# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Monika Sieger' _publ_contact_author_address ; Universit\"at Stuttgart Institut Anorganische Chemie Pfaffenwaldring 55 70569 Stuttgart ; _publ_contact_author_email monika.sieger@iac.uni-stuttgart.de loop_ _publ_author_name W.Kaim C.Duboc A.N.Maity M.Niemeyer B.Sarkar M.Sieger S.Zalis # Attachment 'NEU3.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 687368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(rhenium(tri-carbonyl)(bipyridin)) {m4-(2,3,5,6-tetrafluoro-7,7,8,8-tetracyano-p-quinodimethane)} ; _chemical_name_common ; tetra(rhenium(tri-carbonyl)(bipyridin)) (m4-(2,3,5,6- tetrafluoro-7,7,8,8-tetracyano-p-quinodimethane)) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H36 Cl4 F22 N12 O12 P3 Re4' _chemical_formula_weight 2586.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 17.542(2) _cell_length_b 9.301(5) _cell_length_c 26.235(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.500(17) _cell_angle_gamma 90.00 _cell_volume 4082(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.3 _cell_measurement_theta_max 11.1 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2446 _exptl_absorpt_coefficient_mu 6.216 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 0.315 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 298 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8561 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.52 _reflns_number_total 8282 _reflns_number_gt 4263 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1034P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8282 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2264 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.38474(4) 0.19130(8) 0.26643(2) 0.0540(2) Uani 1 1 d . . . Re2 Re 0.15311(5) 0.22344(12) 0.49585(3) 0.0804(4) Uani 1 1 d . . . N1 N 0.3648(7) 0.2625(17) 0.3382(4) 0.056(4) Uani 1 1 d . . . N2 N 0.3825(9) -0.0219(16) 0.3003(5) 0.058(4) Uani 1 1 d . . . N3 N 0.2582(8) 0.1287(18) 0.2409(5) 0.055(4) Uani 1 1 d . . . N4 N 0.2457(9) 0.280(2) 0.4625(5) 0.074(5) Uani 1 1 d . . . N5 N 0.2181(11) 0.0240(19) 0.5131(7) 0.082(5) Uiso 1 1 d . . . N6 N 0.1061(8) 0.0957(18) 0.4246(4) 0.054(4) Uani 1 1 d . . . O1 O 0.4163(11) 0.0722(18) 0.1650(5) 0.105(6) Uani 1 1 d . . . O2 O 0.3681(14) 0.495(2) 0.2156(9) 0.137(8) Uani 1 1 d . . . O3 O 0.5657(10) 0.255(2) 0.3121(7) 0.109(6) Uani 1 1 d . . . O4 O 0.0273(11) 0.124(2) 0.5491(7) 0.125(7) Uani 1 1 d . . . O5 O 0.0556(12) 0.5040(19) 0.4552(7) 0.106(5) Uani 1 1 d . . . O6 