# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_method SHELXL _publ_contact_author_name 'Julio Perez' _publ_contact_author_address ; JULIO PEREZ Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qu'mica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; _publ_contact_author_phone +34-85-102985 _publ_contact_author_fax +34-85-103446 _publ_contact_author_email japm@sauron.quimica.uniovi.es loop_ _publ_author_name _publ_author_address 'Sonia Nieto' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qu'mica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Julio Perez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qu'mica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Victor Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qu'mica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Daniel Miguel' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Valladolid 47071 Valladolid SPAIN ; 'Celedonio Alvarez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Qu'mica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; _publ_section_title ; Cationic fac-tris(pyrazole) complexes as anion receptors. ; #-------------------------- data section of block --------------------------- data_Compound_1_(sn135am) _database_code_depnum_ccdc_archive 'CCDC 246231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H36 B F24 N6 O3 Re' _chemical_formula_weight 1421.86 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.756(7) _cell_length_b 26.143(12) _cell_length_c 15.501(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.642(9) _cell_angle_gamma 90.00 _cell_volume 5758(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 2.234 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.704985 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26020 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 23.49 _reflns_number_total 8406 _reflns_number_gt 6234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0559P)^2^+27.3091P] 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 8406 _refine_ls_number_parameters 783 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.15377(3) 0.215590(13) 0.12160(2) 0.06327(15) Uani 1 1 d . . . N1 N 0.1402(4) 0.1439(2) 0.1918(4) 0.0523(15) Uani 1 1 d . . . N2 N 0.0923(5) 0.1439(3) 0.2562(5) 0.0643(19) Uani 1 1 d . . . N3 N 0.1230(5) 0.2521(2) 0.2381(5) 0.0618(18) Uani 1 1 d . . . N4 N 0.1835(7) 0.2485(3) 0.3212(6) 0.072(2) Uani 1 1 d . . . N5 N 0.2996(5) 0.2186(3) 0.2036(5) 0.0652(19) Uani 1 1 d . . . N6 N 0.3548(5) 0.1762(4) 0.2262(5) 0.068(2) Uani 1 1 d . . . C1 C 0.1564(9) 0.2806(4) 0.0621(8) 0.097(3) Uani 1 1 d . . . O1 O 0.1520(9) 0.3176(4) 0.0242(7) 0.159(4) Uani 1 1 d . . . C2 C 0.1888(7) 0.1851(4) 0.0221(7) 0.078(3) Uani 1 1 d . . . O2 O 0.2096(6) 0.1689(3) -0.0380(5) 0.120(3) Uani 1 1 d . . . C3 C 0.0242(7) 0.2103(3) 0.0486(6) 0.065(2) Uani 1 1 d . . . O3 O -0.0490(5) 0.2055(3) 0.0032(5) 0.116(3) Uani 1 1 d . . . C11 C 0.0806(7) 0.0972(4) 0.2861(6) 0.074(3) Uani 1 1 d . . . C12 C 0.1212(7) 0.0653(3) 0.2406(6) 0.073(3) Uani 1 1 d . . . H12 H 0.1248 0.0300 0.2468 0.088 Uiso 1 1 calc R . . C13 C 0.1566(6) 0.0939(3) 0.1829(6) 0.061(2) Uani 1 1 d . . . C14 C 0.0299(8) 0.0883(5) 0.3567(7) 0.108(4) Uani 1 1 d . . . H14A H -0.0233 0.1109 0.3467 0.162 Uiso 1 1 calc R . . H14B H 0.0718 0.0948 0.4147 0.162 Uiso 1 1 calc R . . H14C H 0.0086 0.0535 0.3537 0.162 Uiso 1 1 calc R . . C15 C 0.2060(7) 0.0749(4) 0.1169(7) 0.090(3) Uani 1 1 d . . . H15A H 0.1714 0.0849 0.0576 0.134 Uiso 1 1 d R . . H15B H 0.2104 0.0383 0.1203 0.134 Uiso 1 1 d R . . H15C H 0.2681 0.0893 0.1304 0.134 Uiso 1 1 d R . . C21 C 0.1573(8) 0.2762(4) 0.3826(7) 0.083(3) Uani 1 1 d . . . C22 C 0.0751(10) 0.2973(4) 0.3378(8) 0.102(4) Uani 1 1 d . . . H22 H 0.0373 0.3180 0.3625 0.123 Uiso 1 1 calc R . . C23 C 0.0566(8) 0.2834(3) 0.2506(7) 0.080(3) Uani 1 1 d . . . C24 C 0.2163(9) 0.2774(5) 0.4798(8) 0.120(5) Uani 1 1 d . . . H24A H 0.2420 0.2441 0.4971 0.180 Uiso 1 1 calc R . . H24B H 0.1774 0.2874 0.5176 0.180 Uiso 1 1 calc R . . H24C H 0.2665 0.3016 0.4860 0.180 Uiso 1 1 calc R . . C25 C -0.0241(10) 0.2990(5) 0.1748(8) 0.131(5) Uani 1 1 d . . . H25A H -0.0009 0.3152 0.1294 0.196 Uiso 1 1 calc R . . H25B H -0.0633 0.3225 0.1958 0.196 Uiso 1 1 calc R . . H25C H -0.0601 0.2693 0.1501 0.196 Uiso 1 1 calc R . . C31 C 0.4446(7) 0.1852(6) 0.2717(6) 0.086(3) Uani 1 1 d . . . C32 C 0.4471(9) 0.2374(6) 0.2803(8) 0.108(4) Uani 1 1 d . . . H32 H 0.4993 0.2566 0.3097 0.129 Uiso 1 1 calc R . . C33 C 0.3593(8) 0.2567(5) 0.2383(8) 0.095(4) Uani 1 1 d . . . C34 C 0.5130(7) 0.1438(6) 0.2977(7) 0.115(4) Uani 1 1 d . . . H34A H 0.4807 0.1124 0.3018 0.173 Uiso 1 1 calc R . . H34B H 0.5558 0.1515 0.3548 0.173 Uiso 1 1 calc R . . H34C H 0.5475 0.1403 0.2536 0.173 Uiso 1 1 calc R . . C35 C 0.3316(11) 0.3119(5) 0.2325(12) 0.165(7) Uani 1 1 d . . . H35A H 0.3255 0.3242 0.1729 0.248 Uiso 1 1 calc R . . H35B H 0.3790 0.3314 0.2742 0.248 Uiso 1 1 calc R . . H35C H 0.2725 0.3156 0.2468 0.248 Uiso 1 1 calc R . . B51 B 0.7517(6) 0.4198(3) 0.2301(6) 0.050(2) Uani 1 1 d . . . C51 C 0.7172(5) 0.3598(3) 0.2163(4) 0.0448(17) Uani 1 1 d . . . C52 C 0.6355(5) 0.3475(3) 0.1498(5) 0.0529(19) Uani 1 1 d . . . H52 H 0.6027 0.3738 0.1144 0.064 Uiso 1 1 calc R . . C53 C 0.6006(6) 0.2984(3) 0.1337(5) 0.057(2) Uani 1 1 d . . . C54 C 0.6481(6) 0.2587(3) 0.1840(5) 0.061(2) Uani 1 1 d . . . H54 H 0.6260 0.2253 0.1730 0.073 Uiso 1 1 calc R . . C55 C 0.7288(6) 0.2687(3) 0.2509(5) 0.055(2) Uani 1 1 d . . . C56 C 0.7619(5) 0.3182(3) 0.2656(5) 0.0511(18) Uani 1 1 d . . . H56 H 0.8168 0.3240 0.3109 0.061 Uiso 1 1 calc R . . C57 C 0.5139(8) 0.2887(4) 0.0615(7) 0.077(3) Uani 1 1 d . . . C58 C 0.7799(9) 0.2261(4) 0.3066(8) 0.088(3) Uani 1 1 d . . . C61 C 0.8606(5) 0.4236(3) 0.2951(5) 0.0474(17) Uani 1 1 d . . . C62 C 0.9382(6) 0.4358(3) 0.2655(6) 0.061(2) Uani 1 1 d . . . H62 H 0.9299 0.4422 0.2049 0.073 Uiso 1 1 calc R . . C63 C 1.0282(6) 0.4389(4) 0.3231(6) 0.070(2) Uani 1 1 d . . . C64 C 1.0441(6) 0.4303(4) 0.4128(6) 0.071(2) Uani 1 1 d . . . H64 H 1.1046 0.4326 0.4511 0.085 Uiso 1 1 calc R . . C65 C 0.9691(6) 0.4182(3) 0.4453(5) 0.060(2) Uani 1 1 d . . . C66 C 0.8793(5) 0.4151(3) 0.3870(5) 0.0531(19) Uani 1 1 d . . . H66 H 0.8293 0.4071 0.4105 0.064 Uiso 1 1 calc R . . C67 C 1.1088(9) 0.4512(8) 0.2854(9) 0.123(5) Uani 1 1 d . . . C68 C 0.9823(8) 0.4088(6) 0.5415(6) 0.096(4) Uani 1 1 d . . . C71 C 0.7476(5) 0.4428(3) 0.1303(5) 0.0511(18) Uani 1 1 d . . . C72 C 0.7892(5) 0.4153(3) 0.0741(5) 0.056(2) Uani 1 1 d . . . H72 H 0.8144 0.3832 0.0929 0.067 Uiso 1 1 calc R . . C73 C 0.7948(6) 0.4330(3) -0.0072(5) 0.065(2) Uani 1 1 d . . . C74 C 0.7557(7) 0.4801(4) -0.0377(6) 0.078(3) Uani 1 1 d . . . H74 H 0.7600 0.4931 -0.0923 0.094 Uiso 