Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Karsten Gloe' 'David Farrell' 'Gudrun Goretzki' 'Vickie McKee' 'Jane Nelson' 'Mark Nieuwenhuyzen' ; I.Pal ; 'Holger Stephan' 'Raewyn Town' 'Kathrin Wichmann' _publ_contact_author_name 'Prof Karsten Gloe' _publ_contact_author_address ; Institut fur Anorganische Chemie Technische Universitat Dresden TU Dresden Dresden 01062 GERMANY ; _publ_contact_author_email KARSTEN.GLOE@CHEMIE.TU-DRESDEN.DE _publ_section_title ; Towards promising oxoanion extractants: azacages and open-chain counterparts ; data_r3reo4am _database_code_CSD 195731 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H59 Cl N11 O25.50 Re5' _chemical_formula_weight 1984.36 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 30.9119(18) _cell_length_b 12.3210(7) _cell_length_c 27.4541(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10456.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7440 _exptl_absorpt_coefficient_mu 11.678 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 96679 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18419 _reflns_number_gt 16018 _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^)+(0.1131P)^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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(13) _refine_ls_number_reflns 18419 _refine_ls_number_parameters 1359 _refine_ls_number_restraints 295 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1629 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.005 _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 0.99024(2) 0.14102(6) 0.66569(3) 0.01618(16) Uani 1 1 d D . . O11 O 1.0007(4) 0.0104(10) 0.6524(5) 0.025(3) Uani 1 1 d D . . O12 O 0.9371(4) 0.1713(11) 0.6569(5) 0.025(3) Uani 1 1 d D . . O13 O 1.0214(4) 0.2272(11) 0.6328(5) 0.023(3) Uani 1 1 d D . . O14 O 0.9998(5) 0.1571(10) 0.7258(4) 0.023(3) Uani 1 1 d D . . Re2 Re 0.94398(2) -0.01114(6) 0.53725(3) 0.01400(16) Uani 1 1 d . . . O21 O 0.9144(4) -0.0731(11) 0.5818(5) 0.021(3) Uani 1 1 d U . . O22 O 0.9897(4) -0.0864(11) 0.5253(5) 0.025(3) Uani 1 1 d U . . O23 O 0.9138(5) 0.0007(11) 0.4854(5) 0.025(3) Uani 1 1 d . . . O24 O 0.9590(5) 0.1124(11) 0.5585(5) 0.026(3) Uani 1 1 d . . . Re3 Re 0.63511(2) 0.37449(6) 0.69576(3) 0.01641(16) Uani 1 1 d . . . O31 O 0.5913(4) 0.4575(12) 0.6858(5) 0.025(3) Uani 1 1 d . . . O32 O 0.6438(5) 0.3678(12) 0.7583(5) 0.028(3) Uani 1 1 d . . . O33 O 0.6806(4) 0.4272(11) 0.6683(5) 0.024(3) Uani 1 1 d . . . O34 O 0.6249(5) 0.2463(12) 0.6728(5) 0.030(3) Uani 1 1 d . . . Re4 Re 0.77968(3) 0.46796(6) 0.48869(3) 0.01928(17) Uani 1 1 d . . . O41 O 0.8281(5) 0.5031(12) 0.4641(6) 0.034(4) Uani 1 1 d . . . O42 O 0.7714(4) 0.5187(11) 0.5471(5) 0.024(3) Uani 1 1 d . . . O43 O 0.7378(5) 0.5066(11) 0.4500(6) 0.030(3) Uani 1 1 d U . . O44 O 0.7779(5) 0.3275(13) 0.4944(5) 0.034(4) Uani 1 1 d . . . Re5 Re 0.89306(3) 0.85597(7) 0.77764(3) 0.0273(2) Uani 1 1 d . . . O51 O 0.9006(5) 0.8957(15) 0.7199(6) 0.043(4) Uani 1 1 d . . . O52 O 0.9153(10) 0.9424(16) 0.8136(8) 0.089(9) Uani 1 1 d . . . O53 O 0.8416(8) 0.831(5) 0.7871(9) 0.19(2) Uani 1 1 d . . . O54 O 0.9159(14) 0.7392(19) 0.7861(8) 0.150(18) Uani 1 1 d . . . Re6 Re 0.70732(3) 0.10434(7) 0.71448(3) 0.02213(18) Uani 1 1 d . . . O61 O 0.7273(4) 0.2326(10) 0.7024(5) 0.019(3) Uani 1 1 d U . . O62 O 0.6945(5) 0.0402(12) 0.6614(6) 0.038(4) Uani 1 1 d . . . O63 O 0.7466(5) 0.0318(13) 0.7431(6) 0.034(4) Uani 1 1 d . . . O64 O 0.6630(4) 0.1078(10) 0.7529(5) 0.020(3) Uani 1 1 d U . . Re7 Re 0.91092(3) 0.50520(7) 0.69888(3) 0.0279(2) Uani 1 1 d . . . O71 O 0.9012(6) 0.6404(12) 0.6845(7) 0.046(5) Uani 1 1 d . . . O72 O 0.9240(6) 0.4879(13) 0.7590(6) 0.042(4) Uani 1 1 d . . . O73 O 0.8679(5) 0.4262(13) 0.6846(6) 0.042(4) Uani 1 1 d . . . O74 O 0.9543(6) 0.462(2) 0.6641(8) 0.072(7) Uani 1 1 d . . . Re8 Re 0.91489(4) 1.25504(11) 0.90173(5) 0.0586(3) Uani 1 1 d . . . O81 O 0.8889(6) 1.3398(14) 0.8715(7) 0.046(4) Uani 1 1 d . . . O82 O 0.9285(5) 1.1648(14) 0.8611(6) 0.040(4) Uani 1 1 d . . . O83 O 0.8897(8) 1.198(2) 0.9369(8) 0.077(7) Uani 1 1 d . . . O84 O 0.9578(7) 1.3044(17) 0.9232(7) 0.060(5) Uani 1 1 d U . . Re9 Re 0.79460(5) 0.83236(13) 0.46631(7) 0.0797(5) Uani 1 1 d . . . O91 O 0.8290(6) 0.7775(16) 0.4291(7) 0.058(5) Uani 1 1 d U . . O92 O 0.7661(7) 0.7335(17) 0.4847(10) 0.081(7) Uani 1 1 d . . . O93 O 0.7683(7) 0.9153(16) 0.4373(10) 0.077(7) Uani 1 1 d . . . O94 O 0.8262(9) 0.891(2) 0.5122(11) 0.096(8) Uani 1 1 d U . . Re10 Re 0.64791(16) 0.9980(3) 0.52296(14) 0.0799(10) Uani 0.50 1 d PD A 1 O101 O 0.6282(11) 0.946(3) 0.4713(9) 0.055(10) Uiso 0.50 1 d PD A 1 O102 O 0.6147(8) 1.0926(19) 0.5432(10) 0.031(7) Uiso 0.50 1 d PD A 1 O103 O 0.6551(14) 0.898(3) 0.5636(13) 0.087(15) Uiso 0.50 1 d PD A 1 O104 O 0.6953(8) 1.063(3) 0.5086(14) 0.061(11) Uiso 0.50 1 d PD A 1 Re1' Re 0.67866(16) 0.9897(3) 0.52180(14) 0.0799(10) Uani 0.50 1 d PD B 2 O10# O 0.7111(12) 1.087(3) 0.4986(16) 0.086(15) Uiso 0.50 1 d PD B 2 O10' O 0.6501(11) 0.931(3) 0.4781(11) 0.062(11) Uiso 0.50 1 d PD B 2 O10@ O 0.7083(16) 0.903(4) 0.5551(18) 0.16(3) Uiso 0.50 1 d PD B 2 O10? O 0.6411(11) 1.058(3) 0.5575(14) 0.090(15) Uiso 0.50 1 d PD B 2 Cl11 Cl 1.04017(15) 0.7241(4) 0.92172(17) 0.0213(10) Uani 1 1 d . . . O114 O 1.0172(4) 0.6302(10) 0.9341(5) 0.022(3) Uani 1 1 d . . . O113 O 1.0224(4) 0.7704(10) 0.8765(5) 0.020(3) Uani 1 1 d . . . O112 O 1.0372(8) 0.8023(14) 0.9604(7) 0.065(6) Uani 1 1 d . . . O111 O 1.0850(5) 0.6885(14) 0.9129(7) 0.045(4) Uani 1 1 d . . . O1W O 0.7489(11) 0.919(2) 0.5663(10) 0.108(10) Uani 1 1 d . . . O2W O 0.8128(6) 0.4616(15) 0.8840(7) 0.050(5) Uani 1 1 d . . . O3W O 0.8290(6) 0.5561(17) 0.7860(8) 0.065(6) Uani 1 1 d . . . N1 N 1.0610(5) 1.0119(11) 0.8434(6) 0.015(3) Uani 1 1 d . . . N2 N 1.0555(5) 0.4622(11) 0.8138(5) 0.015(3) Uani 1 1 d . . . C2C C 1.0264(6) 1.0829(17) 0.8566(6) 0.020(4) Uani 1 1 d . . . H2CA H 1.0044 1.0829 0.8304 0.025 Uiso 1 1 calc R . . H2CB H 1.0377 1.1577 0.8598 0.025 Uiso 1 1 calc R . . C2B C 1.1049(6) 1.0609(15) 0.8619(7) 0.018(4) Uani 1 1 d . . . H2BA H 1.1137 1.1200 0.8395 0.022 Uiso 1 1 calc R . . H2BB H 1.1001 1.0935 0.8944 0.022 Uiso 1 1 calc R . . C2A C 1.0635(6) 0.9951(14) 0.7899(7) 0.015(4) Uani 1 1 d U . . H2AA H 1.0922 0.9652 0.7811 0.018 Uiso 1 1 calc R . . H2AB H 1.0598 1.0652 0.7728 0.018 Uiso 1 1 calc R . . C3B C 1.1395(6) 0.9848(14) 0.8654(7) 0.016(4) Uani 1 1 d . . . H3BA H 1.1664 1.0238 0.8741 0.019 Uiso 1 1 calc R . . H3BB H 1.1440 0.9503 0.8332 0.019 Uiso 1 1 calc R . . C3C C 1.0058(5) 1.0502(16) 0.9028(7) 0.017(4) Uani 1 1 d U . . H3CA H 1.0283 1.0220 0.9251 0.021 Uiso 1 1 calc R . . H3CB H 0.9927 1.1150 0.9182 0.021 Uiso 1 1 calc R . . C3A C 1.0286(6) 0.9178(16) 0.7751(7) 0.021(4) Uani 1 1 d U . . H3AA H 1.0003 0.9555 0.7758 0.025 Uiso 1 1 calc R . . H3AB H 1.0274 0.8569 0.7986 0.025 Uiso 1 1 calc R . . N4C N 0.9728(6) 0.9684(13) 0.8965(5) 0.023(4) Uani 1 1 d . . . H4C1 H 0.9859 0.9043 0.8877 0.028 Uiso 1 1 calc R . . H4C2 H 0.9550 0.9890 