O 0.2345(13) 0.390(3) 0.5988(7) 0.146(8) Uani 1 1 d . . . P1 P 0.1467(3) 0.4619(6) 0.31692(19) 0.0672(14) Uani 1 1 d . . . P2 P 0.5000 0.0000 0.5000 0.079(2) Uani 1 2 d S . . F1 F 0.0933(9) 0.471(2) 0.3569(6) 0.128(5) Uani 1 1 d . . . F2 F 0.0730(9) 0.3845(15) 0.2752(5) 0.113(5) Uani 1 1 d . . . F3 F 0.1139(8) 0.6217(15) 0.2947(4) 0.097(4) Uani 1 1 d . . . F4 F 0.1985(9) 0.4677(16) 0.2770(5) 0.112(5) Uani 1 1 d . . . F5 F 0.2134(8) 0.5407(14) 0.3629(5) 0.099(4) Uani 1 1 d . . . F6 F 0.1821(8) 0.3074(13) 0.3378(5) 0.089(3) Uani 1 1 d . . . F7 F 0.4512(15) 0.103(2) 0.5235(8) 0.185(10) Uani 1 1 d . . . F8 F 0.4305(19) -0.081(5) 0.4676(10) 0.32(2) Uani 1 1 d . . . F9 F 0.5025(13) 0.100(2) 0.4529(7) 0.170(9) Uani 1 1 d . . . F10 F 0.5010(5) 0.4291(11) 0.3999(3) 0.062(3) Uani 1 1 d . . . F11 F 0.3793(5) 0.4229(11) 0.5388(3) 0.061(3) Uani 1 1 d . . . Cl1 Cl 0.1853(7) 0.8530(12) 0.6667(4) 0.175(4) Uani 1 1 d . . . Cl2 Cl 0.1179(8) 0.7320(16) 0.5657(5) 0.206(6) Uani 1 1 d . . . C1 C 0.4035(12) 0.118(3) 0.2027(7) 0.078(6) Uani 1 1 d . . . C2 C 0.3752(14) 0.387(3) 0.2340(9) 0.086(6) Uiso 1 1 d . . . C3 C 0.5004(13) 0.237(2) 0.2955(8) 0.068(5) Uiso 1 1 d . . . C4 C 0.0703(17) 0.160(3) 0.5271(10) 0.120(11) Uani 1 1 d . . . C5 C 0.0933(14) 0.401(3) 0.4730(9) 0.082(6) Uiso 1 1 d . . . C6 C 0.2003(17) 0.330(4) 0.5604(8) 0.126(12) Uani 1 1 d . . . C7 C 0.3641(9) 0.2980(19) 0.3793(6) 0.050(4) Uani 1 1 d . . . C8 C 0.3663(8) 0.3449(16) 0.4321(5) 0.041(4) Uani 1 1 d . . . C9 C 0.2984(10) 0.3029(18) 0.4488(5) 0.050(4) Uani 1 1 d . . . C10 C 0.4318(9) 0.4198(18) 0.4652(5) 0.044(4) Uani 1 1 d . . . C11 C 0.5002(9) 0.4649(19) 0.4498(5) 0.047(4) Uani 1 1 d . . . C12 C 0.4385(9) 0.4658(18) 0.5187(5) 0.047(4) Uani 1 1 d . . . C13 C 0.4472(12) -0.088(2) 0.3319(7) 0.071(5) Uani 1 1 d . . . H13A H 0.4983 -0.0440 0.3394 0.085 Uiso 1 1 calc R . . C14 C 0.4392(18) -0.220(2) 0.3535(8) 0.090(7) Uani 1 1 d . . . H14A H 0.4857 -0.2648 0.3763 0.108 Uiso 1 1 calc R . . C15 C 0.3668(19) -0.291(3) 0.3438(11) 0.111(9) Uani 1 1 d . . . H15A H 0.3617 -0.3850 0.3562 0.134 Uiso 1 1 calc R . . C16 C 0.3036(17) -0.211(3) 0.3145(10) 0.098(8) Uani 1 1 d . . . H16A H 0.2515 -0.2477 0.3099 0.118 Uiso 1 1 calc R . . C17 C 0.3095(12) -0.086(2) 0.2922(7) 0.059(5) Uani 1 1 d . . . C18 C 0.2426(12) 0.000(2) 0.2579(6) 0.064(5) Uani 1 1 d . . . C19 C 0.1602(13) -0.047(3) 0.2430(8) 0.089(7) Uani 1 1 d . . . H19A H 0.1460 -0.1348 0.2562 0.107 Uiso 1 1 calc R . . C20 C 0.1023(15) 0.039(4) 0.2089(10) 0.108(10) Uani 1 1 d . . . H20A H 