1 1 calc R . . C75 C 0.7108(7) 0.5071(3) 0.0141(6) 0.077(3) Uani 1 1 d . . . C76 C 0.7065(6) 0.4890(3) 0.0960(5) 0.064(2) Uani 1 1 d . . . H76 H 0.6753 0.5081 0.1296 0.077 Uiso 1 1 calc R . . C77 C 0.8445(9) 0.4018(5) -0.0600(7) 0.093(3) Uani 1 1 d . . . C78 C 0.6666(16) 0.5569(6) -0.0193(10) 0.133(6) Uani 1 1 d . . . C81 C 0.6860(5) 0.4516(3) 0.2810(4) 0.0444(17) Uani 1 1 d . . . C82 C 0.6099(5) 0.4310(3) 0.3046(5) 0.0493(18) Uani 1 1 d . . . H82 H 0.5926 0.3974 0.2883 0.059 Uiso 1 1 calc R . . C83 C 0.5584(5) 0.4582(3) 0.3515(5) 0.0544(19) Uani 1 1 d . . . C84 C 0.5820(5) 0.5080(3) 0.3770(5) 0.056(2) Uani 1 1 d . . . H84 H 0.5479 0.5264 0.4088 0.068 Uiso 1 1 calc R . . C85 C 0.6568(5) 0.5296(3) 0.3546(5) 0.0514(18) Uani 1 1 d . . . C86 C 0.7078(5) 0.5024(3) 0.3085(5) 0.0528(19) Uani 1 1 d . . . H86 H 0.7589 0.5180 0.2949 0.063 Uiso 1 1 calc R . . C87 C 0.4791(8) 0.4329(4) 0.3751(7) 0.080(3) Uani 1 1 d . . . C88 C 0.6816(7) 0.5839(4) 0.3813(7) 0.075(3) Uani 1 1 d . . . F1 F 0.4448(5) 0.3177(3) 0.0640(6) 0.152(3) Uani 1 1 d . . . F2 F 0.4846(6) 0.2427(3) 0.0549(6) 0.177(4) Uani 1 1 d . . . F3 F 0.5265(6) 0.2990(4) -0.0176(5) 0.155(3) Uani 1 1 d . . . F4 F 0.7430(6) 0.1825(3) 0.2943(7) 0.168(4) Uani 1 1 d . . . F5 F 0.8612(7) 0.2176(4) 0.2933(9) 0.203(6) Uani 1 1 d . . . F6 F 0.8059(11) 0.2354(4) 0.3888(6) 0.238(7) Uani 1 1 d . . . F7 F 1.1102(7) 0.4243(6) 0.2161(9) 0.239(7) Uani 1 1 d . . . F8 F 1.1036(7) 0.4972(5) 0.2519(9) 0.215(6) Uani 1 1 d . . . F9 F 1.1885(6) 0.4497(5) 0.3396(7) 0.221(6) Uani 1 1 d . . . F10 F 1.0401(7) 0.4418(3) 0.5921(5) 0.165(4) Uani 1 1 d . . . F11 F 1.0357(8) 0.3688(3) 0.5698(5) 0.165(4) Uani 1 1 d . . . F12 F 0.9150(5) 0.4044(7) 0.5686(4) 0.298(10) Uani 1 1 d . . . F13 F 0.9265(6) 0.3871(4) -0.0175(5) 0.167(4) Uani 1 1 d . . . F14 F 0.7977(7) 0.3571(3) -0.0871(6) 0.155(3) Uani 1 1 d . . . F15 F 0.8464(5) 0.4218(3) -0.1373(4) 0.126(3) Uani 1 1 d . . . F16 F 0.5753(11) 0.5540(5) -0.0385(14) 0.287(10) Uani 1 1 d . . . F17 F 0.6783(13) 0.5915(4) 0.0376(8) 0.251(8) Uani 1 1 d . . . F18 F 0.6786(12) 0.5736(4) -0.0881(8) 0.252(8) Uani 1 1 d . . . F19 F 0.4047(5) 0.4278(3) 0.3025(6) 0.141(3) Uani 1 1 d . . . F20 F 0.4924(5) 0.3906(4) 0.4067(9) 0.235(7) Uani 1 1 d . . . F21 F 0.4350(6) 0.4628(3) 0.4192(6) 0.163(4) Uani 1 1 d . . . F22 F 0.7507(6) 0.6027(3) 0.3570(8) 0.171(4) Uani 1 1 d . . . F23 F 0.6162(5) 0.6151(2) 0.3641(7) 0.174(4) Uani 1 1 d . . . F24 F 0.7175(8) 0.5886(3) 0.4689(6) 0.174(4) Uani 1 1 d . . . H6 H 0.331(6) 0.147(3) 0.215(6) 0.06(3) Uiso 1 1 d . . . H4 H 0.231(6) 0.233(3) 0.333(6) 0.06(3) Uiso 1 1 d . . . H2 H 0.084(6) 0.171(3) 0.276(5) 0.06(3) Uiso 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 0.0814(3) 0.0580(2) 0.0574(2) -0.00171(17) 0.03075(18) -0.00102(18) N1 0.054(4) 0.049(4) 0.055(4) 0.001(3) 0.017(3) -0.006(3) N2 0.072(5) 0.060(5) 0.065(5) -0.002(4) 0.026(4) -0.010(4) N3 0.078(5) 0.052(4) 0.060(5) -0.001(3) 0.027(4) 0.003(4) N4 0.067(6) 0.077(6) 0.075(6) -0.017(4) 0.026(5) -0.006(5) N5 0.080(5) 0.066(5) 0.062(4) -0.020(4) 0.040(4) -0.023(4) N6 0.051(5) 0.092(7) 0.063(5) -0.001(4) 0.018(4) -0.017(5) C1 0.149(11) 0.071(7) 0.088(8) 0.003(6) 0.061(8) 0.005(7) O1 0.257(13) 0.091(6) 0.149(8) 0.054(6) 0.091(9) 0.000(7) C2 0.088(7) 0.068(6) 0.079(7) 0.016(5) 0.024(6) -0.001(5) O2 0.169(8) 0.134(7) 0.082(5) -0.031(5) 0.077(6) -0.003(6) C3 0.089(7) 0.064(5) 0.042(5) -0.003(4) 0.019(5) 0.006(5) O3 0.070(5) 0.167(8) 0.088(5) -0.015(5) -0.017(4) 0.018(5) C11 0.070(6) 0.076(7) 0.067(6) 0.010(5) 0.005(5) -0.023(5) C12 0.083(7) 0.052(5) 0.074(6) 0.006(5) 0.003(5) -0.017(5) C13 0.053(5) 0.052(5) 0.068(6) -0.004(4) 0.002(4) 0.001(4) C14 0.123(10) 0.117(9) 0.097(8) 0.012(7) 0.050(7) -0.040(7) C15 0.088(7) 0.068(6) 0.123(9) -0.008(6) 0.047(7) 0.013(5) C21 0.099(8) 0.093(7) 0.073(7) -0.028(6) 0.047(6) -0.030(6) C22 0.134(11) 0.083(7) 0.105(9) -0.025(6) 0.058(8) 0.020(7) C23 0.118(8) 0.062(6) 0.075(6) -0.008(5) 0.050(6) 0.015(6) C24 0.116(10) 0.168(13) 0.084(8) -0.051(8) 0.041(7) -0.041(9) C25 0.156(12) 0.144(11) 0.095(9) 0.016(8) 0.039(9) 0.078(10) C31 0.053(6) 0.152(11) 0.056(6) -0.011(6) 0.021(5) -0.026(7) C32 0.079(9) 0.150(12) 0.098(8) -0.053(8) 0.030(7) -0.073(8) C33 0.074(7) 0.112(9) 0.110(9) -0.040(7) 0.044(7) -0.049(7) C34 0.063(7) 0.203(14) 0.077(7) 0.003(8) 0.015(6) -0.016(8) C35 0.183(15) 0.087(9) 0.25(2) -0.068(11) 0.101(14) -0.066(10) B51 0.062(6) 0.046(5) 0.046(5) 0.001(4) 0.021(4) 0.003(4) C51 0.044(4) 0.054(4) 0.034(4) -0.003(3) 0.009(3) 0.003(3) C52 0.058(5) 0.051(5) 0.046(4) 0.004(4) 0.007(4) 0.007(4) C53 0.060(5) 0.057(5) 0.047(5) -0.003(4) 0.003(4) -0.006(4) C54 0.073(6) 0.050(5) 0.058(5) -0.003(4) 0.014(5) -0.006(4) C55 0.060(5) 0.051(5) 0.050(5) 0.004(4) 0.008(4) 0.006(4) C56 0.049(4) 0.061(5) 0.041(4) 0.001(4) 0.008(4) 0.007(4) C57 0.090(7) 0.060(6) 0.062(6) 0.001(5) -0.010(5) 0.002(5) C58 0.094(8) 0.074(7) 0.082(8) 0.007(6) -0.002(6) 0.008(6) C61 0.051(4) 0.046(4) 0.046(4) -0.003(3) 0.014(4) 0.000(3) C62 0.065(6) 0.066(5) 0.052(5) -0.001(4) 0.015(4) -0.012(4) C63 0.049(5) 0.085(6) 0.075(6) -0.002(5) 0.014(5) -0.014(4) C64 0.048(5) 0.090(7) 0.064(6) -0.007(5) -0.002(4) -0.010(5) C65 0.057(5) 0.068(5) 0.050(5) -0.005(4) 0.004(4) 0.003(4) C66 0.051(5) 0.057(5) 0.054(5) -0.004(4) 0.019(4) 0.001(4) C67 0.070(8) 0.221(18) 0.082(8) 0.014(10) 0.024(7) -0.035(9) C68 0.076(7) 0.149(11) 0.045(6) -0.019(7) -0.015(5) 0.022(7) C71 0.050(4) 0.056(5) 0.045(4) -0.002(4) 0.010(4) -0.004(4) C72 0.055(5) 0.064(5) 0.051(5) 0.004(4) 0.015(4) 0.006(4) C73 0.074(6) 0.079(6) 0.043(5) 0.000(4) 0.019(4) 0.011(5) C74 0.109(8) 0.078(6) 0.049(5) 0.013(5) 0.025(5) 0.002(6) C75 0.114(8) 0.058(5) 0.062(6) 0.010(5) 0.028(6) 0.014(5) C76 0.091(6) 0.051(5) 0.054(5) 0.001(4) 0.023(5) 0.010(4) C77 0.110(9) 0.121(10) 0.053(6) 0.008(6) 0.029(6) 0.031(8) C78 0.221(19) 0.098(11) 0.075(9) 0.025(8) 0.032(10) 0.059(12) C81 0.044(4) 0.050(4) 0.036(4) 0.002(3) 0.005(3) 0.001(3) C82 0.054(5) 0.048(4) 0.044(4) -0.001(3) 0.010(4) -0.002(4) C83 0.055(5) 0.061(5) 0.048(4) -0.005(4) 0.015(4) -0.003(4) C84 0.054(5) 0.062(5) 0.052(5) -0.010(4) 0.014(4) 0.011(4) C85 0.052(5) 0.047(4) 0.050(4) -0.009(4) 0.005(4) 0.003(4) C86 0.053(5) 0.052(5) 0.052(5) 0.001(4) 0.012(4) -0.002(4) C87 0.088(8) 0.086(7) 0.079(7) -0.015(6) 0.045(6) -0.015(6) C88 0.058(6) 0.070(6) 0.094(8) -0.028(5) 0.018(5) -0.009(5) F1 0.083(5) 0.148(7) 0.179(8) -0.052(6) -0.044(5) 0.028(5) F2 0.173(7) 0.082(5) 0.185(8) 0.011(5) -0.106(6) -0.046(5) F3 0.135(6) 0.235(9) 0.063(4) 0.003(5) -0.030(4) -0.044(6) F4 0.143(7) 0.080(5) 0.232(10) 0.065(5) -0.035(6) -0.008(4) F5 0.123(7) 0.165(8) 0.322(16) 0.138(9) 0.065(8) 0.072(6) F6 0.422(19) 0.147(8) 0.090(6) 0.018(5) -0.028(9) 0.152(10) F7 0.160(9) 0.38(2) 