) C6 0.036(4) 0.036(4) 0.034(5) 0.005(4) -0.009(4) 0.008(3) N7 0.043(4) 0.031(4) 0.025(4) 0.004(3) -0.001(3) -0.007(3) C7 0.045(5) 0.034(4) 0.029(5) -0.007(4) 0.008(4) -0.005(4) N8 0.038(4) 0.034(4) 0.030(4) 0.005(3) 0.002(3) -0.002(3) C8 0.090(7) 0.030(4) 0.032(5) -0.018(4) 0.009(5) -0.021(4) N9 0.038(4) 0.027(3) 0.031(4) 0.004(3) 0.000(3) 0.000(3) C9 0.032(4) 0.033(4) 0.032(5) 0.013(4) -0.001(3) 0.005(3) N10 0.039(4) 0.026(3) 0.028(4) 0.001(3) 0.002(3) -0.001(3) C10 0.052(5) 0.040(5) 0.040(5) 0.004(4) 0.014(4) 0.015(4) C11 0.070(7) 0.069(7) 0.054(7) -0.006(6) 0.014(6) -0.016(6) C12 0.162(14) 0.126(12) 0.067(10) 0.007(8) 0.053(10) -0.059(11) C13 0.042(5) 0.027(4) 0.029(5) 0.011(3) 0.000(3) 0.000(3) C14 0.049(5) 0.032(4) 0.035(5) 0.007(4) 0.004(4) 0.003(4) C15 0.041(5) 0.034(4) 0.032(5) -0.007(4) -0.002(4) -0.008(4) C16 0.037(5) 0.042(5) 0.054(6) -0.005(4) 0.000(4) 0.005(4) C17 0.046(5) 0.026(4) 0.030(5) 0.006(4) -0.002(4) 0.001(3) C18 0.099(8) 0.047(6) 0.031(6) -0.010(4) -0.015(5) 0.005(5) C19 0.042(4) 0.021(4) 0.018(4) 0.005(3) 0.000(3) -0.001(3) C20 0.050(5) 0.038(5) 0.040(5) 0.009(4) -0.018(4) -0.014(4) F1A 0.021(2) 0.039(2) 0.057(3) 0.002(2) -0.001(2) -0.0047(18) C1A 0.019(3) 0.019(3) 0.024(4) -0.002(3) 0.006(3) 0.002(3) B1A 0.020(4) 0.020(4) 0.020(4) 0.000(3) 0.006(3) 0.000(3) F2A 0.074(3) 0.049(3) 0.029(3) 0.007(2) 0.010(2) -0.032(3) C2A 0.021(3) 0.027(4) 0.019(4) -0.002(3) 0.003(3) -0.002(3) F3A 0.033(2) 0.027(2) 0.062(3) -0.017(2) 0.007(2) -0.0003(18) C3A 0.016(3) 0.022(3) 0.026(4) -0.003(3) 0.003(3) 0.000(3) F4A 0.093(4) 0.050(3) 0.024(3) 0.012(2) -0.019(3) -0.010(3) C4A 0.028(4) 0.030(4) 0.025(4) 0.005(3) 0.009(3) 0.004(3) F5A 0.055(4) 0.152(6) 0.041(4) 0.006(4) -0.012(3) -0.050(4) C5A 0.024(3) 0.026(4) 0.020(4) 0.001(3) -0.001(3) 0.001(3) F6A 0.119(5) 0.056(4) 0.040(4) -0.019(3) -0.024(3) 0.020(3) C6A 0.017(3) 0.023(3) 0.029(4) 0.002(3) 0.007(3) -0.001(3) F7A 0.045(3) 0.035(3) 0.068(4) 0.006(2) 0.028(3) 0.001(2) C7A 0.026(4) 0.026(4) 0.027(4) 0.001(3) 0.005(3) 0.000(3) F8A 0.046(3) 0.081(4) 0.054(4) -0.036(3) 0.027(3) -0.019(3) C8A 0.042(5) 0.044(5) 0.028(5) -0.002(4) -0.012(4) -0.008(4) F9A 0.017(2) 0.083(4) 0.072(4) 0.025(3) 0.001(2) 0.006(2) C9A 0.020(3) 0.024(4) 0.021(4) -0.003(3) -0.004(3) -0.002(3) F10A 0.042(3) 0.037(3) 0.070(4) 0.020(3) 0.008(2) 0.016(2) C10A 0.023(3) 0.022(3) 0.022(4) -0.005(3) 0.000(3) -0.001(3) F11A 0.039(3) 0.045(3) 0.049(3) 0.019(2) -0.004(2) -0.012(2) C11A 0.017(3) 0.032(4) 0.024(4) -0.001(3) 0.001(3) -0.004(3) F12A 0.127(5) 0.042(3) 0.028(3) 0.010(2) 0.016(3) 0.022(3) C12A 0.024(3) 0.026(4) 0.025(4) -0.012(3) -0.006(3) 0.005(3) C13A 0.024(3) 0.026(4) 0.014(4) -0.004(3) -0.006(3) 0.000(3) C14A 0.020(3) 0.027(4) 0.027(4) -0.009(3) 0.000(3) -0.002(3) C15A 0.020(3) 0.030(4) 0.036(5) -0.005(3) 0.002(3) -0.001(3) F16A 0.051(3) 0.037(3) 0.074(4) 0.024(3) 0.017(3) 0.013(2) C16A 0.039(4) 0.038(4) 0.014(4) -0.005(3) 0.000(3) 0.008(3) F17A 0.068(3) 0.060(3) 0.046(3) -0.006(3) 0.025(3) 0.026(3) C17A 0.025(3) 0.020(3) 0.019(4) -0.003(3) 0.004(3) -0.004(3) F18A 0.036(3) 0.048(3) 0.081(4) -0.017(3) -0.007(3) 0.017(2) C18A 0.028(4) 0.022(4) 0.027(4) -0.005(3) -0.002(3) 0.006(3) C19A 0.047(5) 0.036(4) 0.025(5) -0.003(4) -0.001(4) 0.011(4) C20A 0.043(4) 0.031(4) 0.030(5) -0.004(3) 0.006(4) 0.001(3) C21A 0.030(4) 0.022(4) 0.025(4) -0.002(3) 0.008(3) 0.001(3) F22A 0.031(2) 0.074(4) 0.060(4) -0.036(3) 0.001(2) -0.012(2) C22A 0.031(4) 0.020(3) 0.020(4) 0.004(3) 0.007(3) -0.002(3) F23A 0.079(4) 0.026(2) 0.053(3) -0.007(2) 0.017(3) -0.009(2) F24A 0.037(2) 0.039(3) 0.031(3) -0.012(2) 0.007(2) -0.0073(19) C24A 0.036(4) 0.031(4) 0.032(5) 0.005(3) 0.010(4) 0.005(3) C25A 0.020(3) 0.025(4) 0.021(4) 0.005(3) 0.001(3) 0.001(3) C26A 0.021(3) 0.033(4) 0.023(4) 0.001(3) -0.001(3) -0.002(3) C27A 0.021(3) 0.035(4) 0.029(4) 0.004(3) 0.007(3) -0.006(3) C28A 0.026(4) 0.027(4) 0.025(4) -0.002(3) 0.004(3) -0.006(3) C29A 0.025(3) 0.023(3) 0.025(4) -0.004(3) 0.003(3) 0.000(3) C30A 0.021(3) 0.025(4) 0.027(4) 0.001(3) 0.000(3) 0.000(3) C32A 0.027(4) 0.035(4) 0.035(5) -0.001(4) 0.005(3) -0.003(3) F1B 0.066(4) 0.033(3) 0.080(4) -0.002(3) -0.013(3) -0.015(2) C1B 0.025(3) 0.025(4) 0.018(4) 0.000(3) -0.002(3) -0.006(3) B1B 0.026(4) 0.020(4) 0.022(4) 0.001(3) 0.002(3) -0.005(3) F2B 0.063(4) 0.042(3) 0.080(4) 0.027(3) -0.007(3) 0.003(3) C2B 0.034(4) 0.027(4) 0.023(4) 0.000(3) 0.003(3) -0.005(3) F3B 0.183(7) 0.037(3) 0.093(5) 0.003(3) 0.104(5) -0.013(4) C3B 0.039(4) 0.023(4) 0.017(4) 0.002(3) 0.002(3) -0.007(3) F4B 0.033(2) 0.048(3) 0.054(3) -0.008(2) 0.019(2) -0.006(2) C4B 0.028(4) 0.035(4) 0.019(4) -0.002(3) 0.003(3) -0.005(3) F5B 0.042(3) 0.041(3) 0.035(3) -0.010(2) 0.004(2) 0.005(2) C5B 0.026(4) 0.020(4) 0.025(4) -0.006(3) 0.000(3) -0.004(3) F6B 0.040(3) 0.036(2) 0.039(3) 0.002(2) 0.004(2) 0.010(2) C6B 0.024(3) 0.027(4) 0.021(4) 0.001(3) 0.000(3) -0.005(3) F7B 0.057(3) 0.046(3) 0.023(3) 0.008(2) -0.009(2) -0.017(2) C7B 0.044(5) 0.035(4) 0.035(5) -0.001(4) 0.015(4) -0.008(4) F8B 0.058(3) 0.024(2) 0.035(3) -0.006(2) -0.008(2) -0.002(2) C8B 0.024(4) 0.040(4) 0.024(4) 0.001(3) 0.005(3) 0.001(3) F9B 0.027(2) 0.074(3) 0.047(3) -0.020(3) -0.007(2) -0.002(2) C9B 0.021(3) 0.021(3) 0.026(4) 0.001(3) 0.002(3) 0.001(3) F10B 0.049(3) 0.021(2) 0.033(3) -0.0002(18) 0.013(2) 0.0000(18) C10B 0.022(3) 0.022(3) 0.026(4) -0.003(3) 0.006(3) -0.001(3) F11B 0.048(3) 0.043(3) 0.043(3) 0.012(2) 0.027(2) 0.008(2) C11B 0.022(3) 0.023(3) 0.021(4) -0.005(3) 0.004(3) -0.001(3) F12B 0.061(3) 0.042(3) 0.025(3) 0.007(2) -0.003(2) -0.013(2) C12B 0.026(4) 0.019(3) 0.029(4) -0.007(3) 0.011(3) -0.002(3) F13B 0.082(5) 0.049(3) 0.062(3) 0.003(3) 0.040(3) 0.010(3) C13B 0.022(3) 0.019(3) 0.024(4) 0.001(3) 0.008(3) 0.002(3) F14B 0.082(5) 0.049(3) 0.062(3) 0.003(3) 0.040(3) 0.010(3) C14B 0.027(4) 0.027(4) 0.015(4) 0.001(3) 0.004(3) 0.002(3) F15B 0.082(5) 0.049(3) 0.062(3) 0.003(3) 0.040(3) 0.010(3) C15B 0.037(4) 0.029(4) 0.022(4) -0.003(3) -0.001(3) -0.006(3) F16B 0.095(5) 0.082(4) 0.042(4) 0.015(3) 0.007(3) 0.043(4) C16B 0.029(4) 0.020(4) 0.028(4) -0.001(3) 0.002(3) -0.001(3) F17B 0.089(5) 0.065(4) 0.101(6) 0.047(4) -0.012(4) -0.004(3) C17B 0.025(4) 0.018(3) 0.037(5) 0.003(3) 0.010(3) -0.003(3) F18B 0.057(3) 0.088(4) 0.055(4) 0.009(3) -0.002(3) 0.038(3) C18B 0.032(4) 0.021(4) 0.035(5) -0.002(3) 0.009(3) 0.000(3) C19B 0.040(4) 0.024(4) 0.038(5) 0.000(3) 0.015(4) 0.004(3) C20B 0.031(4) 0.031(4) 0.058(6) -0.002(4) 0.006(4) 0.003(3) C21B 0.029(4) 0.029(4) 0.043(5) -0.003(4) 0.001(4) 0.001(3) C22B 0.030(4) 0.032(4) 0.034(5) -0.006(3) 0.008(3) -0.002(3) C23B 0.055(7) 0.031(5) 0.063(7) 0.004(5) 0.028(5) 0.003(4) C24B 0.042(5) 0.051(6) 0.055(7) 0.010(5) -0.002(5) 0.009(4) C25B 0.031(4) 0.028(4) 0.024(4) -0.002(3) 0.010(3) -0.010(3) C26B 0.043(4) 0.028(4) 0.021(4) 0.000(3) 0.004(3) -0.010(3) C27B 0.044(5) 0.031(4) 0.026(4) -0.004(3) -0.005(3) -0.012(4) C28B 0.040(4) 0.042(5) 0.031(5) 0.003(4) -0.008(4) -0.013(4) C29B 0.025(4) 0.037(4) 0.031(5) 0.007(3) 0.001(3) -0.008(3) C30B 0.029(4) 0.031(4) 0.028(4) 0.004(3) 0.004(3) -0.003(3) C32B 0.035(4) 0.043(5) 0.043(6) 0.017(4) -0.004(4) -0.005(4) F24B 0.041(3) 0.048(3) 0.086(5) -0.004(3) -0.002(3) 0.008(2) F23B 0.048(3) 0.072(4) 0.107(5) 0.057(4) 0.015(3) 0.009(3) F22B 0.025(2) 0.061(3) 0.067(4) 0.008(3) -0.006(2) -0.007(2) F1C 0.095(5) 0.117(6) 0.083(5) -0.056(4) -0.052(4) 0.057(4) C1C 0.017(3) 0.025(3) 0.027(4) 0.002(3) 0.007(3) -0.001(3) B1C 0.020(4) 0.022(4) 0.024(4) 0.003(3) 0.002(3) 0.001(3) F2C 0.063(4) 0.096(5) 0.071(4) 0.054(4) -0.018(3) -0.023(3) C2C 0.024(3) 0.023(4) 0.020(4) -0.002(3) 0.004(3) -0.004(3) F3C 0.034(3) 0.074(4) 0.069(4) 0.023(3) -0.009(3) 0.004(3) C3C 0.025(4) 0.023(4) 0.037(5) -0.001(3) 0.001(3) 0.006(3) F4C 0.079(4) 0.081(4) 0.092(5) -0.040(4) 0.032(4) 0.004(4) C4C 0.028(4) 0.056(5) 0.042(6) -0.001(4) 0.002(4) 0.010(4) F5C 0.052(3) 0.091(4) 0.059(4) 0.001(3) 0.033(3) 0.015(3) C5C 0.022(4) 0.058(5) 0.038(5) -0.002(4) 0.008(3) 0.006(4) F6C 0.064(4) 0.175(7) 0.037(4) -0.023(4) 0.007(3) 0.028(4) C6C 0.019(3) 0.050(5) 0.029(4) 0.004(4) -0.002(3) 0.002(3) C7C 0.032(4) 0.047(5) 0.047(6) -0.003(4) -0.007(4) 0.009(4) C8C 0.035(5) 0.086(8) 0.054(7) -0.009(6) 0.009(5) 0.011(5) C9C 0.026(3) 0.032(4) 0.022(4) 0.007(3) 0.009(3) 0.004(3) F10C 0.038(2) 0.051(3) 0.032(3) 0.018(2) 0.002(2) 0.004(2) C10C 0.032(4) 0.028(4) 0.029(4) 0.001(3) 0.004(3) 0.005(3) F11C 0.022(2) 0.063(3) 0.056(3) 0.025(3) 0.005(2) 0.002(2) C11C 0.034(4) 0.032(4) 0.036(5) -0.001(4) 0.001(4) 0.001(3) F12C 0.050(3) 0.039(3) 0.050(3) -0.005(2) -0.012(2) 0.014(2) C12C 0.030(4) 0.039(4) 0.035(5) -0.002(4) -0.009(3) -0.003(3) F13C 0.137(6) 0.100(5) 0.047(4) 0.032(4) -0.008(4) -0.059(5) C13C 0.023(3) 0.028(4) 0.026(4) 0.005(3) 0.003(3) 0.000(3) F14C 0.076(4) 0.082(5) 0.121(6) 0.073(4) 0.013(4) 0.024(4) C14C 0.023(3) 0.023(3) 0.028(4) 0.002(3) 0.005(3) -0.001(3) F15C 0.044(3) 0.093(4) 0.083(5) 0.057(4) 0.015(3) -0.007(3) F16C 0.082(4) 0.063(4) 0.081(5) -0.033(3) -0.007(3) 0.021(3) C16C 0.032(4) 0.032(4) 0.030(5) 0.004(3) 0.006(3) 0.000(3) F17C 0.058(4) 0.088(5) 0.091(5) -0.028(4) -0.016(3) -0.017(3) C17C 0.017(3) 0.032(4) 0.025(4) 0.001(3) -0.001(3) 0.001(3) F18C 0.144(6) 0.063(4) 0.053(4) -0.011(3) -0.008(4) -0.035(4) C18C 0.023(4) 0.035(4) 0.031(5) 0.007(3) 0.000(3) -0.001(3) C19C 0.022(4) 0.040(5) 0.055(6) 0.018(4) 0.001(4) -0.007(3) C20C 0.050(5) 0.028(4) 0.043(6) 0.008(4) -0.007(4) 0.000(4) C21C 0.039(4) 0.022(4) 0.041(5) 0.001(4) -0.008(4) -0.003(3) F22C 0.092(5) 0.047(3) 0.080(5) 0.022(3) -0.011(4) 0.000(3) C22C 0.029(4) 0.025(4) 0.030(4) 0.003(3) 0.002(3) 0.004(3) F23C 0.089(5) 0.070(4) 0.222(9) 0.081(5) 0.096(6) 0.015(4) C23C 0.042(5) 0.054(6) 0.063(7) 0.025(5) 0.005(5) -0.020(4) F24C 0.147(6) 0.042(3) 0.077(5) 0.003(3) 0.025(4) -0.024(4) C24C 0.071(7) 0.030(5) 0.057(7) -0.002(5) 0.001(5) -0.009(4) C25C 0.021(3) 0.027(4) 0.023(4) -0.001(3) 0.004(3) -0.002(3) C26C 0.020(3) 0.034(4) 0.023(4) 0.001(3) 0.004(3) -0.003(3) C27C 0.026(4) 0.043(5) 0.024(4) -0.005(4) 0.003(3) -0.001(3) C28C 0.028(4) 0.059(6) 0.031(5) 0.000(4) 0.007(3) -0.014(4) C29C 0.022(4) 0.039(4) 0.033(5) 0.010(4) 0.001(3) -0.014(3) C30C 0.025(4) 0.030(4) 0.037(5) 0.001(3) 0.006(3) 0.001(3) C32C 0.052(6) 0.055(6) 0.040(6) 0.015(5) 0.009(5) -0.014(5) C1D 0.022(3) 0.024(4) 0.021(4) 0.005(3) 0.004(3) 0.002(3) B1D 0.024(4) 0.022(4) 0.017(4) 0.002(3) -0.001(3) 0.003(3) C2D 0.028(4) 0.023(4) 0.023(4) 0.005(3) 0.009(3) 0.000(3) C3D 0.025(4) 0.024(4) 0.030(4) 0.003(3) 0.006(3) 0.001(3) F4D 0.062(3) 0.043(3) 0.031(3) -0.004(2) 0.002(2) 0.003(2) C4D 0.023(4) 0.039(4) 0.042(5) 0.015(4) 0.015(3) 0.005(3) F5D 0.033(2) 0.046(3) 0.083(4) -0.026(3) 0.024(3) 0.000(2) C5D 0.019(3) 0.035(4) 0.039(5) -0.001(4) 0.008(3) 0.000(3) F6D 0.038(2) 0.032(2) 0.044(3) -0.002(2) 0.007(2) -0.0057(19) C6D 0.020(3) 0.034(4) 0.031(4) -0.002(3) 0.002(3) -0.001(3) C7D 0.035(4) 0.024(4) 0.046(6) -0.004(4) 0.010(4) 0.006(3) C9D 0.022(3) 0.020(3) 0.024(4) 0.005(3) 0.002(3) 0.005(3) C10D 0.027(4) 0.026(4) 0.021(4) 0.002(3) 0.001(3) 0.002(3) C11D 0.029(4) 0.025(4) 0.029(4) -0.001(3) -0.011(3) 0.003(3) C12D 0.049(5) 0.021(4) 0.029(5) -0.004(3) -0.005(4) 0.002(3) C13D 0.048(5) 0.028(4) 0.029(5) -0.001(3) 0.009(4) 0.004(3) C14D 0.032(4) 0.031(4) 0.018(4) 0.006(3) 0.003(3) 0.004(3) C15D 0.037(4) 0.034(4) 0.030(5) -0.001(4) -0.007(4) -0.005(3) C16D 0.065(6) 0.049(6) 0.030(5) -0.002(4) 0.014(4) -0.001(5) C17D 0.024(3) 0.020(3) 0.017(4) 0.003(3) 0.003(3) 0.005(3) C18D 0.026(4) 0.020(4) 0.038(5) 0.006(3) 0.003(3) 0.001(3) C19D 0.032(4) 0.027(4) 0.029(4) 0.010(3) 0.010(3) 0.002(3) C20D 0.026(4) 0.032(4) 0.035(5) 0.001(3) 0.008(3) -0.003(3) C21D 0.019(3) 0.020(3) 0.030(4) -0.001(3) 0.003(3) 0.001(3) C23D 0.024(3) 0.023(4) 0.026(4) 0.001(3) 0.008(3) 0.009(3) F10D 0.105(5) 0.154(7) 0.069(5) -0.048(5) 0.061(4) -0.071(5) F11D 0.103(5) 0.104(5) 0.034(3) 0.028(3) 0.026(3) 0.049(4) C24D 0.021(4) 0.035(4) 0.040(5) -0.006(4) -0.002(3) -0.001(3) F12D 0.118(5) 0.059(3) 0.049(4) 0.004(3) 0.038(3) 0.034(3) C25D 0.022(3) 0.025(4) 0.023(4) 0.000(3) 0.007(3) -0.003(3) C26D 0.020(3) 0.024(3) 0.016(4) -0.005(3) -0.001(3) -0.003(3) F9D 0.060(3) 0.051(3) 0.045(3) -0.003(3) -0.015(3) -0.018(3) C27D 0.018(3) 0.023(4) 0.031(4) 0.002(3) 0.004(3) 0.000(3) F7D 0.050(3) 0.028(2) 0.046(3) 0.010(2) -0.001(2) -0.003(2) C28D 0.023(3) 0.031(4) 0.028(4) 0.007(3) 0.000(3) -0.007(3) F8D 0.035(3) 0.045(3) 0.073(4) -0.012(3) 0.011(3) -0.013(2) C29D 0.023(3) 0.029(4) 0.021(4) -0.003(3) 0.002(3) -0.001(3) C30D 0.022(3) 0.027(4) 0.022(4) 0.000(3) 0.007(3) -0.005(3) C31D 0.026(4) 0.028(4) 0.033(5) 0.004(3) -0.008(3) -0.002(3) C32D 0.038(5) 0.052(5) 0.027(5) 0.008(4) -0.002(4) -0.006(4) F21D 0.024(2) 0.026(2) 0.048(3) -0.003(2) 0.0000(19) -0.0012(17) F20D 0.078(4) 0.037(3) 0.034(3) 0.005(2) -0.010(2) 0.020(2) F19D 0.021(2) 0.033(2) 0.080(4) -0.006(2) 0.005(2) 0.0017(18) F23D 0.072(4) 0.057(3) 0.038(3) 0.013(2) 0.032(3) -0.001(3) F22D 0.076(4) 0.149(6) 0.042(4) -0.040(4) 0.019(3) -0.066(4) F24D 0.130(6) 0.090(4) 0.032(3) -0.001(3) 0.018(3) 0.063(4) F17D 0.030(2) 0.034(3) 0.061(3) 0.003(2) -0.008(2) 0.0052(19) F18D 0.035(3) 0.100(4) 0.041(3) -0.019(3) -0.007(2) 0.008(3) F16D 0.023(2) 0.044(3) 0.091(4) 0.011(3) -0.006(2) -0.008(2) Cl1S 0.092(2) 0.177(4) 0.067(2) 0.030(2) -0.0190(18) -0.071(3) N1S 