0.8713 0.028 Uiso 1 1 calc R . . N4B N 1.1304(5) 0.8937(12) 0.9047(6) 0.019(3) Uani 1 1 d . . . H4B1 H 1.1122 0.9215 0.9281 0.023 Uiso 1 1 calc R . . H4B2 H 1.1162 0.8370 0.8898 0.023 Uiso 1 1 calc R . . N4A N 1.0371(5) 0.8732(12) 0.7236(6) 0.015(3) Uani 1 1 d U . . H4A1 H 1.0376 0.9297 0.7017 0.019 Uiso 1 1 calc R . . H4A2 H 1.0636 0.8396 0.7228 0.019 Uiso 1 1 calc R . . C5B C 1.1689(8) 0.8518(17) 0.9284(8) 0.035(5) Uani 1 1 d . . . H5BA H 1.1599 0.8047 0.9558 0.042 Uiso 1 1 calc R . . H5BB H 1.1853 0.9135 0.9423 0.042 Uiso 1 1 calc R . . C5C C 0.9453(6) 0.9485(17) 0.9413(7) 0.025(5) Uani 1 1 d . . . H5CA H 0.9643 0.9242 0.9683 0.030 Uiso 1 1 calc R . . H5CB H 0.9317 1.0176 0.9513 0.030 Uiso 1 1 calc R . . C5A C 1.0037(6) 0.7963(16) 0.7098(8) 0.025(5) Uani 1 1 d . . . H5AA H 0.9770 0.8364 0.7012 0.030 Uiso 1 1 calc R . . H5AB H 0.9970 0.7490 0.7380 0.030 Uiso 1 1 calc R . . C6B C 1.1995(5) 0.7861(13) 0.8948(6) 0.011(3) Uani 1 1 d U . . C6A C 1.0171(7) 0.7265(17) 0.6673(9) 0.030(5) Uani 1 1 d U . . C6C C 0.9102(10) 0.8641(17) 0.9334(9) 0.043(7) Uani 1 1 d . . . C7B C 1.2363(7) 0.8234(17) 0.8764(7) 0.027(5) Uani 1 1 d . . . H7BA H 1.2455 0.8954 0.8830 0.033 Uiso 1 1 calc R . . C7C C 0.8680(6) 0.8815(16) 0.9390(6) 0.018(4) Uani 1 1 d U . . H7CA H 0.8582 0.9511 0.9489 0.022 Uiso 1 1 calc R . . C7A C 1.0084(10) 0.752(2) 0.6208(8) 0.045(7) Uani 1 1 d . . . H7AA H 0.9901 0.8126 0.6140 0.054 Uiso 1 1 calc R . . C8B C 1.2617(7) 0.7532(18) 0.8463(9) 0.032(5) Uani 1 1 d . . . H8BA H 1.2892 0.7763 0.8350 0.038 Uiso 1 1 calc R . . C8C C 0.8399(6) 0.8045(17) 0.9311(7) 0.022(4) Uani 1 1 d U . . H8CA H 0.8100 0.8188 0.9357 0.027 Uiso 1 1 calc R . . C8A C 1.0250(8) 0.6943(19) 0.5833(10) 0.047(7) Uani 1 1 d . . . H8AA H 1.0211 0.7164 0.5505 0.056 Uiso 1 1 calc R . . C9A C 1.0492(9) 0.5967(17) 0.5954(9) 0.037(6) Uani 1 1 d . . . H9AA H 1.0598 0.5497 0.5707 0.045 Uiso 1 1 calc R . . C9C C 0.8532(7) 0.7002(18) 0.9158(8) 0.031(5) Uani 1 1 d . . . H9CA H 0.8334 0.6415 0.9124 0.037 Uiso 1 1 calc R . . C9B C 1.2470(6) 0.6578(15) 0.8346(8) 0.021(4) Uani 1 1 d . . . H9BA H 1.2620 0.6119 0.8126 0.026 Uiso 1 1 calc R . . C10A C 1.0563(6) 0.5746(15) 0.6437(7) 0.021(4) Uani 1 1 d U . . C10C C 0.8981(6) 0.6892(15) 0.9058(6) 0.016(4) Uani 1 1 d U . . C10B C 1.2062(6) 0.6248(15) 0.8572(8) 0.020(4) Uani 1 1 d . . . N11A N 1.0415(6) 0.6332(13) 0.6814(6) 0.024(4) Uani 1 1 d . . . N11C N 0.9271(5) 0.7669(12) 0.9129(6) 0.021(3) Uani 1 1 d . . . N11B N 1.1841(5) 0.6890(15) 0.8850(5) 0.021(4) Uani 1 1 d . . . C12B C 1.1886(7) 0.5118(17) 0.8521(9) 0.029(5) Uani 1 1 d . . . H12A H 1.1975 0.4801 0.8205 0.034 Uiso 1 1 calc R . . H12B H 1.1996 0.4649 0.8786 0.034 Uiso 1 1 calc R . . C12A C 1.0868(6) 0.4830(17) 0.6589(8) 0.025(4) Uani 1 1 d U . . H12C H 1.0797 0.4169 0.6399 0.030 Uiso 1 1 calc R . . H12D H 1.1169 0.5039 0.6510 0.030 Uiso 1 1 calc R . . C12C C 0.9149(6) 0.5847(17) 0.8888(8) 0.026(5) Uani 1 1 d . . . H12E H 0.8919 0.5456 0.8709 0.031 Uiso 1 1 calc R . . H12F H 0.9233 0.5399 0.9172 0.031 Uiso 1 1 calc R . . N13C N 0.9543(5) 0.5999(12) 0.8554(5) 0.015(3) Uani 1 1 d . . . H13A H 0.9446 0.6290 0.8266 0.018 Uiso 1 1 calc R . . H13B H 0.9720 0.6508 0.8696 0.018 Uiso 1 1 calc R . . N13A N 1.0836(5) 0.4575(12) 0.7126(6) 0.017(3) Uani 1 1 d . . . H13C H 1.1075 0.4176 0.7213 0.021 Uiso 1 1 calc R . . H13D H 1.0847 0.5219 0.7295 0.021 Uiso 1 1 calc R . . N13B N 1.1409(5) 0.5202(13) 0.8547(6) 0.021(4) Uani 1 1 d . . . H13E H 1.1308 0.5511 0.8264 0.025 Uiso 1 1 calc R . . H13F H 1.1335 0.5654 0.8801 0.025 Uiso 1 1 calc R . . C14B C 1.1186(6) 0.4093(15) 0.8621(7) 0.016(4) Uani 1 1 d U . . H14A H 1.1279 0.3576 0.8365 0.019 Uiso 1 1 calc R . . H14B H 1.1263 0.3787 0.8942 0.019 Uiso 1 1 calc R . . C14C C 0.9814(6) 0.5027(15) 0.8434(8) 0.021(4) Uani 1 1 d U . . H14C H 0.9918 0.4682 0.8738 0.025 Uiso 1 1 calc R . . H14D H 0.9639 0.4489 0.8252 0.025 Uiso 1 1 calc R . . C14A C 1.0450(7) 0.3983(17) 0.7280(7) 0.027(5) Uani 1 1 d U . . H14E H 1.0194 0.4459 0.7241 0.032 Uiso 1 1 calc R . . H14F H 1.0410 0.3346 0.7065 0.032 Uiso 1 1 calc R . . C15C C 1.0179(6) 0.5365(14) 0.8141(8) 0.019(4) Uani 1 1 d . . . H15A H 1.0178 0.6024 0.7961 0.022 Uiso 1 1 calc R . . C15A C 1.0471(7) 0.3610(16) 0.7788(8) 0.026(4) Uani 1 1 d . . . H15B H 1.0707 0.3075 0.7825 0.031 Uiso 1 1 calc R . . H15C H 1.0195 0.3253 0.7877 0.031 Uiso 1 1 calc R . . C15B C 1.0700(6) 0.4284(15) 0.8590(7) 0.016(4) Uani 1 1 d . . . H15D H 1.0549 0.3602 0.8677 0.020 Uiso 1 1 calc R . . H15E H 1.0619 0.4838 0.8835 0.020 Uiso 1 1 calc R . . C2E C 0.7654(6) 0.5721(15) 0.6707(6) 0.018(4) Uani 1 1 d U . . H2EA H 0.7957 0.5457 0.6698 0.022 Uiso 1 1 calc R . . H2EB H 0.7485 0.5278 0.6475 0.022 Uiso 1 1 calc R . . C2F C 0.7991(7) 0.7469(15) 0.6791(7) 0.025(5) Uani 1 1 d . . . H2FA H 0.8194 0.6937 0.6937 0.031 Uiso 1 1 calc R . . H2FB H 0.7868 0.7914 0.7058 0.031 Uiso 1 1 calc R . . C2D C 0.7241(7) 0.7433(15) 0.6548(7) 0.025(4) Uani 1 1 d . . . H2DA H 0.7284 0.8204 0.6461 0.030 Uiso 1 1 calc R . . H2DB H 0.7126 0.7408 0.6884 0.030 Uiso 1 1 calc R . . C3F C 0.8245(5) 0.8229(14) 0.6421(6) 0.012(3) Uani 1 1 d U . . H3FA H 0.8039 0.8510 0.6174 0.015 Uiso 1 1 calc R . . H3FB H 0.8365 0.8858 0.6600 0.015 Uiso 1 1 calc R . . N3 N 0.7646(4) 0.6899(11) 0.6538(5) 0.010(3) Uani 1 1 d U . . C3E C 0.7471(6) 0.5537(15) 0.7229(7) 0.021(4) Uani 1 1 d . . . H3EA H 0.7591 0.6082 0.7458 0.025 Uiso 1 1 calc R . . H3EB H 0.7152 0.5601 0.7229 0.025 Uiso 1 1 calc R . . C3D C 0.6903(6) 0.6940(16) 0.6201(7) 0.023(4) Uani 1 1 d . . . H3DA H 0.6825 0.6207 0.6320 0.028 Uiso 1 1 calc R . . H3DB H 0.6639 0.7393 0.6210 0.028 Uiso 1 1 calc R . . N4 N 0.8389(5) 0.2151(11) 0.6140(5) 0.011(3) Uani 1 1 d U . . N4E N 0.7598(5) 0.4476(12) 0.7372(5) 0.015(3) Uani 1 1 d U . . H4E1 H 0.7895 0.4437 0.7362 0.018 Uiso 1 1 calc R . . H4E2 H 0.7492 0.3991 0.7146 0.018 Uiso 1 1 calc R . . N4D N 0.7054(6) 0.6853(14) 0.5690(6) 0.027(4) Uani 1 1 d U . . H4D1 H 0.7179 0.7501 0.5600 0.032 Uiso 1 1 calc R . . H4D2 H 0.7264 0.6326 0.5672 0.032 Uiso 1 1 calc R . . N4F N 0.8584(6) 0.7680(13) 0.6181(6) 0.024(4) Uani 1 1 d . . . H4F1 H 0.8765 0.7398 0.6416 0.029 Uiso 1 1 calc R . . H4F2 H 0.8741 0.8186 0.6010 0.029 Uiso 1 1 calc R . . C5F C 0.8466(6) 0.6764(16) 0.5833(7) 0.021(4) Uani 1 1 d U . . H5FA H 0.8350 0.6145 0.6022 0.025 Uiso 1 1 calc R . . H5FB H 0.8235 0.7017 0.5610 0.025 Uiso 1 1 calc R . . C5D C 0.6704(8) 0.658(2) 0.5336(8) 0.040(6) Uani 1 1 d . . . H5DA H 0.6491 0.7186 0.5330 0.048 Uiso 1 1 calc R . . H5DB H 0.6830 0.6522 0.5006 0.048 Uiso 1 1 calc R . . C5E C 0.7447(7) 0.4115(17) 0.7880(8) 0.031(5) Uani 1 1 d . . . H5EA H 0.7135 0.3927 0.7871 0.037 Uiso 1 1 calc R . . H5EB H 0.7488 0.4712 0.8116 0.037 Uiso 1 1 calc R . . C6E C 0.7711(6) 0.3130(16) 0.8033(7) 0.020(4) Uani 1 1 d U . . C6D C 0.6478(6) 0.5572(15) 0.5454(7) 0.018(4) Uani 1 1 d U . . C6F C 0.8843(6) 0.6384(15) 0.5537(7) 0.021(4) Uani 1 1 d . . . C7F C 0.9031(6) 0.7003(17) 0.5179(7) 0.020(4) Uani 