0.232(12) -0.116(13) 0.150(9) -0.111(10) F8 0.174(9) 0.241(12) 0.252(13) 0.119(12) 0.094(9) -0.046(8) F9 0.066(5) 0.423(18) 0.175(9) 0.088(10) 0.032(6) -0.047(7) F10 0.236(10) 0.157(7) 0.073(5) -0.029(5) -0.007(5) -0.018(7) F11 0.243(10) 0.151(7) 0.090(5) 0.039(5) 0.028(6) 0.042(7) F12 0.074(5) 0.77(3) 0.050(4) 0.066(9) 0.019(4) 0.003(10) F13 0.125(6) 0.295(12) 0.081(4) -0.002(6) 0.029(4) 0.115(7) F14 0.219(9) 0.129(6) 0.151(7) -0.048(6) 0.108(7) 0.007(6) F15 0.154(6) 0.171(7) 0.074(4) 0.025(4) 0.067(4) 0.049(5) F16 0.221(13) 0.165(12) 0.44(3) 0.150(15) 0.034(16) 0.095(11) F17 0.48(3) 0.097(6) 0.154(9) 0.017(6) 0.042(12) 0.105(10) F18 0.46(2) 0.170(9) 0.182(9) 0.126(8) 0.190(12) 0.167(12) F19 0.095(5) 0.156(7) 0.173(8) -0.014(6) 0.037(5) -0.046(5) F20 0.114(6) 0.208(9) 0.424(17) 0.232(11) 0.140(9) 0.048(6) F21 0.161(7) 0.174(8) 0.206(9) -0.070(7) 0.141(7) -0.065(6) F22 0.172(8) 0.078(4) 0.304(13) -0.068(6) 0.135(8) -0.046(5) F23 0.088(5) 0.067(4) 0.316(12) -0.066(5) -0.031(6) 0.019(4) F24 0.255(11) 0.114(6) 0.113(6) -0.042(5) -0.018(7) -0.050(6) _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 C2 1.926(11) . ? Re1 C1 1.938(11) . ? Re1 C3 1.946(11) . ? Re1 N5 2.186(8) . ? Re1 N3 2.195(7) . ? Re1 N1 2.204(6) . ? N1 C13 1.341(10) . ? N1 N2 1.370(9) . ? N2 C11 1.333(11) . ? N3 C23 1.332(11) . ? N3 N4 1.358(11) . ? N4 C21 1.334(12) . ? N5 C33 1.342(11) . ? N5 N6 1.364(11) . ? N6 C31 1.343(12) . ? C1 O1 1.124(12) . ? C2 O2 1.139(11) . ? C3 O3 1.126(11) . ? C11 C12 1.333(13) . ? C11 C14 1.502(13) . ? C12 C13 1.372(12) . ? C13 C15 1.493(12) . ? C21 C22 1.344(15) . ? C21 C24 1.524(16) . ? C22 C23 1.353(14) . ? C23 C25 1.486(15) . ? C31 C32 1.370(17) . ? C31 C34 1.461(16) . ? C32 C33 1.380(17) . ? C33 C35 1.496(18) . ? B51 C81 1.635(11) . ? B51 C51 1.644(11) . ? B51 C71 1.644(11) . ? B51 C61 1.654(12) . ? C51 C56 1.388(10) . ? C51 C52 1.397(10) . ? C52 C53 1.379(10) . ? C53 C54 1.372(11) . ? C53 C57 1.477(12) . ? C54 C55 1.377(11) . ? C55 C56 1.381(11) . ? C55 C58 1.483(12) . ? C57 F2 1.273(10) . ? C57 F1 1.280(12) . ? C57 F3 1.316(12) . ? C58 F6 1.252(13) . ? C58 F4 1.256(12) . ? C58 F5 1.291(14) . ? C61 C62 1.381(10) . ? C61 C66 1.394(10) . ? C62 C63 1.389(11) . ? C63 C64 1.366(12) . ? C63 C67 1.495(14) . ? C64 C65 1.371(12) . ? C65 C66 1.391(11) . ? C65 C68 1.472(13) . ? C67 F9 1.249(14) . ? C67 F7 1.289(17) . ? C67 F8 1.303(19) . ? C68 F12 1.183(13) . ? C68 F11 1.310(13) . ? C68 F10 1.314(13) . ? C71 C76 1.391(11) . ? C71 C72 1.393(10) . ? C72 C73 1.366(11) . ? C73 C74 1.388(12) . ? C73 C77 1.483(13) . ? C74 C75 1.366(12) . ? C75 C76 1.372(11) . ? C75 C78 1.486(15) . ? C77 F13 1.270(12) . ? C77 F15 1.314(11) . ? C77 F14 1.365(14) . ? C78 F18 1.208(15) . ? C78 F17 1.243(17) . ? C78 F16 1.30(2) . ? C81 C82 1.382(10) . ? C81 C86 1.404(10) . ? C82 C83 1.382(10) . ? C83 C84 1.377(11) . ? C83 C87 1.474(12) . ? C84 C85 1.365(11) . ? C85 C86 1.369(10) . ? C85 C88 1.496(11) . ? C87 F20 1.205(12) . ? C87 F21 1.318(11) . ? C87 F19 1.350(12) . ? C88 F23 1.236(11) . ? C88 F22 1.277(11) . ? C88 F24 1.324(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 C2 Re1 C1 86.4(4) . . ? C2 Re1 C3 86.5(4) . . ? C1 Re1 C3 85.8(5) . . ? C2 Re1 N5 92.7(3) . . ? C1 Re1 N5 95.9(4) . . ? C3 Re1 N5 178.0(3) . . ? C2 Re1 N3 176.4(4) . . ? C1 Re1 N3 92.6(3) . . ? C3 Re1 N3 96.9(3) . . ? N5 Re1 N3 84.0(3) . . ? C2 Re1 N1 97.0(3) . . ? C1 Re1 N1 175.3(4) . . ? C3 Re1 N1 91.2(3) . . ? N5 Re1 N1 87.2(2) . . ? N3 Re1 N1 84.1(2) . . ? C13 N1 N2 102.7(7) . . ? C13 N1 Re1 137.2(6) . . ? N2 N1 Re1 119.5(5) . . ? C11 N2 N1 113.1(8) . . ? C23 N3 N4 103.0(8) . . ? C23 N3 Re1 135.3(7) . . ? N4 N3 Re1 121.4(5) . . ? C21 N4 N3 113.3(9) . . ? C33 N5 N6 102.6(9) . . ? C33 N5 Re1 134.2(8) . . ? N6 N5 Re1 123.1(5) . . ? C31 N6 N5 115.4(10) . . ? O1 C1 Re1 175.4(13) . . ? O2 C2 Re1 177.3(9) . . ? O3 C3 Re1 176.1(8) . . ? C12 C11 N2 105.7(8) . . ? C12 C11 C14 132.2(10) . . ? N2 C11 C14 122.1(10) . . ? C11 C12 C13 108.0(8) . . ? N1 C13 C12 110.6(8) . . ? N1 C13 C15 122.0(8) . . ? C12 C13 C15 127.4(8) . . ? N4 C21 C22 104.4(10) . . ? N4 C21 C24 121.3(11) . . ? C22 C21 C24 134.2(10) . . ? C21 C22 C23 108.5(9) . . ? N3 C23 C22 110.6(10) . . ? N3 C23 C25 121.1(9) . . ? C22 C23 C25 128.3(10) . . ? N6 C31 C32 102.8(11) . . ? N6 C31 C34 121.8(12) . . ? C32 C31 C34 135.4(11) . . ? C31 C32 C33 108.8(9) . . ? N5 C33 C32 110.4(11) . . ? N5 C33 C35 123.6(12) . . ? C32 C33 C35 126.1(11) . . ? C81 B51 C51 110.2(6) . . ? C81 B51 C71 113.1(6) . . ? C51 B51 C71 107.1(6) . . ? C81 B51 C61 106.2(6) . . ? C51 B51 C61 110.7(6) . . ? C71 B51 C61 109.5(6) . . ? C56 C51 C52 114.4(7) . . ? C56 C51 B51 126.2(7) . . ? C52 C51 B51 119.4(6) . . ? C53 C52 C51 123.6(7) . . ? C54 C53 C52 119.5(7) . . ? C54 C53 C57 120.4(8) . . ? C52 C53 C57 120.1(7) . . ? C53 C54 C55 119.3(7) . . ? C54 C55 C56 119.9(7) . . ? C54 C55 C58 119.8(8) . . ? C56 C55 C58 120.4(8) . . ? C55 C56 C51 123.3(7) . . ? F2 C57 F1 107.8(10) . . ? F2 C57 F3 104.4(9) . . ? F1 C57 F3 102.8(9) . . ? F2 C57 C53 115.4(8) . . ? F1 C57 C53 114.1(8) . . ? F3 C57 C53 111.1(9) . . ? F6 C58 F4 109.3(12) . . ? F6 C58 F5 98.8(12) . . ? F4 C58 F5 101.7(11) . . ? F6 C58 C55 114.6(10) . . ? F4 C58 C55 117.4(10) . . ? F5 C58 C55 112.8(10) . . ? C62 C61 C66 115.0(7) . . ? C62 C61 B51 124.6(7) . . ? C66 C61 B51 120.4(6) . . ? C61 C62 C63 122.3(8) . . ? C64 C63 C62 121.1(8) . . ? C64 C63 C67 119.9(9) . . ? C62 C63 C67 119.0(9) . . ? C63 C64 C65 118.6(8) . . ? C64 C65 C66 119.8(8) . . ? C64 C65 C68 120.8(8) . . ? C66 C65 C68 119.4(8) . . ? C65 C66 C61 123.1(7) . . ? F9 C67 F7 108.7(16) . . ? F9 C67 F8 104.0(14) . . ? F7 C67 F8 100.6(13) . . ? F9 C67 C63 115.7(11) . . ? F7 C67 C63 113.6(13) . . ? F8 C67 C63 112.8(15) . . ? F12 C68 F11 106.9(14) . . ? F12 C68 F10 108.9(12) . . ? F11 C68 F10 95.1(9) . . ? F12 C68 C65 118.8(9) . . ? F11 C68 C65 112.0(9) . . ? F10 C68 C65 112.4(11) . . ? C76 C71 C72 115.4(7) . . ? C76 C71 B51 125.3(7) . . ? C72 C71 B51 119.3(7) . . ? C73 C72 C71 123.2(8) . . ? C72 C73 C74 119.5(8) . . ? C72 C73 C77 119.0(8) . . ? C74 C73 C77 121.5(8) . . ? C75 C74 C73 118.8(8) . . ? C74 C75 C76 121.1(8) . . ? C74 C75 C78 119.0(10) . . ? C76 C75 C78 120.0(10) . . ? C75 C76 C71 122.0(8) . . ? F13 C77 F15 110.1(10) . . ? F13 C77 F14 103.5(11) . . ? F15 C77 F14 101.2(9) . . ? F13 C77 C73 115.0(9) . . ? F15 C77 C73 114.7(9) . . ? F14 C77 C73 110.9(10) . . ? F18 C78 F17 109.8(18) . . ? F18 C78 F16 102.0(16) . . ? F17 C78 F16 98.2(17) . . ? F18 C78 C75 118.0(14) . . ? F17 C78 C75 115.2(13) . . ? F16 C78 C75 111.0(16) . . ? C82 C81 C86 115.2(7) . . ? C82 C81 B51 124.0(6) . . ? C86 C81 B51 120.7(6) . . ? C81 C82 C83 122.6(7) . . ? C84 C83 C82 120.3(7) . . ? C84 C83 C87 120.6(7) . . ? C82 C83 C87 119.0(7) . . ? C85 C84 