0.052(5) 0.063(6) 0.090(8) 0.022(5) 0.010(5) 0.013(4) C1S 0.057(6) 0.040(5) 0.036(5) 0.004(4) 0.010(4) -0.010(4) Cl2S 0.094(2) 0.0642(16) 0.0569(18) -0.0095(13) 0.0234(15) 0.0206(15) C2S 0.043(5) 0.058(6) 0.042(6) 0.009(4) 0.018(4) 0.013(4) Cl3S 0.104(3) 0.068(2) 0.167(4) -0.021(2) -0.032(3) -0.0178(19) C3S 0.062(6) 0.065(7) 0.052(7) -0.010(5) -0.003(5) -0.005(5) Cl4S 0.100(3) 0.199(5) 0.066(2) 0.034(3) -0.016(2) 0.011(3) C4S 0.065(7) 0.074(8) 0.084(9) 0.004(7) -0.022(6) 0.003(6) Cl5S 0.141(4) 0.210(6) 0.153(5) 0.073(4) -0.005(4) -0.042(4) C5S 0.119(10) 0.069(7) 0.035(6) 0.001(5) -0.003(6) -0.015(7) Cl6S 0.170(5) 0.193(5) 0.115(4) 0.042(4) 0.005(3) -0.033(4) Cl7S 0.120(3) 0.0623(19) 0.133(3) -0.025(2) -0.055(2) 0.0411(19) Cl8S 0.162(3) 0.0450(16) 0.109(3) 0.0088(17) -0.074(3) 0.0013(19) C6S 0.32(3) 0.152(17) 0.30(3) 0.020(19) 0.28(3) 0.074(19) C22E 0.039(5) 0.047(5) 0.052(6) 0.017(5) 0.006(4) -0.010(4) F15F 0.072(3) 0.060(4) 0.068(4) 0.038(3) -0.005(3) -0.017(3) F14F 0.072(3) 0.060(4) 0.068(4) 0.038(3) -0.005(3) -0.017(3) F13F 0.072(3) 0.060(4) 0.068(4) 0.038(3) -0.005(3) -0.017(3) C23F 0.055(7) 0.031(5) 0.063(7) 0.004(5) 0.028(5) 0.003(4) F13G 0.082(5) 0.049(3) 0.062(3) 0.003(3) 0.040(3) 0.010(3) F14G 0.082(5) 0.049(3) 0.062(3) 0.003(3) 0.040(3) 0.010(3) F15G 0.082(5) 0.049(3) 0.062(3) 0.003(3) 0.040(3) 0.010(3) _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 C8D F3D 1.310(16) . ? C8D F1D 1.323(16) . ? C8D F2D 1.371(17) . ? C8D C5D 1.498(11) . ? C8E F2E 1.321(14) . ? C8E F3E 1.371(12) . ? C8E F1E 1.374(14) . ? C8E C5D 1.498(11) . ? C15C F9C 1.322(17) . ? C15C F8C 1.349(17) . ? C15C F7C 1.354(17) . ? C15C C11C 1.48(3) . ? C15E F9E 1.326(17) . ? C15E F7E 1.343(17) . ? C15E F8E 1.361(17) . ? C15E C11C 1.48(3) . ? C22D F15D 1.309(16) . ? C22D F14D 1.32(2) . ? C22D F13D 1.355(16) . ? C22D C19D 1.489(12) . ? C31A F20A 1.326(15) . ? C31A F19A 1.345(15) . ? C31A F21A 1.358(15) . ? C31A C27A 1.498(10) . ? C31E F20E 1.336(15) . ? C31E F19E 1.338(15) . ? C31E F21E 1.367(15) . ? C31E C27A 1.498(10) . ? C31B F20B 1.34(2) . ? C31B F19B 1.34(2) . ? C31B F21B 1.34(2) . ? C31B C27B 1.45(4) . ? C31F F20F 1.28(3) . ? C31F F21F 1.34(3) . ? C31F C27B 1.46(4) . ? C31F F19F 1.47(3) . ? C31C F20C 1.322(9) . ? C31C F19C 1.344(8) . ? C31C F21C 1.351(9) . ? C31C C27C 1.496(11) . ? C23A F13A 1.338(16) . ? C23A F14A 1.336(16) . ? C23A F15A 1.362(16) . ? C23A C19A 1.496(15) . ? C23E F13E 1.336(16) . ? C23E F15E 1.347(16) . ? C23E F14E 1.354(16) . ? C23E C19A 1.496(15) . ? Re1 N4 2.045(6) . ? Re1 N2 2.058(6) . ? Re1 N5 2.060(6) . ? Re1 N3 2.062(7) . ? Re1 Re2 2.2628(4) . ? Re1 N1 2.410(5) . ? N1 C1 1.169(10) . ? C1 C2 1.455(12) . ? Re2 N9 2.052(7) . ? Re2 N10 2.054(7) . ? Re2 N7 2.070(7) . ? Re2 N8 2.075(7) . ? Re2 N6 2.375(5) . ? N2 C3 1.124(9) . ? N3 C5 1.131(9) . ? C3 C4 1.463(11) . ? N4 C7 1.136(9) . ? N5 C9 1.122(9) . ? C5 C6 1.458(11) . ? N6 C11 1.172(11) . ? N7 C13 1.136(9) . ? C7 C8 1.457(11) . ? N8 C15 1.129(9) . ? N9 C17 1.144(9) . ? C9 C10 1.478(11) . ? N10 C19 1.138(9) . ? C11 C12 1.464(14) . ? C13 C14 1.449(10) . ? C15 C16 1.458(11) . ? C17 C18 1.440(12) . ? C19 C20 1.477(10) . ? F1A C7A 1.354(8) . ? C1A C6A 1.381(9) . ? C1A C2A 1.404(9) . ? C1A B1A 1.644(10) . ? B1A C25A 1.634(10) . ? B1A C17A 1.642(10) . ? B1A C9A 1.650(10) . ? F2A C7A 1.328(8) . ? C2A C3A 1.369(9) . ? F3A C7A 1.334(8) . ? C3A C4A 1.377(10) . ? C3A C7A 1.496(9) . ? F4A C8A 1.318(9) . ? C4A C5A 1.387(9) . ? F5A C8A 1.327(9) . ? C5A C6A 1.405(9) . ? C5A C8A 1.490(10) . ? F6A C8A 1.336(10) . ? F7A C15A 1.333(8) . ? F8A C15A 1.339(8) . ? F9A C15A 1.329(8) . ? C9A C10A 1.392(9) . ? C9A C14A 1.399(9) . ? F10A C16A 1.336(8) . ? C10A C11A 1.406(9) . ? F11A C16A 1.329(9) . ? C11A C12A 1.387(10) . ? C11A C15A 1.487(9) . ? F12A C16A 1.327(8) . ? C12A C13A 1.375(9) . ? C13A C14A 1.380(9) . ? C13A C16A 1.499(10) . ? F16A C24A 1.356(8) . ? F17A C24A 1.347(9) . ? C17A C18A 1.382(9) . ? C17A C22A 1.411(9) . ? F18A C24A 1.327(9) . ? C18A C19A 1.405(10) . ? C19A C20A 1.385(10) . ? C20A C21A 1.382(10) . ? C21A C22A 1.402(9) . ? C21A C24A 1.481(10) . ? F22A C32A 1.337(9) . ? F23A C32A 1.350(9) . ? F24A C32A 1.343(8) . ? C25A C26A 1.385(9) . ? C25A C30A 1.405(9) . ? C26A C27A 1.393(9) . ? C27A C28A 1.362(10) . ? C28A C29A 1.393(9) . ? C29A C30A 1.384(9) . ? C29A C32A 1.483(10) . ? F1B C7B 1.327(10) . ? C1B C2B 1.396(9) . ? C1B C6B 1.402(9) . ? C1B B1B 1.652(10) . ? B1B C25B 1.626(11) . ? B1B C17B 1.632(10) . ? B1B C9B 1.634(10) . ? F2B C7B 1.329(9) . ? C2B C3B 1.375(9) . ? F3B C7B 1.317(9) . ? C3B C4B 1.383(10) . ? C3B C7B 1.486(10) . ? F4B C8B 1.348(8) . ? C4B C5B 1.393(9) . ? F5B C8B 1.357(8) . ? C5B C6B 1.374(9) . ? C5B C8B 1.496(9) . ? F6B C8B 1.340(8) . ? F7B C15B 1.359(8) . ? F8B C15B 1.353(8) . ? F9B C15B 1.358(8) . ? C9B C14B 1.399(9) . ? C9B C10B 1.396(9) . ? F10B C16B 1.350(8) . ? C10B C11B 1.396(9) . ? F11B C16B 1.340(8) . ? C11B C12B 1.379(9) . ? C11B C15B 1.479(10) . ? F12B C16B 1.338(8) . ? C12B C13B 1.382(10) . ? F13B C23B 1.321(16) . ? C13B C14B 1.399(9) . ? C13B C16B 1.484(9) . ? F14B C23B 1.352(17) . ? F15B C23B 1.352(16) . ? F16B C24B 1.331(11) . ? F17B C24B 1.355(10) . ? C17B C22B 1.396(10) . ? C17B C18B 1.399(10) . ? F18B C24B 1.314(9) . ? C18B C19B 1.398(10) . ? C19B C20B 1.397(11) . ? C19B C23F 1.493(15) . ? C19B C23B 1.496(15) . ? C20B C21B 1.372(11) . ? C21B C22B 1.399(10) . ? C21B C24B 1.500(12) . ? C25B C30B 1.395(10) . ? C25B C26B 1.389(10) . ? C26B C27B 1.410(10) . ? C27B C28B 1.393(11) . ? C28B C29B 1.386(11) . ? C29B C30B 1.393(10) . ? C29B C32B 1.461(11) . ? C32B F23B 1.319(9) . ? C32B F22B 1.339(9) . ? C32B F24B 1.392(10) . ? F1C C7C 1.312(10) . ? C1C C2C 1.379(10) . ? C1C C6C 1.390(10) . ? C1C B1C 1.649(9) . ? B1C C9C 1.608(11) . ? B1C C17C 1.644(10) . ? B1C C25C 1.633(10) . ? F2C C7C 1.308(10) . ? C2C C3C 1.392(9) . ? F3C C7C 1.351(9) . ? C3C C4C 1.356(11) . ? C3C C7C 1.497(11) . ? F4C C8C 1.369(12) . ? C4C C5C 1.369(11) . ? F5C C8C 1.345(11) . ? C5C C6C 1.407(10) . ? C5C C8C 1.503(12) . ? F6C C8C 1.306(11) . ? C9C C14C 1.405(9) . ? C9C C10C 1.425(10) . ? F10C C16C 1.333(8) . ? C10C C11C 1.391(11) . ? F11C C16C 1.332(8) . ? C11C C12C 1.381(10) . ? F12C C16C 1.339(9) . ? C12C C13C 1.384(10) . ? F13C C23C 1.345(11) . ? C13C C14C 1.382(10) . ? C13C C16C 1.505(10) . ? F14C C23C 1.342(11) . ? F15C C23C 1.326(9) . ? F16C C24C 1.340(10) . ? F17C C24C 1.357(11) . ? C17C C18C 1.395(10) . ? C17C C22C 1.405(10) . ? F18C C24C 1.306(11) . ? C18C C19C 1.389(10) . ? C19C C20C 1.389(12) . ? C19C C23C 1.473(12) . ? C20C C21C 1.379(11) . ? C21C C22C 1.390(10) . ? C21C C24C 1.503(12) . ? F22C C32C 1.335(11) . ? F23C C32C 1.282(10) . ? F24C C32C 1.374(11) . ? C25C C30C 1.401(10) . ? C25C C26C 1.400(9) . ? C26C C27C 1.390(10) . ? C27C C28C 1.363(11) . ? C28C C29C 1.384(11) . ? C29C C30C 1.378(10) . ? C29C C32C 1.478(11) . ? C1D C2D 1.390(9) . ? C1D C6D 1.387(9) . ? C1D B1D 1.642(10) . ? B1D C9D 1.622(10) . ? B1D C25D 1.641(10) . ? B1D C17D 1.647(10) . ? C2D C3D 1.400(9) . ? C3D C4D 1.368(10) . ? C3D C7D 1.505(10) . ? F4D C7D 1.345(9) . ? C4D C5D 1.388(11) . ? F5D C7D 1.327(8) . ? C5D C6D 1.385(9) . ? F6D C7D 1.351(8) . ? C9D C14D 1.413(9) . ? C9D C10D 1.420(9) . ? C10D C11D 1.392(10) . ? C11D C12D 1.382(11) . ? C11D C15D 1.478(10) . ? C12D C13D 1.372(11) . ? C13D C14D 1.403(10) . ? C13D C16D 1.481(11) . ? C15D F8D 1.337(9) . ? C15D F7D 1.343(9) . ? C15D F9D 1.343(9) . ? C16D F10D 1.281(10) . ? C16D F12D 1.345(10) . ? C16D F11D 1.344(11) . ? C17D C23D 1.403(9) . ? C17D C18D 1.409(9) . ? C18D C19D 1.384(9) . ? C19D C20D 1.382(10) . ? C19D C22E 1.469(14) . ? C20D C21D 1.386(10) . ? C21D C23D 1.384(9) . ? C21D C24D 1.491(10) . ? C24D F16D 1.329(8) . ? C24D F17D 1.345(8) . ? C24D F18D 1.348(9) . ? C25D C30D 1.400(9) . ? C25D C26D 1.415(9) . ? C26D C27D 1.393(9) . ? C27D C28D 1.367(10) . ? C27D C31D 1.500(9) . ? C28D C29D 1.408(10) . ? C29D C30D 1.372(10) . ? C29D C32D 1.475(10) . ? C31D F20D 1.317(8) . ? C31D F21D 1.345(8) . ? C31D F19D 1.354(8) . ? C32D F24D 1.314(9) . ? C32D F23D 1.332(9) . ? C32D F22D 1.347(9) . ? Cl1S C3S 1.728(9) . ? N1S C1S 1.133(11) . ? C1S C2S 1.449(12) . ? Cl2S C3S 1.737(9) . ? Cl3S C4S 1.751(10) . ? Cl4S C4S 1.733(10) . ? Cl5S C6S 1.808(8) . ? C5S Cl7S 1.698(10) . ? C5S Cl8S 1.779(10) . ? Cl6S C6S 1.808(8) . ? C22E F13F 1.295(15) . ? C22E F14F 1.303(16) . ? C22E F15F 1.45(2) . ? C23F F13G 1.316(16) . ? C23F F14G 1.347(16) . ? C23F F15G 1.349(16) . ? 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 F3D C8D F1D 117.5(14) . . ? F3D C8D F2D 103.1(13) . . ? F1D C8D F2D 100.1(12) . . ? F3D C8D C5D 110.6(14) . . ? F1D C8D C5D 110.7(12) . . ? F2D C8D C5D 114.4(13) . . ? F2E C8E F3E 105.1(10) . . ? F2E C8E F1E 105.1(10) . . ? F3E C8E F1E 102.2(10) . . ? F2E C8E C5D 118.3(10) . . ? F3E C8E C5D 111.5(10) . . ? F1E C8E C5D 113.2(12) . . ? F9C C15C F8C 106.4(16) . . ? F9C C15C F7C 104.2(16) . . ? F8C C15C F7C 105.2(16) . . ? F9C C15C C11C 114.9(16) . . ? F8C C15C C11C 110.3(15) . . ? F7C C15C C11C 115.1(16) . . ? F9E C15E F7E 106.8(17) . . ? F9E C15E F8E 103.8(15) . . ? F7E C15E F8E 105.2(16) . . ? F9E C15E C11C 115.5(16) . . ? F7E C15E C11C 110.3(15) . . ? F8E C15E C11C 114.4(16) . . ? F15D C22D F14D 107.9(12) . . ? F15D C22D F13D 107.7(13) . . ? F14D C22D F13D 106.2(12) . . ? F15D C22D C19D 111.1(12) . . ? F14D C22D C19D 114.9(14) . . ? F13D C22D C19D 108.6(11) . . ? F20A C31A F19A 107.4(11) . . ? F20A C31A F21A 105.2(12) . . ? F19A C31A F21A 106.4(12) . . ? F20A C31A C27A 114.0(11) . . ? F19A C31A C27A 112.1(13) . . ? F21A C31A C27A 111.3(11) . . ? F20E C31E F19E 108.9(11) . . ? F20E C31E F21E 101.9(11) . . ? F19E C31E F21E 102.1(12) . . ? F20E C31E C27A 114.0(11) . . ? F19E C31E C27A 114.1(13) . . ? F21E C31E C27A 114.5(11) . . ? F20B C31B F19B 105(2) . . ? F20B C31B F21B 108(2) . . ? F19B C31B F21B 105(2) . . ? F20B C31B C27B 112(2) . . ? F19B C31B C27B 113(2) . . ? F21B C31B C27B 115(2) . . ? F20F C31F F21F 112(3) . . ? F20F C31F C27B 120(3) . . ? F21F C31F C27B 116(2) . . ? F20F C31F F19F 95(2) . . ? F21F C31F F19F 94(2) . . ? C27B C31F F19F 114(2) . . ? F20C C31C F19C 106.1(7) . . ? F20C C31C F21C 106.5(7) . . ? F19C C31C F21C 104.4(6) . . ? F20C C31C C27C 114.6(7) . . ? F19C C31C C27C 112.7(7) . . ? F21C C31C C27C 111.7(7) . . ? F13A C23A F14A 105.8(14) . . ? F13A C23A F15A 106.4(15) . . ? F14A C23A F15A 104.2(13) . . ? F13A C23A C19A 112(2) . . ? F14A C23A C19A 117.6(13) . . ? F15A C23A C19A 110.2(13) . . ? F13E C23E F15E 106.9(14) . . ? F13E C23E F14E 103.5(14) . . ? F15E C23E F14E 103.2(13) . . ? F13E C23E C19A 116(2) . . ? F15E C23E C19A 109.1(13) . . ? F14E C23E C19A 117.6(13) . . ? N4 Re1 N2 89.3(2) . . ? N4 Re1 N5 163.5(2) . . ? N2 Re1 N5 88.5(2) . . ? N4 Re1 N3 87.2(2) . . ? N2 Re1 N3 164.5(2) . . ? N5 Re1 N3 90.6(2) . . ? N4 Re1 Re2 97.02(17) . . ? N2 Re1 Re2 96.85(17) . . ? N5 Re1 Re2 99.48(16) . . ? N3 Re1 Re2 98.52(16) . . ? N4 Re1 N1 82.3(2) . . ? N2 Re1 N1 80.0(2) . . ? N5 Re1 N1 81.2(2) . . ? N3 Re1 N1 84.6(2) . . ? Re2 Re1 N1 176.79(14) . . ? C1 N1 Re1 167.9(6) . . ? N1 C1 C2 178.3(10) . . ? N9 Re2 N10 164.1(2) . . ? N9 Re2 N7 90.5(2) . . ? N10 Re2 N7 88.9(2) . . ? N9 Re2 N8 88.3(2) . . ? N10 Re2 N8 88.8(2) . . ? N7 Re2 N8 167.6(2) . . ? N9 Re2 Re1 96.28(17) . . ? N10 Re2 Re1 99.59(17) . . ? N7 Re2 Re1 95.53(17) . . ? N8 Re2 Re1 96.89(17) . . ? N9 Re2 N6 80.2(2) . . ? N10 Re2 N6 83.9(2) . . ? N7 Re2 N6 84.3(2) . . ? N8 Re2 N6 83.3(2) . . ? Re1 Re2 N6 176.47(16) . . ? C3 N2 Re1 172.7(7) . . ? C5 N3 Re1 173.0(6) . . ? N2 C3 C4 178.4(11) . . ? C7 N4 Re1 172.3(6) . . ? C9 N5 Re1 169.6(6) . . ? N3 C5 C6 179.2(9) . . ? C11 N6 Re2 167.3(7) . . ? C13 N7 Re2 177.8(7) . . ? N4 C7 C8 178.7(9) . . ? C15 N8 Re2 175.9(7) . . ? C17 N9 Re2 170.3(6) . . ? N5 C9 C10 177.1(8) . . ? C19 N10 Re2 170.6(6) . . ? N6 C11 C12 176.8(12) . . ? N7 C13 C14 178.8(9) . . ? N8 C15 C16 178.6(9) . . ? N9 C17 C18 178.0(9) . . ? N10 C19 C20 177.8(8) . . ? C6A C1A C2A 115.8(6) . . ? C6A C1A B1A 124.4(6) . . ? C2A C1A B1A 119.8(6) . . ? C25A B1A C1A 113.2(6) . . ? C25A B1A C17A 109.5(5) . . ? C1A B1A C17A 106.5(5) . . ? C25A B1A C9A 105.9(5) . . ? C1A B1A C9A 109.6(5) . . ? C17A B1A C9A 112.1(6) . . ? C3A C2A C1A 122.1(7) . . ? C2A C3A C4A 121.9(6) . . ? C2A C3A C7A 118.8(6) . . ? C4A C3A C7A 119.2(6) . . ? C3A C4A C5A 117.5(6) . . ? C4A C5A C6A 120.4(7) . . ? C4A C5A C8A 120.1(6) . . ? C6A C5A C8A 119.5(6) . . ? C1A C6A C5A 122.2(6) . . ? F2A C7A F3A 107.3(6) . . ? F2A C7A F1A 104.4(5) . . ? F3A C7A F1A 104.6(6) . . ? F2A C7A C3A 114.2(6) . . ? F3A C7A C3A 113.2(5) . . ? F1A C7A C3A 112.4(6) . . ? F4A C8A F5A 107.4(7) . . ? F4A C8A F6A 105.8(7) . . ? F5A C8A F6A 103.9(7) . . ? F4A C8A C5A 114.3(7) . . ? F5A C8A C5A 112.8(7) . . ? F6A C8A C5A 111.9(7) . . ? C10A C9A C14A 114.4(6) . . ? C10A C9A B1A 124.3(6) . . ? C14A C9A B1A 121.1(6) . . ? C9A C10A C11A 123.2(6) . . ? C12A C11A C10A 119.4(6) . . ? C12A C11A C15A 119.2(6) . . ? C10A C11A C15A 121.3(6) . . ? C13A C12A C11A 119.0(6) . . ? C12A C13A C14A 120.2(7) . . ? C12A C13A C16A 120.3(6) . . ? C14A C13A C16A 119.4(6) . . ? C13A C14A C9A 123.7(6) . . ? F9A C15A F7A 106.0(6) . . ? F9A C15A F8A 105.3(6) . . ? F7A C15A F8A 105.6(6) . . ? F9A C15A C11A 112.8(6) . . ? F7A C15A C11A 113.5(6) . . ? F8A C15A C11A 113.1(6) . . ? F12A C16A F11A 