1 1 d U . . H7FA H 0.8924 0.7710 0.5112 0.024 Uiso 1 1 calc R . . C7E C 0.7576(6) 0.2473(16) 0.8414(6) 0.020(4) Uani 1 1 d . . . H7EA H 0.7296 0.2574 0.8549 0.024 Uiso 1 1 calc R . . C7D C 0.6014(7) 0.556(2) 0.5521(8) 0.033(5) Uani 1 1 d . . . H7DA H 0.5849 0.6215 0.5519 0.039 Uiso 1 1 calc R . . C8F C 0.9380(7) 0.6594(16) 0.4915(8) 0.028(5) Uani 1 1 d . . . H8FA H 0.9502 0.6996 0.4654 0.034 Uiso 1 1 calc R . . C8D C 0.5817(8) 0.453(2) 0.5590(8) 0.045(7) Uani 1 1 d . . . H8DA H 0.5511 0.4461 0.5599 0.054 Uiso 1 1 calc R . . C8E C 0.7813(8) 0.176(2) 0.8580(9) 0.049(8) Uani 1 1 d . . . H8EA H 0.7735 0.1413 0.8876 0.059 Uiso 1 1 calc R . . C9E C 0.8210(6) 0.1439(15) 0.8334(7) 0.022(4) Uani 1 1 d . . . H9EA H 0.8383 0.0842 0.8434 0.026 Uiso 1 1 calc R . . C9F C 0.9548(7) 0.5547(19) 0.5049(7) 0.029(5) Uani 1 1 d . . . H9FA H 0.9795 0.5249 0.4892 0.035 Uiso 1 1 calc R . . C9D C 0.6072(7) 0.363(2) 0.5642(7) 0.033(5) Uani 1 1 d . . . H9DA H 0.5945 0.2936 0.5692 0.039 Uiso 1 1 calc R . . C10E C 0.8306(6) 0.2077(15) 0.7949(7) 0.018(4) Uani 1 1 d . . . C10F C 0.9332(5) 0.4983(15) 0.5421(7) 0.016(4) Uani 1 1 d . . . C10D C 0.6526(7) 0.3747(19) 0.5622(8) 0.032(5) Uani 1 1 d . . . N11F N 0.8998(5) 0.5420(13) 0.5672(6) 0.017(3) Uani 1 1 d U . . N11D N 0.6707(5) 0.4662(14) 0.5511(5) 0.020(4) Uani 1 1 d . . . N11E N 0.8073(5) 0.2949(12) 0.7806(5) 0.016(3) Uani 1 1 d . . . C12F C 0.9496(7) 0.3932(17) 0.5590(8) 0.028(5) Uani 1 1 d U . . H12G H 0.9721 0.4054 0.5841 0.034 Uiso 1 1 calc R . . H12H H 0.9632 0.3545 0.5314 0.034 Uiso 1 1 calc R . . C12E C 0.8743(6) 0.1995(17) 0.7665(7) 0.020(4) Uani 1 1 d U . . H12I H 0.8934 0.2606 0.7758 0.025 Uiso 1 1 calc R . . H12J H 0.8891 0.1309 0.7751 0.025 Uiso 1 1 calc R . . C12D C 0.6813(5) 0.2771(16) 0.5675(7) 0.019(4) Uani 1 1 d U . . H12K H 0.6871 0.2447 0.5351 0.023 Uiso 1 1 calc R . . H12L H 0.6671 0.2218 0.5881 0.023 Uiso 1 1 calc R . . N13E N 0.8659(5) 0.2027(11) 0.7134(6) 0.017(3) Uani 1 1 d U . . H13G H 0.8598 0.2731 0.7046 0.020 Uiso 1 1 calc R . . H13H H 0.8907 0.1824 0.6973 0.020 Uiso 1 1 calc R . . N13D N 0.7243(4) 0.3149(12) 0.5914(5) 0.013(3) Uani 1 1 d . . . H13I H 0.7344 0.3749 0.5750 0.015 Uiso 1 1 calc R . . H13J H 0.7188 0.3354 0.6230 0.015 Uiso 1 1 calc R . . N13F N 0.9133(6) 0.3219(15) 0.5807(6) 0.030(4) Uani 1 1 d . . . H13K H 0.9255 0.2600 0.5935 0.036 Uiso 1 1 calc R . . H13L H 0.9004 0.3590 0.6058 0.036 Uiso 1 1 calc R . . C14E C 0.8306(5) 0.1334(14) 0.6970(7) 0.016(4) Uani 1 1 d U . . H14G H 0.8026 0.1690 0.7040 0.019 Uiso 1 1 calc R . . H14H H 0.8315 0.0637 0.7149 0.019 Uiso 1 1 calc R . . C14F C 0.8801(6) 0.2906(16) 0.5455(7) 0.022(4) Uani 1 1 d U . . H14I H 0.8601 0.3523 0.5399 0.027 Uiso 1 1 calc R . . H14J H 0.8938 0.2719 0.5140 0.027 Uiso 1 1 calc R . . C14D C 0.7586(6) 0.2302(14) 0.5915(6) 0.013(4) Uani 1 1 d U . . H14K H 0.7650 0.2072 0.5577 0.016 Uiso 1 1 calc R . . H14L H 0.7487 0.1660 0.6101 0.016 Uiso 1 1 calc R . . C15F C 0.8553(6) 0.1954(16) 0.5641(7) 0.022(4) Uani 1 1 d . . . H15F H 0.8743 0.1306 0.5643 0.026 Uiso 1 1 calc R . . H15G H 0.8307 0.1805 0.5421 0.026 Uiso 1 1 calc R . . C15D C 0.7987(6) 0.2772(15) 0.6147(6) 0.014(4) Uani 1 1 d U . . H15H H 0.7978 0.3467 0.6297 0.017 Uiso 1 1 calc R . . C15E C 0.8346(6) 0.1118(15) 0.6412(7) 0.021(4) Uani 1 1 d U . . H15I H 0.8603 0.0658 0.6349 0.025 Uiso 1 1 calc R . . H15J H 0.8087 0.0722 0.6297 0.025 Uiso 1 1 calc R . . Cl12 Cl 1.13681(13) 0.7393(3) 0.76089(16) 0.0146(8) Uani 1 1 d . . . O121 O 1.1217(4) 0.7845(11) 0.7169(5) 0.024(3) Uani 1 1 d . . . O122 O 1.1739(5) 0.7953(13) 0.7768(5) 0.033(3) Uani 1 1 d . . . O123 O 1.1450(6) 0.6227(11) 0.7570(6) 0.041(4) Uani 1 1 d . . . O124 O 1.1041(5) 0.7499(17) 0.7969(6) 0.048(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 0.0144(4) 0.0154(4) 0.0187(4) 0.0003(3) -0.0022(3) 0.0021(3) O11 0.020(7) 0.020(7) 0.036(9) 0.002(6) 0.002(6) 0.010(6) O12 0.026(7) 0.029(8) 0.021(7) -0.004(6) -0.004(6) 0.012(6) O13 0.019(7) 0.021(7) 0.028(7) 0.005(6) -0.009(6) -0.014(6) O14 0.038(8) 0.016(7) 0.015(7) -0.009(5) -0.003(6) 0.007(6) Re2 0.0130(3) 0.0141(4) 0.0149(3) 0.0022(3) 0.0003(3) -0.0008(3) O21 0.021(3) 0.021(3) 0.020(3) 0.0022(19) 0.0016(19) -0.0016(19) O22 0.025(3) 0.024(3) 0.025(3) 0.0004(19) -0.0003(19) 0.002(2) O23 0.029(8) 0.029(8) 0.017(7) -0.008(6) -0.011(6) -0.004(6) O24 0.028(8) 0.027(8) 0.022(7) 0.003(6) -0.006(6) -0.014(6) Re3 0.0128(3) 0.0202(4) 0.0162(4) 0.0000(3) 0.0021(3) 0.0000(3) O31 0.026(7) 0.031(8) 0.017(7) -0.008(6) 0.006(6) 0.000(6) O32 0.030(8) 0.036(9) 0.019(7) -0.003(6) 0.008(6) 0.018(7) O33 0.023(7) 0.022(7) 0.028(7) 0.008(6) 0.015(6) 0.000(6) O34 0.032(8) 0.034(9) 0.023(7) 0.009(6) -0.004(6) -0.005(7) Re4 0.0225(4) 0.0195(4) 0.0158(4) 0.0031(3) -0.0008(3) 0.0004(3) O41 0.037(9) 0.041(9) 0.023(8) 0.006(7) 0.008(7) 0.001(7) O42 0.023(7) 0.026(7) 0.023(8) -0.005(6) -0.001(6) -0.003(6) O43 0.031(4) 0.030(4) 0.030(4) 0.002(2) -0.001(2) 0.002(2) O44 0.035(9) 0.043(9) 0.024(8) 0.008(7) 0.003(7) 0.010(7) Re5 0.0238(4) 0.0288(5) 0.0293(4) -0.0008(4) 0.0004(3) -0.0011(4) O51 0.034(9) 0.062(12) 0.033(9) 0.009(8) 0.000(7) 0.003(8) O52 0.17(3) 0.025(10) 0.071(15) 0.009(10) -0.047(16) -0.021(13) O53 0.050(16) 0.48(7) 0.045(15) -0.01(3) -0.003(12) -0.10(3) O54 0.35(5) 0.057(15) 0.044(13) 0.000(11) -0.04(2) 0.13(2) Re6 0.0198(4) 0.0238(4) 0.0229(4) 0.0067(3) 0.0012(3) -0.0036(3) O61 0.020(3) 0.017(3) 0.020(3) 0.0009(19) 0.0009(19) -0.0026(19) O62 0.060(11) 0.024(8) 0.031(8) -0.012(7) -0.011(8) -0.006(7) O63 0.023(8) 0.041(9) 0.038(9) 0.034(7) -0.003(7) -0.013(7) O64 0.021(3) 0.021(3) 0.019(3) 0.0030(19) -0.0010(19) -0.0007(19) Re7 0.0294(5) 0.0215(4) 0.0328(5) 0.0034(4) -0.0114(4) -0.0006(3) O71 0.051(10) 0.027(9) 0.062(12) 0.021(8) -0.025(9) -0.005(7) O72 0.053(11) 0.031(9) 0.041(10) -0.002(7) -0.006(8) 0.009(8) O73 0.038(9) 0.034(9) 0.055(11) 0.007(8) -0.009(8) -0.030(7) O74 0.046(11) 0.108(18) 0.063(13) -0.037(13) -0.023(10) 0.050(12) Re8 0.0625(8) 0.0497(7) 0.0636(8) 0.0023(6) 0.0048(6) 0.0010(6) O81 0.050(11) 0.030(9) 0.057(11) 0.005(8) -0.002(9) -0.012(8) O82 0.039(9) 0.044(10) 0.038(9) 0.006(8) -0.005(7) 0.010(8) O83 0.085(16) 0.083(17) 0.063(14) 0.037(12) 0.027(12) 0.009(13) O84 0.061(5) 0.060(5) 0.060(5) 0.001(2) -0.002(2) 0.000(2) Re9 0.0702(10) 0.0655(9) 0.1034(12) 0.0203(9) 0.0085(8) -0.0030(7) O91 0.057(5) 0.057(5) 0.058(5) 0.000(2) 0.000(2) 0.003(2) O92 0.070(14) 0.056(13) 0.12(2) -0.013(14) -0.037(14) -0.017(11) O93 0.084(16) 0.037(12) 0.111(19) 0.041(12) 0.011(14) -0.010(11) O94 0.096(8) 0.095(8) 0.097(8) 0.000(2) 0.000(2) -0.001(2) Re10 0.135(3) 0.0480(10) 0.0563(11) -0.0012(8) 0.004(2) -0.008(2) Re1' 0.135(3) 0.0480(10) 0.0563(11) -0.0012(8) 0.004(2) -0.008(2) Cl11 0.020(2) 0.023(2) 0.021(2) -0.0043(19) -0.0102(18) 0.0019(19) O114 0.020(7) 0.011(7) 0.035(8) 0.003(6) 0.005(6) 0.003(5) O113 0.019(7) 0.015(7) 0.026(7) 0.010(6) -0.002(6) 0.004(5) O112 0.114(18) 0.029(10) 0.051(11) -0.030(9) 0.009(12) -0.017(10) O111 0.023(8) 0.037(10) 