C83 118.6(7) . . ? C84 C85 C86 120.9(7) . . ? C84 C85 C88 118.5(7) . . ? C86 C85 C88 120.6(8) . . ? C85 C86 C81 122.4(7) . . ? F20 C87 F21 112.5(10) . . ? F20 C87 F19 104.7(10) . . ? F21 C87 F19 95.0(9) . . ? F20 C87 C83 117.3(10) . . ? F21 C87 C83 113.5(8) . . ? F19 C87 C83 111.0(8) . . ? F23 C88 F22 108.8(10) . . ? F23 C88 F24 103.4(9) . . ? F22 C88 F24 97.9(9) . . ? F23 C88 C85 116.6(8) . . ? F22 C88 C85 116.1(8) . . ? F24 C88 C85 111.9(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.361 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.092 #===END data_Compound_2_(sn189am) _database_code_depnum_ccdc_archive 'CCDC 246232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H48 B F24 N6 O3 Re' _chemical_formula_weight 1506.01 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.819(6) _cell_length_b 15.760(8) _cell_length_c 19.839(10) _cell_angle_alpha 74.846(11) _cell_angle_beta 76.806(9) _cell_angle_gamma 82.664(10) _cell_volume 3170(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 2.033 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.830411 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14258 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 23.32 _reflns_number_total 8980 _reflns_number_gt 7076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0510P)^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 SHELXL _refine_ls_extinction_coef 0.00067(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8980 _refine_ls_number_parameters 842 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.35445(2) 0.217039(17) 0.393238(15) 0.04340(12) Uani 1 1 d . . . N1 N 0.4532(5) 0.3321(3) 0.3902(3) 0.0445(13) Uani 1 1 d . . . N2 N 0.4096(5) 0.4170(4) 0.3658(3) 0.0484(14) Uani 1 1 d . . . H2 H 0.340(6) 0.425(4) 0.357(3) 0.05(2) Uiso 1 1 d . . . N3 N 0.4362(4) 0.2464(3) 0.2780(3) 0.0438(12) Uani 1 1 d . . . N4 N 0.5121(5) 0.3117(4) 0.2411(3) 0.0517(15) Uani 1 1 d . . . H4 H 0.527(6) 0.342(4) 0.262(3) 0.04(2) Uiso 1 1 d . . . N5 N 0.5383(4) 0.1453(3) 0.4053(3) 0.0428(12) Uani 1 1 d . . . N6 N 0.6393(5) 0.1442(4) 0.3506(3) 0.0457(14) Uani 1 1 d . . . H6 H 0.637(6) 0.165(4) 0.313(4) 0.06(3) Uiso 1 1 d . . . C1 C 0.2790(6) 0.1145(5) 0.3915(3) 0.0543(18) Uani 1 1 d . . . O1 O 0.2337(5) 0.0524(3) 0.3910(3) 0.0824(17) Uani 1 1 d . . . C2 C 0.2909(5) 0.1908(4) 0.4945(4) 0.0499(17) Uani 1 1 d . . . O2 O 0.2512(5) 0.1741(4) 0.5556(3) 0.0793(16) Uani 1 1 d . . . C3 C 0.1968(7) 0.2831(4) 0.3812(3) 0.0466(16) Uani 1 1 d . . . O3 O 0.1006(5) 0.3225(4) 0.3750(3) 0.0755(15) Uani 1 1 d . . . C11 C 0.4909(6) 0.4762(4) 0.3628(4) 0.0495(16) Uani 1 1 d . . . C12 C 0.5938(7) 0.4264(5) 0.3857(5) 0.078(2) Uani 1 1 d . . . H12 H 0.6682 0.4475 0.3889 0.093 Uiso 1 1 calc R . . C13 C 0.5663(7) 0.3393(4) 0.4031(4) 0.066(2) Uani 1 1 d . . . H13 H 0.6197 0.2920 0.4214 0.079 Uiso 1 1 calc R . . C14 C 0.4623(7) 0.5743(4) 0.3400(4) 0.0595(19) Uani 1 1 d . . . C15 C 0.5817(8) 0.6154(5) 0.2920(5) 0.092(3) Uani 1 1 d . . . H15A H 0.6501 0.6017 0.3175 0.137 Uiso 1 1 calc R . . H15B H 0.5653 0.6782 0.2781 0.137 Uiso 1 1 calc R . . H15C H 0.6048 0.5923 0.2503 0.137 Uiso 1 1 calc R . . C16 C 0.4270(8) 0.6098(5) 0.4079(5) 0.086(3) Uani 1 1 d . . . H16A H 0.3526 0.5832 0.4384 0.129 Uiso 1 1 calc R . . H16B H 0.4101 0.6726 0.3950 0.129 Uiso 1 1 calc R . . H16C H 0.4965 0.5956 0.4326 0.129 Uiso 1 1 calc R . . C17 C 0.3516(8) 0.5969(5) 0.3011(5) 0.094(3) Uani 1 1 d . . . H17A H 0.3722 0.5734 0.2595 0.141 Uiso 1 1 calc R . . H17B H 0.3362 0.6598 0.2871 0.141 Uiso 1 1 calc R . . H17C H 0.2767 0.5717 0.3323 0.141 Uiso 1 1 calc R . . C21 C 0.5502(7) 0.3143(5) 0.1710(4) 0.0603(19) Uani 1 1 d . . . C22 C 0.4962(8) 0.2464(6) 0.1621(4) 0.090(3) Uani 1 1 d . . . H22 H 0.5041 0.2294 0.1197 0.108 Uiso 1 1 calc R . . C23 C 0.4269(7) 0.2070(5) 0.2283(4) 0.078(2) Uani 1 1 d . . . H23 H 0.3795 0.1586 0.2368 0.093 Uiso 1 1 calc R . . C24 C 0.6321(8) 0.3838(6) 0.1203(4) 0.082(3) Uani 1 1 d . . . C25 C 0.6809(18) 0.3583(11) 0.0523(7) 0.272(12) Uani 1 1 d . . . H25A H 0.6130 0.3651 0.0270 0.407 Uiso 1 1 calc R . . H25B H 0.7142 0.2978 0.0615 0.407 Uiso 1 1 calc R . . H25C H 0.7473 0.3952 0.0239 0.407 Uiso 1 1 calc R . . C26 C 0.7461(13) 0.3903(11) 0.1480(8) 0.221(9) Uani 1 1 d . . . H26A H 0.7841 0.3322 0.1644 0.332 Uiso 1 1 calc R . . H26B H 0.7215 0.4188 0.1868 0.332 Uiso 1 1 calc R . . H26C H 0.8065 0.4240 0.1106 0.332 Uiso 1 1 calc R . . C27 C 0.5597(14) 0.4694(8) 0.1093(10) 0.264(12) Uani 1 1 d . . . H27A H 0.5905 0.5039 0.0621 0.397 Uiso 1 1 calc R . . H27B H 0.5696 0.4997 0.1437 0.397 Uiso 1 1 calc R . . H27C H 0.4713 0.4609 0.1149 0.397 Uiso 1 1 calc R . . C31 C 0.7469(6) 0.1055(4) 0.3722(4) 0.0462(15) Uani 1 1 d . . . C32 C 0.7130(6) 0.0810(4) 0.4453(4) 0.0605(19) Uani 1 1 d . . . H32 H 0.7658 0.0524 0.4766 0.073 Uiso 1 1 calc R . . C33 C 0.5854(7) 0.1068(4) 0.4634(4) 0.0592(18) Uani 1 1 d . . . H33 H 0.5385 0.0984 0.5099 0.071 Uiso 1 1 calc R . . C34 C 0.8735(6) 0.1008(4) 0.3206(4) 0.0544(17) Uani 1 1 d . . . C35 C 0.8564(7) 0.1054(6) 0.2464(4) 0.091(3) Uani 1 1 d . . . H35A H 0.8097 0.1597 0.2291 0.136 Uiso 1 1 calc R . . H35B H 0.8102 0.0567 0.2475 0.136 Uiso 1 1 calc R . . H35C H 0.9382 0.1025 0.2153 0.136 Uiso 1 1 calc R . . C36 C 0.9470(7) 0.0125(5) 0.3467(5) 0.104(3) Uani 1 1 d . . . H36A H 1.0263 0.0081 0.3137 0.155 Uiso 1 1 calc R . . H36B H 0.8972 -0.0351 0.3498 0.155 Uiso 1 1 calc R . . H36C H 0.9633 0.0095 0.3929 0.155 Uiso 1 1 calc R . . C37 C 0.9476(8) 0.1769(6) 0.3194(5) 0.101(3) Uani 1 1 d . . . H37A H 0.8996 0.2316 0.3048 0.152 Uiso 1 1 calc R . . H37B H 1.0276 0.1755 0.2864 0.152 Uiso 1 1 calc R . . H37C H 0.9626 0.1716 0.3663 0.152 Uiso 1 1 calc R . . B51 B 0.0115(6) 0.7793(4) 0.2142(3) 0.0361(15) Uani 1 1 d . . . C51 C 0.0109(5) 0.7413(4) 0.2997(3) 0.0371(14) Uani 1 1 d . . . C52 C 0.0773(5) 0.7776(4) 0.3369(3) 0.0384(14) Uani 1 1 d . . . H52 H 0.1269 0.8243 0.3118 0.046 Uiso 1 1 calc R . . C53 C 0.0720(5) 0.7468(4) 0.4097(3) 0.0372(14) Uani 1 1 d . . . C54 C -0.0002(5) 0.6760(4) 0.4497(3) 0.0418(15) Uani 1 1 d . . . H54 H -0.0018 0.6540 0.4982 0.050 Uiso 1 1 calc R . . C55 C -0.0682(5) 0.6401(4) 0.4150(3) 0.0392(14) Uani 1 1 d . . . C56 C -0.0623(5) 0.6716(4) 0.3422(3) 0.0398(14) Uani 1 1 d . . . H56 H -0.1092 0.6452 0.3204 0.048 Uiso 1 1 calc R . . C57 C 0.1384(7) 0.7903(5) 0.4480(4) 0.0547(17) Uani 1 1 d . . . C58 C -0.1530(7) 0.5688(5) 0.4552(4) 0.0589(19) Uani 1 1 d . . . C61 C 0.1447(5) 0.8286(4) 0.1754(3) 0.0358(14) Uani 1 1 d . . . C62 C 0.1552(5) 0.9160(4) 0.1745(3) 0.0405(14) Uani 1 1 d . . . H62 H 0.0838 0.9479 0.1940 0.049 Uiso 1 1 calc R . . C63 C 0.2683(6) 0.9577(4) 0.1457(3) 0.0421(15) Uani 1 1 d . . . C64 C 0.3764(6) 0.9125(4) 0.1164(3) 0.0486(16) Uani 1 1 d . . . H64 H 0.4520 