106.3(6) . . ? F12A C16A F10A 106.5(6) . . ? F11A C16A F10A 106.3(6) . . ? F12A C16A C13A 111.7(6) . . ? F11A C16A C13A 112.2(6) . . ? F10A C16A C13A 113.4(6) . . ? C18A C17A C22A 116.6(6) . . ? C18A C17A B1A 125.2(6) . . ? C22A C17A B1A 118.1(6) . . ? C17A C18A C19A 121.2(6) . . ? C20A C19A C18A 121.9(7) . . ? C20A C19A C23E 114.7(10) . . ? C18A C19A C23E 123.0(10) . . ? C20A C19A C23A 121.1(10) . . ? C18A C19A C23A 116.4(10) . . ? C23E C19A C23A 15.8(11) . . ? C19A C20A C21A 117.7(7) . . ? C20A C21A C22A 120.7(7) . . ? C20A C21A C24A 120.7(7) . . ? C22A C21A C24A 118.5(7) . . ? C21A C22A C17A 121.9(7) . . ? F18A C24A F17A 106.0(6) . . ? F18A C24A F16A 105.6(6) . . ? F17A C24A F16A 104.6(6) . . ? F18A C24A C21A 114.6(6) . . ? F17A C24A C21A 113.0(7) . . ? F16A C24A C21A 112.2(6) . . ? C26A C25A C30A 114.6(6) . . ? C26A C25A B1A 125.0(6) . . ? C30A C25A B1A 120.4(6) . . ? C25A C26A C27A 122.9(7) . . ? C28A C27A C26A 121.0(6) . . ? C28A C27A C31E 122.4(9) . . ? C26A C27A C31E 116.2(9) . . ? C28A C27A C31A 117.7(9) . . ? C26A C27A C31A 121.2(9) . . ? C31E C27A C31A 10.1(11) . . ? C27A C28A C29A 118.5(6) . . ? C30A C29A C28A 119.7(6) . . ? C30A C29A C32A 121.5(6) . . ? C28A C29A C32A 118.8(6) . . ? C29A C30A C25A 123.4(6) . . ? F22A C32A F24A 105.9(6) . . ? F22A C32A F23A 105.9(6) . . ? F24A C32A F23A 105.1(6) . . ? F22A C32A C29A 113.1(6) . . ? F24A C32A C29A 113.7(6) . . ? F23A C32A C29A 112.4(7) . . ? C2B C1B C6B 115.7(6) . . ? C2B C1B B1B 120.8(6) . . ? C6B C1B B1B 122.3(6) . . ? C25B B1B C17B 112.6(6) . . ? C25B B1B C9B 112.8(6) . . ? C17B B1B C9B 103.6(5) . . ? C25B B1B C1B 102.9(5) . . ? C17B B1B C1B 113.3(6) . . ? C9B B1B C1B 112.1(6) . . ? C3B C2B C1B 122.3(7) . . ? C2B C3B C4B 121.1(6) . . ? C2B C3B C7B 117.7(7) . . ? C4B C3B C7B 121.0(6) . . ? C3B C4B C5B 117.7(6) . . ? C6B C5B C4B 120.8(6) . . ? C6B C5B C8B 120.9(6) . . ? C4B C5B C8B 118.2(6) . . ? C5B C6B C1B 122.3(6) . . ? F1B C7B F3B 105.3(7) . . ? F1B C7B F2B 103.2(6) . . ? F3B C7B F2B 108.1(8) . . ? F1B C7B C3B 112.2(7) . . ? F3B C7B C3B 114.0(7) . . ? F2B C7B C3B 113.3(6) . . ? F6B C8B F4B 106.2(6) . . ? F6B C8B F5B 105.8(6) . . ? F4B C8B F5B 106.6(6) . . ? F6B C8B C5B 112.7(6) . . ? F4B C8B C5B 112.8(6) . . ? F5B C8B C5B 112.1(6) . . ? C14B C9B C10B 116.5(6) . . ? C14B C9B B1B 121.6(6) . . ? C10B C9B B1B 121.5(6) . . ? C11B C10B C9B 121.1(6) . . ? C12B C11B C10B 121.4(7) . . ? C12B C11B C15B 119.1(6) . . ? C10B C11B C15B 119.4(6) . . ? C11B C12B C13B 118.7(6) . . ? C12B C13B C14B 119.9(6) . . ? C12B C13B C16B 120.3(6) . . ? C14B C13B C16B 119.7(6) . . ? C13B C14B C9B 122.3(7) . . ? F8B C15B F9B 105.7(6) . . ? F8B C15B F7B 105.1(6) . . ? F9B C15B F7B 105.0(6) . . ? F8B C15B C11B 113.1(6) . . ? F9B C15B C11B 113.2(6) . . ? F7B C15B C11B 113.9(6) . . ? F12B C16B F11B 105.4(6) . . ? F12B C16B F10B 105.1(6) . . ? F11B C16B F10B 105.6(5) . . ? F12B C16B C13B 114.5(6) . . ? F11B C16B C13B 113.1(6) . . ? F10B C16B C13B 112.4(6) . . ? C22B C17B C18B 115.7(6) . . ? C22B C17B B1B 124.2(6) . . ? C18B C17B B1B 120.0(6) . . ? C19B C18B C17B 122.3(7) . . ? C20B C19B C18B 120.5(7) . . ? C20B C19B C23F 120.1(10) . . ? C18B C19B C23F 119.1(11) . . ? C20B C19B C23B 118.0(11) . . ? C18B C19B C23B 121.5(11) . . ? C23F C19B C23B 6.7(14) . . ? C21B C20B C19B 118.0(7) . . ? C20B C21B C22B 121.1(8) . . ? C20B C21B C24B 119.7(7) . . ? C22B C21B C24B 119.1(7) . . ? C17B C22B C21B 122.3(7) . . ? F13B C23B F14B 119.8(17) . . ? F13B C23B F15B 94.6(15) . . ? F14B C23B F15B 104.3(14) . . ? F13B C23B C19B 113.0(17) . . ? F14B C23B C19B 110.8(13) . . ? F15B C23B C19B 112.8(14) . . ? F18B C24B F16B 106.8(8) . . ? F18B C24B F17B 106.6(8) . . ? F16B C24B F17B 105.9(8) . . ? F18B C24B C21B 113.9(8) . . ? F16B C24B C21B 112.6(7) . . ? F17B C24B C21B 110.6(7) . . ? C30B C25B C26B 115.7(7) . . ? C30B C25B B1B 122.1(6) . . ? C26B C25B B1B 121.4(7) . . ? C25B C26B C27B 122.2(7) . . ? C28B C27B C26B 120.7(7) . . ? C28B C27B C31B 120.6(11) . . ? C26B C27B C31B 118.6(11) . . ? C28B C27B C31F 120.8(13) . . ? C26B C27B C31F 118.1(13) . . ? C31B C27B C31F 2(2) . . ? C29B C28B C27B 117.7(7) . . ? C28B C29B C30B 120.7(7) . . ? C28B C29B C32B 118.1(7) . . ? C30B C29B C32B 121.3(7) . . ? C25B C30B C29B 123.1(7) . . ? F23B C32B F22B 106.7(7) . . ? F23B C32B F24B 102.9(7) . . ? F22B C32B F24B 104.2(7) . . ? F23B C32B C29B 115.1(7) . . ? F22B C32B C29B 113.7(7) . . ? F24B C32B C29B 113.0(7) . . ? C2C C1C C6C 115.7(6) . . ? C2C C1C B1C 121.9(6) . . ? C6C C1C B1C 122.1(6) . . ? C9C B1C C17C 111.7(6) . . ? C9C B1C C25C 105.4(5) . . ? C17C B1C C25C 112.2(6) . . ? C9C B1C C1C 113.9(6) . . ? C17C B1C C1C 101.9(5) . . ? C25C B1C C1C 112.0(6) . . ? C1C C2C C3C 122.5(6) . . ? C4C C3C C2C 120.8(7) . . ? C4C C3C C7C 120.4(7) . . ? C2C C3C C7C 118.9(7) . . ? C3C C4C C5C 119.0(7) . . ? C4C C5C C6C 120.0(7) . . ? C4C C5C C8C 119.7(7) . . ? C6C C5C C8C 120.3(8) . . ? C1C C6C C5C 121.9(7) . . ? F2C C7C F1C 108.6(9) . . ? F2C C7C F3C 105.2(7) . . ? F1C C7C F3C 103.0(7) . . ? F2C C7C C3C 114.1(7) . . ? F1C C7C C3C 113.1(7) . . ? F3C C7C C3C 112.0(7) . . ? F6C C8C F5C 106.9(9) . . ? F6C C8C F4C 106.8(9) . . ? F5C C8C F4C 105.3(7) . . ? F6C C8C C5C 114.9(8) . . ? F5C C8C C5C 111.1(8) . . ? F4C C8C C5C 111.3(9) . . ? C14C C9C C10C 114.7(7) . . ? C14C C9C B1C 122.3(6) . . ? C10C C9C B1C 122.6(6) . . ? C11C C10C C9C 121.9(7) . . ? C12C C11C C10C 120.8(7) . . ? C12C C11C C15C 119.2(10) . . ? C10C C11C C15C 120.0(9) . . ? C12C C11C C15E 121.3(10) . . ? C10C C11C C15E 117.8(9) . . ? C15C C11C C15E 5.6(13) . . ? C13C C12C C11C 119.0(7) . . ? C12C C13C C14C 120.2(7) . . ? C12C C13C C16C 118.2(7) . . ? C14C C13C C16C 121.6(6) . . ? C13C C14C C9C 123.3(7) . . ? F10C C16C F11C 106.6(6) . . ? F10C C16C F12C 106.9(6) . . ? F11C C16C F12C 107.4(6) . . ? F10C C16C C13C 111.1(6) . . ? F11C C16C C13C 112.0(6) . . ? F12C C16C C13C 112.4(6) . . ? C18C C17C C22C 115.3(7) . . ? C18C C17C B1C 121.1(6) . . ? C22C C17C B1C 123.2(6) . . ? C19C C18C C17C 123.3(8) . . ? C18C C19C C20C 120.0(8) . . ? C18C C19C C23C 120.9(8) . . ? C20C C19C C23C 119.2(8) . . ? C21C C20C C19C 118.1(7) . . ? C20C C21C C22C 121.5(8) . . ? C20C C21C C24C 118.5(7) . . ? C22C C21C C24C 120.0(7) . . ? C21C C22C C17C 121.8(7) . . ? F15C C23C F14C 104.2(7) . . ? F15C C23C F13C 106.3(9) . . ? F14C C23C F13C 104.4(8) . . ? F15C C23C C19C 113.6(8) . . ? F14C C23C C19C 112.7(9) . . ? F13C C23C C19C 114.6(7) . . ? F18C C24C F16C 109.6(9) . . ? F18C C24C F17C 104.2(9) . . ? F16C C24C F17C 102.6(7) . . ? F18C C24C C21C 115.5(7) . . ? F16C C24C C21C 112.5(8) . . ? F17C C24C C21C 111.2(8) . . ? C30C C25C C26C 115.6(6) . . ? C30C C25C B1C 121.7(6) . . ? C26C C25C B1C 122.4(6) . . ? C27C C26C C25C 121.7(7) . . ? C28C C27C C26C 121.0(7) . . ? C28C C27C C31C 118.1(7) . . ? C26C C27C C31C 120.8(7) . . ? C27C C28C C29C 118.7(7) . . ? C30C C29C C28C 120.4(7) . . ? C30C C29C C32C 121.3(7) . . ? C28C C29C C32C 118.2(7) . . ? C29C C30C C25C 122.4(7) . . ? F23C C32C F22C 109.0(8) . . ? F23C C32C F24C 104.0(8) . . ? F22C C32C F24C 98.5(8) . . ? F23C C32C C29C 116.7(8) . . ? F22C C32C C29C 114.6(7) . . ? F24C C32C C29C 112.2(7) . . ? C2D C1D C6D 115.2(6) . . ? C2D C1D B1D 120.5(6) . . ? C6D C1D B1D 124.2(6) . . ? C9D B1D C25D 108.4(5) . . ? C9D B1D C17D 113.0(5) . . ? C25D B1D C17D 108.4(5) . . ? C9D B1D C1D 109.7(6) . . ? C25D B1D C1D 110.0(5) . . ? C17D B1D C1D 107.3(5) . . ? C1D C2D C3D 122.1(7) . . ? C4D C3D C2D 121.4(7) . . ? C4D C3D C7D 120.3(6) . . ? C2D C3D C7D 118.3(6) . . ? C3D C4D C5D 117.3(7) . . ? C6D C5D C4D 120.9(7) . . ? C6D C5D C8E 114.9(8) . . ? C4D C5D C8E 124.2(8) . . ? C6D C5D C8D 123.8(10) . . ? C4D C5D C8D 114.4(9) . . ? C8E C5D C8D 16.3(10) . . ? C5D C6D C1D 122.9(7) . . ? F5D C7D F6D 105.5(6) . . ? F5D C7D F4D 106.6(7) . . ? F6D C7D F4D 105.2(6) . . ? F5D C7D C3D 113.5(6) . . ? F6D C7D C3D 112.8(6) . . ? F4D C7D C3D 112.5(6) . . ? C14D C9D C10D 115.4(6) . . ? C14D C9D B1D 124.2(6) . . ? C10D C9D B1D 120.4(6) . . ? C11D C10D C9D 122.2(6) . . ? C12D C11D C10D 120.4(7) . . ? C12D C11D C15D 119.8(7) . . ? C10D C11D C15D 119.8(7) . . ? C13D C12D C11D 119.5(7) . . ? C12D C13D C14D 120.8(7) . . ? C12D C13D C16D 119.5(8) . . ? C14D C13D C16D 119.7(7) . . ? C13D C14D C9D 121.8(7) . . ? F8D C15D F7D 105.0(6) . . ? F8D C15D F9D 105.1(6) . . ? F7D C15D F9D 106.1(6) . . ? F8D C15D C11D 113.3(6) . . ? F7D C15D C11D 113.2(6) . . ? F9D C15D C11D 113.4(7) . . ? F10D C16D F12D 106.3(8) . . ? F10D C16D F11D 106.3(8) . . ? F12D C16D F11D 102.8(7) . . ? F10D C16D C13D 115.8(8) . . ? F12D C16D C13D 112.4(7) . . ? F11D C16D C13D 112.3(8) . . ? C23D C17D C18D 115.6(6) . . ? C23D C17D B1D 124.1(6) . . ? C18D C17D B1D 120.2(6) . . ? C19D C18D C17D 122.5(7) . . ? C18D C19D C20D 120.5(7) . . ? C18D C19D C22E 119.7(8) . . ? C20D C19D C22E 119.8(8) . . ? C18D C19D C22D 120.5(10) . . ? C20D C19D C22D 118.9(10) . . ? C22E C19D C22D 1.5(12) . . ? C19D C20D C21D 118.3(6) . . ? C23D C21D C20D 121.4(7) . . ? C23D C21D C24D 117.5(6) . . ? C20D C21D C24D 121.1(6) . . ? C21D C23D C17D 121.7(7) . . ? F16D C24D F17D 106.1(6) . . ? F16D C24D F18D 106.6(6) . . ? F17D C24D F18D 104.9(7) . . ? F16D C24D C21D 113.9(7) . . ? F17D C24D C21D 111.7(6) . . ? F18D C24D C21D 113.1(6) . . ? C30D C25D C26D 114.9(6) . . ? C30D C25D B1D 124.3(6) . . ? C26D C25D B1D 120.7(6) . . ? C27D C26D C25D 122.1(6) . . ? C28D C27D C26D 121.1(6) . . ? C28D C27D C31D 120.9(7) . . ? C26D C27D C31D 118.0(6) . . ? C27D C28D C29D 118.3(7) . . ? C30D C29D C28D 120.2(6) . . ? C30D C29D C32D 121.2(7) . . ? C28D C29D C32D 118.4(7) . . ? C29D C30D C25D 123.4(7) . . ? F20D C31D F21D 107.2(6) . . ? F20D C31D F19D 107.4(6) . . ? F21D C31D F19D 105.1(6) . . ? F20D C31D C27D 113.5(6) . . ? F21D C31D C27D 111.4(6) . . ? F19D C31D C27D 111.7(6) . . ? F24D C32D F23D 106.1(7) . . ? F24D C32D F22D 105.1(8) . . ? F23D C32D F22D 103.6(7) . . ? F24D C32D C29D 114.2(7) . . ? F23D C32D C29D 114.8(7) . . ? F22D C32D C29D 112.1(7) . . ? N1S C1S C2S 177.9(10) . . ? Cl1S C3S Cl2S 114.1(6) . . ? Cl4S C4S Cl3S 110.7(6) . . ? Cl7S C5S Cl8S 109.7(5) . . ? Cl5S C6S Cl6S 107.0(7) . . ? F13F C22E F14F 112.5(13) . . ? F13F C22E F15F 100.2(13) . . ? F14F C22E F15F 99.7(13) . . ? F13F C22E C19D 117.2(12) . . ? F14F C22E C19D 115.2(14) . . ? F15F C22E C19D 109.4(13) . . ? F13G C23F F14G 92.8(15) . . ? F13G C23F F15G 113.5(17) . . ? F14G C23F F15G 107.2(15) . . ? F13G C23F C19B 115.8(18) . . ? F14G C23F C19B 113.0(13) . . ? F15G C23F C19B 112.7(14) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.558 _refine_diff_density_min -2.026 _refine_diff_density_rms 0.156 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 604232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 N10 O Re2 4(B F4) 2(C2 H3 N)' _chemical_formula_sum 'C12 H18 B2 F8 N6 O0.50 Re' _chemical_formula_weight 614.14 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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.899(2) _cell_length_b 22.286(5) _cell_length_c 10.654(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.58(3) _cell_angle_gamma 90.00 _cell_volume 2214.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 928 _cell_measurement_theta_min 2.255 _cell_measurement_theta_max 27.332 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 5.565 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2143 _exptl_absorpt_correction_T_max 0.5796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16051 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5237 _reflns_number_gt 3907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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^)+(0.0362P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5237 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 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 Re1 Re -0.08254(2) 0.441774(9) 0.56631(2) 0.01873(7) Uani 1 1 d . . . O1 O 0.0000 0.5000 0.5000 0.0380(14) Uani 1 2 d S . . N1 N -0.1814(5) 0.37220(19) 0.6485(4) 0.0249(10) Uani 1 1 d . . . N2 N -0.2128(4) 0.4173(2) 0.3780(4) 0.0227(9) Uani 1 1 d . . . N3 N 0.0425(4) 0.45775(18) 0.7618(4) 0.0208(9) Uani 1 1 d . . . N4 N 0.0638(4) 0.37779(18) 0.5559(4) 0.0224(9) Uani 1 1 d . . . N5 N -0.2360(4) 0.49873(17) 0.5911(4) 0.0181(8) Uani 1 1 d . . . C1 C -0.2254(6) 0.3385(2) 0.7056(5) 0.0275(12) Uani 1 1 d . . . C2 C -0.2750(7) 0.2955(3) 0.7820(7) 0.0457(17) Uani 1 1 d . . . H1A H -0.2592 0.2548 0.7553 0.069 Uiso 1 1 calc R . . H1B H -0.3775 0.3017 0.7655 0.069 Uiso 1 1 calc R . . H1C H -0.2218 0.3010 0.8770 0.069 Uiso 1 1 calc R . . C3 C -0.2773(5) 0.4052(2) 0.2709(6) 0.0256(12) Uani 1 1 d . . . C4 C -0.3623(6) 0.3916(3) 0.1324(5) 0.0322(13) Uani 1 1 d . . . H4A H -0.4249 0.3572 0.1300 0.048 Uiso 1 1 calc R . . H4B H -0.2980 0.3819 0.0825 0.048 Uiso 1 1 calc R . . H4C H -0.4210 0.4265 0.0920 0.048 Uiso 1 1 calc R . . C5 C 0.1116(6) 0.4639(3) 0.8704(6) 0.0294(12) Uani 1 1 d . . . C6 C 0.1981(6) 0.4721(3) 1.0083(6) 0.0416(15) Uani 1 1 d . . . H7A H 0.1950 0.5143 1.0329 0.062 Uiso 1 1 calc R . . H7B H 0.2974 0.4606 1.0211 0.062 Uiso 1 1 calc R . . H7C H 0.1605 0.4470 1.0646 0.062 Uiso 1 1 calc R . . C7 C 0.1468(6) 0.3424(2) 0.5547(5) 0.0281(12) Uani 1 1 d . . . C8 C 0.2500(7) 0.2974(3) 0.5534(7) 0.0446(16) Uani 1 1 d . . . H5A H 0.3280 0.2972 0.6393 0.067 Uiso 1 1 calc R . . H5B H 0.2890 