0.075(13) -0.014(9) -0.001(8) 0.006(7) O1W 0.16(3) 0.080(18) 0.082(18) 0.017(15) -0.052(19) -0.045(19) O2W 0.041(10) 0.040(10) 0.069(13) 0.012(9) -0.006(9) -0.003(8) O3W 0.054(12) 0.054(13) 0.088(16) -0.023(11) -0.003(11) -0.018(10) N1 0.017(8) 0.010(7) 0.017(8) -0.011(6) 0.011(6) -0.009(6) N2 0.029(9) 0.001(7) 0.014(8) -0.002(6) 0.002(6) 0.002(6) C2C 0.014(9) 0.036(12) 0.011(9) -0.002(8) -0.007(7) 0.001(8) C2B 0.017(10) 0.014(9) 0.023(10) 0.004(8) -0.008(8) -0.007(7) C2A 0.008(7) 0.011(7) 0.026(8) -0.006(6) 0.004(6) 0.004(6) C3B 0.023(10) 0.008(9) 0.017(9) 0.003(7) 0.003(7) -0.006(7) C3C 0.007(7) 0.022(8) 0.023(7) 0.009(6) -0.004(6) 0.000(6) C3A 0.024(7) 0.021(7) 0.017(7) 0.003(6) -0.004(6) 0.007(6) N4C 0.046(11) 0.018(8) 0.006(7) 0.002(6) -0.004(7) 0.012(8) N4B 0.024(9) 0.014(8) 0.019(8) -0.008(6) 0.011(7) 0.004(7) N4A 0.013(6) 0.012(6) 0.021(6) -0.002(5) -0.003(5) 0.011(5) C5B 0.055(15) 0.019(11) 0.031(12) -0.001(9) 0.004(11) 0.018(10) C5C 0.025(11) 0.026(11) 0.025(11) -0.002(9) 0.023(8) 0.002(9) C5A 0.017(10) 0.023(10) 0.037(12) -0.014(9) 0.001(8) -0.006(8) C6B 0.013(7) 0.005(7) 0.016(7) 0.005(6) -0.004(6) 0.003(6) C6A 0.034(8) 0.021(8) 0.035(8) -0.010(7) 0.001(7) 0.009(7) C6C 0.09(2) 0.009(10) 0.030(13) -0.009(9) -0.008(13) 0.000(11) C7B 0.041(13) 0.017(10) 0.024(10) -0.002(8) 0.001(9) -0.005(9) C7C 0.015(7) 0.026(8) 0.013(7) 0.002(6) 0.010(6) 0.001(6) C7A 0.08(2) 0.032(13) 0.026(12) 0.007(10) -0.023(12) 0.006(12) C8B 0.014(10) 0.033(13) 0.049(14) 0.009(10) -0.013(9) -0.003(9) C8C 0.015(7) 0.030(8) 0.022(7) -0.006(6) 0.003(6) 0.012(7) C8A 0.053(16) 0.027(13) 0.061(17) -0.017(12) -0.046(13) 0.014(11) C9A 0.064(17) 0.011(10) 0.038(13) 0.008(9) -0.021(12) -0.004(10) C9C 0.031(12) 0.032(12) 0.029(12) 0.010(9) -0.019(9) -0.007(10) C9B 0.006(9) 0.017(10) 0.041(12) -0.012(9) 0.006(8) 0.004(7) C10A 0.024(8) 0.011(7) 0.029(8) -0.001(6) -0.002(6) -0.003(6) C10C 0.017(7) 0.020(7) 0.010(7) -0.005(6) 0.009(6) -0.001(6) C10B 0.013(9) 0.016(10) 0.033(11) -0.007(8) -0.011(8) -0.006(7) N11A 0.030(9) 0.015(8) 0.026(9) 0.004(7) -0.011(7) -0.002(7) N11C 0.027(9) 0.010(8) 0.025(9) -0.004(6) 0.006(7) -0.002(7) N11B 0.013(8) 0.042(11) 0.009(7) 0.012(7) 0.004(6) 0.013(7) C12B 0.018(11) 0.028(12) 0.040(13) -0.018(9) -0.010(9) 0.007(9) C12A 0.022(8) 0.026(8) 0.028(8) 0.003(7) 0.008(7) 0.013(7) C12C 0.009(9) 0.019(10) 0.051(14) -0.009(9) 0.004(9) -0.001(8) N13C 0.024(8) 0.007(7) 0.014(8) 0.005(6) -0.001(6) -0.002(6) N13A 0.014(8) 0.012(7) 0.026(8) 0.005(6) -0.004(6) 0.005(6) N13B 0.016(8) 0.025(9) 0.021(9) 0.008(7) -0.007(6) -0.002(7) C14B 0.013(7) 0.017(7) 0.017(7) 0.002(6) -0.005(6) -0.009(6) C14C 0.017(7) 0.018(7) 0.028(8) -0.004(6) 0.005(6) 0.009(6) C14A 0.032(8) 0.028(8) 0.020(8) -0.006(6) -0.015(7) 0.006(7) C15C 0.011(9) 0.002(8) 0.042(12) 0.008(8) 0.013(8) 0.001(7) C15A 0.027(11) 0.022(11) 0.029(11) -0.007(9) 0.005(9) -0.009(8) C15B 0.009(9) 0.018(10) 0.022(9) -0.005(7) 0.001(7) -0.004(7) C2E 0.025(7) 0.018(7) 0.010(7) 0.007(6) -0.003(6) -0.001(6) C2F 0.049(13) 0.007(9) 0.021(10) 0.000(7) 0.012(9) -0.006(9) C2D 0.034(12) 0.014(10) 0.026(11) -0.003(8) 0.003(8) -0.008(8) C3F 0.012(7) 0.011(7) 0.014(7) -0.003(6) 0.006(6) 0.006(6) N3 0.010(3) 0.009(3) 0.009(3) 0.0016(19) 0.0003(19) -0.0011(19) C3E 0.021(10) 0.013(9) 0.029(11) -0.001(8) 0.006(8) 0.012(8) C3D 0.024(11) 0.020(10) 0.025(10) 0.014(8) 0.006(8) 0.012(8) N4 0.014(4) 0.008(4) 0.012(4) 0.000(3) 0.001(3) 0.000(3) N4E 0.015(4) 0.014(4) 0.016(4) -0.001(2) 0.000(2) 0.001(2) N4D 0.032(7) 0.016(7) 0.032(7) 0.000(6) -0.006(6) 0.014(6) N4F 0.037(10) 0.013(8) 0.021(9) -0.002(7) -0.011(7) -0.001(7) C5F 0.021(4) 0.020(4) 0.022(4) -0.001(2) 0.000(2) -0.001(2) C5D 0.057(16) 0.046(14) 0.018(11) 0.000(10) -0.021(11) 0.025(12) C5E 0.034(13) 0.023(11) 0.037(13) -0.001(9) 0.005(10) -0.002(9) C6E 0.023(8) 0.022(8) 0.015(7) 0.006(6) 0.011(6) -0.006(6) C6D 0.018(4) 0.018(4) 0.018(4) -0.001(2) 0.000(2) 0.001(2) C6F 0.021(10) 0.014(10) 0.029(11) -0.011(8) 0.003(8) -0.010(8) C7F 0.018(7) 0.022(8) 0.020(7) 0.001(6) -0.003(6) -0.016(6) C7E 0.022(10) 0.031(12) 0.007(8) -0.005(8) 0.001(7) -0.012(9) C7D 0.019(11) 0.047(14) 0.032(12) -0.017(10) -0.008(9) 0.019(10) C8F 0.038(12) 0.017(10) 0.030(11) -0.007(9) 0.005(10) -0.003(9) C8D 0.039(14) 0.07(2) 0.021(11) -0.001(12) 0.002(10) 0.037(14) C8E 0.035(14) 0.073(19) 0.039(14) 0.043(14) -0.031(11) -0.025(13) C9E 0.015(10) 0.017(10) 0.034(11) 0.001(8) 0.002(8) 0.001(8) C9F 0.018(10) 0.044(13) 0.024(11) 0.014(10) 0.007(8) -0.002(9) C9D 0.020(11) 0.063(16) 0.015(10) 0.004(10) 0.003(8) -0.009(10) C10E 0.019(10) 0.015(9) 0.020(9) 0.004(7) 0.012(7) 0.002(8) C10F 0.007(8) 0.023(10) 0.018(9) 0.006(7) 0.003(7) 0.002(7) C10D 0.034(13) 0.045(14) 0.017(10) 0.004(9) 0.003(9) 0.019(11) N11F 0.017(4) 0.017(4) 0.018(4) 0.001(2) 0.000(2) 0.000(2) N11D 0.015(8) 0.034(10) 0.011(8) -0.010(7) -0.008(6) -0.003(7) N11E 0.016(8) 0.015(8) 0.018(8) 0.008(6) -0.009(6) -0.004(6) C12F 0.022(8) 0.028(8) 0.034(8) 0.005(7) -0.007(7) -0.003(7) C12E 0.006(7) 0.030(8) 0.026(8) -0.005(6) -0.001(6) 0.002(6) C12D 0.009(7) 0.025(8) 0.022(7) 0.007(6) -0.006(6) -0.011(6) N13E 0.017(6) 0.007(6) 0.027(7) -0.001(5) 0.000(5) 0.006(5) N13D 0.013(7) 0.012(7) 0.013(7) -0.004(6) 0.001(6) 0.001(6) N13F 0.038(11) 0.033(10) 0.020(9) 0.014(8) -0.007(8) -0.016(8) C14E 0.008(6) 0.011(7) 0.030(7) 0.010(6) -0.001(6) 0.000(6) C14F 0.022(4) 0.023(4) 0.022(4) 0.000(2) 0.000(2) 0.001(2) C14D 0.024(7) 0.012(7) 0.003(6) 0.005(5) 0.000(6) 0.000(6) C15F 0.017(9) 0.024(10) 0.025(10) -0.014(8) 0.012(8) -0.013(8) C15D 0.014(4) 0.014(4) 0.014(4) 0.001(2) 0.000(2) 0.000(2) C15E 0.018(7) 0.014(7) 0.031(8) 0.009(6) 0.005(6) 0.004(6) Cl12 0.013(2) 0.011(2) 0.020(2) 0.0012(16) 0.0022(16) 0.0017(16) O121 0.021(7) 0.030(8) 0.021(7) -0.002(6) 0.002(6) 0.004(6) O122 0.029(8) 0.044(9) 0.027(8) -0.006(7) 0.004(6) -0.006(7) O123 0.075(12) 0.004(7) 0.045(10) -0.004(6) -0.007(9) 0.012(7) O124 0.028(9) 0.095(15) 0.022(8) 0.024(9) 0.016(6) 0.011(9) _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 O11 1.681(12) . ? Re1 O13 1.695(12) . ? Re1 O14 1.688(12) . ? Re1 O12 1.702(12) . ? Re2 O24 1.695(13) . ? Re2 O21 1.709(13) . ? Re2 O23 1.707(13) . ? Re2 O22 1.723(13) . ? Re3 O31 1.719(14) . ? Re3 O33 1.722(12) . ? Re3 O34 1.729(15) . ? Re3 O32 1.741(14) . ? Re4 O41 1.698(15) . ? Re4 O43 1.741(15) . ? Re4 O44 1.739(16) . ? Re4 O42 1.739(13) . ? Re5 O52 1.61(2) . ? Re5 O54 1.619(18) . ? Re5 O53 1.64(2) . ? Re5 O51 1.677(16) . ? Re6 O62 1.704(14) . ? Re6 O63 1.700(14) . ? Re6 O61 1.729(12) . ? Re6 O64 1.730(13) . ? Re7 O73 1.695(14) . ? Re7 O72 1.713(17) . ? Re7 O74 1.728(19) . ? Re7 O71 1.738(15) . ? Re8 O83 1.43(2) . ? Re8 O84 1.57(2) . ? Re8 O81 1.556(18) . ? Re8 O82 1.630(17) . ? Re9 O93 1.53(2) . ? Re9 O92 1.59(2) . ? Re9 O91 1.62(2) . ? Re9 O94 1.75(3) . ? Re10 O102 1.649(18) . ? Re10 O103 1.68(2) . ? Re10 O101 1.671(19) . ? Re10 O104 1.72(2) . ? Re1' O10' 1.657(19) . ? Re1' O10@ 1.68(2) . ? Re1' O10# 1.69(2) . ? Re1' O10? 