0.9399 0.0968 0.058 Uiso 1 1 calc R . . C65 C 0.3694(5) 0.8254(4) 0.1169(3) 0.0466(16) Uani 1 1 d . . . C66 C 0.2568(5) 0.7853(4) 0.1451(3) 0.0410(14) Uani 1 1 d . . . H66 H 0.2550 0.7269 0.1440 0.049 Uiso 1 1 calc R . . C67 C 0.2702(7) 1.0505(5) 0.1458(5) 0.069(2) Uani 1 1 d . . . C68 C 0.4836(7) 0.7748(6) 0.0862(5) 0.074(2) Uani 1 1 d . . . C71 C -0.1139(5) 0.8495(3) 0.2046(3) 0.0352(13) Uani 1 1 d . . . C72 C -0.2262(5) 0.8480(4) 0.2562(3) 0.0408(14) Uani 1 1 d . . . H72 H -0.2291 0.8070 0.2997 0.049 Uiso 1 1 calc R . . C73 C -0.3333(5) 0.9041(4) 0.2464(3) 0.0424(15) Uani 1 1 d . . . C74 C -0.3325(6) 0.9665(4) 0.1828(3) 0.0497(16) Uani 1 1 d . . . H74 H -0.4038 1.0046 0.1755 0.060 Uiso 1 1 calc R . . C75 C -0.2223(6) 0.9710(4) 0.1299(3) 0.0469(16) Uani 1 1 d . . . C76 C -0.1163(5) 0.9143(4) 0.1412(3) 0.0396(14) Uani 1 1 d . . . H76 H -0.0436 0.9194 0.1053 0.048 Uiso 1 1 calc R . . C77 C -0.4500(7) 0.9005(6) 0.3033(4) 0.065(2) Uani 1 1 d . . . C78 C -0.2217(9) 1.0368(7) 0.0621(5) 0.086(3) Uani 1 1 d . . . C81 C 0.0073(5) 0.6992(4) 0.1767(3) 0.0411(15) Uani 1 1 d . . . C82 C 0.0695(5) 0.6173(4) 0.1967(3) 0.0463(16) Uani 1 1 d . . . H82 H 0.1094 0.6067 0.2352 0.056 Uiso 1 1 calc R . . C83 C 0.0757(6) 0.5497(4) 0.1625(4) 0.0510(17) Uani 1 1 d . . . C84 C 0.0192(6) 0.5627(4) 0.1044(4) 0.0527(17) Uani 1 1 d . . . H84 H 0.0236 0.5184 0.0806 0.063 Uiso 1 1 calc R . . C85 C -0.0441(6) 0.6437(4) 0.0828(3) 0.0485(16) Uani 1 1 d . . . C86 C -0.0501(5) 0.7093(4) 0.1182(3) 0.0439(15) Uani 1 1 d . . . H86 H -0.0945 0.7627 0.1025 0.053 Uiso 1 1 calc R . . C87 C 0.1437(11) 0.4619(6) 0.1875(6) 0.092(3) Uani 1 1 d . . . C88 C -0.1049(9) 0.6589(6) 0.0212(5) 0.077(2) Uani 1 1 d . . . F1 F 0.2315(5) 0.8372(4) 0.4066(3) 0.1125(19) Uani 1 1 d . . . F2 F 0.0598(5) 0.8455(3) 0.4816(3) 0.1006(16) Uani 1 1 d . . . F3 F 0.1882(5) 0.7344(3) 0.4997(3) 0.0931(15) Uani 1 1 d . . . F4 F -0.1424(4) 0.5372(3) 0.5239(2) 0.0796(13) Uani 1 1 d . . . F5 F -0.2763(4) 0.5952(3) 0.4593(3) 0.1005(17) Uani 1 1 d . . . F6 F -0.1341(5) 0.4985(3) 0.4281(2) 0.0940(15) Uani 1 1 d . . . F7 F 0.1898(6) 1.1033(3) 0.1137(4) 0.149(3) Uani 1 1 d . . . F8 F 0.2351(6) 1.0650(4) 0.2124(3) 0.134(2) Uani 1 1 d . . . F9 F 0.3823(4) 1.0834(3) 0.1220(3) 0.1131(19) Uani 1 1 d . . . F10 F 0.5080(8) 0.7856(7) 0.0220(4) 0.230(6) Uani 1 1 d . . . F11 F 0.4893(6) 0.6930(5) 0.1102(5) 0.196(4) Uani 1 1 d . . . F12 F 0.5846(6) 0.7924(7) 0.0984(7) 0.254(7) Uani 1 1 d . . . F13 F -0.4570(4) 0.8299(3) 0.3554(3) 0.1098(18) Uani 1 1 d . . . F14 F -0.4593(7) 0.9620(5) 0.3380(4) 0.177(4) Uani 1 1 d . . . F15 F -0.5529(4) 0.9093(7) 0.2822(3) 0.210(5) Uani 1 1 d . . . F16 F -0.3216(6) 1.0762(6) 0.0501(4) 0.226(5) Uani 1 1 d . . . F17 F -0.1585(8) 1.0162(5) 0.0068(3) 0.184(4) Uani 1 1 d . . . F18 F -0.1506(12) 1.1012(6) 0.0559(5) 0.244(6) Uani 1 1 d . . . F19 F 0.2216(9) 0.4342(5) 0.1335(4) 0.200(4) Uani 1 1 d . . . F20 F 0.0677(8) 0.3995(4) 0.2149(5) 0.200(5) Uani 1 1 d . . . F21 F 0.2139(6) 0.4577(3) 0.2329(4) 0.130(2) Uani 1 1 d . . . F22 F -0.0850(14) 0.7294(6) -0.0229(5) 0.266(7) Uani 1 1 d . . . F23 F -0.2224(7) 0.6672(9) 0.0351(5) 0.257(7) Uani 1 1 d . . . F24 F -0.0809(9) 0.6028(5) -0.0141(4) 0.210(5) 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 0.04075(16) 0.04735(17) 0.04164(17) -0.00957(11) -0.00593(11) -0.00833(11) N1 0.048(3) 0.044(3) 0.046(3) -0.016(3) -0.017(3) 0.004(3) N2 0.040(3) 0.052(4) 0.056(4) -0.014(3) -0.015(3) -0.002(3) N3 0.043(3) 0.048(3) 0.041(3) -0.009(3) -0.008(2) -0.011(2) N4 0.059(4) 0.055(4) 0.044(4) -0.011(3) -0.005(3) -0.024(3) N5 0.039(3) 0.045(3) 0.042(3) -0.010(3) -0.004(3) -0.003(2) N6 0.045(3) 0.049(3) 0.041(4) -0.009(3) -0.006(3) -0.005(3) C1 0.052(4) 0.058(5) 0.044(4) 0.002(3) -0.009(3) -0.007(4) O1 0.098(4) 0.065(3) 0.089(4) -0.010(3) -0.021(3) -0.040(3) C2 0.034(3) 0.050(4) 0.064(5) -0.011(4) -0.012(3) 0.002(3) O2 0.075(3) 0.109(4) 0.039(3) -0.007(3) 0.000(3) 0.005(3) C3 0.058(4) 0.051(4) 0.029(4) -0.008(3) 0.000(3) -0.014(3) O3 0.053(3) 0.099(4) 0.070(4) -0.014(3) -0.020(3) 0.012(3) C11 0.052(4) 0.048(4) 0.056(4) -0.017(3) -0.016(3) -0.010(3) C12 0.074(5) 0.055(5) 0.123(8) -0.018(5) -0.059(5) -0.013(4) C13 0.065(5) 0.053(4) 0.093(6) -0.018(4) -0.048(4) 0.001(4) C14 0.069(5) 0.039(4) 0.072(5) -0.008(4) -0.019(4) -0.014(3) C15 0.109(7) 0.067(5) 0.090(7) -0.001(5) -0.010(5) -0.026(5) C16 0.100(6) 0.062(5) 0.097(7) -0.032(5) -0.004(5) -0.011(5) C17 0.104(7) 0.064(5) 0.119(8) -0.004(5) -0.061(6) 0.004(5) C21 0.065(5) 0.066(5) 0.043(5) -0.007(4) -0.003(4) -0.004(4) C22 0.122(7) 0.107(7) 0.049(5) -0.030(5) 0.000(5) -0.048(6) C23 0.095(6) 0.090(6) 0.057(5) -0.026(5) -0.004(4) -0.046(5) C24 0.089(6) 0.085(6) 0.054(5) 0.004(4) 0.012(4) -0.031(5) C25 0.40(3) 0.30(2) 0.094(11) -0.065(12) 0.135(14) -0.24(2) C26 0.170(13) 0.274(18) 0.185(16) 0.088(13) -0.053(11) -0.160(13) C27 0.192(15) 0.103(10) 0.35(3) 0.102(13) 0.065(15) -0.010(10) C31 0.047(4) 0.044(4) 0.053(4) -0.013(3) -0.020(3) 0.000(3) C32 0.059(5) 0.068(5) 0.047(5) -0.002(4) -0.016(4) 0.004(4) C33 0.067(5) 0.057(4) 0.046(4) -0.006(3) -0.011(4) 0.005(4) C34 0.045(4) 0.061(4) 0.063(5) -0.021(4) -0.014(3) -0.007(3) C35 0.061(5) 0.147(8) 0.072(6) -0.048(6) -0.006(4) -0.003(5) C36 0.065(5) 0.083(6) 0.137(9) -0.014(6) -0.002(5) 0.027(5) C37 0.084(6) 0.113(7) 0.114(8) -0.047(6) 0.012(5) -0.043(6) B51 0.038(4) 0.040(4) 0.032(4) -0.010(3) -0.007(3) -0.008(3) C51 0.031(3) 0.040(3) 0.042(4) -0.011(3) -0.009(3) -0.003(3) C52 0.041(3) 0.036(3) 0.036(4) -0.006(3) -0.007(3) -0.006(3) C53 0.036(3) 0.039(3) 0.039(4) -0.013(3) -0.010(3) 0.001(3) C54 0.043(3) 0.050(4) 0.029(3) -0.006(3) -0.006(3) 0.000(3) C55 0.035(3) 0.036(3) 0.042(4) -0.003(3) -0.004(3) -0.006(3) C56 0.038(3) 0.044(3) 0.039(4) -0.010(3) -0.010(3) -0.005(3) C57 0.057(4) 0.064(5) 0.049(4) -0.018(4) -0.015(4) -0.009(4) C58 0.059(5) 0.065(5) 0.045(5) 0.006(4) -0.011(3) -0.020(4) C61 0.033(3) 0.044(4) 0.030(3) -0.007(3) -0.006(3) -0.003(3) C62 0.033(3) 0.048(4) 0.040(4) -0.012(3) -0.008(3) 0.000(3) C63 0.046(4) 0.047(4) 0.035(4) -0.004(3) -0.012(3) -0.012(3) C64 0.038(4) 0.061(4) 0.043(4) -0.005(3) -0.006(3) -0.013(3) C65 0.037(4) 0.060(4) 0.039(4) -0.010(3) -0.007(3) 0.003(3) C66 0.041(4) 0.040(3) 0.043(4) -0.014(3) -0.009(3) 0.003(3) C67 0.060(5) 0.066(5) 0.083(6) -0.016(5) -0.011(4) -0.020(4) C68 0.033(4) 0.082(6) 0.080(7) 0.001(5) 0.009(4) 0.008(4) C71 0.042(3) 0.039(3) 0.031(3) -0.015(3) -0.012(3) -0.007(3) C72 0.045(4) 0.044(4) 0.034(4) -0.008(3) -0.008(3) -0.008(3) C73 0.033(3) 0.053(4) 0.043(4) -0.017(3) -0.004(3) -0.004(3) C74 0.042(4) 0.059(4) 0.050(4) -0.016(3) -0.014(3) 0.005(3) C75 0.050(4) 0.052(4) 0.038(4) -0.004(3) -0.016(3) -0.002(3) C76 0.034(3) 0.048(4) 0.037(4) -0.012(3) -0.005(3) -0.004(3) C77 