0.3062 0.4821 0.067 Uiso 1 1 calc R . . H5C H 0.2035 0.2579 0.5378 0.067 Uiso 1 1 calc R . . C9 C -0.3190(5) 0.5290(2) 0.6117(5) 0.0227(11) Uani 1 1 d . . . C10 C -0.4271(5) 0.5670(2) 0.6363(6) 0.0293(13) Uani 1 1 d . . . H10A H -0.4896 0.5838 0.5518 0.044 Uiso 1 1 calc R . . H10B H -0.3800 0.5997 0.6966 0.044 Uiso 1 1 calc R . . H10C H -0.4846 0.5430 0.6769 0.044 Uiso 1 1 calc R . . B1 B -0.0166(8) 0.6574(4) 0.8419(8) 0.0419(18) Uani 1 1 d . . . B2 B 0.0277(7) -0.0779(3) -0.2832(7) 0.0306(15) Uani 1 1 d . . . F11 F 0.0438(4) 0.6032(2) 0.8847(6) 0.0952(18) Uani 1 1 d . . . F12 F -0.0012(6) 0.6983(3) 0.9421(5) 0.114(2) Uani 1 1 d . . . F13 F 0.0473(5) 0.68499(18) 0.7602(5) 0.0702(13) Uani 1 1 d . . . F14 F -0.1604(4) 0.65042(18) 0.7738(5) 0.0792(15) Uani 1 1 d . . . F21 F 0.0805(5) -0.0813(2) -0.1490(4) 0.0790(14) Uani 1 1 d . . . F22 F 0.0715(5) -0.0273(2) -0.3319(5) 0.0826(15) Uani 1 1 d . . . F23 F -0.1202(4) -0.07510(17) -0.3220(4) 0.0556(11) Uani 1 1 d . . . F24 F 0.0653(5) -0.12791(18) -0.3379(4) 0.0620(12) Uani 1 1 d . . . N1S N 0.0374(8) 0.2304(4) -0.2310(8) 0.091(3) Uani 1 1 d . . . C1S C 0.2700(8) 0.2697(4) -0.0582(7) 0.063(2) Uani 1 1 d . . . H1S1 H 0.2491 0.2877 0.0172 0.094 Uiso 1 1 calc R . . H1S2 H 0.3138 0.2998 -0.0994 0.094 Uiso 1 1 calc R . . H1S3 H 0.3362 0.2359 -0.0267 0.094 Uiso 1 1 calc R . . C2S C 0.1391(9) 0.2485(3) -0.1547(8) 0.0537(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01676(10) 0.02131(11) 0.01721(11) 0.00027(10) 0.00448(7) 0.00068(9) O1 0.022(3) 0.046(3) 0.036(3) 0.005(3) -0.004(2) 0.019(3) N1 0.026(2) 0.026(2) 0.021(2) 0.004(2) 0.006(2) 0.005(2) N2 0.019(2) 0.027(2) 0.021(2) 0.000(2) 0.0060(19) -0.0014(19) N3 0.017(2) 0.024(2) 0.020(2) 0.0013(19) 0.0044(19) 0.0054(18) N4 0.027(2) 0.018(2) 0.021(2) -0.0050(19) 0.008(2) -0.0013(19) N5 0.0165(19) 0.021(2) 0.015(2) -0.0006(18) 0.0023(17) -0.0013(18) C1 0.031(3) 0.025(3) 0.025(3) 0.001(2) 0.008(3) 0.002(2) C2 0.055(4) 0.032(3) 0.062(5) 0.014(3) 0.035(4) -0.001(3) C3 0.023(3) 0.026(3) 0.028(3) -0.003(2) 0.010(2) -0.001(2) C4 0.030(3) 0.040(3) 0.024(3) -0.006(3) 0.006(3) -0.001(3) C5 0.029(3) 0.029(3) 0.029(3) 0.001(3) 0.008(3) -0.004(3) C6 0.037(3) 0.059(4) 0.021(3) -0.003(3) -0.001(3) -0.009(3) C7 0.031(3) 0.027(3) 0.024(3) -0.002(2) 0.007(2) 0.000(2) C8 0.048(4) 0.039(4) 0.043(4) -0.013(3) 0.011(3) 0.016(3) C9 0.020(2) 0.024(3) 0.024(3) 0.003(2) 0.007(2) -0.006(2) C10 0.021(3) 0.036(3) 0.032(3) -0.008(3) 0.010(2) 0.001(2) B1 0.035(4) 0.051(5) 0.037(4) -0.001(4) 0.007(3) 0.015(4) B2 0.029(3) 0.037(4) 0.025(4) 0.000(3) 0.007(3) 0.002(3) F11 0.045(2) 0.073(3) 0.169(5) 0.065(4) 0.039(3) 0.023(2) F12 0.114(4) 0.159(6) 0.065(4) -0.048(4) 0.025(3) -0.022(4) F13 0.067(3) 0.050(3) 0.104(4) 0.009(3) 0.043(3) -0.003(2) F14 0.029(2) 0.047(2) 0.130(4) 0.014(3) -0.015(2) -0.0109(19) F21 0.085(3) 0.114(4) 0.025(2) -0.012(3) 0.001(2) 0.020(3) F22 0.088(3) 0.056(3) 0.122(4) 0.010(3) 0.059(3) -0.019(3) F23 0.0319(19) 0.061(2) 0.071(3) 0.020(2) 0.013(2) 0.0101(18) F24 0.083(3) 0.059(3) 0.039(2) -0.008(2) 0.014(2) 0.035(2) N1S 0.062(5) 0.099(6) 0.097(6) -0.046(5) 0.007(4) 0.030(5) C1S 0.062(5) 0.071(5) 0.051(5) 0.005(4) 0.015(4) -0.027(4) C2S 0.053(5) 0.051(4) 0.056(5) -0.007(4) 0.017(4) 0.001(4) _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 O1 1.7993(3) . ? Re1 N4 2.062(4) . ? Re1 N2 2.062(5) . ? Re1 N5 2.064(4) . ? Re1 N3 2.066(4) . ? Re1 N1 2.169(4) . ? O1 Re1 1.7993(3) 3_566 ? N1 C1 1.141(6) . ? N2 C3 1.138(6) . ? N3 C5 1.138(7) . ? N4 C7 1.142(6) . ? N5 C9 1.140(6) . ? C1 C2 1.445(8) . ? C3 C4 1.464(7) . ? C5 C6 1.443(8) . ? C7 C8 1.436(7) . ? C9 C10 1.455(7) . ? B1 F11 1.357(8) . ? B1 F14 1.373(8) . ? B1 F12 1.374(9) . ? B1 F13 1.379(8) . ? B2 F21 1.350(7) . ? B2 F24 1.366(7) . ? B2 F22 1.370(8) . ? B2 F23 1.383(7) . ? N1S C2S 1.136(9) . ? C1S C2S 1.436(10) . ? 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 O1 Re1 N4 93.33(11) . . ? O1 Re1 N2 91.54(11) . . ? N4 Re1 N2 89.20(17) . . ? O1 Re1 N5 93.28(11) . . ? N4 Re1 N5 173.17(15) . . ? N2 Re1 N5 92.32(16) . . ? O1 Re1 N3 94.24(11) . . ? N4 Re1 N3 88.78(16) . . ? N2 Re1 N3 173.98(16) . . ? N5 Re1 N3 89.04(15) . . ? O1 Re1 N1 179.29(11) . . ? N4 Re1 N1 86.99(16) . . ? N2 Re1 N1 89.10(16) . . ? N5 Re1 N1 86.38(15) . . ? N3 Re1 N1 85.14(16) . . ? Re1 O1 Re1 180.000 . 3_566 ? C1 N1 Re1 172.2(4) . . ? C3 N2 Re1 175.2(4) . . ? C5 N3 Re1 177.0(4) . . ? C7 N4 Re1 177.7(4) . . ? C9 N5 Re1 176.2(4) . . ? N1 C1 C2 177.5(6) . . ? N2 C3 C4 178.2(6) . . ? N3 C5 C6 179.4(7) . . ? N4 C7 C8 179.3(6) . . ? N5 C9 C10 178.9(6) . . ? F11 B1 F14 109.8(6) . . ? F11 B1 F12 114.1(7) . . ? F14 B1 F12 108.1(6) . . ? F11 B1 F13 111.5(5) . . ? F14 B1 F13 109.3(6) . . ? F12 B1 F13 103.8(6) . . ? F21 B2 F24 110.0(5) . . ? F21 B2 F22 112.8(6) . . ? F24 B2 F22 110.1(5) . . ? F21 B2 F23 108.3(5) . . ? F24 B2 F23 108.8(5) . . ? F22 B2 F23 106.7(5) . . ? N1S C2S C1S 178.3(9) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 2.241 _refine_diff_density_min -1.718 _refine_diff_density_rms 0.161 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 604233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H62 N6 P4 Re2 4(B F4)' _chemical_formula_sum 'C62 H62 B4 F16 N6 P4 Re2' _chemical_formula_weight 1734.70 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.082(3) _cell_length_b 22.310(5) _cell_length_c 19.884(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.58(3) _cell_angle_gamma 90.00 _cell_volume 7120(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 224 _cell_measurement_theta_min 2.114 _cell_measurement_theta_max 21.447 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3400 _exptl_absorpt_coefficient_mu 3.571 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3440 _exptl_absorpt_correction_T_max 0.7882 _exptl_absorpt_process_details XABS2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12095 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.71 _reflns_number_total 12095 _reflns_number_gt 7485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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^)+(0.0835P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12095 _refine_ls_number_parameters 751 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 Re1 Re 0.52239(3) 0.17228(2) 0.25733(2) 0.02567(14) Uani 1 1 d D . . Re2 Re 0.42623(3) 0.103062(19) 0.289011(19) 0.02290(13) Uani 1 1 d . . . P1 P 0.43493(18) 0.25919(13) 0.23052(13) 0.0254(6) Uani 1 1 d . . . P2 P 0.33563(17) 0.18406(12) 0.32328(12) 0.0232(6) Uani 1 1 d . . . P3 P 0.51181(19) 0.13214(14) 0.14287(13) 0.0300(7) Uani 1 1 d . . . P4 P 0.34611(18) 0.08640(12) 0.18208(12) 0.0234(6) Uani 1 1 d . . . F33' F 0.8634(14) 0.3146(13) 0.3715(11) 0.066(8) Uiso 0.38(2) 1 d P A 1 F11 F 0.4480(6) -0.1942(4) 0.3217(5) 0.091(3) Uiso 1 1 d D A . F12 F 0.4027(4) -0.1013(3) 0.3419(3) 0.0407(16) Uiso 1 1 d D A . F13 F 0.3629(4) -0.1795(3) 0.4061(3) 0.0476(18) Uiso 1 1 d D A . F14 F 0.3018(9) -0.1614(8) 0.3019(7) 0.019(5) Uiso 0.38(2) 1 d PD A 1 F21 F 0.3473(5) 0.0480(4) 0.4940(4) 0.071(2) Uiso 1 1 d D . . F22 F 0.3073(6) 0.0995(4) 0.5860(5) 0.090(3) Uiso 1 1 d D . . F23 F 0.2348(6) 0.0207(5) 0.5413(5) 0.102(3) Uiso 1 1 d D . . F24 F 0.3572(5) 0.0050(4) 0.5986(4) 0.069(2) Uiso 1 1 d D . . F31 F 0.7304(6) 0.3234(4) 0.3638(5) 0.089(3) Uiso 1 1 d D A . F32 F 0.7659(6) 0.2305(4) 0.3963(5) 0.088(3) Uiso 1 1 d D A . F33 F 0.8644(10) 0.2841(9) 0.3661(8) 0.081(6) Uiso 0.62(2) 1 d PD A 2 F34 F 0.7965(6) 0.3115(4) 0.4631(4) 0.080(3) Uiso 1 1 d D A . F41 F 0.9142(9) 0.1105(7) 0.2410(7) 0.080(6) Uiso 0.62(2) 1 d PD A 2 F42 F 0.8363(13) 0.0438(10) 0.2101(11) 0.247(9) Uiso 1 1 d D . . F43 F 0.7856(7) 0.1385(5) 0.1997(6) 0.119(4) Uiso 1 1 d D . . F44 F 0.8758(9) 0.1010(6) 0.1264(8) 0.156(5) Uiso 1 1 d D . . N1 N 0.5519(6) 0.2129(4) 0.3511(4) 0.033(2) Uani 1 1 d . . . N2 N 0.4823(6) 0.0919(4) 0.3862(4) 0.035(2) Uani 1 1 d . . . N3 N 0.6262(6) 0.1221(4) 0.2901(5) 0.038(2) Uani 1 1 d . . . N4 N 0.4925(6) 0.0237(4) 0.2738(4) 0.032(2) Uani 1 1 d . . . N6 N 0.3299(5) 0.0351(4) 0.3319(4) 0.0199(19) Uani 1 1 d . . . C1 C 0.5755(7) 0.2337(5) 0.3999(5) 0.030(3) Uani 1 1 d . . . C2 C 0.6001(7) 0.2639(6) 0.4628(5) 0.047(3) Uani 1 1 d . . . H2A H 0.6021 0.3073 0.4550 0.070 Uiso 1 1 calc R . . H2B H 0.6553 0.2498 0.4794 0.070 Uiso 1 1 calc R . . H2C H 0.5596 0.2551 0.4962 0.070 Uiso 1 1 calc R . . C3 C 0.5123(8) 0.0834(5) 0.4372(6) 0.036(3) Uani 1 1 d . . . C4 C 0.5470(9) 0.0769(6) 0.5072(5) 0.052(4) Uani 1 1 d . . . H4A H 0.5795 0.1126 0.5202 0.077 Uiso 1 1 calc R . . H4B H 0.5832 0.0415 0.5106 0.077 Uiso 1 1 calc R . . H4C H 0.5015 0.0721 0.5373 0.077 Uiso 1 1 calc R . . C6 C 0.6887(9) 0.1091(6) 0.3165(6) 0.045(3) Uani 1 1 d . . . C7 C 0.5296(7) -0.0189(6) 0.2721(5) 0.037(3) Uani 1 1 d . . . C8 C 0.5720(9) -0.0772(6) 0.2705(6) 0.053(4) Uani 1 1 d . . . H8A H 0.5351 -0.1085 0.2863 0.079 Uiso 1 1 calc R . . H8B H 0.6232 -0.0759 0.2999 0.079 Uiso 1 1 calc R . . H8C H 0.5859 -0.0862 0.2243 0.079 Uiso 1 1 calc R . . C11 C 0.2870(7) 0.0014(5) 0.3580(5) 0.030(3) Uani 1 1 d . . . C12 C 0.2308(8) -0.0390(6) 0.3879(7) 0.054(4) Uani 1 1 d . . . H12A H 0.1773 -0.0391 0.3613 0.080 Uiso 1 1 calc R . . H12B H 0.2221 -0.0262 0.4340 0.080 Uiso 1 1 calc R . . H12C H 0.2544 -0.0795 0.3886 0.080 Uiso 1 1 calc R . . C5 C 0.7704(8) 0.0922(7) 0.3479(7) 0.066(5) Uani 1 1 d . . . H51A H 0.8023 0.1285 0.3599 0.099 Uiso 1 1 calc R . . H51B H 0.8007 0.0682 0.3162 0.099 Uiso 1 1 calc R . . H51C H 0.7627 0.0687 0.3887 0.099 Uiso 1 1 calc R . . C111 C 0.4208(7) 0.2880(5) 0.1447(5) 0.028(3) Uani 1 1 d . . . C112 C 0.4908(7) 0.3112(5) 0.1166(5) 0.034(3) Uani 1 1 d . . . H112 H 0.5438 0.3072 0.1400 0.041 Uiso 1 1 calc R . . C113 C 0.4843(8) 0.3402(5) 0.0551(5) 0.039(3) Uani 1 1 d . . . H113 H 0.5321 0.3579 0.0375 0.046 Uiso 1 1 calc R . . C114 C 0.4085(8) 0.3433(6) 0.0197(6) 0.045(3) Uani 1 1 d . . . H114 H 0.4044 0.3619 -0.0233 0.054 Uiso 1 1 calc R . . C115 C 0.3388(8) 0.3198(5) 0.0456(5) 0.035(3) Uani 1 1 d . . . H115 H 0.2865 0.3224 0.0207 0.043 Uiso 1 1 calc R . . C116 C 0.3444(7) 0.2920(5) 0.1084(5) 0.031(3) Uani 1 1 d . . . H116 H 0.2959 0.2757 0.1264 0.038 Uiso 1 1 calc R . . C121 C 0.4594(8) 0.3306(5) 0.2727(5) 0.034(3) Uani 1 1 d . . . C122 C 0.3988(9) 0.3735(6) 0.2721(6) 0.050(4) Uani 1 1 d . . . H122 H 0.3459 0.3659 0.2496 0.061 Uiso 1 1 calc R . . C123 C 0.4138(10) 0.4289(6) 0.3044(6) 0.058(4) Uani 1 1 d . . . H123 H 0.3706 0.4578 0.3050 0.070 Uiso 1 1 calc R . . C124 C 0.4898(12) 0.4412(7) 0.3348(6) 0.079(6) Uani 1 1 d . . . H124 H 0.4994 0.4783 0.3575 0.095 Uiso 1 1 calc R . . C125 C 0.5536(11) 0.3994(6) 0.3324(7) 0.064(5) Uani 1 1 d . . . H125 H 0.6072 0.4089 0.3523 0.077 Uiso 1 1 calc R . . C126 C 0.5411(8) 0.3450(5) 0.3023(5) 0.040(3) Uani 1 1 d . . . H126 H 0.5855 0.3171 0.3008 0.048 Uiso 1 1 calc R . . C211 C 0.2240(7) 0.1695(5) 0.3370(5) 0.030(3) Uani 1 1 d . . . C212 C 0.1624(7) 0.2007(6) 0.2994(5) 0.038(3) Uani 1 1 d . . . H212 H 0.1761 0.2287 0.2659 0.045 Uiso 1 1 calc R . . C213 C 0.0810(8) 0.1896(6) 0.3124(6) 0.049(4) Uani 1 1 d . . . H213 H 0.0377 0.2112 0.2884 0.058 Uiso 1 1 calc R . . C214 C 0.0604(8) 0.1464(7) 0.3609(7) 0.057(4) Uani 1 1 d . . . H214 H 0.0039 0.1377 0.3686 0.068 Uiso 1 1 calc R . . C215 C 0.1235(8) 0.1180(5) 0.3959(5) 0.041(3) Uani 1 1 d . . . H215 H 0.1104 0.0903 0.4300 0.049 Uiso 1 1 calc R . . C216 C 0.2047(7) 0.1274(5) 0.3844(5) 0.034(3) Uani 1 1 d . . . H216 H 0.2475 0.1054 0.4085 0.040 Uiso 1 1 calc R . . C221 C 0.3649(7) 0.2236(5) 0.4023(5) 0.028(3) Uani 1 1 d . . . C222 C 0.3794(7) 0.1889(5) 0.4608(5) 0.034(3) Uani 1 1 d . . . H222 H 0.3767 0.1464 0.4586 0.041 Uiso 1 1 calc R . . C223 C 0.3976(7) 0.2176(6) 0.5223(5) 0.042(3) Uani 1 1 d . . . H223 H 0.4094 0.1944 0.5619 0.050 Uiso 1 1 calc R . . C224 C 0.3989(7) 0.2793(6) 0.5264(6) 0.045(3) Uani 1 1 d . . . H224 H 0.4129 0.2982 0.5683 0.055 Uiso 1 1 calc R . . C225 C 0.3797(8) 0.3141(5) 0.4692(5) 0.046(3) Uani 1 1 d . . . H225 H 0.3773 0.3566 0.4724 0.055 Uiso 1 1 calc R . . C226 C 0.3640(7) 0.2855(5) 0.4069(5) 0.035(3) Uani 1 1 d . . . H226 H 0.3526 0.3088 0.3674 0.042 Uiso 1 1 calc R . . C311 C 0.5584(9) 0.0595(6) 0.1283(6) 0.049(4) Uani 1 1 d . . . C312 C 0.5185(11) 0.0136(6) 0.0920(6) 0.063(4) Uani 1 1 d . . . H312 H 0.4622 0.0195 0.0761 0.076 Uiso 1 1 calc R . . C313 C 0.5552(16) -0.0391(8) 0.0778(10) 0.095(7) Uani 1 1 d . . . H313 H 0.5238 -0.0695 0.0544 0.115 Uiso 1 1 calc R . . C314 C 0.633(2) -0.0483(11) 0.0960(10) 0.130(13) Uani 1 1 d . . . H314 H 0.6581 -0.0854 0.0854 0.156 Uiso 1 1 calc R . . C315 C 0.6778(15) -0.0072(11) 0.1287(11) 0.114(9) Uani 1 1 d . . . H315 H 0.7352 -0.0145 0.1401 0.137 Uiso 1 1 calc R . . C316 C 0.6403(11) 0.0500(8) 0.1480(7) 0.078(5) Uani 1 1 d . . . H316 H 0.6719 0.0793 0.1733 0.093 Uiso 1 1 calc R . . C321 C 0.5512(7) 0.1758(5) 0.0735(5) 0.032(3) Uani 1 1 d . . . C322 C 0.5029(7) 0.1918(5) 0.0176(5) 0.030(3) Uani 1 1 d . . . H322 H 0.4453 0.1819 0.0145 0.036 Uiso 1 1 calc R . . C323 C 0.5371(8) 0.2224(5) -0.0347(6) 0.042(3) Uani 1 1 d . . . H323 H 0.5028 0.2331 -0.0735 0.051 Uiso 1 1 calc R . . C324 C 0.6214(8) 0.2376(6) -0.0308(6) 0.046(3) Uani 1 1 d . . . H324 H 0.6455 0.2585 -0.0663 0.055 Uiso 1 1 calc R . . C325 C 0.6690(8) 0.2208(6) 0.0274(6) 0.054(4) Uani 1 1 d . . . H325 H 0.7262 