1.74(2) . ? O10@ O1W 1.30(5) . ? Cl11 O114 1.400(14) . ? Cl11 O112 1.436(17) . ? Cl11 O111 1.473(16) . ? Cl11 O113 1.472(13) . ? N1 C2C 1.43(2) . ? N1 C2A 1.48(2) . ? N1 C2B 1.57(2) . ? N2 C15B 1.38(2) . ? N2 C15C 1.48(2) . ? N2 C15A 1.60(2) . ? C2C C3C 1.47(3) . ? C2B C3B 1.43(3) . ? C2A C3A 1.50(3) . ? C3B N4B 1.58(2) . ? C3C N4C 1.44(2) . ? C3A N4A 1.54(2) . ? N4C C5C 1.51(2) . ? N4B C5B 1.45(3) . ? N4A C5A 1.45(2) . ? C5B C6B 1.55(3) . ? C5C C6C 1.52(3) . ? C5A C6A 1.51(3) . ? C6B N11B 1.32(2) . ? C6B C7B 1.33(3) . ? C6A C7A 1.34(3) . ? C6A N11A 1.43(3) . ? C6C C7C 1.33(3) . ? C6C N11C 1.42(3) . ? C7B C8B 1.43(3) . ? C7C C8C 1.31(3) . ? C7A C8A 1.36(4) . ? C8B C9B 1.30(3) . ? C8C C9C 1.41(3) . ? C8A C9A 1.45(3) . ? C9A C10A 1.37(3) . ? C9C C10C 1.42(3) . ? C9B C10B 1.46(3) . ? C10A N11A 1.34(3) . ? C10A C12A 1.53(3) . ? C10C N11C 1.33(2) . ? C10C C12C 1.47(3) . ? C10B N11B 1.29(3) . ? C10B C12B 1.50(3) . ? C12B N13B 1.48(3) . ? C12A N13A 1.51(3) . ? C12C N13C 1.53(2) . ? N13C C14C 1.50(2) . ? N13A C14A 1.46(3) . ? N13B C14B 1.54(2) . ? C14B C15B 1.52(2) . ? C14C C15C 1.45(3) . ? C14A C15A 1.47(3) . ? C2E N3 1.52(2) . ? C2E C3E 1.56(3) . ? C2F N3 1.45(2) . ? C2F C3F 1.59(2) . ? C2D N3 1.41(2) . ? C2D C3D 1.54(3) . ? C3F N4F 1.41(2) . ? C3E N4E 1.42(2) . ? C3D N4D 1.48(3) . ? N4 C15D 1.46(2) . ? N4 C15F 1.48(2) . ? N4 C15E 1.48(2) . ? N4E C5E 1.54(3) . ? N4D C5D 1.49(3) . ? N4F C5F 1.52(2) . ? C5F C6F 1.50(3) . ? C5D C6D 1.47(3) . ? C5E C6E 1.52(3) . ? C6E N11E 1.30(2) . ? C6E C7E 1.39(3) . ? C6D N11D 1.34(2) . ? C6D C7D 1.44(3) . ? C6F N11F 1.33(3) . ? C6F C7F 1.37(3) . ? C7F C8F 1.39(3) . ? C7E C8E 1.23(3) . ? C7D C8D 1.43(4) . ? C8F C9F 1.44(3) . ? C8D C9D 1.36(3) . ? C8E C9E 1.46(3) . ? C9E C10E 1.35(3) . ? C9F C10F 1.41(3) . ? C9D C10D 1.41(3) . ? C10E N11E 1.35(2) . ? C10E C12E 1.56(2) . ? C10F N11F 1.35(2) . ? C10F C12F 1.47(3) . ? C10D N11D 1.30(3) . ? C10D C12D 1.50(3) . ? C12F N13F 1.54(3) . ? C12E N13E 1.48(2) . ? C12D N13D 1.55(2) . ? N13E C14E 1.46(2) . ? N13D C14D 1.49(2) . ? N13F C14F 1.46(2) . ? C14E C15E 1.56(3) . ? C14F C15F 1.49(3) . ? C14D C15D 1.51(2) . ? Cl12 O122 1.408(16) . ? Cl12 O121 1.411(14) . ? Cl12 O124 1.419(15) . ? Cl12 O123 1.462(13) . ? 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 O11 Re1 O13 112.0(7) . . ? O11 Re1 O14 106.9(6) . . ? O13 Re1 O14 110.3(6) . . ? O11 Re1 O12 111.4(6) . . ? O13 Re1 O12 109.7(6) . . ? O14 Re1 O12 106.4(6) . . ? O24 Re2 O21 107.6(6) . . ? O24 Re2 O23 111.1(6) . . ? O21 Re2 O23 110.0(7) . . ? O24 Re2 O22 108.9(7) . . ? O21 Re2 O22 109.6(6) . . ? O23 Re2 O22 109.6(7) . . ? O31 Re3 O33 110.5(6) . . ? O31 Re3 O34 109.9(7) . . ? O33 Re3 O34 109.6(7) . . ? O31 Re3 O32 107.8(6) . . ? O33 Re3 O32 108.9(7) . . ? O34 Re3 O32 110.1(7) . . ? O41 Re4 O43 110.1(7) . . ? O41 Re4 O44 108.5(7) . . ? O43 Re4 O44 107.7(7) . . ? O41 Re4 O42 113.8(7) . . ? O43 Re4 O42 110.8(7) . . ? O44 Re4 O42 105.7(7) . . ? O52 Re5 O54 108.3(15) . . ? O52 Re5 O53 116.2(18) . . ? O54 Re5 O53 104(3) . . ? O52 Re5 O51 109.1(11) . . ? O54 Re5 O51 109.6(11) . . ? O53 Re5 O51 109.9(12) . . ? O62 Re6 O63 108.5(8) . . ? O62 Re6 O61 110.1(7) . . ? O63 Re6 O61 108.4(6) . . ? O62 Re6 O64 110.4(7) . . ? O63 Re6 O64 107.3(7) . . ? O61 Re6 O64 112.1(6) . . ? O73 Re7 O72 109.7(8) . . ? O73 Re7 O74 107.7(10) . . ? O72 Re7 O74 108.2(9) . . ? O73 Re7 O71 111.2(8) . . ? O72 Re7 O71 112.3(8) . . ? O74 Re7 O71 107.6(11) . . ? O83 Re8 O84 113.4(13) . . ? O83 Re8 O81 114.3(11) . . ? O84 Re8 O81 112.0(10) . . ? O83 Re8 O82 105.5(12) . . ? O84 Re8 O82 107.6(10) . . ? O81 Re8 O82 103.1(9) . . ? O93 Re9 O92 112.6(11) . . ? O93 Re9 O91 107.4(12) . . ? O92 Re9 O91 104.1(12) . . ? O93 Re9 O94 113.3(13) . . ? O92 Re9 O94 113.5(13) . . ? O91 Re9 O94 105.1(12) . . ? O102 Re10 O103 112.2(16) . . ? O102 Re10 O101 109.3(14) . . ? O103 Re10 O101 109.3(16) . . ? O102 Re10 O104 106.2(14) . . ? O103 Re10 O104 112.4(17) . . ? O101 Re10 O104 107.2(15) . . ? O10' Re1' O10@ 114(2) . . ? O10' Re1' O10# 110.7(17) . . ? O10@ Re1' O10# 109.5(19) . . ? O10' Re1' O10? 105.4(16) . . ? O10@ Re1' O10? 111.4(19) . . ? O10# Re1' O10? 105.5(17) . . ? O1W O10@ Re1' 124(4) . . ? O114 Cl11 O112 110.1(11) . . ? O114 Cl11 O111 105.7(9) . . ? O112 Cl11 O111 112.3(12) . . ? O114 Cl11 O113 109.6(8) . . ? O112 Cl11 O113 109.8(11) . . ? O111 Cl11 O113 109.2(10) . . ? C2C N1 C2A 112.1(15) . . ? C2C N1 C2B 109.2(14) . . ? C2A N1 C2B 109.1(13) . . ? C15B N2 C15C 115.9(15) . . ? C15B N2 C15A 111.0(14) . . ? C15C N2 C15A 111.0(15) . . ? N1 C2C C3C 112.0(16) . . ? C3B C2B N1 114.7(15) . . ? N1 C2A C3A 108.5(15) . . ? C2B C3B N4B 112.2(15) . . ? N4C C3C C2C 113.2(16) . . ? C2A C3A N4A 110.7(15) . . ? C3C N4C C5C 114.4(15) . . ? C5B N4B C3B 114.3(16) . . ? C5A N4A C3A 110.6(15) . . ? N4B C5B C6B 114.7(17) . . ? C6C C5C N4C 113.3(17) . . ? N4A C5A C6A 112.2(16) . . ? N11B C6B C7B 123.2(17) . . ? N11B C6B C5B 112.1(16) . . ? C7B C6B C5B 124.7(18) . . ? C7A C6A N11A 124(2) . . ? C7A C6A C5A 123(2) . . ? N11A C6A C5A 113.2(19) . . ? C7C C6C N11C 123(2) . . ? C7C C6C C5C 125.0(19) . . ? N11C C6C C5C 112(2) . . ? C6B C7B C8B 118.8(19) . . ? C8C C7C C6C 121.1(19) . . ? C6A C7A C8A 121(2) . . ? C9B C8B C7B 120(2) . . ? C7C C8C C9C 121.2(18) . . ? C7A C8A C9A 117(2) . . ? C10A C9A C8A 118(2) . . ? C8C C9C C10C 115.3(19) . . ? C8B C9B C10B 116.5(18) . . ? N11A C10A C9A 125.7(19) . . ? N11A C10A C12A 113.5(17) . . ? C9A C10A C12A 120.6(19) . . ? N11C C10C C9C 124.3(18) . . ? N11C C10C C12C 116.1(16) . . ? C9C C10C C12C 119.5(17) . . ? N11B C10B C9B 122.4(17) . . ? N11B C10B C12B 115.4(18) . . ? C9B C10B C12B 122.1(18) . . ? C10A N11A C6A 113.9(17) . . ? C10C N11C C6C 114.7(18) . . ? C6B N11B C10B 119.0(16) . . ? N13B C12B C10B 107.0(16) . . ? N13A C12A C10A 112.3(15) . . ? C10C C12C N13C 111.4(16) . . ? C14C N13C C12C 118.6(14) . . ? C14A N13A C12A 116.1(15) . . ? C12B N13B C14B 112.9(15) . . ? C15B C14B N13B 107.2(15) . . ? C15C C14C N13C 109.3(15) . . ? C15A C14A N13A 113.4(16) . . ? C14C C15C N2 115.9(15) . . ? C14A C15A N2 109.5(16) . . ? N2 C15B C14B 114.6(15) . . ? N3 C2E C3E 114.4(15) . . ? N3 C2F C3F 109.9(15) . . ? N3 C2D C3D 114.0(15) . . ? N4F C3F C2F 112.5(15) . . ? C2D N3 C2F 114.6(15) . . ? C2D N3 C2E 116.8(14) . . ? C2F N3 C2E 107.5(13) . . ? N4E C3E C2E 106.7(14) . . ? N4D C3D C2D 113.6(16) . . ? C15D N4 C15F 113.0(14) . . ? C15D N4 C15E 111.7(14) . . ? C15F N4 C15E 110.8(15) . . ? C3E N4E C5E 115.6(14) . . ? C5D N4D C3D 113.8(17) . . ? C3F N4F C5F 118.0(15) . . ? C6F C5F N4F 112.7(15) . . ? C6D C5D N4D 113.0(17) . . ? N4E C5E C6E 108.6(16) . . ? N11E C6E C7E 121.3(18) . . ? N11E C6E C5E 117.8(16) . . ? C7E C6E C5E 120.8(17) . . ? N11D C6D C7D 120.5(19) . . ? N11D C6D C5D 119.1(18) . . ? C7D C6D C5D 120.4(19) . . ? N11F C6F C7F 122.8(18) . . ? N11F C6F C5F 114.1(17) . . ? C7F C6F C5F 123.0(18) . . ? C6F C7F C8F 119.9(19) . . ? C8E C7E C6E 121(2) . . ? C8D C7D C6D 116(2) . . ? C7F C8F C9F 118.1(19) . . ? C9D C8D C7D 119(2) . . ? C7E C8E C9E 