0.052(5) 0.081(6) 0.052(5) -0.008(4) -0.004(4) 0.005(4) C78 0.081(6) 0.089(7) 0.059(6) 0.013(5) -0.002(5) 0.019(5) C81 0.038(3) 0.046(4) 0.040(4) -0.012(3) -0.005(3) -0.008(3) C82 0.044(4) 0.056(4) 0.049(4) -0.023(3) -0.017(3) -0.007(3) C83 0.062(4) 0.041(4) 0.052(4) -0.012(3) -0.016(3) -0.002(3) C84 0.060(4) 0.046(4) 0.060(5) -0.027(3) -0.008(4) -0.010(3) C85 0.054(4) 0.052(4) 0.046(4) -0.024(3) -0.012(3) 0.001(3) C86 0.043(4) 0.041(4) 0.049(4) -0.014(3) -0.014(3) 0.005(3) C87 0.135(8) 0.061(6) 0.095(7) -0.036(5) -0.050(7) 0.023(6) C88 0.096(7) 0.081(6) 0.076(6) -0.041(5) -0.051(5) 0.023(5) F1 0.126(4) 0.166(5) 0.066(3) -0.028(3) -0.008(3) -0.104(4) F2 0.102(3) 0.113(4) 0.122(4) -0.082(3) -0.045(3) 0.016(3) F3 0.115(4) 0.089(3) 0.099(4) -0.015(3) -0.075(3) -0.012(3) F4 0.090(3) 0.086(3) 0.052(3) 0.016(2) -0.011(2) -0.042(2) F5 0.049(3) 0.115(4) 0.115(4) 0.022(3) -0.017(2) -0.027(2) F6 0.139(4) 0.068(3) 0.079(3) -0.010(3) -0.014(3) -0.053(3) F7 0.159(5) 0.052(3) 0.259(9) -0.015(4) -0.121(6) 0.001(3) F8 0.173(6) 0.109(4) 0.132(5) -0.073(4) 0.032(4) -0.071(4) F9 0.077(3) 0.080(3) 0.178(6) -0.043(3) 0.015(3) -0.039(3) F10 0.208(8) 0.327(11) 0.074(5) -0.038(6) 0.011(5) 0.185(8) F11 0.134(6) 0.112(5) 0.242(9) -0.004(6) 0.083(6) 0.058(4) F12 0.055(4) 0.319(12) 0.488(19) -0.309(13) -0.044(6) 0.049(5) F13 0.073(3) 0.115(4) 0.100(4) 0.005(3) 0.028(3) -0.004(3) F14 0.181(7) 0.134(5) 0.176(7) -0.083(5) 0.115(6) -0.040(5) F15 0.032(3) 0.481(14) 0.077(4) -0.009(6) -0.005(3) -0.006(5) F16 0.098(4) 0.331(10) 0.113(5) 0.117(6) -0.001(4) 0.084(6) F17 0.215(7) 0.204(8) 0.055(4) 0.027(4) 0.009(4) 0.079(6) F18 0.421(16) 0.149(7) 0.162(8) 0.095(6) -0.148(9) -0.135(9) F19 0.285(10) 0.144(6) 0.157(7) -0.061(6) -0.074(7) 0.136(7) F20 0.226(8) 0.057(3) 0.324(13) 0.038(5) -0.154(9) -0.040(5) F21 0.187(6) 0.064(3) 0.172(6) -0.035(3) -0.121(5) 0.037(3) F22 0.50(2) 0.184(7) 0.172(8) 0.065(7) -0.257(12) -0.137(10) F23 0.113(5) 0.53(2) 0.194(9) -0.203(12) -0.110(6) 0.116(9) F24 0.328(10) 0.203(7) 0.196(7) -0.162(7) -0.210(8) 0.151(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.911(7) . ? Re1 C1 1.912(8) . ? Re1 C2 1.920(8) . ? Re1 N5 2.190(5) . ? Re1 N1 2.200(5) . ? Re1 N3 2.203(5) . ? N1 C13 1.331(8) . ? N1 N2 1.361(7) . ? N2 C11 1.345(8) . ? N3 C23 1.322(8) . ? N3 N4 1.348(7) . ? N4 C21 1.347(9) . ? N5 C33 1.334(8) . ? N5 N6 1.356(7) . ? N6 C31 1.349(8) . ? C1 O1 1.153(8) . ? C2 O2 1.162(8) . ? C3 O3 1.156(7) . ? C11 C12 1.372(9) . ? C11 C14 1.505(9) . ? C12 C13 1.379(9) . ? C14 C15 1.525(10) . ? C14 C17 1.525(10) . ? C14 C16 1.541(10) . ? C21 C22 1.350(10) . ? C21 C24 1.505(10) . ? C22 C23 1.384(10) . ? C24 C27 1.461(14) . ? C24 C25 1.472(14) . ? C24 C26 1.484(14) . ? C31 C32 1.374(9) . ? C31 C34 1.518(9) . ? C32 C33 1.381(9) . ? C34 C35 1.509(10) . ? C34 C37 1.517(9) . ? C34 C36 1.538(10) . ? B51 C81 1.635(9) . ? B51 C51 1.643(8) . ? B51 C71 1.651(8) . ? B51 C61 1.655(8) . ? C51 C52 1.398(8) . ? C51 C56 1.406(7) . ? C52 C53 1.390(8) . ? C53 C54 1.401(8) . ? C53 C57 1.487(8) . ? C54 C55 1.370(8) . ? C55 C56 1.389(8) . ? C55 C58 1.484(8) . ? C57 F1 1.315(7) . ? C57 F3 1.332(8) . ? C57 F2 1.334(8) . ? C58 F6 1.328(8) . ? C58 F5 1.336(7) . ? C58 F4 1.348(7) . ? C61 C62 1.392(8) . ? C61 C66 1.403(8) . ? C62 C63 1.395(8) . ? C63 C64 1.381(8) . ? C63 C67 1.466(9) . ? C64 C65 1.381(9) . ? C65 C66 1.378(8) . ? C65 C68 1.481(9) . ? C67 F7 1.283(9) . ? C67 F9 1.316(8) . ? C67 F8 1.359(9) . ? C68 F10 1.210(10) . ? C68 F12 1.249(10) . ? C68 F11 1.251(9) . ? C71 C72 1.397(8) . ? C71 C76 1.400(8) . ? C72 C73 1.384(8) . ? C73 C74 1.381(8) . ? C73 C77 1.485(9) . ? C74 C75 1.392(8) . ? C75 C76 1.385(8) . ? C75 C78 1.466(10) . ? C77 F15 1.255(9) . ? C77 F13 1.303(8) . ? C77 F14 1.310(10) . ? C78 F16 1.216(9) . ? C78 F17 1.251(10) . ? C78 F18 1.315(12) . ? C81 C82 1.381(8) . ? C81 C86 1.401(8) . ? C82 C83 1.394(8) . ? C83 C84 1.381(9) . ? C83 C87 1.500(10) . ? C84 C85 1.380(9) . ? C85 C86 1.381(8) . ? C85 C88 1.470(10) . ? C87 F21 1.289(10) . ? C87 F20 1.290(12) . ? C87 F19 1.337(11) . ? C88 F22 1.230(10) . ? C88 F24 1.233(9) . ? C88 F23 1.235(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 C3 Re1 C1 88.2(3) . . ? C3 Re1 C2 88.6(2) . . ? C1 Re1 C2 87.9(3) . . ? C3 Re1 N5 178.2(2) . . ? C1 Re1 N5 93.4(2) . . ? C2 Re1 N5 92.3(2) . . ? C3 Re1 N1 94.6(2) . . ? C1 Re1 N1 176.0(2) . . ? C2 Re1 N1 94.9(2) . . ? N5 Re1 N1 83.71(18) . . ? C3 Re1 N3 93.7(2) . . ? C1 Re1 N3 93.3(2) . . ? C2 Re1 N3 177.4(2) . . ? N5 Re1 N3 85.33(18) . . ? N1 Re1 N3 83.76(18) . . ? C13 N1 N2 103.9(5) . . ? C13 N1 Re1 132.1(4) . . ? N2 N1 Re1 123.7(4) . . ? C11 N2 N1 113.4(5) . . ? C23 N3 N4 102.7(6) . . ? C23 N3 Re1 130.9(5) . . ? N4 N3 Re1 126.4(4) . . ? C21 N4 N3 114.2(6) . . ? C33 N5 N6 104.2(5) . . ? C33 N5 Re1 131.1(4) . . ? N6 N5 Re1 123.9(4) . . ? C31 N6 N5 113.1(6) . . ? O1 C1 Re1 179.5(6) . . ? O2 C2 Re1 179.0(6) . . ? O3 C3 Re1 179.0(6) . . ? N2 C11 C12 104.6(6) . . ? N2 C11 C14 123.4(6) . . ? C12 C11 C14 132.0(6) . . ? C11 C12 C13 107.2(6) . . ? N1 C13 C12 110.9(6) . . ? C11 C14 C15 108.6(6) . . ? C11 C14 C17 111.6(5) . . ? C15 C14 C17 110.4(7) . . ? C11 C14 C16 107.5(6) . . ? C15 C14 C16 109.5(6) . . ? C17 C14 C16 109.2(7) . . ? N4 C21 C22 104.6(6) . . ? N4 C21 C24 122.4(7) . . ? C22 C21 C24 133.0(7) . . ? C21 C22 C23 106.7(7) . . ? N3 C23 C22 111.8(7) . . ? C27 C24 C25 111.0(13) . . ? C27 C24 C26 109.4(12) . . ? C25 C24 C26 105.8(11) . . ? C27 C24 C21 110.3(8) . . ? C25 C24 C21 109.5(8) . . ? C26 C24 C21 110.8(8) . . ? N6 C31 C32 104.9(6) . . ? N6 C31 C34 122.5(6) . . ? C32 C31 C34 132.4(6) . . ? C31 C32 C33 106.8(6) . . ? N5 C33 C32 110.9(6) . . ? C35 C34 C37 109.9(7) . . ? C35 C34 C31 111.9(5) . . ? C37 C34 C31 108.3(6) . . ? C35 C34 C36 107.9(7) . . ? C37 C34 C36 110.1(6) . . ? C31 C34 C36 108.7(6) . . ? C81 B51 C51 111.0(5) . . ? C81 B51 C71 109.5(5) . . ? C51 B51 C71 108.9(4) . . ? C81 B51 C61 108.2(5) . . ? C51 B51 C61 108.6(4) . . ? C71 B51 C61 110.7(4) . . ? C52 C51 C56 114.5(5) . . ? C52 C51 B51 123.4(5) . . ? C56 C51 B51 122.1(5) . . ? C53 C52 C51 122.7(5) . . ? C52 C53 C54 120.8(5) . . ? C52 C53 C57 121.0(5) . . ? C54 C53 C57 118.1(5) . . ? C55 C54 C53 117.8(5) . . ? C54 C55 C56 120.7(5) . . ? C54 C55 C58 120.4(6) . . ? C56 C55 C58 118.9(6) . . ? C55 C56 C51 123.4(5) . . ? F1 C57 F3 106.3(6) . . ? F1 C57 F2 105.7(6) . . ? F3 C57 F2 103.9(6) . . ? F1 C57 C53 114.1(6) . . ? F3 C57 C53 113.7(6) . . ? F2 C57 C53 112.3(5) . . ? F6 C58 F5 106.1(6) . . ? F6 C58 F4 105.0(5) . . ? F5 C58 F4 103.9(6) . . ? F6 C58 C55 114.1(6) . . ? F5 C58 C55 112.7(6) . . ? F4 C58 C55 114.0(6) . . ? C62 C61 C66 114.9(5) . . ? C62 C61 B51 121.6(5) . . ? C66 C61 B51 123.4(5) . . ? C61 C62 C63 122.8(5) . . ? C64 C63 C62 120.3(6) . . ? C64 