0.2317 0.0316 0.065 Uiso 1 1 calc R . . C326 C 0.6367(7) 0.1896(6) 0.0780(6) 0.042(3) Uani 1 1 d . . . H326 H 0.6712 0.1771 0.1160 0.050 Uiso 1 1 calc R . . C411 C 0.3320(7) 0.0100(5) 0.1506(5) 0.030(3) Uani 1 1 d . . . C412 C 0.3463(7) -0.0406(5) 0.1881(6) 0.033(3) Uani 1 1 d . . . H412 H 0.3645 -0.0372 0.2343 0.040 Uiso 1 1 calc R . . C413 C 0.3348(8) -0.0969(6) 0.1595(6) 0.046(3) Uani 1 1 d . . . H413 H 0.3476 -0.1320 0.1852 0.056 Uiso 1 1 calc R . . C414 C 0.3044(10) -0.1014(6) 0.0932(7) 0.063(4) Uani 1 1 d . . . H414 H 0.2949 -0.1400 0.0739 0.075 Uiso 1 1 calc R . . C415 C 0.2878(10) -0.0520(6) 0.0553(6) 0.057(4) Uani 1 1 d . . . H415 H 0.2674 -0.0557 0.0096 0.069 Uiso 1 1 calc R . . C416 C 0.3008(9) 0.0040(6) 0.0835(5) 0.050(4) Uani 1 1 d . . . H416 H 0.2885 0.0388 0.0572 0.059 Uiso 1 1 calc R . . C421 C 0.2384(7) 0.1109(5) 0.1709(5) 0.028(3) Uani 1 1 d . . . C422 C 0.2114(7) 0.1559(6) 0.1271(5) 0.041(3) Uani 1 1 d . . . H422 H 0.2497 0.1763 0.1007 0.049 Uiso 1 1 calc R . . C423 C 0.1265(8) 0.1713(6) 0.1221(6) 0.048(4) Uani 1 1 d . . . H423 H 0.1079 0.2051 0.0963 0.058 Uiso 1 1 calc R . . C424 C 0.0714(7) 0.1378(6) 0.1542(6) 0.045(3) Uani 1 1 d . . . H424 H 0.0135 0.1459 0.1468 0.053 Uiso 1 1 calc R . . C425 C 0.0968(7) 0.0923(5) 0.1971(5) 0.037(3) Uani 1 1 d . . . H425 H 0.0577 0.0701 0.2211 0.044 Uiso 1 1 calc R . . C426 C 0.1825(7) 0.0794(5) 0.2045(6) 0.036(3) Uani 1 1 d . . . H426 H 0.2014 0.0480 0.2338 0.043 Uiso 1 1 calc R . . B1 B 0.3783(6) -0.1617(3) 0.3404(4) 0.043(4) Uiso 1 1 d D . . B2 B 0.3133(6) 0.0441(4) 0.5558(4) 0.066(5) Uiso 1 1 d D . . B3 B 0.7912(7) 0.2896(4) 0.3982(5) 0.070(5) Uiso 1 1 d D . . B4 B 0.8529(10) 0.1021(9) 0.1917(7) 0.175(15) Uiso 1 1 d D A . F14' F 0.3208(10) -0.1811(7) 0.2967(7) 0.057(5) Uiso 0.62(2) 1 d P A 2 F41' F 0.880(3) 0.1647(12) 0.197(2) 0.177(19) Uiso 0.38(2) 1 d PD A 1 C1B C 0.3318(6) 0.2400(4) 0.2564(4) 0.022(2) Uani 1 1 d . . . H1B1 H 0.2977 0.2245 0.2170 0.027 Uiso 1 1 calc R . . H1B2 H 0.3044 0.2767 0.2723 0.027 Uiso 1 1 calc R . . C2B C 0.4018(7) 0.1248(5) 0.1180(5) 0.026(3) Uani 1 1 d . . . H2B1 H 0.3952 0.1021 0.0752 0.032 Uiso 1 1 calc R . . H2B2 H 0.3774 0.1651 0.1102 0.032 Uiso 1 1 calc R . . N5 N 0.6323(5) 0.2370(3) 0.2250(4) 0.0208(14) Uiso 1 1 d D . . C9 C 0.6950(5) 0.2532(4) 0.2193(5) 0.0208(14) Uiso 1 1 d D . . C10 C 0.7802(8) 0.2805(8) 0.2089(9) 0.104(6) Uiso 1 1 d D . . H10A H 0.7791 0.3001 0.1647 0.155 Uiso 1 1 calc R . . H10B H 0.8225 0.2489 0.2110 0.155 Uiso 1 1 calc R . . H10C H 0.7938 0.3102 0.2443 0.155 Uiso 1 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 0.0282(3) 0.0316(3) 0.0161(2) 0.00291(18) -0.00767(17) 0.0025(2) Re2 0.0299(3) 0.0252(2) 0.0124(2) 0.00200(18) -0.00802(17) 0.0044(2) P1 0.0305(16) 0.0296(16) 0.0152(13) 0.0009(12) -0.0050(11) 0.0017(13) P2 0.0264(15) 0.0299(17) 0.0126(13) 0.0015(11) -0.0043(11) 0.0024(13) P3 0.0315(17) 0.0373(18) 0.0209(15) -0.0018(13) -0.0003(13) 0.0055(14) P4 0.0317(16) 0.0239(15) 0.0137(13) 0.0003(11) -0.0066(11) -0.0003(13) N1 0.039(6) 0.038(6) 0.021(5) 0.002(4) -0.013(4) 0.003(5) N2 0.043(6) 0.035(6) 0.025(5) 0.005(4) -0.006(5) 0.010(5) N3 0.033(6) 0.040(6) 0.041(6) 0.016(5) -0.001(5) -0.004(5) N4 0.039(6) 0.037(6) 0.020(5) 0.001(4) -0.008(4) 0.005(5) N6 0.021(5) 0.024(5) 0.013(4) -0.008(4) -0.009(4) 0.009(4) C1 0.033(7) 0.037(7) 0.019(6) 0.006(5) -0.009(5) -0.004(6) C2 0.046(8) 0.063(9) 0.029(6) -0.001(6) -0.020(6) -0.014(7) C3 0.050(8) 0.032(7) 0.025(6) 0.006(5) -0.011(6) 0.009(6) C4 0.072(9) 0.055(9) 0.024(6) 0.006(6) -0.033(6) -0.001(7) C6 0.053(9) 0.037(8) 0.046(8) 0.004(6) 0.001(7) 0.010(7) C7 0.042(7) 0.048(8) 0.022(6) 0.013(5) -0.002(5) 0.019(7) C8 0.066(10) 0.045(8) 0.046(8) 0.005(6) 0.002(7) 0.026(8) C11 0.034(7) 0.030(7) 0.024(6) 0.006(5) 0.004(5) -0.002(6) C12 0.058(9) 0.045(8) 0.056(8) -0.013(7) -0.006(7) -0.010(7) C5 0.026(7) 0.097(13) 0.072(10) -0.013(9) -0.012(7) 0.017(8) C111 0.042(7) 0.027(6) 0.015(5) 0.000(4) -0.005(5) -0.001(5) C112 0.039(7) 0.034(7) 0.029(6) 0.002(5) 0.002(5) 0.001(6) C113 0.046(8) 0.038(8) 0.032(7) 0.003(5) 0.006(6) -0.004(6) C114 0.062(9) 0.047(8) 0.025(6) 0.014(6) -0.002(6) 0.019(7) C115 0.043(7) 0.031(7) 0.031(6) -0.003(5) -0.010(6) 0.013(6) C116 0.041(7) 0.029(7) 0.023(6) 0.002(5) -0.009(5) 0.005(6) C121 0.064(8) 0.015(6) 0.022(6) -0.004(5) -0.006(6) -0.004(6) C122 0.078(10) 0.048(8) 0.023(6) -0.006(6) -0.016(6) 0.009(8) C123 0.092(12) 0.029(8) 0.051(8) -0.012(6) -0.016(8) 0.024(8) C124 0.148(16) 0.046(9) 0.035(8) -0.013(7) -0.060(9) 0.012(11) C125 0.098(12) 0.036(8) 0.053(9) -0.003(7) -0.037(8) -0.002(9) C126 0.049(8) 0.041(8) 0.028(6) -0.003(5) -0.012(6) -0.001(6) C211 0.034(7) 0.031(7) 0.023(6) 0.000(5) -0.002(5) -0.002(6) C212 0.027(7) 0.070(9) 0.014(5) -0.006(5) -0.013(5) 0.024(6) C213 0.038(8) 0.071(10) 0.036(7) -0.009(7) -0.003(6) 0.011(7) C214 0.032(8) 0.088(12) 0.052(9) -0.020(8) 0.011(7) -0.007(8) C215 0.058(9) 0.043(8) 0.021(6) 0.000(5) 0.013(6) 0.003(7) C216 0.039(7) 0.035(7) 0.026(6) -0.005(5) -0.004(5) 0.003(6) C221 0.041(7) 0.025(6) 0.017(5) -0.006(5) -0.001(5) 0.005(5) C222 0.040(7) 0.040(7) 0.021(6) 0.000(5) -0.006(5) 0.012(6) C223 0.041(8) 0.063(10) 0.020(6) 0.007(6) 0.000(5) 0.005(7) C224 0.042(8) 0.071(10) 0.022(6) -0.015(6) -0.003(5) 0.000(7) C225 0.079(10) 0.031(7) 0.027(6) -0.012(5) -0.004(6) -0.001(7) C226 0.048(8) 0.045(8) 0.012(5) 0.000(5) 0.000(5) -0.003(6) C311 0.060(9) 0.056(9) 0.034(7) 0.010(7) 0.014(6) 0.034(8) C312 0.117(14) 0.038(8) 0.038(8) -0.013(6) 0.033(8) 0.009(9) C313 0.16(2) 0.047(11) 0.090(15) 0.008(10) 0.067(15) 0.031(13) C314 0.26(4) 0.084(17) 0.053(13) 0.019(11) 0.079(19) 0.07(2) C315 0.125(19) 0.13(2) 0.093(16) 0.027(14) 0.014(14) 0.090(17) C316 0.107(14) 0.088(13) 0.039(8) 0.004(8) 0.015(9) 0.038(11) C321 0.032(7) 0.036(7) 0.030(6) -0.008(5) 0.014(5) -0.002(6) C322 0.039(7) 0.035(7) 0.017(5) 0.004(5) -0.003(5) 0.001(6) C323 0.055(9) 0.041(8) 0.031(7) -0.003(6) 0.008(6) -0.004(7) C324 0.049(8) 0.049(9) 0.043(8) -0.008(6) 0.020(7) -0.005(7) C325 0.035(8) 0.082(11) 0.046(8) -0.015(7) 0.014(7) -0.018(7) C326 0.028(7) 0.069(9) 0.030(7) -0.012(6) 0.010(5) 0.005(6) C411 0.036(7) 0.026(6) 0.025(6) -0.006(5) -0.007(5) -0.004(5) C412 0.036(7) 0.030(7) 0.032(6) 0.002(5) -0.003(5) 0.001(6) C413 0.065(9) 0.035(8) 0.039(7) -0.004(6) 0.004(6) -0.005(7) C414 0.105(13) 0.041(9) 0.044(8) -0.023(7) 0.016(8) -0.017(9) C415 0.098(12) 0.043(9) 0.032(7) -0.011(7) 0.010(7) -0.018(8) C416 0.087(11) 0.042(8) 0.018(6) 0.004(5) -0.004(6) -0.015(8) C421 0.038(7) 0.029(7) 0.015(5) 0.002(5) -0.007(5) 0.008(6) C422 0.043(8) 0.053(8) 0.024(6) 0.012(6) -0.016(5) 0.004(7) C423 0.055(9) 0.053(9) 0.035(7) 0.021(6) -0.017(6) 0.030(8) C424 0.025(7) 0.067(10) 0.039(7) -0.005(7) -0.021(6) 0.001(7) C425 0.046(8) 0.044(8) 0.020(6) 0.006(5) 0.002(5) 0.012(6) C426 0.022(6) 0.043(7) 0.040(7) -0.003(6) -0.019(5) 0.008(6) C1B 0.035(6) 0.024(6) 0.006(5) -0.007(4) -0.008(4) 0.008(5) C2B 0.044(7) 0.024(6) 0.011(5) -0.001(4) 0.000(5) -0.004(5) _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 N3 2.082(10) . ? Re1 N1 2.101(9) . ? Re1 Re2 2.3010(7) . ? Re1 N5 2.401(7) . ? Re1 P1 2.435(3) . ? Re1 P3 2.442(3) . ? Re2 N2 2.096(9) . ? Re2 N4 2.099(10) . ? Re2 N6 2.364(9) . ? Re2 P4 2.445(3) . ? Re2 P2 2.445(3) . ? P1 C1B 1.818(10) . ? P1 C111 1.825(10) . ? P1 C121 1.831(10) . ? P2 C1B 1.823(9) . ? P2 C221 1.836(10) . ? P2 C211 1.861(11) . ? P3 C2B 1.814(11) . ? P3 C311 1.817(13) . ? P3 C321 1.834(11) . ? P4 C421 1.816(11) . ? P4 C2B 1.817(10) . ? P4 C411 1.825(11) . ? F33' B3 1.42(3) . ? F11 B1 1.404(6) . ? F12 B1 1.403(6) . ? F13 B1 1.402(6) . ? F14 B1 1.410(6) . ? F21 B2 1.379(5) . ? F22 B2 1.379(5) . ? F23 B2 1.380(5) . ? F24 B2 1.381(5) . ? F31 B3 1.382(6) . ? F32 B3 1.379(6) . ? F33 B3 1.379(7) . ? F34 B3 1.379(6) . ? F41 B4 1.360(9) . ? F42 B4 1.383(10) . ? F43 B4 1.371(9) . ? F43 F41' 1.62(4) . ? F44 B4 1.371(9) . ? N1 C1 1.121(12) . ? N2 C3 1.111(12) . ? N3 C6 1.140(14) . ? N4 C7 1.124(13) . ? N6 C11 1.164(13) . ? C1 C2 1.453(14) . ? C3 C4 1.475(14) . ? C6 C5 1.469(17) . ? C7 C8 1.470(16) . ? C11 C12 1.433(16) . ? C111 C112 1.387(15) . ? C111 C116 1.389(14) . ? C112 C113 1.381(15) . ? C113 C114 1.371(16) . ? C114 C115 1.368(16) . ? C115 C116 1.391(14) . ? C121 C122 1.366(16) . ? C121 C126 1.443(16) . ? C122 C123 1.407(17) . ? C123 C124 1.36(2) . ? C124 C125 1.39(2) . ? C125 C126 1.361(16) . ? C211 C216 1.381(15) . ? C211 C212 1.389(14) . ? C212 C213 1.373(16) . ? C213 C214 1.417(18) . ? C214 C215 1.352(17) . ? C215 C216 1.356(16) . ? C221 C226 1.385(14) . ? C221 C222 1.405(14) . ? C222 C223 1.396(15) . ? C223 C224 1.378(17) . ? C224 C225 1.396(16) . ? C225 C226 1.402(14) . ? C311 C316 1.37(2) . ? C311 C312 1.386(19) . ? C312 C313 1.35(2) . ? C313 C314 1.30(3) . ? C314 C315 1.31(3) . ? C315 C316 1.47(2) . ? C321 C322 1.363(14) . ? C321 C326 1.405(15) . ? C322 C323 1.385(15) . ? C323 C324 1.396(16) . ? C324 C325 1.397(17) . ? C325 C326 1.355(17) . ? C411 C412 1.364(14) . ? C411 C416 1.403(14) . ? C412 C413 1.386(15) . ? C413 C414 1.380(17) . ? C414 C415 1.354(18) . ? C415 C416 1.379(16) . ? C421 C426 1.351(15) . ? C421 C422 1.382(14) . ? C422 C423 1.405(16) . ? C423 C424 1.350(17) . ? C424 C425 1.372(16) . ? C425 C426 1.407(15) . ? B1 F14' 1.304(18) . ? B4 F41' 1.462(19) . ? N5 C9 1.083(9) . ? C9 C10 1.527(10) . ? 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 N3 Re1 N1 79.7(4) . . ? N3 Re1 Re2 95.3(3) . . ? N1 Re1 Re2 99.5(3) . . ? N3 Re1 N5 79.5(3) . . ? N1 Re1 N5 81.4(3) . . ? Re2 Re1 N5 174.59(19) . . ? N3 Re1 P1 159.8(3) . . ? N1 Re1 P1 86.9(3) . . ? Re2 Re1 P1 101.85(7) . . ? N5 Re1 P1 83.5(2) . . ? N3 Re1 P3 95.9(3) . . ? N1 Re1 P3 169.9(3) . . ? Re2 Re1 P3 90.01(8) . . ? N5 Re1 P3 88.87(19) . . ? P1 Re1 P3 94.72(9) . . ? N2 Re2 N4 80.8(3) . . ? N2 Re2 Re1 94.3(3) . . ? N4 Re2 Re1 99.8(3) . . ? N2 Re2 N6 81.1(3) . . ? N4 Re2 N6 82.0(3) . . ? Re1 Re2 N6 174.68(17) . . ? N2 Re2 P4 163.1(3) . . ? N4 Re2 P4 89.5(2) . . ? Re1 Re2 P4 100.99(7) . . ? N6 Re2 P4 83.96(18) . . ? N2 Re2 P2 93.5(3) . . ? N4 Re2 P2 168.8(3) . . ? Re1 Re2 P2 90.16(7) . . ? N6 Re2 P2 87.6(2) . . ? P4 Re2 P2 93.67(9) . . ? C1B P1 C111 106.6(5) . . ? C1B P1 C121 104.4(5) . . ? C111 P1 C121 97.6(5) . . ? C1B P1 Re1 106.0(3) . . ? C111 P1 Re1 121.4(4) . . ? C121 P1 Re1 119.2(4) . . ? C1B P2 C221 106.9(5) . . ? C1B P2 C211 103.7(5) . . ? C221 P2 C211 99.0(5) . . ? C1B P2 Re2 107.3(3) . . ? C221 P2 Re2 117.9(4) . . ? C211 P2 Re2 120.6(4) . . ? C2B P3 C311 106.3(6) . . ? C2B P3 C321 102.7(5) . . ? C311 P3 C321 100.9(5) . . ? C2B P3 Re1 107.3(3) . . ? C311 P3 Re1 118.1(4) . . ? C321 P3 Re1 119.9(4) . . ? C421 P4 C2B 106.3(5) . . ? C421 P4 C411 98.2(5) . . ? C2B P4 C411 104.8(5) . . ? C421 P4 Re2 120.5(3) . . ? C2B P4 Re2 106.4(3) . . ? C411 P4 Re2 119.2(3) . . ? B4 F43 F41' 57.7(12) . . ? C1 N1 Re1 173.3(9) . . ? C3 N2 Re2 176.9(9) . . ? C6 N3 Re1 161.2(11) . . ? C7 N4 Re2 173.4(8) . . ? C11 N6 Re2 174.1(8) . . ? N1 C1 C2 175.3(12) . . ? N2 C3 C4 174.4(13) . . ? N3 C6 C5 177.9(15) . . ? N4 C7 C8 175.5(14) . . ? N6 C11 C12 177.1(12) . . ? C112 C111 C116 118.7(10) . . ? C112 C111 P1 116.8(8) . . ? C116 C111 P1 124.3(9) . . ? C113 C112 C111 120.9(11) . . ? C114 C113 C112 119.6(12) . . ? C115 C114 C113 120.8(11) . . ? C114 C115 C116 120.0(11) . . ? C111 C116 C115 120.0(11) . . ? C122 C121 C126 118.6(10) . . ? C122 C121 P1 118.2(9) . . ? C126 C121 P1 123.1(9) . . ? C121 C122 C123 120.6(12) . . ? C124 C123 C122 120.4(13) . . ? C123 C124 C125 119.7(13) . . ? C126 C125 C124 121.6(14) . . ? C125 C126 C121 118.9(13) . . ? C216 C211 C212 121.6(11) . . ? C216 C211 P2 118.6(9) . . ? C212 C211 P2 119.8(9) . . ? C213 C212 C211 117.8(12) . . ? C212 C213 C214 121.1(12) . . ? C215 C214 C213 118.0(12) . . ? C214 C215 C216 122.7(12) . . ? C215 C216 C211 118.7(11) . . ? C226 C221 C222 119.7(9) . . ? C226 C221 P2 122.2(8) . . ? C222 C221 P2 117.7(8) . . ? C223 C222 C221 119.2(11) . . ? C224 C223 C222 120.7(11) . . ? C223 C224 C225 120.5(11) . . ? C224 C225 C226 119.0(11) . . ? C221 C226 C225 120.7(10) . . ? C316 C311 C312 116.3(14) . . ? C316 C311 P3 119.4(13) . . ? C312 C311 P3 124.0(11) . . ? C313 C312 C311 123.8(18) . . ? C314 C313 C312 120(2) . . ? C313 C314 C315 121(2) . . ? C314 C315 C316 121(2) . . ? C311 C316 C315 117.5(18) . . ? C322 C321 C326 120.0(10) . . ? C322 C321 P3 123.1(9) . . ? C326 C321 P3 116.8(9) . . ? C321 C322 C323 120.5(11) . . ? C322 C323 C324 120.5(12) . . ? C323 C324 C325 117.4(12) . . ? C326 C325 C324 122.5(12) . . ? C325 C326 C321 119.0(12) . . ? C412 C411 C416 118.6(10) . . ? C412 C411 P4 124.9(8) . . ? C416 C411 P4 116.4(9) . . ? C411 C412 C413 120.8(10) . . ? C414 C413 C412 119.2(12) . . ? C415 C414 C413 121.2(12) . . ? C414 C415 C416 119.5(12) . . ? C415 C416 C411 120.6(12) . . ? C426 C421 C422 119.7(11) . . ? C426 C421 P4 116.3(8) . . ? C422 C421 P4 123.8(9) . . ? C421 C422 C423 119.2(12) . . ? C424 C423 C422 119.7(11) . . ? C423 C424 C425 121.7(11) . . ? C424 C425 C426 117.8(12) . . ? C421 C426 C425 121.4(11) . . ? F14' B1 F13 111.5(8) . . ? F14' B1 F12 121.2(9) . . ? F13 B1 F12 108.6(7) . . ? F14' B1 F11 101.4(11) . . ? F13 B1 F11 106.9(7) . . ? F12 B1 F11 106.0(7) . . ? F14' B1 F14 22.9(9) . . ? F13 B1 F14 108.0(8) . . ? F12 B1 F14 103.8(9) . . ? F11 B1 F14 122.9(11) . . ? F22 B2 F21 112.0(8) . . ? F22 B2 F23 110.0(8) . . ? F21 B2 F23 104.2(8) . . ? F22 B2 F24 110.2(8) . . ? F21 B2 F24 111.9(8) . . ? F23 B2 F24 108.3(8) . . ? F34 B3 F32 111.4(9) . . ? F34 B3 F33 117.4(11) . . ? F32 B3 F33 99.3(11) . . ? F34 B3 F31 105.6(8) . . ? F32 B3 F31 108.0(9) . . ? F33 B3 F31 114.7(11) . . ? F34 B3 F33' 101.9(13) . . ? F32 B3 F33' 127.8(15) . . ? F33 B3 F33' 28.5(11) . . ? F31 B3 F33' 99.8(12) . . ? F41 B4 F43 112.2(13) . . ? F41 B4 F44 117.5(15) . . ? F43 B4 F44 112.4(13) . . ? F41 B4 F42 94.6(14) . . ? F43 B4 F42 111.0(16) . . ? F44 B4 F42 107.6(15) . . ? F41 B4 F41' 67.5(18) . . ? F43 B4 F41' 69.8(18) . . ? F44 B4 F41' 90(2) . . ? F42 B4 F41' 160(2) . . ? B4 F41' F43 52.4(10) . . ? P1 C1B P2 112.2(5) . . ? P3 C2B P4 111.5(5) . . ? C9 N5 Re1 159.0(8) . . ? N5 C9 C10 175.4(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.704 _refine_diff_density_min -2.258 _refine_diff_density_rms 0.189 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 604234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H62 N6 P4 Re2, 4(B F4), 2(C2 H3 N)' _chemical_formula_sum 'C66 H68 B4 F16 N8 P4 Re2' _chemical_formula_weight 1816.80 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' N N 0.0061 0.0033 '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' 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 12.510(3) _cell_length_b 12.791(3) _cell_length_c 23.341(5) _cell_angle_alpha 84.69(3) _cell_angle_beta 89.50(3) _cell_angle_gamma 79.08(3) _cell_volume 3651.