122(2) . . ? C10E C9E C8E 113.0(18) . . ? C10F C9F C8F 117.2(19) . . ? C8D C9D C10D 119(2) . . ? N11E C10E C9E 124.8(17) . . ? N11E C10E C12E 111.6(15) . . ? C9E C10E C12E 123.0(17) . . ? N11F C10F C9F 122.5(18) . . ? N11F C10F C12F 116.9(17) . . ? C9F C10F C12F 120.2(17) . . ? N11D C10D C9D 122(2) . . ? N11D C10D C12D 117.6(19) . . ? C9D C10D C12D 120(2) . . ? C6F N11F C10F 119.1(16) . . ? C10D N11D C6D 121.9(17) . . ? C6E N11E C10E 117.2(15) . . ? C10F C12F N13F 112.0(17) . . ? N13E C12E C10E 109.8(14) . . ? C10D C12D N13D 107.9(16) . . ? C14E N13E C12E 114.7(15) . . ? C14D N13D C12D 113.6(13) . . ? C14F N13F C12F 113.9(15) . . ? N13E C14E C15E 110.1(15) . . ? C15F C14F N13F 109.9(16) . . ? N13D C14D C15D 108.5(14) . . ? C14F C15F N4 111.4(15) . . ? N4 C15D C14D 119.5(15) . . ? N4 C15E C14E 110.8(15) . . ? O122 Cl12 O121 110.0(9) . . ? O122 Cl12 O124 108.7(10) . . ? O121 Cl12 O124 108.9(9) . . ? O122 Cl12 O123 111.2(10) . . ? O121 Cl12 O123 112.5(9) . . ? O124 Cl12 O123 105.3(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.146 _refine_diff_density_min -4.702 _refine_diff_density_rms 0.353 data_r3bmre _database_code_CSD 195732 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 N8 O29 Re6' _chemical_formula_weight 2196.20 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' 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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 14.8844(10) _cell_length_b 12.5582(8) _cell_length_c 16.5916(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.7290(10) _cell_angle_gamma 90.00 _cell_volume 2860.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'triangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 12.736 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.652 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 33445 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.91 _reflns_number_total 12954 _reflns_number_gt 10712 _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 ; SHELX DELU and ISOR restraints were applied to all the carbon atoms of the cryptand ligand. Hydrogen atoms of the water molecules were not located or included in the model. The residual peaks are all close to Re atoms. 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^)+(0.1195P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(16) _refine_ls_number_reflns 12954 _refine_ls_number_parameters 712 _refine_ls_number_restraints 278 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1714 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.004 _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 0.86743(4) 0.16214(5) 0.43301(4) 0.02102(13) Uani 1 1 d . . . O11 O 0.7703(8) 0.0959(8) 0.3558(8) 0.027(2) Uani 1 1 d . . . O12 O 0.9247(10) 0.2418(10) 0.3845(8) 0.038(3) Uani 1 1 d . . . O13 O 0.8268(9) 0.2398(10) 0.4978(8) 0.032(3) Uani 1 1 d . . . O14 O 0.9518(9) 0.0721(9) 0.5001(8) 0.027(2) Uani 1 1 d . . . Re2 Re 0.39305(5) 0.09480(5) 0.77520(5) 0.03054(16) Uani 1 1 d . . . O21 O 0.4707(11) 0.1788(12) 0.7479(10) 0.046(3) Uani 1 1 d . . . O22 O 0.2866(9) 0.0749(11) 0.6806(8) 0.036(3) Uani 1 1 d . . . O23 O 0.3660(11) 0.1529(13) 0.8552(10) 0.048(4) Uani 1 1 d . . . O24 O 0.4510(10) -0.0219(10) 0.8117(9) 0.036(3) Uani 1 1 d . . . Re3 Re 0.70187(7) 0.59555(6) 1.13668(6) 0.0472(2) Uani 1 1 d . . . O31 O 0.6019(16) 0.5478(12) 1.1491(16) 0.077(6) Uani 1 1 d . . . O32 O 0.7227(10) 0.5220(11) 1.0643(10) 0.043(3) Uani 1 1 d . . . O33 O 0.6772(14) 0.7235(11) 1.1008(13) 0.061(5) Uani 1 1 d . . . O34 O 0.8031(17) 0.5917(16) 1.2280(15) 0.081(6) Uani 1 1 d . . . Re4 Re 1.12339(6) 0.62344(5) 0.81668(5) 0.03767(19) Uani 1 1 d . . . O41 O 1.1131(11) 0.7212(15) 0.8798(11) 0.061(5) Uani 1 1 d . . . O42 O 1.0146(15) 0.629(2) 0.7249(14) 0.085(7) Uani 1 1 d . . . O43 O 1.2188(11) 0.6483(10) 0.7878(10) 0.041(3) Uani 1 1 d . . . O44 O 1.1442(16) 0.5082(11) 0.8687(13) 0.067(5) Uani 1 1 d . . . Re5 Re 0.70188(6) 0.03119(7) 0.58801(6) 0.0435(2) Uani 1 1 d . . . O51 O 0.6709(10) 0.1460(12) 0.6195(9) 0.045(3) Uani 1 1 d . . . O52 O 0.6427(13) 0.0116(13) 0.4763(10) 0.056(4) Uani 1 1 d . . . O53 O 0.6830(12) -0.0692(15) 0.6388(13) 0.066(5) Uani 1 1 d . . . O54 O 0.8220(9) 0.0333(10) 0.6103(10) 0.039(3) Uani 1 1 d . . . Re6 Re 0.86469(7) 0.18944(8) 0.89821(6) 0.0515(2) Uani 1 1 d . . . O61 O 0.7693(14) 0.2005(14) 0.9243(13) 0.069(6) Uani 1 1 d . . . O62 O 0.9087(14) 0.3062(14) 0.8932(13) 0.067(5) Uani 1 1 d . . . O63 O 0.8348(11) 0.1345(12) 0.7984(9) 0.042(3) Uani 1 1 d . . . O64 O 0.9514(13) 0.1191(15) 0.9661(11) 0.063(5) Uani 1 1 d . . . N1 N 1.0575(9) 0.1779(10) 0.7813(9) 0.021(3) Uani 1 1 d . . . C1A C 1.1070(11) 0.0721(11) 0.7848(11) 0.025(3) Uani 1 1 d U . . H1A1 H 1.1456 0.0757 0.7479 0.029 Uiso 1 1 calc R . . H1A2 H 1.1526 0.0581 0.8456 0.029 Uiso 1 1 calc R . . C2A C 1.0361(11) -0.0182(10) 0.7542(10) 0.017(3) Uani 1 1 d U . . H2A1 H 1.0704 -0.0848 0.7516 0.020 Uiso 1 1 calc R . . H2A2 H 0.9867 -0.0030 0.6952 0.020 Uiso 1 1 calc R . . N3A N 0.9875(10) -0.0298(9) 0.8188(9) 0.021(3) Uani 1 1 d . . . H3A1 H 0.9533 0.0314 0.8181 0.026 Uiso 1 1 calc R . . H3A2 H 1.0349 -0.0372 0.8741 0.026 Uiso 1 1 calc R . . C3A C 0.9179(14) -0.1252(12) 0.7998(13) 0.033(4) Uani 1 1 d U . . H3A3 H 0.8585 -0.1099 0.7474 0.040 Uiso 1 1 calc R . . H3A4 H 0.9497 -0.1888 0.7874 0.040 Uiso 1 1 calc R . . C4A C 0.8900(12) -0.1477(11) 0.8763(11) 0.021(3) Uani 1 1 d U . . C5A C 0.9587(11) -0.1810(11) 0.9547(12) 0.025(3) Uani 1 1 d U . . H5A H 1.0240 -0.1895 0.9595 0.031 Uiso 1 1 calc R . . C6A C 0.9361(13) -0.2037(14) 1.0303(11) 0.029(3) Uani 1 1 d U . . H6A H 0.9847 -0.2254 1.0844 0.034 Uiso 1 1 calc R . . C7A C 0.8378(12) -0.1916(14) 1.0190(11) 0.028(3) Uani 1 1 d U . . H7A H 0.8188 -0.2033 1.0667 0.034 Uiso 1 1 calc R . . C8A C 0.7681(11) -0.1623(11) 0.9371(12) 0.025(3) Uani 1 1 d U . . C9A C 0.7945(11) -0.1399(11) 0.8699(11) 0.023(3) Uani 1 1 d U . . H9A H 0.7457 -0.1179 0.8160 0.027 Uiso 1 1 calc R . . C10A C 0.6612(12) -0.1587(13) 0.9294(13) 0.032(4) Uani 1 1 d U . . H10A H 0.6201 -0.1326 0.8703 0.039 Uiso 1 1 calc R . . H10B H 0.6403 -0.2323 0.9345 0.039 Uiso 1 1 calc R . . N4A N 0.6418(10) -0.0921(9) 0.9938(9) 0.024(3) Uani 1 1 d . . . H4A1 H 0.6731 -0.1213 1.0484 0.028 Uiso 1 1 calc R . . H4A2 H 0.5760 -0.0928 0.9815 0.028 Uiso 1 1 calc R . . C11A C 0.6750(13) 0.0232(12) 0.9955(12) 0.028(3) Uani 1 1 d U . . H11A H 0.6578 0.0493 0.9351 0.034 Uiso 1 1 calc R . . H11B H 0.7466 0.0278 1.0266 0.034 Uiso 1 1 calc R . . C12A C 0.6247(12) 0.0917(11) 1.0423(12) 0.026(3) Uani 1 1 d U . . H12A H 0.5556 0.1027 1.0037 0.031 Uiso 1 1 calc R . . H12B H 0.6271 0.0550 1.0959 0.031 Uiso 1 1 calc R . . N2 N 0.6737(9) 0.1929(10) 1.0647(8) 0.020(3) Uani 1 1 d . . . C1B C 1.1353(14) 0.2554(16) 0.8405(12) 0.037(4) Uani 1 1 d U . . H1B1 H 1.2002 0.2342 0.8426 0.045 Uiso 1 1 calc R . . H1B2 H 1.1212 0.3283 0.8161 0.045 Uiso 1 1 calc R . . C2B C 1.1357(14) 0.254(2) 0.9335(12) 0.044(5) Uani 1 1 d U . . H2B1 H 1.0738 0.2841 0.9326 