C63 C67 120.5(6) . . ? C62 C63 C67 119.1(6) . . ? C65 C64 C63 118.4(6) . . ? C66 C65 C64 120.6(5) . . ? C66 C65 C68 119.6(6) . . ? C64 C65 C68 119.8(6) . . ? C65 C66 C61 123.0(5) . . ? F7 C67 F9 108.1(7) . . ? F7 C67 F8 101.4(8) . . ? F9 C67 F8 102.9(6) . . ? F7 C67 C63 114.8(7) . . ? F9 C67 C63 115.4(7) . . ? F8 C67 C63 112.7(7) . . ? F10 C68 F12 102.3(9) . . ? F10 C68 F11 104.9(10) . . ? F12 C68 F11 100.2(9) . . ? F10 C68 C65 116.8(7) . . ? F12 C68 C65 113.5(8) . . ? F11 C68 C65 116.9(7) . . ? C72 C71 C76 114.6(5) . . ? C72 C71 B51 124.1(5) . . ? C76 C71 B51 121.3(5) . . ? C73 C72 C71 123.7(5) . . ? C74 C73 C72 119.9(5) . . ? C74 C73 C77 118.4(6) . . ? C72 C73 C77 121.7(6) . . ? C73 C74 C75 118.5(6) . . ? C76 C75 C74 120.4(6) . . ? C76 C75 C78 121.1(6) . . ? C74 C75 C78 118.5(6) . . ? C75 C76 C71 122.8(5) . . ? F15 C77 F13 105.6(7) . . ? F15 C77 F14 105.0(8) . . ? F13 C77 F14 101.1(7) . . ? F15 C77 C73 115.1(7) . . ? F13 C77 C73 115.9(6) . . ? F14 C77 C73 112.6(7) . . ? F16 C78 F17 109.4(9) . . ? F16 C78 F18 102.5(10) . . ? F17 C78 F18 93.6(9) . . ? F16 C78 C75 118.9(8) . . ? F17 C78 C75 117.2(8) . . ? F18 C78 C75 111.3(9) . . ? C82 C81 C86 114.2(5) . . ? C82 C81 B51 122.2(5) . . ? C86 C81 B51 123.4(5) . . ? C81 C82 C83 123.7(6) . . ? C84 C83 C82 120.2(6) . . ? C84 C83 C87 118.8(6) . . ? C82 C83 C87 120.9(7) . . ? C85 C84 C83 117.8(6) . . ? C84 C85 C86 120.9(6) . . ? C84 C85 C88 118.6(6) . . ? C86 C85 C88 120.5(6) . . ? C85 C86 C81 123.2(6) . . ? F21 C87 F20 106.6(9) . . ? F21 C87 F19 104.9(9) . . ? F20 C87 F19 103.0(9) . . ? F21 C87 C83 116.5(7) . . ? F20 C87 C83 112.9(9) . . ? F19 C87 C83 111.9(8) . . ? F22 C88 F24 104.9(10) . . ? F22 C88 F23 98.6(10) . . ? F24 C88 F23 103.7(9) . . ? F22 C88 C85 115.1(8) . . ? F24 C88 C85 117.1(7) . . ? F23 C88 C85 115.1(9) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.012 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.098 #===END data_Compound_3_(sn126a) _database_code_depnum_ccdc_archive 'CCDC 246233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 Cl2 N8 O6 Re2' _chemical_formula_weight 995.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.765(3) _cell_length_b 18.596(4) _cell_length_c 13.707(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.329(4) _cell_angle_gamma 90.00 _cell_volume 3479.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 7.153 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.595932 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15207 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4993 _reflns_number_gt 4223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0344P)^2^+4.2306P] 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 SHELXL _refine_ls_extinction_coef 0.00099(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4993 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 1.001845(16) 0.052896(13) 0.276588(18) 0.04179(10) Uani 1 1 d . . . Cl1 Cl 0.92695(11) 0.08903(8) 0.42581(11) 0.0491(4) Uani 1 1 d . . . N1 N 0.9149(3) -0.0456(2) 0.2848(4) 0.0413(11) Uani 1 1 d . . . N2 N 0.9154(4) -0.0811(3) 0.3714(4) 0.0425(13) Uani 1 1 d . . . H2 H 0.942(4) -0.070(3) 0.418(4) 0.034(19) Uiso 1 1 d . . . N3 N 0.8670(3) 0.0974(3) 0.1968(4) 0.0448(12) Uani 1 1 d . . . N4 N 0.7793(4) 0.0865(3) 0.2285(5) 0.0515(15) Uani 1 1 d . . . H4 H 0.772(5) 0.069(3) 0.271(5) 0.04(2) Uiso 1 1 d . . . C1 C 1.0550(5) 0.0223(4) 0.1627(5) 0.0600(18) Uani 1 1 d . . . O1 O 1.0926(4) 0.0023(3) 0.0969(4) 0.0876(17) Uani 1 1 d . . . C2 C 1.1186(5) 0.0141(3) 0.3503(5) 0.0468(15) Uani 1 1 d . . . O2 O 1.1900(3) -0.0073(3) 0.3909(4) 0.0670(13) Uani 1 1 d . . . C3 C 1.0702(5) 0.1418(4) 0.2710(5) 0.0585(18) Uani 1 1 d . . . O3 O 1.1125(4) 0.1940(3) 0.2682(5) 0.102(2) Uani 1 1 d . . . C11 C 0.8642(4) -0.1417(3) 0.3625(5) 0.0447(15) Uani 1 1 d . . . C12 C 0.8274(4) -0.1457(3) 0.2656(5) 0.0477(15) Uani 1 1 d . . . H12 H 0.7872 -0.1819 0.2362 0.057 Uiso 1 1 calc R . . C13 C 0.8603(4) -0.0870(3) 0.2189(5) 0.0444(15) Uani 1 1 d . . . C14 C 0.8574(5) -0.1901(4) 0.4482(5) 0.069(2) Uani 1 1 d . . . H14A H 0.9122 -0.1816 0.4976 0.103 Uiso 1 1 calc R . . H14B H 0.8578 -0.2393 0.4271 0.103 Uiso 1 1 calc R . . H14C H 0.7977 -0.1804 0.4752 0.103 Uiso 1 1 calc R . . C15 C 0.8420(5) -0.0686(4) 0.1127(5) 0.0665(19) Uani 1 1 d . . . H15A H 0.7919 -0.0325 0.1025 0.100 Uiso 1 1 calc R . . H15B H 0.8211 -0.1109 0.0756 0.100 Uiso 1 1 calc R . . H15C H 0.9012 -0.0506 0.0915 0.100 Uiso 1 1 calc R . . C21 C 0.7051(5) 0.1151(4) 0.1680(6) 0.0594(18) Uani 1 1 d . . . C22 C 0.7462(5) 0.1456(4) 0.0934(5) 0.0636(19) Uani 1 1 d . . . H22 H 0.7132 0.1698 0.0398 0.076 Uiso 1 1 calc R . . C23 C 0.8463(5) 0.1341(4) 0.1115(5) 0.0562(17) Uani 1 1 d . . . C24 C 0.6015(5) 0.1090(5) 0.1871(8) 0.095(3) Uani 1 1 d . . . H24A H 0.5719 0.0678 0.1531 0.142 Uiso 1 1 calc R . . H24B H 0.5664 0.1515 0.1640 0.142 Uiso 1 1 calc R . . H24C H 0.5994 0.1036 0.2565 0.142 Uiso 1 1 calc R . . C25 C 0.9235(5) 0.1554(4) 0.0504(5) 0.077(2) Uani 1 1 d . . . H25A H 0.9843 0.1624 0.0920 0.116 Uiso 1 1 calc R . . H25B H 0.9048 0.1992 0.0162 0.116 Uiso 1 1 calc R . . H25C H 0.9313 0.1181 0.0035 0.116 Uiso 1 1 calc R . . Re51 Re 0.496616(17) 0.395596(13) 0.195575(19) 0.04366(10) Uani 1 1 d . . . Cl51 Cl 0.56350(11) 0.40347(8) 0.03506(11) 0.0483(4) Uani 1 1 d . . . N51 N 0.5843(3) 0.4931(3) 0.2301(3) 0.0440(12) Uani 1 1 d . . . N52 N 0.5877(3) 0.5447(3) 0.1604(4) 0.0419(12) Uani 1 1 d . . . H52 H 0.560(4) 0.539(3) 0.102(5) 0.042(18) Uiso 1 1 d . . . N53 N 0.6344(3) 0.3386(3) 0.2461(4) 0.0482(13) Uani 1 1 d . . . N54 N 0.7179(4) 0.3545(3) 0.2088(5) 0.0539(15) Uani 1 1 d . . . H54 H 0.718(5) 0.376(3) 0.166(5) 0.04(2) Uiso 1 1 d . . . C51 C 0.4466(5) 0.3929(4) 0.3171(6) 0.0634(19) Uani 1 1 d . . . O51 O 0.4116(4) 0.3918(4) 0.3906(5) 0.102(2) Uani 1 1 d . . . C52 C 0.3815(5) 0.4490(3) 0.1458(5) 0.0500(16) Uani 1 1 d . . . O52 O 0.3116(3) 0.4803(3) 0.1202(4) 0.0723(14) Uani 1 1 d . . . C53 C 0.4278(5) 0.3094(4) 0.1592(5) 0.0587(18) Uani 1 1 d . . . O53 O 0.3864(4) 0.2573(3) 0.1354(5) 0.0949(19) Uani 1 1 d . . . C61 C 0.6411(4) 0.6017(3) 0.1950(5) 0.0467(15) Uani 1 1 d . . . C62 C 0.6737(5) 0.5865(3) 0.2907(5) 0.0553(17) Uani 1 1 d . . . H62 H 0.7131 0.6156 0.3344 0.066 Uiso 1 1 calc R . . C63 C 0.6372(4) 0.5195(3) 0.3107(5) 0.0503(16) Uani 1 1 d . . . C64 C 0.6562(5) 0.6626(4) 0.1285(6) 0.0658(19) Uani 1 1 d . . . H64A H 0.7024 0.6488 0.0849 0.099 Uiso 1 1 calc R . . H64B H 0.6811 0.7033 0.1668 0.099 Uiso 1 1 calc R . . H64C H 0.5950 0.6750 0.0906 0.099 Uiso 1 1 calc R . . C65 C 0.6521(6) 0.4798(4) 0.4051(5) 0.080(2) Uani 1 1 d . . . H65A H 0.5897 0.4663 0.4237 0.121 Uiso 1 1 calc R . . H65B H 0.6860 0.5100 0.4552 0.121 Uiso 1 1 calc R . . H65C H 0.6903 0.4374 0.3977 0.121 Uiso 