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 111 _cell_measurement_theta_min 2.871 _cell_measurement_theta_max 21.553 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 3.486 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4761 _exptl_absorpt_correction_T_max 0.6600 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker SMART APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22186 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 23.34 _reflns_number_total 10464 _reflns_number_gt 6541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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^)+(0.1007P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00103(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10464 _refine_ls_number_parameters 473 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1813 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 Re1 Re 0.99170(5) -0.44544(5) 0.45734(2) 0.0238(2) Uani 1 1 d . . . Re2 Re 0.49719(4) 0.03420(4) 0.04426(2) 0.0180(2) Uani 1 1 d . . . P1 P 1.1825(3) -0.4230(3) 0.45611(17) 0.0356(11) Uani 1 1 d . . . P2 P 0.7944(3) -0.4292(3) 0.43619(17) 0.0316(10) Uani 1 1 d . . . P3 P 0.6876(3) -0.0394(3) 0.07535(15) 0.0234(9) Uani 1 1 d . . . P4 P 0.3070(3) 0.1278(3) 0.03680(16) 0.0290(9) Uani 1 1 d . . . N1 N 1.0389(9) -0.5704(9) 0.4084(5) 0.025(3) Uiso 1 1 d . . . N2 N 0.9419(9) -0.2949(9) 0.4824(5) 0.025(3) Uani 1 1 d . . . N3 N 0.9808(10) -0.3482(9) 0.3662(5) 0.030(3) Uani 1 1 d . . . N4 N 0.4349(8) -0.0864(9) 0.0878(5) 0.022(3) Uani 1 1 d . . . N5 N 0.4940(9) 0.0966(9) 0.1367(5) 0.025(3) Uani 1 1 d . . . N6 N 0.5554(9) 0.1717(8) 0.0236(5) 0.028(3) Uani 1 1 d . . . C11 C 1.0651(13) -0.6302(14) 0.3769(7) 0.041(4) Uiso 1 1 d . . . C12 C 1.0886(15) -0.7125(15) 0.3370(8) 0.058(5) Uiso 1 1 d . . . H12A H 1.0634 -0.7769 0.3533 0.087 Uiso 1 1 calc R . . H12B H 1.1673 -0.7296 0.3306 0.087 Uiso 1 1 calc R . . H12C H 1.0510 -0.6864 0.3003 0.087 Uiso 1 1 calc R . . C12A C 0.7365(12) -0.4571(13) 0.5057(6) 0.038(4) Uiso 1 1 d . . . H12D H 0.6609 -0.4678 0.5008 0.045 Uiso 1 1 calc R . . H12E H 0.7344 -0.3954 0.5287 0.045 Uiso 1 1 calc R . . C13 C 0.9110(11) -0.2095(12) 0.4902(6) 0.024(3) Uiso 1 1 d . . . C14 C 0.8747(13) -0.0973(13) 0.4981(7) 0.046(4) Uiso 1 1 d . . . H14A H 0.9057 -0.0812 0.5339 0.070 Uiso 1 1 calc R . . H14B H 0.7951 -0.0813 0.5000 0.070 Uiso 1 1 calc R . . H14C H 0.8988 -0.0535 0.4656 0.070 Uiso 1 1 calc R . . C15 C 0.9693(13) -0.2958(14) 0.3252(8) 0.044(4) Uiso 1 1 d . . . C16 C 0.9607(17) -0.2337(17) 0.2682(9) 0.072(6) Uiso 1 1 d . . . H16A H 1.0338 -0.2298 0.2538 0.108 Uiso 1 1 calc R . . H16B H 0.9198 -0.1613 0.2717 0.108 Uiso 1 1 calc R . . H16C H 0.9228 -0.2689 0.2413 0.108 Uiso 1 1 calc R . . C17 C 0.3985(11) -0.1467(12) 0.1166(6) 0.030(4) Uiso 1 1 d . . . C18 C 0.3576(13) -0.2288(13) 0.1530(7) 0.044(4) Uiso 1 1 d . . . H18A H 0.2778 -0.2118 0.1533 0.067 Uiso 1 1 calc R . . H18B H 0.3857 -0.2315 0.1923 0.067 Uiso 1 1 calc R . . H18C H 0.3817 -0.2983 0.1379 0.067 Uiso 1 1 calc R . . C19 C 0.5020(12) 0.1260(12) 0.1795(7) 0.031(4) Uiso 1 1 d . . . C20 C 0.5111(13) 0.1622(14) 0.2368(7) 0.046(4) Uiso 1 1 d . . . H20A H 0.5155 0.2382 0.2329 0.069 Uiso 1 1 calc R . . H20B H 0.5769 0.1208 0.2562 0.069 Uiso 1 1 calc R . . H20C H 0.4471 0.1518 0.2595 0.069 Uiso 1 1 calc R . . C21 C 0.5879(13) 0.2475(14) 0.0160(7) 0.042(4) Uiso 1 1 d . . . C22 C 0.6229(16) 0.3494(16) 0.0048(9) 0.066(6) Uiso 1 1 d . . . H22A H 0.6807 0.3430 -0.0240 0.098 Uiso 1 1 calc R . . H22B H 0.6505 0.3697 0.0405 0.098 Uiso 1 1 calc R . . H22C H 0.5611 0.4043 -0.0097 0.098 Uiso 1 1 calc R . . C34A C 0.2363(11) 0.0566(11) -0.0082(6) 0.023(3) Uiso 1 1 d . . . H34A H 0.1617 0.0973 -0.0167 0.028 Uiso 1 1 calc R . . H34B H 0.2308 -0.0141 0.0115 0.028 Uiso 1 1 calc R . . C212 C 0.6463(16) -0.5460(16) 0.3943(9) 0.064(5) Uiso 1 1 d . . . H212 H 0.6011 -0.5342 0.4269 0.076 Uiso 1 1 calc R . . C111 C 1.2206(14) -0.3127(15) 0.4887(8) 0.052(5) Uiso 1 1 d . . . C112 C 1.1645(15) -0.2671(15) 0.5352(8) 0.055(5) Uiso 1 1 d . . . H112 H 1.0976 -0.2871 0.5469 0.067 Uiso 1 1 calc R . . C113 C 1.2053(16) -0.1927(16) 0.5648(9) 0.064(6) Uiso 1 1 d . . . H113 H 1.1663 -0.1620 0.5961 0.077 Uiso 1 1 calc R . . C114 C 1.3001(17) -0.1649(17) 0.5485(9) 0.070(6) Uiso 1 1 d . . . H114 H 1.3250 -0.1115 0.5676 0.084 Uiso 1 1 calc R . . C115 C 1.3585(19) -0.2077(19) 0.5082(10) 0.082(7) Uiso 1 1 d . . . H115 H 1.4261 -0.1861 0.5002 0.098 Uiso 1 1 calc R . . C116 C 1.3276(19) -0.2880(19) 0.4736(10) 0.083(7) Uiso 1 1 d . . . H116 H 1.3723 -0.3205 0.4446 0.100 Uiso 1 1 calc R . . C121 C 1.2359(13) -0.4157(14) 0.3830(7) 0.045(4) Uiso 1 1 d . . . C122 C 1.2872(14) -0.5080(15) 0.3601(8) 0.054(5) Uiso 1 1 d . . . H122 H 1.2997 -0.5745 0.3831 0.065 Uiso 1 1 calc R . . C123 C 1.3202(14) -0.5021(16) 0.3031(8) 0.056(5) Uiso 1 1 d . . . H123 H 1.3547 -0.5652 0.2869 0.067 Uiso 1 1 calc R . . C124 C 1.3037(16) -0.4070(17) 0.2701(9) 0.072(6) Uiso 1 1 d . . . H124 H 1.3255 -0.4035 0.2310 0.086 Uiso 1 1 calc R . . C125 C 1.2533(15) -0.3123(17) 0.2951(8) 0.060(5) Uiso 1 1 d . . . H125 H 1.2420 -0.2450 0.2729 0.072 Uiso 1 1 calc R . . C126 C 1.2220(13) -0.3197(14) 0.3505(7) 0.041(4) Uiso 1 1 d . . . H126 H 1.1895 -0.2566 0.3673 0.050 Uiso 1 1 calc R . . C221 C 0.7234(12) -0.2958(13) 0.4110(7) 0.036(4) Uiso 1 1 d . . . C226 C 0.6727(13) -0.2261(14) 0.4485(8) 0.049(5) Uiso 1 1 d . . . H226 H 0.6699 -0.2486 0.4883 0.058 Uiso 1 1 calc R . . C225 C 0.6232(13) -0.1171(14) 0.4267(7) 0.049(5) Uiso 1 1 d . . . H225 H 0.5937 -0.0668 0.4529 0.058 Uiso 1 1 calc R . . C224 C 0.6192(14) -0.0880(15) 0.3706(7) 0.049(5) Uiso 1 1 d . . . H224 H 0.5865 -0.0169 0.3570 0.059 Uiso 1 1 calc R . . C223 C 0.6619(14) -0.1591(14) 0.3316(8) 0.052(5) Uiso 1 1 d . . . H223 H 0.6556 -0.1379 0.2915 0.063 Uiso 1 1 calc R . . C222 C 0.7164(14) -0.2665(15) 0.3519(8) 0.053(5) Uiso 1 1 d . . . H222 H 0.7467 -0.3159 0.3255 0.064 Uiso 1 1 calc R . . C211 C 0.7472(14) -0.5089(14) 0.3843(7) 0.047(4) Uiso 1 1 d . . . C213 C 0.6246(18) -0.6054(18) 0.3457(9) 0.076(6) Uiso 1 1 d . . . H213 H 0.5583 -0.6315 0.3476 0.092 Uiso 1 1 calc R . . C214 C 0.6831(18) -0.6265(18) 0.3011(10) 0.076(6) Uiso 1 1 d . . . H214 H 0.6585 -0.6637 0.2720 0.092 Uiso 1 1 calc R . . C215 C 0.7816(16) -0.5943(16) 0.2966(9) 0.062(5) Uiso 1 1 d . . . H215 H 0.8273 -0.6119 0.2648 0.074 Uiso 1 1 calc R . . C216 C 0.8151(14) -0.5360(13) 0.3384(7) 0.043(4) Uiso 1 1 d . . . H216 H 0.8840 -0.5149 0.3355 0.052 Uiso 1 1 calc R . . C311 C 0.7190(12) -0.1614(10) 0.1210(5) 0.040(4) Uiso 1 1 d G . . C312 C 0.6431(9) -0.1884(9) 0.1619(5) 0.055(5) Uiso 1 1 d G . . H312 H 0.5752 -0.1415 0.1655 0.066 Uiso 1 1 calc R . . C313 C 0.6678(15) -0.2848(13) 0.1976(6) 0.076(6) Uiso 1 1 d G . . H313 H 0.6197 -0.3018 0.2273 0.091 Uiso 1 1 calc R . . C314 C 0.765(2) -0.354(2) 0.1880(11) 0.099(8) Uiso 1 1 d . . . H314 H 0.7766 -0.4255 0.2061 0.119 Uiso 1 1 calc R . . C315 C 0.8415(14) -0.3244(14) 0.1546(7) 0.047(4) Uiso 1 1 d . . . H315 H 0.9120 -0.3675 0.1529 0.057 Uiso 1 1 calc R . . C316 C 0.8142(15) -0.2288(15) 0.1228(8) 0.053(5) Uiso 1 1 d . . . H316 H 0.8696 -0.2076 0.0989 0.064 Uiso 1 1 calc R . . C321 C 0.7588(14) 0.0484(14) 0.1113(8) 0.048(5) Uiso 1 1 d . . . C322 C 0.7601(16) 0.0415(15) 0.1722(8) 0.069(6) Uiso 1 1 d G . . H322 H 0.7221 -0.0063 0.1938 0.082 Uiso 1 1 calc R . . C323 C 0.818(2) 0.106(2) 0.2005(11) 0.094(8) Uiso 1 1 d . . . H323 H 0.8242 0.1013 0.2412 0.113 Uiso 1 1 calc R . . C324 C 0.864(2) 0.175(2) 0.1668(11) 0.094(8) Uiso 1 1 d . . . H324 H 0.9034 0.2176 0.1866 0.113 Uiso 1 1 calc R . . C325 C 0.8641(19) 0.192(2) 0.1136(11) 0.089(7) Uiso 1 1 d . . . H325 H 0.8972 0.2459 0.0944 0.107 Uiso 1 1 calc R . . C326 C 0.8098(15) 0.1228(16) 0.0828(9) 0.061(5) Uiso 1 1 d . . . H326 H 0.8098 0.1297 0.0419 0.073 Uiso 1 1 calc R . . C411 C 0.2387(13) 0.1280(13) 0.1046(7) 0.041(4) Uiso 1 1 d . . . C412 C 0.2571(15) 0.1979(15) 0.1423(8) 0.056(5) Uiso 1 1 d . . . H412 H 0.3014 0.2487 0.1308 0.067 Uiso 1 1 calc R . . C413 C 0.2139(15) 0.1971(17) 0.1961(9) 0.064(5) Uiso 1 1 d . . . H413 H 0.2234 0.2488 0.2214 0.076 Uiso 1 1 calc R . . C414 C 0.1592(15) 0.1227(15) 0.2112(8) 0.058(5) Uiso 1 1 d . . . H414 H 0.1324 0.1211 0.2494 0.069 Uiso 1 1 calc R . . C415 C 0.1355(16) 0.0473(17) 0.1792(9) 0.066(6) Uiso 1 1 d . . . H415 H 0.0939 -0.0044 0.1933 0.080 Uiso 1 1 calc R . . C416 C 0.1777(14) 0.0516(15) 0.1228(8) 0.055(5) Uiso 1 1 d . . . H416 H 0.1642 0.0018 0.0972 0.066 Uiso 1 1 calc R . . C421 C 0.2783(8) 0.2717(10) 0.0060(6) 0.041(4) Uiso 1 1 d G . . C422 C 0.3486(8) 0.3071(9) -0.0346(4) 0.053(5) Uiso 1 1 d G . . H422 H 0.4149 0.2615 -0.0430 0.063 Uiso 1 1 calc R . . C423 C 0.3218(9) 0.4093(11) -0.0628(6) 0.071(6) Uiso 1 1 d G . . H423 H 0.3700 0.4339 -0.0903 0.086 Uiso 1 1 calc R . . C424 C 0.2242(19) 0.475(2) -0.0505(10) 0.091(7) Uiso 1 1 d . . . H424 H 0.2048 0.5444 -0.0703 0.110 Uiso 1 1 calc R . . C425 C 0.1549(17) 0.4396(17) -0.0093(9) 0.071(6) Uiso 1 1 d . . . H425 H 0.0935 0.4874 0.0035 0.085 Uiso 1 1 calc R . . C426 C 0.1772(18) 0.3314(18) 0.0134(10) 0.079(7) Uiso 1 1 d . . . H426 H 0.1226 0.3006 0.0335 0.095 Uiso 1 1 calc R . . N1S N 1.0236(15) -0.5199(15) 0.2407(8) 0.086(6) Uiso 1 1 d . . . C1S C 1.0822(14) -0.5148(14) 0.2032(8) 0.074(6) Uiso 1 1 d G . . C2S C 1.1440(14) -0.5059(14) 0.1507(8) 0.108(9) Uiso 1 1 d G . . H2S1 H 1.1314 -0.5603 0.1259 0.162 Uiso 1 1 calc R . . H2S2 H 1.2217 -0.5168 0.1602 0.162 Uiso 1 1 calc R . . H2S3 H 1.1206 -0.4347 0.1305 0.162 Uiso 1 1 calc R . . N2S N 0.4233(13) -0.0800(13) 0.2512(7) 0.064(5) Uiso 1 1 d . . . C3S C 0.3833(15) -0.0691(15) 0.2919(8) 0.056(5) Uiso 1 1 d . . . C4S C 0.3280(19) -0.064(2) 0.3471(10) 0.091(7) Uiso 1 1 d . . . H4S1 H 0.2495 -0.0575 0.3409 0.137 Uiso 1 1 calc R . . H4S2 H 0.3421 -0.0026 0.3656 0.137 Uiso 1 1 calc R . . H4S3 H 0.3553 -0.1300 0.3718 0.137 Uiso 1 1 calc R . . B3 B 1.0121(12) -0.0319(12) 0.3590(7) 0.073(7) Uiso 1 1 d D . . F33 F 0.9073(10) -0.0403(11) 0.3546(5) 0.106(5) Uiso 1 1 d D . . F31 F 1.0688(10) -0.0589(11) 0.3114(5) 0.110(5) Uiso 1 1 d D . . F32 F 1.0589(12) -0.0953(14) 0.4049(6) 0.145(6) Uiso 1 1 d D . . F34 F 1.0221(14) 0.0650(14) 0.3723(8) 0.167(7) Uiso 1 1 d D . . B4 B 1.3760(12) -0.8078(12) 0.3994(7) 0.097(10) Uiso 1 1 d D . . F42 F 1.2749(8) -0.7719(8) 0.4187(4) 0.063(3) Uiso 1 1 d D A . F44 F 1.4171(11) -0.9039(11) 0.4267(6) 0.109(5) Uiso 1 1 d D A . F43 F 1.3660(14) -0.8164(14) 0.3435(7) 0.174(8) Uiso 1 1 d D A . F41 F 1.4348(12) -0.7359(12) 0.4128(7) 0.098(7) Uiso 0.740(18) 1 d PD A 1 F41' F 1.440(3) -0.760(3) 0.3647(15) 0.051(12) Uiso 0.260(18) 1 d PD A 2 B1 B 0.4662(10) 0.4245(10) 0.1440(6) 0.040(5) Uiso 1 1 d D . . F13 F 0.4012(8) 0.3887(9) 0.1857(5) 0.076(3) Uiso 1 1 d D A . F12 F 0.4320(10) 0.3919(12) 0.0936(5) 0.110(5) Uiso 1 1 d D A . F11 F 0.5730(10) 0.3830(12) 0.1530(7) 0.081(5) Uiso 0.740(18) 1 d PD A 1 F11' F 0.548(2) 0.352(2) 0.1227(16) 0.047(11) Uiso 0.260(18) 1 d PD A 2 F14 F 0.4472(11) 0.5326(10) 0.1381(8) 0.075(5) Uiso 0.740(18) 1 d PD A 1 F14' F 0.442(3) 0.520(3) 0.103(2) 0.057(12) Uiso 0.260(18) 1 d P A 2 B2 B 0.1036(9) -0.2082(11) 0.0704(6) 0.058(6) Uiso 1 1 d D . . F22 F 0.0970(9) -0.2357(9) 0.1292(5) 0.080(3) Uiso 1 1 d D A . F24 F 0.0958(10) -0.2972(10) 0.0446(6) 0.102(4) Uiso 1 1 d D A . F21 F 0.2022(7) -0.1766(9) 0.0598(5) 0.032(3) Uiso 0.740(18) 1 d PD A 1 F21' F 0.196(2) -0.201(3) 0.0369(16) 0.039(10) Uiso 0.260(18) 1 d PD A 2 F23 F 0.0192(9) -0.1242(10) 0.0558(6) 0.057(4) Uiso 0.740(18) 1 d PD A 1 F23' F 0.027(2) -0.149(3) 0.0298(13) 0.034(9) Uiso 0.260(18) 1 d PD 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 Re1 0.0410(4) 0.0221(4) 0.0114(3) 0.0003(3) 0.0017(3) -0.0151(3) Re2 0.0202(3) 0.0188(3) 0.0152(3) 0.0009(2) 0.0046(2) -0.0051(2) P1 0.045(3) 