0.053 Uiso 1 1 calc R . . H2B2 H 1.1417 0.1801 0.9552 0.053 Uiso 1 1 calc R . . N3B N 1.2154(12) 0.3159(13) 0.9896(10) 0.036(3) Uani 1 1 d . . . H3B1 H 1.2117 0.3832 0.9665 0.043 Uiso 1 1 calc R . . H3B2 H 1.2726 0.2855 0.9921 0.043 Uiso 1 1 calc R . . C3B C 1.2174(18) 0.3249(18) 1.0843(17) 0.050(5) Uani 1 1 d U . . H3B3 H 1.2249 0.2529 1.1102 0.060 Uiso 1 1 calc R . . H3B4 H 1.2747 0.3677 1.1204 0.060 Uiso 1 1 calc R . . C4B C 1.1273(16) 0.3752(14) 1.0864(13) 0.037(4) Uani 1 1 d U . . C5B C 1.0743(15) 0.4631(13) 1.0362(11) 0.034(3) Uani 1 1 d U . . H5B H 1.0918 0.4917 0.9912 0.041 Uiso 1 1 calc R . . C6B C 0.9995(13) 0.5061(13) 1.0517(11) 0.034(3) Uani 1 1 d U . . H6B H 0.9629 0.5608 1.0136 0.040 Uiso 1 1 calc R . . C7B C 0.9738(13) 0.4778(13) 1.1157(12) 0.032(3) Uani 1 1 d U . . H7B H 0.9250 0.5162 1.1271 0.039 Uiso 1 1 calc R . . C8B C 1.0225(12) 0.3842(12) 1.1701(10) 0.025(3) Uani 1 1 d U . . C9B C 1.0954(11) 0.3391(11) 1.1530(10) 0.023(3) Uani 1 1 d U . . H9B H 1.1277 0.2796 1.1873 0.027 Uiso 1 1 calc R . . C10B C 0.9991(12) 0.3444(13) 1.2442(12) 0.029(3) Uani 1 1 d U . . H10C H 0.9702 0.4029 1.2663 0.035 Uiso 1 1 calc R . . H10D H 1.0599 0.3216 1.2923 0.035 Uiso 1 1 calc R . . N4B N 0.9284(10) 0.2515(11) 1.2169(9) 0.027(3) Uani 1 1 d . . . H4B1 H 0.9549 0.1981 1.1951 0.032 Uiso 1 1 calc R . . H4B2 H 0.9203 0.2252 1.2655 0.032 Uiso 1 1 calc R . . C11B C 0.8326(13) 0.2801(12) 1.1509(12) 0.029(4) Uani 1 1 d U . . H11C H 0.8369 0.2923 1.0935 0.035 Uiso 1 1 calc R . . H11D H 0.8077 0.3456 1.1682 0.035 Uiso 1 1 calc R . . C12B C 0.7641(13) 0.1830(11) 1.1459(11) 0.028(3) Uani 1 1 d U . . H12C H 0.7979 0.1155 1.1447 0.033 Uiso 1 1 calc R . . H12D H 0.7470 0.1823 1.1980 0.033 Uiso 1 1 calc R . . C1C C 1.0083(13) 0.2179(13) 0.6984(12) 0.030(3) Uani 1 1 d U . . H1C1 H 0.9673 0.1607 0.6610 0.036 Uiso 1 1 calc R . . H1C2 H 1.0563 0.2392 0.6735 0.036 Uiso 1 1 calc R . . C2C C 0.9434(12) 0.3138(14) 0.6956(11) 0.029(3) Uani 1 1 d U . . H2C1 H 0.9632 0.3444 0.7549 0.035 Uiso 1 1 calc R . . H2C2 H 0.9524 0.3693 0.6569 0.035 Uiso 1 1 calc R . . N3C N 0.8390(9) 0.2828(10) 0.6629(8) 0.022(3) Uani 1 1 d . . . H3C1 H 0.8303 0.2392 0.7039 0.026 Uiso 1 1 calc R . . H3C2 H 0.8249 0.2432 0.6129 0.026 Uiso 1 1 calc R . . C3C C 0.7645(14) 0.3742(14) 0.6425(11) 0.029(3) Uani 1 1 d U . . H3C3 H 0.7813 0.4293 0.6079 0.035 Uiso 1 1 calc R . . H3C4 H 0.6990 0.3464 0.6063 0.035 Uiso 1 1 calc R . . C4C C 0.7613(12) 0.4238(11) 0.7223(10) 0.022(3) Uani 1 1 d U . . C5C C 0.8233(12) 0.5093(13) 0.7637(10) 0.025(3) Uani 1 1 d U . . H5C H 0.8715 0.5355 0.7445 0.030 Uiso 1 1 calc R . . C6C C 0.8078(14) 0.5540(12) 0.8373(12) 0.031(3) Uani 1 1 d U . . H6C H 0.8498 0.6097 0.8692 0.038 Uiso 1 1 calc R . . C7C C 0.7394(11) 0.5223(11) 0.8626(11) 0.023(3) Uani 1 1 d U . . H7C H 0.7311 0.5572 0.9101 0.028 Uiso 1 1 calc R . . C8C C 0.6772(12) 0.4366(11) 0.8203(11) 0.024(3) Uani 1 1 d U . . C9C C 0.6921(11) 0.3844(12) 0.7503(9) 0.023(3) Uani 1 1 d U . . H9C H 0.6548 0.3234 0.7235 0.027 Uiso 1 1 calc R . . C10C C 0.5963(13) 0.3988(12) 0.8483(11) 0.026(3) Uani 1 1 d U . . H10E H 0.5588 0.3413 0.8088 0.031 Uiso 1 1 calc R . . H10F H 0.5511 0.4585 0.8438 0.031 Uiso 1 1 calc R . . N4C N 0.6397(10) 0.3565(11) 0.9451(9) 0.025(3) Uani 1 1 d . . . H4C1 H 0.6811 0.3004 0.9493 0.030 Uiso 1 1 calc R . . H4C2 H 0.6750 0.4097 0.9818 0.030 Uiso 1 1 calc R . . C11C C 0.5574(12) 0.3198(12) 0.9729(12) 0.027(3) Uani 1 1 d U . . H11E H 0.5141 0.3800 0.9718 0.033 Uiso 1 1 calc R . . H11F H 0.5182 0.2630 0.9337 0.033 Uiso 1 1 calc R . . C12C C 0.6088(13) 0.2783(11) 1.0646(12) 0.029(3) Uani 1 1 d U . . H12E H 0.6463 0.3365 1.1032 0.035 Uiso 1 1 calc R . . H12F H 0.5602 0.2520 1.0872 0.035 Uiso 1 1 calc R . . O1W O 0.9871(11) 0.0854(9) 1.1463(10) 0.040(3) Uani 1 1 d . . . O2W O 1.3823(12) 0.4502(14) 1.0488(12) 0.056(4) Uani 1 1 d . . . O3W O 0.9080(15) 0.4747(13) 1.3989(12) 0.064(5) Uani 1 1 d . . . O4W O 1.3639(13) 0.1547(14) 1.0176(11) 0.062(5) Uani 1 1 d . . . O5W O 0.6253(12) 0.0493(17) 0.7637(13) 0.069(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 0.0217(3) 0.0265(3) 0.0183(3) -0.0001(2) 0.0115(2) 0.0012(2) O11 0.024(6) 0.024(5) 0.034(6) 0.004(5) 0.011(5) 0.004(4) O12 0.052(8) 0.040(7) 0.019(6) 0.010(5) 0.012(6) -0.003(6) O13 0.036(7) 0.046(7) 0.021(6) 0.005(5) 0.018(5) 0.010(5) O14 0.028(6) 0.027(6) 0.026(6) -0.001(4) 0.009(5) 0.005(5) Re2 0.0319(4) 0.0324(3) 0.0286(3) -0.0033(3) 0.0130(3) -0.0074(3) O21 0.041(8) 0.050(8) 0.054(9) 0.005(7) 0.025(7) 0.003(6) O22 0.029(7) 0.050(7) 0.026(6) -0.008(6) 0.008(5) -0.009(6) O23 0.045(9) 0.065(9) 0.047(9) -0.018(7) 0.031(8) -0.017(7) O24 0.036(7) 0.040(7) 0.038(7) 0.002(5) 0.020(6) -0.004(5) Re3 0.0664(6) 0.0306(4) 0.0627(6) -0.0065(4) 0.0449(5) -0.0042(4) O31 0.107(16) 0.028(7) 0.131(19) -0.006(9) 0.083(15) -0.008(8) O32 0.042(8) 0.044(7) 0.052(9) -0.006(6) 0.028(7) -0.008(6) O33 0.083(12) 0.032(7) 0.105(14) 0.007(8) 0.076(12) 0.008(7) O34 0.084(15) 0.068(12) 0.081(15) 0.007(10) 0.021(12) -0.006(10) Re4 0.0547(5) 0.0262(3) 0.0507(5) -0.0013(3) 0.0408(4) -0.0042(3) O41 0.041(9) 0.088(12) 0.054(10) -0.028(9) 0.018(8) 0.001(8) O42 0.063(12) 0.127(18) 0.074(14) -0.044(12) 0.038(11) -0.061(12) O43 0.050(8) 0.038(7) 0.046(8) 0.011(6) 0.029(7) 0.006(6) O44 0.120(16) 0.026(7) 0.085(12) 0.007(7) 0.073(12) -0.008(8) Re5 0.0372(4) 0.0454(4) 0.0372(4) 0.0048(3) 0.0025(3) -0.0099(3) O51 0.032(7) 0.062(9) 0.032(7) 0.012(6) 0.004(6) -0.005(6) O52 0.070(11) 0.045(8) 0.035(8) -0.009(6) 0.000(8) -0.004(7) O53 0.035(9) 0.065(10) 0.076(12) 0.015(9) -0.002(8) -0.009(8) O54 0.028(7) 0.035(7) 0.051(8) 0.008(6) 0.011(6) 0.001(5) Re6 0.0656(6) 0.0495(5) 0.0389(5) 0.0007(4) 0.0198(4) 0.0181(4) O61 0.081(13) 0.066(10) 0.104(15) 0.025(10) 0.083(12) 0.035(9) O62 0.063(11) 0.049(9) 0.071(12) -0.003(8) 0.008(10) 0.014(8) O63 0.042(8) 0.052(8) 0.027(7) 0.009(6) 0.008(6) -0.010(6) O64 0.059(11) 0.069(11) 0.048(10) -0.008(8) 0.008(8) 0.031(9) N1 0.016(6) 0.025(6) 0.022(7) -0.006(5) 0.009(5) -0.004(5) C1A 0.016(7) 0.020(7) 0.032(9) -0.007(6) 0.002(6) 0.003(5) C2A 0.026(8) 0.014(6) 0.018(7) -0.002(5) 0.015(6) -0.002(5) N3A 0.024(7) 0.019(6) 0.027(7) -0.007(5) 0.016(6) -0.004(5) C3A 0.049(11) 0.014(6) 0.059(10) -0.007(6) 0.045(9) -0.002(6) C4A 0.026(7) 0.017(6) 0.026(6) -0.003(5) 0.016(5) -0.006(5) C5A 0.019(6) 0.014(6) 0.051(8) 0.007(6) 0.023(6) 0.002(5) C6A 0.029(7) 0.034(8) 0.025(7) -0.003(6) 0.013(6) 0.016(7) C7A 0.027(6) 0.038(8) 0.031(7) -0.001(6) 0.023(6) -0.011(6) C8A 0.012(6) 0.020(6) 0.047(8) -0.009(6) 0.016(5) 0.003(5) C9A 0.020(6) 0.015(6) 0.032(7) -0.003(5) 0.009(5) 0.001(5) C10A 0.021(6) 0.030(8) 0.047(11) -0.024(7) 0.015(7) -0.018(6) N4A 0.029(7) 0.017(5) 0.033(7) -0.006(5) 0.021(6) -0.001(5) C11A 0.033(9) 0.023(7) 0.038(10) -0.001(6) 0.025(8) 0.001(6) C12A 0.021(8) 0.016(6) 0.045(10) -0.006(6) 0.017(7) -0.001(6) N2 0.017(6) 0.027(6) 0.021(6) -0.006(5) 0.014(5) 0.002(5) C1B 0.033(10) 0.041(9) 0.035(9) -0.003(8) 0.010(8) -0.011(8) C2B 