1 1 calc R . . C71 C 0.7939(5) 0.3150(3) 0.2478(6) 0.0572(18) Uani 1 1 d . . . C72 C 0.7581(5) 0.2719(3) 0.3145(5) 0.0619(19) Uani 1 1 d . . . H72 H 0.7936 0.2382 0.3548 0.074 Uiso 1 1 calc R . . C73 C 0.6601(5) 0.2868(3) 0.3120(5) 0.0583(18) Uani 1 1 d . . . C74 C 0.8936(5) 0.3231(4) 0.2170(7) 0.090(3) Uani 1 1 d . . . H74A H 0.8885 0.3237 0.1465 0.135 Uiso 1 1 calc R . . H74B H 0.9340 0.2834 0.2420 0.135 Uiso 1 1 calc R . . H74C H 0.9224 0.3673 0.2428 0.135 Uiso 1 1 calc R . . C75 C 0.5885(6) 0.2549(4) 0.3727(6) 0.080(2) Uani 1 1 d . . . H75A H 0.5677 0.2910 0.4157 0.120 Uiso 1 1 calc R . . H75B H 0.6189 0.2160 0.4113 0.120 Uiso 1 1 calc R . . H75C H 0.5327 0.2372 0.3304 0.120 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 0.03286(14) 0.04659(16) 0.04467(17) 0.00542(11) 0.00011(10) -0.00446(11) Cl1 0.0441(8) 0.0586(9) 0.0428(9) -0.0057(7) -0.0018(7) -0.0006(7) N1 0.037(3) 0.047(3) 0.040(3) -0.001(2) 0.002(2) -0.002(2) N2 0.040(3) 0.047(3) 0.039(4) 0.000(3) 0.000(3) -0.003(3) N3 0.033(3) 0.051(3) 0.048(3) 0.004(2) -0.001(2) -0.005(2) N4 0.043(3) 0.051(3) 0.059(4) 0.007(3) -0.002(3) -0.005(3) C1 0.044(4) 0.082(5) 0.050(5) 0.009(4) -0.012(3) -0.010(4) O1 0.071(4) 0.130(5) 0.066(4) -0.004(3) 0.026(3) 0.000(3) C2 0.044(4) 0.044(4) 0.052(4) 0.005(3) 0.009(3) -0.003(3) O2 0.040(3) 0.085(3) 0.073(3) 0.020(3) -0.006(2) 0.005(3) C3 0.037(4) 0.062(4) 0.070(5) 0.015(4) -0.017(3) -0.006(3) O3 0.065(3) 0.064(3) 0.167(6) 0.039(4) -0.020(4) -0.028(3) C11 0.035(3) 0.043(4) 0.057(4) -0.001(3) 0.010(3) -0.002(3) C12 0.036(3) 0.048(4) 0.058(4) -0.014(3) -0.002(3) -0.003(3) C13 0.036(3) 0.046(4) 0.049(4) -0.006(3) 0.001(3) 0.003(3) C14 0.068(5) 0.067(4) 0.072(5) 0.011(4) 0.013(4) -0.011(4) C15 0.070(5) 0.080(5) 0.045(4) -0.005(4) -0.008(3) -0.006(4) C21 0.043(4) 0.059(4) 0.070(5) -0.002(4) -0.014(4) 0.003(3) C22 0.061(5) 0.064(4) 0.058(5) 0.006(4) -0.024(4) 0.004(4) C23 0.059(4) 0.056(4) 0.050(4) 0.006(3) -0.009(3) 0.003(3) C24 0.045(5) 0.096(6) 0.138(9) 0.010(6) -0.007(5) 0.011(4) C25 0.079(5) 0.095(6) 0.057(5) 0.031(4) 0.004(4) -0.001(5) Re51 0.03197(15) 0.04832(16) 0.04910(17) 0.00324(11) -0.00092(11) -0.00493(11) Cl51 0.0452(8) 0.0533(9) 0.0444(9) -0.0040(7) -0.0016(7) 0.0028(7) N51 0.040(3) 0.051(3) 0.040(3) -0.001(2) 0.000(2) -0.004(2) N52 0.034(3) 0.050(3) 0.040(3) -0.001(3) -0.001(2) -0.007(2) N53 0.035(3) 0.051(3) 0.057(3) 0.010(3) 0.000(2) -0.007(2) N54 0.045(3) 0.051(4) 0.065(4) 0.012(3) 0.003(3) 0.000(3) C51 0.042(4) 0.074(5) 0.068(5) 0.007(4) -0.013(4) -0.004(3) O51 0.084(4) 0.153(6) 0.075(4) 0.020(4) 0.033(4) -0.006(4) C52 0.038(4) 0.059(4) 0.052(4) 0.005(3) 0.005(3) -0.010(3) O52 0.037(3) 0.085(4) 0.093(4) 0.020(3) 0.002(3) 0.009(3) C53 0.046(4) 0.056(4) 0.072(5) 0.016(4) -0.005(3) -0.005(3) O53 0.079(4) 0.062(3) 0.134(5) 0.014(3) -0.023(3) -0.023(3) C61 0.031(3) 0.049(4) 0.060(5) -0.007(3) 0.006(3) 0.000(3) C62 0.051(4) 0.054(4) 0.056(5) -0.015(3) -0.009(3) -0.005(3) C63 0.038(3) 0.055(4) 0.054(4) -0.003(3) -0.007(3) 0.002(3) C64 0.048(4) 0.061(4) 0.087(6) 0.010(4) 0.004(4) -0.010(4) C65 0.089(6) 0.091(6) 0.055(5) 0.007(4) -0.015(4) -0.020(5) C71 0.039(4) 0.047(4) 0.082(5) -0.001(4) -0.008(3) 0.004(3) C72 0.054(4) 0.047(4) 0.077(5) 0.008(4) -0.021(4) 0.001(3) C73 0.058(4) 0.053(4) 0.059(4) 0.009(3) -0.013(3) -0.012(3) C74 0.048(4) 0.077(5) 0.146(9) -0.003(5) 0.014(5) 0.013(4) C75 0.080(5) 0.077(5) 0.080(6) 0.030(4) -0.002(4) -0.020(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 C1 1.894(8) . ? Re1 C3 1.908(7) . ? Re1 C2 1.926(7) . ? Re1 N3 2.192(5) . ? Re1 N1 2.199(5) . ? Re1 Cl1 2.4971(16) . ? N1 C13 1.341(7) . ? N1 N2 1.358(7) . ? N2 C11 1.327(8) . ? N3 N4 1.349(7) . ? N3 C23 1.353(8) . ? N4 C21 1.340(9) . ? C1 O1 1.158(8) . ? C2 O2 1.138(7) . ? C3 O3 1.135(7) . ? C11 C12 1.362(8) . ? C11 C14 1.492(9) . ? C12 C13 1.371(8) . ? C13 C15 1.485(9) . ? C21 C22 1.355(10) . ? C21 C24 1.487(10) . ? C22 C23 1.384(9) . ? C23 C25 1.489(9) . ? Re51 C51 1.883(8) . ? Re51 C53 1.896(7) . ? Re51 C52 1.920(7) . ? Re51 N51 2.195(5) . ? Re51 N53 2.205(5) . ? Re51 Cl51 2.4952(16) . ? N51 C63 1.337(7) . ? N51 N52 1.360(7) . ? N52 C61 1.341(7) . ? N53 C73 1.337(8) . ? N53 N54 1.350(7) . ? N54 C71 1.333(8) . ? C51 O51 1.172(9) . ? C52 O52 1.141(7) . ? C53 O53 1.150(8) . ? C61 C62 1.361(9) . ? C61 C64 1.485(9) . ? C62 C63 1.384(9) . ? C63 C65 1.480(9) . ? C71 C72 1.356(9) . ? C71 C74 1.495(9) . ? C72 C73 1.374(9) . ? C73 C75 1.492(9) . ? 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 C1 Re1 C3 89.0(3) . . ? C1 Re1 C2 86.3(3) . . ? C3 Re1 C2 87.9(2) . . ? C1 Re1 N3 95.4(2) . . ? C3 Re1 N3 92.4(2) . . ? C2 Re1 N3 178.3(2) . . ? C1 Re1 N1 93.5(2) . . ? C3 Re1 N1 176.4(2) . . ? C2 Re1 N1 94.8(2) . . ? N3 Re1 N1 84.75(17) . . ? C1 Re1 Cl1 177.7(2) . . ? C3 Re1 Cl1 93.3(2) . . ? C2 Re1 Cl1 94.30(18) . . ? N3 Re1 Cl1 83.98(13) . . ? N1 Re1 Cl1 84.14(13) . . ? C13 N1 N2 104.5(5) . . ? C13 N1 Re1 134.8(4) . . ? N2 N1 Re1 120.5(4) . . ? C11 N2 N1 112.9(6) . . ? N4 N3 C23 104.8(5) . . ? N4 N3 Re1 121.2(4) . . ? C23 N3 Re1 133.9(4) . . ? C21 N4 N3 112.6(6) . . ? O1 C1 Re1 175.8(6) . . ? O2 C2 Re1 176.9(5) . . ? O3 C3 Re1 178.7(6) . . ? N2 C11 C12 105.3(6) . . ? N2 C11 C14 121.7(6) . . ? C12 C11 C14 133.1(6) . . ? C11 C12 C13 107.9(5) . . ? N1 C13 C12 109.4(6) . . ? N1 C13 C15 122.6(6) . . ? C12 C13 C15 128.0(6) . . ? N4 C21 C22 105.9(6) . . ? N4 C21 C24 122.3(7) . . ? C22 C21 C24 131.8(7) . . ? C21 C22 C23 107.6(6) . . ? N3 C23 C22 109.2(6) . . ? N3 C23 C25 122.2(6) . . ? C22 C23 C25 128.6(6) . . ? C51 Re51 C53 89.1(3) . . ? C51 Re51 C52 87.1(3) . . ? C53 Re51 C52 89.0(3) . . ? C51 Re51 N51 94.8(2) . . ? C53 Re51 N51 175.6(2) . . ? C52 Re51 N51 93.2(2) . . ? C51 Re51 N53 96.1(2) . . ? C53 Re51 N53 93.3(2) . . ? C52 Re51 N53 176.1(2) . . ? N51 Re51 N53 84.39(18) . . ? C51 Re51 Cl51 178.1(2) . . ? C53 Re51 Cl51 92.6(2) . . ? C52 Re51 Cl51 92.12(19) . . ? N51 Re51 Cl51 83.51(13) . . ? N53 Re51 Cl51 84.61(14) . . ? C63 N51 N52 104.9(5) . . ? C63 N51 Re51 135.0(4) . . ? N52 N51 Re51 120.0(4) . . ? C61 N52 N51 112.1(5) . . ? C73 N53 N54 104.4(5) . . ? C73 N53 Re51 134.5(4) . . ? N54 N53 Re51 121.0(4) . . ? C71 N54 N53 112.9(6) . . ? O51 C51 Re51 177.2(6) . . ? O52 C52 Re51 176.9(6) . . ? O53 C53 Re51 178.8(7) . . ? N52 C61 C62 106.0(5) . . ? N52 C61 C64 119.9(6) . . ? C62 C61 C64 134.1(6) . . ? C61 C62 C63 107.2(6) . . ? N51 C63 C62 109.8(6) . . ? N51 C63 C65 122.7(6) . . ? C62 C63 C65 127.5(6) . . ? N54 C71 C72 105.3(6) . . ? N54 C71 C74 122.2(7) . . ? C72 C71 C74 132.5(7) . . ? C71 C72 C73 107.7(6) . . ? N53 C73 C72 109.7(6) . . ? N53 C73 C75 121.8(6) . . ? C72 C73 C75 128.5(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.971 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.095 #===END