0.042(3) 0.024(2) 0.0074(19) 0.0036(18) -0.023(2) P2 0.045(2) 0.027(2) 0.026(2) 0.0042(18) -0.0065(18) -0.017(2) P3 0.0190(19) 0.033(2) 0.0185(19) -0.0030(17) 0.0002(15) -0.0052(17) P4 0.026(2) 0.031(2) 0.027(2) -0.0083(18) -0.0029(16) 0.0075(18) N2 0.031(7) 0.029(8) 0.017(6) -0.001(5) 0.011(5) -0.011(6) N3 0.058(8) 0.021(7) 0.017(6) 0.002(6) -0.005(6) -0.023(6) N4 0.014(6) 0.027(7) 0.025(6) 0.008(5) 0.002(5) -0.009(5) N5 0.023(6) 0.031(7) 0.020(7) -0.012(6) 0.013(5) 0.001(6) N6 0.033(7) 0.005(6) 0.048(8) -0.002(5) 0.015(6) -0.010(5) _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 2.044(12) . ? Re1 N2 2.046(12) . ? Re1 Re1 2.3109(13) 2_746 ? Re1 N3 2.354(11) . ? Re1 P1 2.457(4) . ? Re1 P2 2.488(4) . ? Re2 N4 2.043(10) . ? Re2 N6 2.044(10) . ? Re2 Re2 2.3126(12) 2_655 ? Re2 N5 2.366(11) . ? Re2 P4 2.452(4) . ? Re2 P3 2.479(4) . ? P1 C111 1.80(2) . ? P1 C12A 1.829(15) 2_746 ? P1 C121 1.828(17) . ? P2 C12A 1.804(15) . ? P2 C221 1.816(16) . ? P2 C211 1.823(19) . ? P3 C311 1.787(13) . ? P3 C321 1.824(19) . ? P3 C34A 1.834(13) 2_655 ? P4 C411 1.792(16) . ? P4 C34A 1.793(14) . ? P4 C421 1.882(12) . ? N1 C11 1.113(18) . ? N2 C13 1.118(17) . ? N3 C15 1.110(18) . ? N4 C17 1.134(16) . ? N5 C19 1.112(18) . ? N6 C21 1.120(19) . ? C11 C12 1.46(2) . ? C12A P1 1.829(15) 2_746 ? C13 C14 1.45(2) . ? C15 C16 1.48(2) . ? C17 C18 1.46(2) . ? C19 C20 1.47(2) . ? C21 C22 1.45(2) . ? C34A P3 1.834(13) 2_655 ? C212 C211 1.44(2) . ? C212 C213 1.48(3) . ? C111 C112 1.40(2) . ? C111 C116 1.46(3) . ? C112 C113 1.40(3) . ? C113 C114 1.34(3) . ? C114 C115 1.28(3) . ? C115 C116 1.47(3) . ? C121 C126 1.36(2) . ? C121 C122 1.38(2) . ? C122 C123 1.39(2) . ? C123 C124 1.36(2) . ? C124 C125 1.43(3) . ? C125 C126 1.35(2) . ? C221 C226 1.37(2) . ? C221 C222 1.39(2) . ? C226 C225 1.46(2) . ? C225 C224 1.33(2) . ? C224 C223 1.38(2) . ? C223 C222 1.45(2) . ? C211 C216 1.39(2) . ? C213 C214 1.29(3) . ? C214 C215 1.37(3) . ? C215 C216 1.40(2) . ? C311 C316 1.33(2) . ? C311 C312 1.408(8) . ? C312 C313 1.407(8) . ? C313 C314 1.40(3) . ? C314 C315 1.32(3) . ? C315 C316 1.36(2) . ? C321 C326 1.36(2) . ? C321 C322 1.42(2) . ? C322 C323 1.41(3) . ? C323 C324 1.33(3) . ? C324 C325 1.24(3) . ? C325 C326 1.45(3) . ? C411 C412 1.36(2) . ? C411 C416 1.38(2) . ? C412 C413 1.36(2) . ? C413 C414 1.30(2) . ? C414 C415 1.35(3) . ? C415 C416 1.41(2) . ? C421 C426 1.37(2) . ? C421 C422 1.391(2) . ? C422 C423 1.391(2) . ? C423 C424 1.39(3) . ? C424 C425 1.39(3) . ? C425 C426 1.41(3) . ? N1S C1S 1.14(2) . ? C1S C2S 1.449(2) . ? N2S C3S 1.08(2) . ? C3S C4S 1.46(3) . ? B3 F34 1.335(14) . ? B3 F33 1.341(14) . ? B3 F31 1.348(14) . ? B3 F32 1.349(14) . ? B4 F41' 1.326(16) . ? B4 F43 1.330(14) . ? B4 F41 1.341(14) . ? B4 F44 1.344(13) . ? B4 F42 1.349(13) . ? F43 F41' 1.40(4) . ? B1 F14 1.351(13) . ? B1 F11 1.351(13) . ? B1 F11' 1.365(16) . ? B1 F13 1.366(12) . ? B1 F12 1.380(13) . ? B1 F14' 1.47(4) . ? F12 F11' 1.57(3) . ? F12 F14' 1.70(4) . ? B2 F24 1.356(13) . ? B2 F23 1.377(13) . ? B2 F21 1.383(13) . ? B2 F22 1.389(12) . ? B2 F21' 1.402(15) . ? B2 F23' 1.414(15) . ? 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 162.7(4) . . ? N1 Re1 Re1 93.4(3) . 2_746 ? N2 Re1 Re1 104.0(3) . 2_746 ? N1 Re1 N3 81.5(4) . . ? N2 Re1 N3 81.2(4) . . ? Re1 Re1 N3 174.8(3) 2_746 . ? N1 Re1 P1 87.2(3) . . ? N2 Re1 P1 91.1(3) . . ? Re1 Re1 P1 94.88(10) 2_746 . ? N3 Re1 P1 84.6(3) . . ? N1 Re1 P2 94.3(3) . . ? N2 Re1 P2 82.8(3) . . ? Re1 Re1 P2 100.68(9) 2_746 . ? N3 Re1 P2 80.1(3) . . ? P1 Re1 P2 164.23(13) . . ? N4 Re2 N6 163.4(5) . . ? N4 Re2 Re2 95.7(3) . 2_655 ? N6 Re2 Re2 100.9(3) . 2_655 ? N4 Re2 N5 82.4(4) . . ? N6 Re2 N5 81.0(4) . . ? Re2 Re2 N5 177.5(3) 2_655 . ? N4 Re2 P4 84.7(3) . . ? N6 Re2 P4 92.8(3) . . ? Re2 Re2 P4 96.23(10) 2_655 . ? N5 Re2 P4 85.2(3) . . ? N4 Re2 P3 94.5(3) . . ? N6 Re2 P3 83.8(3) . . ? Re2 Re2 P3 98.39(10) 2_655 . ? N5 Re2 P3 80.2(3) . . ? P4 Re2 P3 165.36(13) . . ? C111 P1 C12A 105.0(8) . 2_746 ? C111 P1 C121 105.4(8) . . ? C12A P1 C121 106.1(7) 2_746 . ? C111 P1 Re1 120.0(6) . . ? C12A P1 Re1 107.6(5) 2_746 . ? C121 P1 Re1 111.8(6) . . ? C12A P2 C221 104.6(7) . . ? C12A P2 C211 109.8(8) . . ? C221 P2 C211 101.2(8) . . ? C12A P2 Re1 103.7(5) . . ? C221 P2 Re1 115.3(5) . . ? C211 P2 Re1 121.2(6) . . ? C311 P3 C321 102.2(7) . . ? C311 P3 C34A 108.5(6) . 2_655 ? C321 P3 C34A 102.7(7) . 2_655 ? C311 P3 Re2 120.3(5) . . ? C321 P3 Re2 116.9(6) . . ? C34A P3 Re2 104.8(5) 2_655 . ? C411 P4 C34A 106.3(7) . . ? C411 P4 C421 104.6(7) . . ? C34A P4 C421 106.5(7) . . ? C411 P4 Re2 112.9(5) . . ? C34A P4 Re2 107.6(5) . . ? C421 P4 Re2 118.2(4) . . ? C11 N1 Re1 172.3(12) . . ? C13 N2 Re1 172.5(12) . . ? C15 N3 Re1 174.0(13) . . ? C17 N4 Re2 172.8(12) . . ? C19 N5 Re2 173.8(11) . . ? C21 N6 Re2 175.3(14) . . ? N1 C11 C12 173.8(18) . . ? P2 C12A P1 110.4(8) . 2_746 ? N2 C13 C14 177.2(15) . . ? N3 C15 C16 174.8(19) . . ? N4 C17 C18 176.6(16) . . ? N5 C19 C20 178.3(17) . . ? N6 C21 C22 176.2(19) . . ? P4 C34A P3 108.3(7) . 2_655 ? C211 C212 C213 108.9(18) . . ? C112 C111 C116 119.3(19) . . ? C112 C111 P1 122.6(14) . . ? C116 C111 P1 116.7(15) . . ? C111 C112 C113 121.0(18) . . ? C114 C113 C112 120(2) . . ? C115 C114 C113 123(2) . . ? C114 C115 C116 124(2) . . ? C115 C116 C111 113(2) . . ? C126 C121 C122 120.2(16) . . ? C126 C121 P1 119.9(13) . . ? C122 C121 P1 119.9(13) . . ? C123 C122 C121 119.1(18) . . ? C124 C123 C122 121(2) . . ? C123 C124 C125 119(2) . . ? C126 C125 C124 119.1(19) . . ? C125 C126 C121 121.6(18) . . ? C226 C221 C222 119.9(16) . . ? C226 C221 P2 121.5(12) . . ? C222 C221 P2 118.6(13) . . ? C221 C226 C225 119.6(16) . . ? C224 C225 C226 120.3(18) . . ? C225 C224 C223 121.1(18) . . ? C224 C223 C222 120.0(17) . . ? C221 C222 C223 118.8(17) . . ? C216 C211 C212 123.3(18) . . ? C216 C211 P2 117.3(13) . . ? C212 C211 P2 119.3(14) . . ? C214 C213 C212 129(2) . . ? C213 C214 C215 119(2) . . ? C214 C215 C216 120(2) . . ? C215 C216 C211 119.6(17) . . ? C316 C311 C312 114.8(11) . . ? C316 C311 P3 125.0(11) . . ? C312 C311 P3 120.1(9) . . ? C313 C312 C311 120.0 . . ? C312 C313 C314 117.8(14) . . ? C315 C314 C313 122(2) . . ? C316 C315 C314 117(2) . . ? C315 C316 C311 127.7(17) . . ? C326 C321 C322 117.4(18) . . ? C326 C321 P3 123.7(15) . . ? C322 C321 P3 118.9(13) . . ? C323 C322 C321 119.3(19) . . ? C324 C323 C322 116(2) . . ? C325 C324 C323 130(3) . . ? C324 C325 C326 115(3) . . ? C321 C326 C325 121(2) . . ? C412 C411 C416 118.5(16) . . ? C412 C411 P4 118.9(13) . . ? C416 C411 P4 122.2(14) . . ? C413 C412 C411 121.8(19) . . ? C414 C413 C412 117(2) . . ? C413 C414 C415 128(2) . . ? C414 C415 C416 114.4(19) . . ? C411 C416 C415 120.3(19) . . ? C426 C421 C422 120.3(11) . . ? C426 C421 P4 118.6(12) . . ? C422 C421 P4 119.3(5) . . ? C423 C422 C421 120.0 . . ? C422 C423 C424 119.6(12) . . ? C425 C424 C423 120(2) . . ? C424 C425 C426 119(2) . . ? C425 C426 C421 119(2) . . ? N1S C1S C2S 172.4(15) . . ? N2S C3S C4S 175(2) . . ? F34 B3 F33 111.5(12) . . ? F34 B3 F31 111.6(12) . . ? F33 B3 F31 112.2(12) . . ? F34 B3 F32 102.1(16) . . ? F33 B3 F32 110.0(11) . . ? F31 B3 F32 109.0(11) . . ? F41' B4 F43 63.6(18) . . ? F41' B4 F41 52.9(18) . . ? F43 B4 F41 115.3(12) . . ? F41' B4 F44 119(2) . . ? F43 B4 F44 109.9(12) . . ? F41 B4 F44 109.8(11) . . ? F41' B4 F42 131(2) . . ? F43 B4 F42 106.5(11) . . ? F41 B4 F42 105.2(11) . . ? F44 B4 F42 109.9(14) . . ? B4 F43 F41' 58.1(10) . . ? B4 F41' F43 58.3(12) . . ? F14 B1 F11 111.7(11) . . ? F14 B1 F11' 130.7(18) . . ? F11 B1 F11' 40.1(16) . . ? F14 B1 F13 110.1(10) . . ? F11 B1 F13 112.9(10) . . ? F11' B1 F13 118.2(18) . . ? F14 B1 F12 107.2(14) . . ? F11 B1 F12 109.6(10) . . ? F11' B1 F12 70.0(18) . . ? F13 B1 F12 105.0(10) . . ? F14 B1 F14' 35.2(17) . . ? F11 B1 F14' 115.7(18) . . ? F11' B1 F14' 109(2) . . ? F13 B1 F14' 128.7(18) . . ? F12 B1 F14' 73(2) . . ? B1 F12 F11' 54.5(10) . . ? B1 F12 F14' 55.9(17) . . ? F11' F12 F14' 89.8(19) . . ? B1 F11' F12 55.4(11) . . ? B1 F14' F12 50.8(14) . . ? F24 B2 F23 112.8(10) . . ? F24 B2 F21 112.1(10) . . ? F23 B2 F21 110.1(10) . . ? F24 B2 F22 106.1(12) . . ? F23 B2 F22 107.4(10) . . ? F21 B2 F22 108.2(10) . . ? F24 B2 F21' 87.6(19) . . ? F23 B2 F21' 111.8(18) . . ? F21 B2 F21' 27.3(17) . . ? F22 B2 F21' 129.0(19) . . ? F24 B2 F23' 88.4(17) . . ? F23 B2 F23' 29.2(15) . . ? F21 B2 F23' 107.5(16) . . ? F22 B2 F23' 132.4(17) . . ? F21' B2 F23' 96(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.311 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.234 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 604235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 N10 Re2, 2(C2 H3 N), 4(B F4)' _chemical_formula_sum 'C38 H36 B4 F16 N12 Re2' _chemical_formula_weight 1380.43 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' 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' Re Re -1.0185 7.2310 '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' _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 10.682(2) _cell_length_b 11.634(2) _cell_length_c 12.320(3) _cell_angle_alpha 62.42(3) _cell_angle_beta 73.43(3) _cell_angle_gamma 83.90(3) _cell_volume 1300.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 110 _cell_measurement_theta_min 3.322 _cell_measurement_theta_max 23.719 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 4.749 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1155 _exptl_absorpt_correction_T_max 0.1999 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11978 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5974 _reflns_number_gt 5491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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^)+(0.0803P)^2^+1.2706P] 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 5974 _refine_ls_number_parameters 253 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Re1 Re 0.439696(15) 0.579622(16) 0.518044(16) 0.02148(8) Uani 1 1 d . . . N1 N 0.2956(4) 0.4519(4) 0.6680(4) 0.0245(8) Uani 1 1 d . . . N2 N 0.4053(4) 0.2875(4) 0.6248(4) 0.0254(9) Uani 1 1 d . . . N3 N 0.6261(5) 0.2159(4) 0.5233(4) 0.0284(9) Uiso 1 1 d . . . N7 N 0.3245(4) 0.6057(4) 0.4015(4) 0.0247(8) Uani 1 1 d . . . N8 N 0.5138(4) 0.5881(4) 0.6500(4) 0.0265(8) Uani 1 1 d . . . C1 C 0.2015(5) 0.4865(5) 0.7447(5) 0.0295(10) Uani 1 1 d . . . H1 H 0.2050 0.5725 0.7340 0.035 Uiso 1 1 calc R . . C2 C 0.0988(6) 0.4043(6) 0.8392(5) 0.0330(11) Uani 1 1 d . . . H2 H 0.0344 0.4341 0.8909 0.040 Uiso 1 1 calc R . . C4 C 0.1921(5) 0.2371(6) 0.7817(5) 0.0294(11) Uani 1 1 d . . . C5 C 0.2965(5) 0.3244(5) 0.6906(5) 0.0258(10) Uani 1 1 d . . . C6 C 0.4079(6) 0.1623(6) 0.6470(6) 0.0339(12) Uani 1 1 d . . . C7 C 0.3026(6) 0.0735(6) 0.7276(7) 0.0434(15) Uani 1 1 d . . . H7 H 0.3064 -0.0119 0.7355 0.052 Uiso 1 1 calc R . . C8 C 0.1952(6) 0.1101(6) 0.7943(6) 0.0392(13) Uani 1 1 d . . . H8 H 0.1234 0.0509 0.8486 0.047 Uiso 1 1 calc R . . C9 C 0.5334(6) 0.1213(6) 0.5890(7) 0.0347(12) Uani 1 1 d . . . C10 C 0.7499(5) 0.1866(5) 0.4785(5) 0.0303(10) Uani 1 1 d . . . H10 H 0.8162 0.2530 0.4354 0.036 Uiso 1 1 calc R . . C11 C 0.7832(6) 0.0623(6) 0.4936(6) 0.0378(13) Uani 1 1 d . . . H11 H 0.8702 0.0438 0.4600 0.045 Uiso 1 1 calc R . . C12 C 0.6850(7) -0.0347(7) 0.5596(8) 0.0520(18) Uani 1 1 d . . . H12 H 0.7044 -0.1207 0.5715 0.062 Uiso 1 1 calc R . . C13 C 0.5596(7) -0.0046(7) 0.6072(8) 0.0506(18) Uani 1 1 d . . . H13 H 0.4918 -0.0696 0.6520 0.061 Uiso 1 1 calc R . . C71 C 0.2501(5) 0.6229(5) 0.3452(5) 0.0266(10) Uani 1 1 d . . . C72 C 0.1554(6) 0.6429(6) 0.2745(5) 0.0355(12) Uani 1 1 d . . . H72A H 0.0994 0.5647 0.3145 0.053 Uiso 1 1 calc R . . H72B H 0.2011 0.6610 0.1869 0.053 Uiso 1 1 calc R . . H72C H 0.1015 0.7166 0.2745 0.053 Uiso 1 1 calc R . . C81 C 0.5506(5) 0.5972(5) 0.7248(5) 0.0296(10) Uani 1 1 d . . . C82 C 0.5995(6) 0.6084(6) 0.8170(6) 0.0417(13) Uiso 1 1 d . . . H82A H 0.6231 0.5225 0.8751 0.062 Uiso 1 1 calc R . . H82B H 0.5319 0.6434 0.8653 0.062 Uiso 1 1 calc R . . H82C H 0.6769 0.6667 0.7733 0.062 Uiso 1 1 calc R . . N1S N 0.5749(12) 0.7087(12) 0.0992(12) 0.110(3) Uiso 1 1 d . . . C1S C 0.5250(12) 0.7909(12) 0.0319(12) 0.087(3) Uiso 1 1 d . . . C2S C 0.4581(14) 0.8879(13) -0.0531(13) 0.104(4) Uiso 1 1 d . . . H2S1 H 0.4154 0.8483 -0.0889 0.156 Uiso 1 1 calc R . . H2S2 H 0.5209 0.9557 -0.1221 0.156 Uiso 1 1 calc R . . H2S3 H 0.3921 0.9262 -0.0069 0.156 Uiso 1 1 calc R . . C3 C 0.0920(5) 0.2794(6) 0.8567(5) 0.0316(11) Uani 1 1 d . . . H3 H 0.0209 0.2225 0.9182 0.038 Uiso 1 1 calc R . . B1 B 0.9314(5) -0.2778(5) 0.5276(5) 0.0363(13) Uiso 1 1 d D . . F14 F 0.8129(4) -0.3201(4) 0.5335(4) 0.0568(10) Uiso 1 1 d D . . F12 F 0.9162(6) -0.2376(6) 0.6194(6) 0.0882(17) Uiso 1 1 d D . . F13 F 0.9769(6) -0.1692(5) 0.4118(5) 0.0811(15) Uiso 1 1 d D . . F11 F 1.0220(4) -0.3744(4) 0.5438(4) 0.0441(8) Uiso 1 1 d D . . B2 B 0.2312(5) -0.2921(5) 0.8956(5) 0.0367(13) Uiso 1 1 d D . . F21 F 0.3220(4) -0.2428(4) 0.7787(3) 0.0453(8) Uiso 1 1 d D . . F23 F 0.1310(7) -0.3511(7) 0.8863(7) 0.102(2) Uiso 1 1 d D . . F22 F 0.2954(9) -0.3573(8) 0.9869(8) 0.134(3) Uiso 1 1 d D . . F24 F 0.1691(5) -0.1946(4) 0.9234(4) 0.0618(11) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01556(11) 0.02763(12) 0.02703(12) -0.01742(9) -0.00664(8) 0.00471(7) N1 0.020(2) 0.031(2) 0.027(2) -0.0176(17) -0.0082(16) 0.0073(16) N2 