0.028(9) 0.076(14) 0.024(8) 0.004(9) 0.005(8) -0.008(9) N3B 0.031(8) 0.037(8) 0.033(8) 0.002(7) 0.005(7) 0.005(6) C3B 0.062(13) 0.049(11) 0.061(14) 0.002(10) 0.048(12) 0.001(9) C4B 0.053(10) 0.025(7) 0.047(11) -0.005(7) 0.036(9) -0.010(6) C5B 0.060(10) 0.026(7) 0.019(8) -0.008(5) 0.017(7) -0.018(6) C6B 0.031(8) 0.027(7) 0.023(8) 0.008(6) -0.011(6) -0.006(6) C7B 0.019(8) 0.029(7) 0.039(9) 0.000(6) 0.000(6) 0.001(6) C8B 0.022(7) 0.031(7) 0.021(7) 0.000(5) 0.008(6) -0.011(5) C9B 0.026(7) 0.017(6) 0.023(7) 0.000(5) 0.008(6) -0.009(5) C10B 0.020(8) 0.032(8) 0.033(8) -0.004(6) 0.007(7) -0.016(6) N4B 0.028(7) 0.032(7) 0.025(7) -0.001(5) 0.014(6) -0.014(6) C11B 0.031(9) 0.022(7) 0.042(10) -0.005(7) 0.022(8) -0.002(6) C12B 0.041(10) 0.014(6) 0.029(9) -0.009(6) 0.015(8) -0.008(6) C1C 0.031(9) 0.024(7) 0.033(9) 0.007(6) 0.011(7) 0.001(6) C2C 0.018(8) 0.037(8) 0.022(8) 0.002(6) -0.005(6) 0.006(6) N3C 0.028(7) 0.027(6) 0.011(6) -0.003(5) 0.008(5) -0.005(5) C3C 0.033(9) 0.036(8) 0.013(7) -0.003(6) 0.003(6) 0.012(7) C4C 0.033(8) 0.018(6) 0.013(6) 0.004(5) 0.005(6) 0.005(5) C5C 0.029(8) 0.027(7) 0.013(7) 0.009(5) 0.002(6) 0.002(5) C6C 0.039(9) 0.018(7) 0.033(8) 0.000(6) 0.009(7) -0.007(6) C7C 0.023(7) 0.016(6) 0.029(8) 0.000(5) 0.008(6) 0.014(4) C8C 0.027(7) 0.014(6) 0.038(9) 0.001(5) 0.020(7) 0.007(5) C9C 0.021(7) 0.027(7) 0.009(6) -0.001(5) -0.006(5) 0.003(5) C10C 0.030(8) 0.023(7) 0.026(8) 0.005(6) 0.012(7) 0.010(5) N4C 0.020(7) 0.031(7) 0.029(8) 0.008(6) 0.014(6) 0.008(5) C11C 0.024(8) 0.027(7) 0.038(8) -0.006(6) 0.021(7) 0.001(6) C12C 0.039(10) 0.014(6) 0.044(9) 0.006(6) 0.028(8) 0.011(6) O1W 0.050(8) 0.024(6) 0.057(9) 0.000(6) 0.030(7) 0.003(5) O2W 0.053(10) 0.063(10) 0.070(11) 0.004(8) 0.047(9) -0.005(8) O3W 0.103(15) 0.044(9) 0.064(11) -0.016(7) 0.053(11) -0.021(9) O4W 0.057(11) 0.060(10) 0.050(10) -0.006(8) -0.001(8) 0.012(8) O5W 0.041(9) 0.094(14) 0.075(12) 0.014(11) 0.025(9) 0.000(9) _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 O12 1.704(12) . ? Re1 O13 1.724(11) . ? Re1 O11 1.730(12) . ? Re1 O14 1.736(11) . ? Re2 O24 1.690(13) . ? Re2 O23 1.694(14) . ? Re2 O21 1.748(14) . ? Re2 O22 1.765(13) . ? Re3 O32 1.637(14) . ? Re3 O34 1.67(2) . ? Re3 O31 1.689(19) . ? Re3 O33 1.704(15) . ? Re4 O44 1.652(15) . ? Re4 O41 1.659(16) . ? Re4 O43 1.693(14) . ? Re4 O42 1.74(2) . ? Re5 O53 1.600(18) . ? Re5 O51 1.658(16) . ? Re5 O54 1.681(13) . ? Re5 O52 1.734(15) . ? Re6 O64 1.610(16) . ? Re6 O62 1.621(19) . ? Re6 O61 1.643(13) . ? Re6 O63 1.687(14) . ? N1 C1C 1.38(2) . ? N1 C1A 1.509(18) . ? N1 C1B 1.54(2) . ? C1A C2A 1.50(2) . ? C2A N3A 1.513(17) . ? N3A C3A 1.53(2) . ? C3A C4A 1.51(2) . ? C4A C5A 1.37(2) . ? C4A C9A 1.39(2) . ? C5A C6A 1.45(2) . ? C6A C7A 1.41(2) . ? C7A C8A 1.40(3) . ? C8A C9A 1.35(2) . ? C8A C10A 1.55(2) . ? C10A N4A 1.470(19) . ? N4A C11A 1.526(19) . ? C11A C12A 1.53(2) . ? C12A N2 1.441(19) . ? N2 C12C 1.442(18) . ? N2 C12B 1.50(2) . ? C1B C2B 1.54(3) . ? C2B N3B 1.42(3) . ? N3B C3B 1.56(3) . ? C3B C4B 1.50(3) . ? C4B C5B 1.42(3) . ? C4B C9B 1.43(2) . ? C5B C6B 1.35(3) . ? C6B C7B 1.31(3) . ? C7B C8B 1.49(2) . ? C8B C9B 1.35(2) . ? C8B C10B 1.49(2) . ? C10B N4B 1.519(19) . ? N4B C11B 1.47(2) . ? C11B C12B 1.57(2) . ? C1C C2C 1.53(2) . ? C2C N3C 1.49(2) . ? N3C C3C 1.54(2) . ? C3C C4C 1.48(2) . ? C4C C9C 1.38(2) . ? C4C C5C 1.41(2) . ? C5C C6C 1.44(2) . ? C6C C7C 1.31(2) . ? C7C C8C 1.42(2) . ? C8C C9C 1.42(2) . ? C8C C10C 1.53(2) . ? C10C N4C 1.57(2) . ? N4C C11C 1.54(2) . ? C11C C12C 1.51(2) . ? 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 O12 Re1 O13 108.8(6) . . ? O12 Re1 O11 111.1(6) . . ? O13 Re1 O11 109.9(6) . . ? O12 Re1 O14 108.3(6) . . ? O13 Re1 O14 108.1(5) . . ? O11 Re1 O14 110.6(5) . . ? O24 Re2 O23 109.6(7) . . ? O24 Re2 O21 108.6(6) . . ? O23 Re2 O21 108.9(7) . . ? O24 Re2 O22 110.8(6) . . ? O23 Re2 O22 110.8(7) . . ? O21 Re2 O22 108.1(7) . . ? O32 Re3 O34 106.8(10) . . ? O32 Re3 O31 108.3(8) . . ? O34 Re3 O31 114.0(12) . . ? O32 Re3 O33 110.6(8) . . ? O34 Re3 O33 109.9(10) . . ? O31 Re3 O33 107.3(8) . . ? O44 Re4 O41 111.3(9) . . ? O44 Re4 O43 107.5(8) . . ? O41 Re4 O43 109.5(8) . . ? O44 Re4 O42 114.6(11) . . ? O41 Re4 O42 103.8(10) . . ? O43 Re4 O42 110.1(8) . . ? O53 Re5 O51 113.1(9) . . ? O53 Re5 O54 106.5(8) . . ? O51 Re5 O54 108.6(7) . . ? O53 Re5 O52 109.3(9) . . ? O51 Re5 O52 111.8(7) . . ? O54 Re5 O52 107.2(8) . . ? O64 Re6 O62 107.5(10) . . ? O64 Re6 O61 113.7(10) . . ? O62 Re6 O61 110.2(10) . . ? O64 Re6 O63 107.4(8) . . ? O62 Re6 O63 106.1(8) . . ? O61 Re6 O63 111.5(9) . . ? C1C N1 C1A 115.0(13) . . ? C1C N1 C1B 112.6(13) . . ? C1A N1 C1B 107.3(13) . . ? C2A C1A N1 112.6(12) . . ? C1A C2A N3A 107.5(12) . . ? C2A N3A C3A 113.5(11) . . ? C4A C3A N3A 111.0(14) . . ? C5A C4A C9A 117.4(14) . . ? C5A C4A C3A 120.6(15) . . ? C9A C4A C3A 122.0(16) . . ? C4A C5A C6A 122.9(14) . . ? C7A C6A C5A 116.1(15) . . ? C8A C7A C6A 119.9(14) . . ? C9A C8A C7A 120.8(14) . . ? C9A C8A C10A 123.0(16) . . ? C7A C8A C10A 116.1(15) . . ? C8A C9A C4A 122.7(16) . . ? N4A C10A C8A 116.2(13) . . ? C10A N4A C11A 113.6(12) . . ? N4A C11A C12A 108.8(12) . . ? N2 C12A C11A 109.2(12) . . ? C12A N2 C12C 112.6(12) . . ? C12A N2 C12B 110.4(12) . . ? C12C N2 C12B 115.6(13) . . ? C2B C1B N1 110.1(14) . . ? N3B C2B C1B 109.3(16) . . ? C2B N3B C3B 112.7(16) . . ? C4B C3B N3B 112.7(19) . . ? C5B C4B C9B 115.0(16) . . ? C5B C4B C3B 127.7(16) . . ? C9B C4B C3B 116.9(18) . . ? C6B C5B C4B 120.6(15) . . ? C7B C6B C5B 124.6(16) . . ? C6B C7B C8B 118.7(16) . . ? C9B C8B C10B 119.8(15) . . ? C9B C8B C7B 116.5(14) . . ? C10B C8B C7B 123.5(16) . . ? C8B C9B C4B 124.2(16) . . ? C8B C10B N4B 111.7(13) . . ? C11B N4B C10B 113.3(13) . . ? N4B C11B C12B 105.8(13) . . ? N2 C12B C11B 108.8(13) . . ? N1 C1C C2C 113.7(15) . . ? N3C C2C C1C 111.3(14) . . ? C2C N3C C3C 116.6(13) . . ? C4C C3C N3C 112.7(13) . . ? C9C C4C C5C 122.9(14) . . ? C9C C4C C3C 116.0(15) . . ? C5C C4C C3C 121.1(15) . . ? C4C C5C C6C 115.0(15) . . ? C7C C6C C5C 123.6(16) . . ? C6C C7C C8C 120.9(15) . . ? C7C C8C C9C 118.5(14) . . ? C7C C8C C10C 121.8(14) . . ? C9C C8C C10C 119.7(14) . . ? C4C C9C C8C 118.9(14) . . ? C8C C10C N4C 110.8(14) . . ? C11C N4C C10C 110.3(13) . . ? C12C C11C N4C 104.8(13) . . ? N2 C12C C11C 109.7(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3A1 O63 0.92 2.11 2.99(2) 160.1 . N3A H3A2 O52 0.92 1.86 2.75(2) 162.1 2 N4A H4A1 O33 0.92 2.13 2.84(2) 133.8 1_545 N4A H4A1 O22 0.92 2.27 3.023(19) 139.0 2 N4A H4A2 O14 0.92 2.01 2.881(17) 158.4 2_455 N3B H3B1 O44 0.92 2.20 3.05(2) 153.9 . N3B H3B2 O4W 0.92 2.07 2.90(2) 149.6 . N3B H3B1 O2W 0.92 2.52 2.85(2) 101.2 . N4B H4B1 O1W 0.92 1.79 2.698(19) 170.8 . N4B H4B2 O12 0.92 1.96 2.805(18) 151.5 1_556 N3C H3C1 O63 0.92 2.03 2.938(18) 170.2 . N3C H3C2 O13 0.92 1.92 2.729(16) 145.4 . N4C H4C1 O61 0.92 1.97 2.862(19) 162.0 . N4C H4C2 O32 0.92 1.90 2.81(2) 167.0 . _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.779 _refine_diff_density_min -5.696 _refine_diff_density_rms 0.351