0.018(2) 0.032(2) 0.033(2) -0.0201(18) -0.0071(17) 0.0051(16) N7 0.021(2) 0.029(2) 0.0265(19) -0.0160(16) -0.0040(16) 0.0026(15) N8 0.020(2) 0.031(2) 0.034(2) -0.0189(18) -0.0081(17) 0.0039(16) C1 0.026(3) 0.036(3) 0.027(2) -0.016(2) -0.007(2) 0.008(2) C2 0.029(3) 0.041(3) 0.027(2) -0.016(2) -0.004(2) 0.008(2) C4 0.022(2) 0.036(3) 0.032(3) -0.016(2) -0.007(2) 0.004(2) C5 0.021(2) 0.032(2) 0.030(2) -0.018(2) -0.0095(19) 0.0036(19) C6 0.025(3) 0.033(3) 0.047(3) -0.024(2) -0.003(2) 0.001(2) C7 0.033(3) 0.037(3) 0.064(4) -0.032(3) 0.000(3) -0.002(2) C8 0.028(3) 0.037(3) 0.049(3) -0.021(3) -0.002(2) -0.004(2) C9 0.022(3) 0.035(3) 0.050(3) -0.026(3) -0.003(2) 0.003(2) C10 0.020(2) 0.032(3) 0.040(3) -0.018(2) -0.008(2) 0.0033(19) C11 0.024(3) 0.038(3) 0.053(3) -0.027(3) -0.005(2) 0.009(2) C12 0.042(4) 0.033(3) 0.077(5) -0.031(3) -0.001(3) 0.005(3) C13 0.033(3) 0.039(3) 0.079(5) -0.036(3) 0.004(3) -0.002(3) C71 0.023(2) 0.031(2) 0.029(2) -0.0157(19) -0.0081(19) 0.0034(18) C72 0.035(3) 0.041(3) 0.033(3) -0.014(2) -0.020(2) 0.005(2) C81 0.024(2) 0.033(3) 0.034(3) -0.019(2) -0.006(2) 0.0054(19) C3 0.024(2) 0.041(3) 0.027(2) -0.014(2) -0.008(2) 0.006(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 N8 2.044(4) . ? Re1 N7 2.048(4) . ? Re1 N1 2.076(5) . ? Re1 N2 2.143(5) 2_666 ? Re1 N3 2.267(5) 2_666 ? Re1 Re1 2.2844(7) 2_666 ? N1 C1 1.338(7) . ? N1 C5 1.376(7) . ? N2 C6 1.351(7) . ? N2 C5 1.369(7) . ? N2 Re1 2.143(5) 2_666 ? N3 C9 1.340(7) . ? N3 C10 1.353(7) . ? N3 Re1 2.267(5) 2_666 ? N7 C71 1.141(6) . ? N8 C81 1.149(7) . ? C1 C2 1.392(8) . ? C2 C3 1.374(8) . ? C4 C3 1.408(8) . ? C4 C8 1.411(8) . ? C4 C5 1.416(8) . ? C6 C7 1.406(8) . ? C6 C9 1.473(8) . ? C7 C8 1.362(9) . ? C9 C13 1.386(9) . ? C10 C11 1.389(8) . ? C11 C12 1.396(9) . ? C12 C13 1.380(9) . ? C71 C72 1.450(7) . ? C81 C82 1.439(8) . ? N1S C1S 1.139(15) . ? C1S C2S 1.429(17) . ? B1 F12 1.376(6) . ? B1 F14 1.377(5) . ? B1 F11 1.383(5) . ? B1 F13 1.390(6) . ? B2 F22 1.360(7) . ? B2 F21 1.379(5) . ? B2 F24 1.384(6) . ? B2 F23 1.389(6) . ? 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 N8 Re1 N7 162.77(18) . . ? N8 Re1 N1 87.76(17) . . ? N7 Re1 N1 87.77(16) . . ? N8 Re1 N2 87.35(17) . 2_666 ? N7 Re1 N2 96.88(17) . 2_666 ? N1 Re1 N2 175.11(15) . 2_666 ? N8 Re1 N3 85.44(16) . 2_666 ? N7 Re1 N3 80.10(16) . 2_666 ? N1 Re1 N3 107.74(17) . 2_666 ? N2 Re1 N3 71.73(17) 2_666 2_666 ? N8 Re1 Re1 101.68(12) . 2_666 ? N7 Re1 Re1 95.24(12) . 2_666 ? N1 Re1 Re1 94.30(12) . 2_666 ? N2 Re1 Re1 86.82(13) 2_666 2_666 ? N3 Re1 Re1 157.17(12) 2_666 2_666 ? C1 N1 C5 117.8(5) . . ? C1 N1 Re1 123.6(4) . . ? C5 N1 Re1 118.6(3) . . ? C6 N2 C5 116.7(5) . . ? C6 N2 Re1 119.9(4) . 2_666 ? C5 N2 Re1 123.2(4) . 2_666 ? C9 N3 C10 119.2(5) . . ? C9 N3 Re1 116.8(4) . 2_666 ? C10 N3 Re1 123.9(4) . 2_666 ? C71 N7 Re1 172.9(4) . . ? C81 N8 Re1 176.5(4) . . ? N1 C1 C2 124.1(5) . . ? C3 C2 C1 119.0(5) . . ? C3 C4 C8 123.1(5) . . ? C3 C4 C5 119.2(5) . . ? C8 C4 C5 117.7(5) . . ? N2 C5 N1 116.1(5) . . ? N2 C5 C4 123.1(5) . . ? N1 C5 C4 120.8(5) . . ? N2 C6 C7 123.0(6) . . ? N2 C6 C9 115.2(5) . . ? C7 C6 C9 121.6(5) . . ? C8 C7 C6 120.0(6) . . ? C7 C8 C4 119.0(6) . . ? N3 C9 C13 121.7(6) . . ? N3 C9 C6 113.7(5) . . ? C13 C9 C6 124.4(6) . . ? N3 C10 C11 122.1(5) . . ? C10 C11 C12 118.1(5) . . ? C13 C12 C11 119.5(6) . . ? C12 C13 C9 119.3(6) . . ? N7 C71 C72 179.2(5) . . ? N8 C81 C82 178.8(6) . . ? N1S C1S C2S 176.3(14) . . ? C2 C3 C4 118.8(5) . . ? F12 B1 F14 110.1(5) . . ? F12 B1 F11 109.4(5) . . ? F14 B1 F11 111.3(4) . . ? F12 B1 F13 105.9(5) . . ? F14 B1 F13 109.7(5) . . ? F11 B1 F13 110.4(5) . . ? F22 B2 F21 108.4(6) . . ? F22 B2 F24 104.5(5) . . ? F21 B2 F24 111.8(5) . . ? F22 B2 F23 121.6(6) . . ? F21 B2 F23 107.2(5) . . ? F24 B2 F23 103.2(5) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 2.882 _refine_diff_density_min -1.470 _refine_diff_density_rms 0.179 #===END data_compound6 _database_code_depnum_ccdc_archive 'CCDC 604236' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 N10 Re2 S2, 3(B F4), (P F6), 2(C2 H3 N)' _chemical_formula_sum 'C34 H32 B3 F18 N12 P Re2 S2' _chemical_formula_weight 1450.64 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' 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' Re Re -1.0185 7.2310 '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' P P 0.1023 0.0942 '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' _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 10.514(2) _cell_length_b 11.705(2) _cell_length_c 12.235(2) _cell_angle_alpha 65.40(3) _cell_angle_beta 73.15(3) _cell_angle_gamma 83.09(3) _cell_volume 1310.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 221 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 22.71 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 4.829 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2483 _exptl_absorpt_correction_T_max 0.3252 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6557 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4374 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ciftab _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^)+(0.0591P)^2^+2.2734P] 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 4374 _refine_ls_number_parameters 289 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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 Re1 Re 0.435790(17) 0.576344(16) 0.523359(16) 0.02380(10) Uani 1 1 d . . . N1 N 0.2943(4) 0.4516(4) 0.6685(4) 0.0251(9) Uani 1 1 d . . . N2 N 0.4155(4) 0.2921(4) 0.6188(4) 0.0250(9) Uani 1 1 d . . . N3 N 0.6415(4) 0.2255(4) 0.4987(4) 0.0289(9) Uani 1 1 d . . . N7 N 0.3156(4) 0.6038(4) 0.4095(4) 0.0265(9) Uani 1 1 d . . . N8 N 0.5119(4) 0.5840(4) 0.6566(4) 0.0268(9) Uani 1 1 d . . . C1 C 0.1949(5) 0.4880(5) 0.7448(5) 0.0312(11) Uani 1 1 d . B . H1 H 0.1910 0.5738 0.7329 0.037 Uiso 1 1 calc R A 1 C2 C 0.0979(6) 0.4070(6) 0.8398(5) 0.0375(13) Uani 1 1 d . B 1 H2 H 0.0306 0.4349 0.8942 0.045 Uiso 1 1 calc R B 1 C3 C 0.10338(14) 0.28735(12) 0.85149(13) 0.0359(12) Uani 1 1 d . B 1 H3 H 0.0332 0.2322 0.9109 0.043 Uiso 1 1 calc R B 1 S1 S 0.60997(14) -0.01231(12) 0.59301(13) 0.0381(3) Uani 1 1 d R B 1 C11 C 0.76153(14) 0.17728(12) 0.45044(13) 0.0357(12) Uani 1 1 d R B 1 H11 H 0.8357 0.2322 0.3936 0.043 Uiso 1 1 d R B 1 C10 C 0.76211(14) 0.05000(12) 0.49069(13) 0.0367(12) Uani 1 1 d R B 1 H10 H 0.8354 0.0019 0.4663 0.044 Uiso 1 1 calc R B 1 C4 C 0.2052(5) 0.2405(5) 0.7820(5) 0.0314(12) Uani 1 1 d . B 1 C5 C 0.3035(5) 0.3264(5) 0.6898(5) 0.0270(11) Uani 1 1 d . B 1 C6 C 0.4268(6) 0.1682(5) 0.6417(5) 0.0315(12) Uani 1 1 d . B 1 C7 C 0.3280(6) 0.0789(5) 0.7246(6) 0.0386(13) Uani 1 1 d . B 1 H7 H 0.3371 -0.0053 0.7313 0.046 Uiso 1 1 calc R B 1 C8 C 0.2188(6) 0.1148(6) 0.7953(6) 0.0395(13) Uani 1 1 d . B 1 H8 H 0.1521 0.0550 0.8534 0.047 Uiso 1 1 calc R B 1 C9 C 0.5536(6) 0.1354(5) 0.5744(5) 0.0311(11) Uani 1 1 d . B 1 B1 B 0.7734(6) 0.2761(6) 1.1044(6) 0.0342(14) Uani 1 1 d . C 1 F11 F 0.8718(4) 0.3286(4) 1.1257(4) 0.0596(10) Uani 1 1 d . C 1 F12 F 0.7328(4) 0.3579(4) 1.0048(4) 0.0676(12) Uani 1 1 d . C 1 F13 F 0.8336(4) 0.1726(3) 1.0777(4) 0.0530(10) Uani 1 1 d . C 1 F14 F 0.6695(3) 0.2316(3) 1.2110(3) 0.0419(8) Uani 1 1 d . C 1 B2 B 0.1023(4) 0.2806(3) 0.4622(3) 0.0662(8) Uiso 0.50 1 d PD D 1 F21 F 0.1605(11) 0.3466(10) 0.5015(10) 0.062(3) Uiso 0.50 1 d PD D 1 F22 F 0.0364(7) 0.3393(6) 0.3767(6) 0.0401(15) Uiso 0.50 1 d PD D 1 F23 F 0.2094(8) 0.2299(7) 0.3946(8) 0.0511(18) Uiso 0.50 1 d PD D 1 F24 F 0.0282(7) 0.1723(6) 0.5534(7) 0.0335(17) Uiso 0.50 1 d PD D 1 P1 P 0.1023(4) 0.2806(3) 0.4622(3) 0.0662(8) Uiso 0.50 1 d PD E 2 F31 F 0.1248(9) 0.3627(8) 0.5178(8) 0.039(2) Uiso 0.50 1 d PD E 2 F32 F 0.0863(18) 0.2061(16) 0.3904(16) 0.142(6) Uiso 0.50 1 d PD E 2 F33 F 0.2422(8) 0.2275(8) 0.4425(8) 0.0505(18) Uiso 0.50 1 d PD E 2 F34 F -0.0243(10) 0.3482(9) 0.4410(10) 0.073(3) Uiso 0.50 1 d PD E 2 F35 F 0.0431(8) 0.1725(7) 0.5880(8) 0.046(2) Uiso 0.50 1 d PD E 2 F36 F 0.147(2) 0.3857(17) 0.3265(13) 0.179(7) Uiso 0.50 1 d PD E 2 C71 C 0.2409(6) 0.6224(5) 0.3534(5) 0.0342(12) Uani 1 1 d . B . C72 C 0.1437(7) 0.6447(7) 0.2822(6) 0.0471(15) Uani 1 1 d . . . H72A H 0.0944 0.5671 0.3109 0.071 Uiso 1 1 calc R B . H72B H 0.1898 0.6716 0.1935 0.071 Uiso 1 1 calc R . . H72C H 0.0817 0.7106 0.2946 0.071 Uiso 1 1 calc R . . C81 C 0.5453(5) 0.5922(5) 0.7332(5) 0.0305(11) Uani 1 1 d . B . C82 C 0.5867(6) 0.6009(6) 0.8328(6) 0.0398(13) Uiso 1 1 d . . . H82A H 0.6297 0.5222 0.8753 0.060 Uiso 1 1 calc R B . H82B H 0.5088 0.6158 0.8926 0.060 Uiso 1 1 calc R . . H82C H 0.6495 0.6706 0.7978 0.060 Uiso 1 1 calc R . . N1S N 0.5709(9) 0.6975(9) 0.1006(9) 0.097(3) Uiso 1 1 d . . . C1S C 0.5210(8) 0.7796(8) 0.0374(8) 0.067(2) Uiso 1 1 d . . . C2S C 0.4609(9) 0.8786(8) -0.0472(8) 0.073(2) Uiso 1 1 d . . . H2S1 H 0.4312 0.8468 -0.0982 0.109 Uiso 1 1 calc R . . H2S2 H 0.5256 0.9463 -0.1014 0.109 Uiso 1 1 calc R . . H2S3 H 0.3844 0.9111 -0.0004 0.109 Uiso 1 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 0.02436(13) 0.02067(13) 0.02679(14) -0.01018(9) -0.00698(9) 0.00146(8) N1 0.025(2) 0.024(2) 0.025(2) -0.0086(18) -0.0062(17) -0.0001(17) N2 0.027(2) 0.021(2) 0.027(2) -0.0098(18) -0.0073(17) -0.0006(17) N3 0.030(2) 0.026(2) 0.036(2) -0.016(2) -0.0111(19) 0.0047(18) N7 0.028(2) 0.023(2) 0.030(2) -0.0113(18) -0.0096(19) 0.0015(17) N8 0.029(2) 0.025(2) 0.028(2) -0.0129(18) -0.0079(18) 0.0033(17) C1 0.034(3) 0.029(3) 0.029(3) -0.012(2) -0.008(2) 0.007(2) C2 0.034(3) 0.041(3) 0.031(3) -0.013(3) -0.004(2) 0.007(2) C3 0.028(3) 0.038(3) 0.034(3) -0.008(2) -0.008(2) 0.000(2) S1 0.0415(8) 0.0227(7) 0.0479(8) -0.0155(6) -0.0077(6) 0.0028(6) C11 0.039(3) 0.032(3) 0.037(3) -0.017(2) -0.008(2) 0.003(2) C10 0.040(3) 0.028(3) 0.041(3) -0.015(3) -0.011(3) 0.007(2) C4 0.028(3) 0.031(3) 0.030(3) -0.005(2) -0.009(2) -0.002(2) C5 0.028(3) 0.027(3) 0.026(2) -0.009(2) -0.011(2) 0.002(2) C6 0.035(3) 0.026(3) 0.033(3) -0.012(2) -0.007(2) -0.004(2) C7 0.042(3) 0.023(3) 0.047(3) -0.011(3) -0.008(3) -0.004(2) C8 0.036(3) 0.036(3) 0.039(3) -0.009(3) -0.004(2) -0.007(2) C9 0.037(3) 0.021(3) 0.039(3) -0.013(2) -0.013(2) 0.001(2) B1 0.036(3) 0.038(3) 0.025(3) -0.015(3) 0.004(2) -0.012(3) F11 0.054(2) 0.068(3) 0.067(3) -0.038(2) -0.0089(19) -0.0130(19) F12 0.074(3) 0.066(3) 0.042(2) -0.007(2) -0.012(2) 0.012(2) F13 0.044(2) 0.039(2) 0.066(2) -0.0266(18) 0.0131(17) -0.0084(15) F14 0.0438(19) 0.0387(18) 0.0341(17) -0.0129(15) -0.0017(14) 0.0037(15) C71 0.038(3) 0.024(3) 0.039(3) -0.014(2) -0.008(3) 0.007(2) C72 0.051(4) 0.055(4) 0.043(3) -0.021(3) -0.029(3) 0.014(3) C81 0.029(3) 0.025(3) 0.029(3) -0.006(2) -0.003(2) 0.001(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 N7 2.047(4) . ? Re1 N8 2.049(4) . ? Re1 N1 2.081(4) . ? Re1 N2 2.148(4) 2_666 ? Re1 Re1 2.2730(8) 2_666 ? Re1 N3 2.295(4) 2_666 ? N1 C1 1.343(7) . ? N1 C5 1.374(7) . ? N2 C6 1.355(7) . ? N2 C5 1.373(7) . ? N2 Re1 2.148(4) 2_666 ? N3 C9 1.323(7) . ? N3 C11 1.391(4) . ? N3 Re1 2.295(4) 2_666 ? N7 C71 1.132(7) . ? N8 C81 1.134(7) . ? C1 C2 1.385(8) . ? C2 C3 1.343(6) . ? C3 C4 1.374(6) . ? S1 C9 1.702(5) . ? S1 C10 1.7371 . ? C11 C10 1.3604 . ? C4 C8 1.407(8) . ? C4 C5 1.407(8) . ? C6 C7 1.403(8) . ? C6 C9 1.451(8) . ? C7 C8 1.361(9) . ? B1 F12 1.348(8) . ? B1 F14 1.382(7) . ? B1 F11 1.400(7) . ? B1 F13 1.415(8) . ? B2 F22 1.324(7) . ? B2 F21 1.340(9) . ? B2 F23 1.418(8) . ? B2 F24 1.420(7) . ? C71 C72 1.460(8) . ? C81 C82 1.451(8) . ? N1S C1S 1.136(11) . ? C1S C2S 1.421(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 N7 Re1 N8 161.98(17) . . ? N7 Re1 N1 88.16(16) . . ? N8 Re1 N1 87.31(17) . . ? N7 Re1 N2 94.60(16) . 2_666 ? N8 Re1 N2 89.55(17) . 2_666 ? N1 Re1 N2 176.75(14) . 2_666 ? N7 Re1 Re1 96.62(12) . 2_666 ? N8 Re1 Re1 101.11(12) . 2_666 ? N1 Re1 Re1 94.39(12) . 2_666 ? N2 Re1 Re1 87.00(12) 2_666 2_666 ? N7 Re1 N3 80.08(16) . 2_666 ? N8 Re1 N3 84.51(16) . 2_666 ? N1 Re1 N3 106.47(16) . 2_666 ? N2 Re1 N3 72.40(16) 2_666 2_666 ? Re1 Re1 N3 158.68(12) 2_666 2_666 ? C1 N1 C5 118.1(5) . . ? C1 N1 Re1 122.5(4) . . ? C5 N1 Re1 119.4(3) . . ? C6 N2 C5 115.8(5) . . ? C6 N2 Re1 120.7(4) . 2_666 ? C5 N2 Re1 123.4(4) . 2_666 ? C9 N3 C11 111.6(4) . . ? C9 N3 Re1 114.0(3) . 2_666 ? C11 N3 Re1 134.4(3) . 2_666 ? C71 N7 Re1 174.1(4) . . ? C81 N8 Re1 174.9(4) . . ? N1 C1 C2 123.4(5) . . ? C3 C2 C1 117.0(5) . . ? C2 C3 C4 123.4(4) . . ? C9 S1 C10 89.7(2) . . ? C10 C11 N3 113.70(19) . . ? C11 C10 S1 110.5 . . ? C3 C4 C8 125.5(5) . . ? C3 C4 C5 116.9(5) . . ? C8 C4 C5 117.6(5) . . ? N2 C5 N1 115.5(5) . . ? N2 C5 C4 123.5(5) . . ? N1 C5 C4 120.9(5) . . ? N2 C6 C7 123.8(5) . . ? N2 C6 C9 113.3(5) . . ? C7 C6 C9 122.8(5) . . ? C8 C7 C6 119.0(5) . . ? C7 C8 C4 119.8(5) . . ? N3 C9 C6 118.8(5) . . ? N3 C9 S1 114.5(4) . . ? C6 C9 S1 126.4(4) . . ? F12 B1 F14 112.5(5) . . ? F12 B1 F11 111.4(5) . . ? F14 B1 F11 110.3(5) . . ? F12 B1 F13 108.2(5) . . ? F14 B1 F13 108.2(5) . . ? F11 B1 F13 106.0(5) . . ? F22 B2 F21 120.1(6) . . ? F22 B2 F23 100.2(5) . . ? F21 B2 F23 104.7(6) . . ? F22 B2 F24 107.8(5) . . ? F21 B2 F24 117.9(6) . . ? F23 B2 F24 103.0(5) . . ? N7 C71 C72 179.2(7) . . ? N8 C81 C82 179.1(6) . . ? N1S C1S C2S 176.4(10) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.983 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.147 #===END