0.0482 0.0082 0.1979 0.129 Uiso 1 1 calc R . . C21 C 0.1216(13) 0.170(3) 0.1907(10) 0.092(7) Uani 1 1 d . . . H21A H 0.0818 0.2289 0.1676 0.111 Uiso 1 1 calc R . . C22 C 0.2009(13) 0.210(3) 0.2072(8) 0.085(7) Uani 1 1 d . . . H22A H 0.2157 0.2984 0.1946 0.102 Uiso 1 1 calc R . . C23 C 0.2779(16) 0.010(3) 0.5622(11) 0.105(8) Uiso 1 1 d . . . H23A H 0.2893 0.0795 0.5901 0.126 Uiso 1 1 calc R . . C24 C 0.315(2) -0.111(4) 0.5637(13) 0.140(11) Uiso 1 1 d . . . H24A H 0.3596 -0.1206 0.5951 0.168 Uiso 1 1 calc R . . C25 C 0.306(2) -0.229(3) 0.5304(12) 0.122(9) Uiso 1 1 d . . . H25A H 0.3379 -0.3138 0.5391 0.146 Uiso 1 1 calc R . . C26 C 0.244(3) -0.209(4) 0.4814(17) 0.173(15) Uiso 1 1 d . . . H26A H 0.2298 -0.2791 0.4539 0.208 Uiso 1 1 calc R . . C27 C 0.2039(12) -0.074(2) 0.4775(8) 0.072(5) Uiso 1 1 d . . . C28 C 0.1385(13) -0.042(3) 0.4251(8) 0.081(7) Uani 1 1 d . . . C29 C 0.1111(15) -0.127(3) 0.3834(11) 0.096(7) Uani 1 1 d . . . H29A H 0.1310 -0.2229 0.3852 0.115 Uiso 1 1 calc R . . C30 C 0.0554(15) -0.083(3) 0.3382(10) 0.094(8) Uani 1 1 d . . . H30A H 0.0397 -0.1457 0.3081 0.113 Uiso 1 1 calc R . . C31 C 0.0226(12) 0.046(3) 0.3355(7) 0.081(7) Uani 1 1 d . . . H31A H -0.0179 0.0772 0.3046 0.098 Uiso 1 1 calc R . . C32 C 0.0512(12) 0.134(3) 0.3810(8) 0.075(6) Uani 1 1 d . . . H32A H 0.0289 0.2272 0.3798 0.090 Uiso 1 1 calc R . . C33 C 0.188(3) 0.700(4) 0.6272(11) 0.169(17) Uani 1 1 d . . . H33A H 0.2418 0.6875 0.6231 0.203 Uiso 1 1 calc R . . H33B H 0.1739 0.6123 0.6438 0.203 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 0.0587(4) 0.0730(5) 0.0403(3) -0.0072(3) 0.0298(3) -0.0067(4) Re2 0.0659(5) 0.1438(9) 0.0425(4) -0.0253(4) 0.0329(4) -0.0465(5) N1 0.034(7) 0.111(12) 0.023(6) -0.021(6) 0.007(5) -0.022(7) N2 0.056(9) 0.072(10) 0.051(8) 0.010(7) 0.023(7) 0.005(8) N3 0.038(7) 0.092(11) 0.037(7) -0.004(7) 0.013(6) 0.000(7) N4 0.058(9) 0.138(15) 0.036(7) -0.013(8) 0.031(7) -0.050(9) N6 0.040(7) 0.097(12) 0.026(6) -0.015(7) 0.012(5) -0.020(8) O1 0.148(15) 0.126(13) 0.070(9) -0.033(9) 0.076(10) 0.005(11) O2 0.18(2) 0.088(12) 0.181(19) 0.050(13) 0.110(17) 0.007(13) O3 0.063(10) 0.141(15) 0.125(14) -0.032(11) 0.029(9) -0.022(10) O4 0.119(14) 0.185(18) 0.106(12) -0.042(12) 0.086(11) -0.070(13) O5 0.141(16) 0.088(11) 0.103(12) 0.003(9) 0.058(11) 0.002(11) O6 0.139(17) 0.24(2) 0.065(10) -0.046(14) 0.031(10) -0.062(17) P1 0.066(3) 0.086(4) 0.051(3) 0.007(3) 0.019(2) 0.005(3) P2 0.086(6) 0.092(6) 0.064(4) 0.012(4) 0.029(4) 0.026(5) F1 0.110(12) 0.178(15) 0.117(11) 0.003(10) 0.066(9) -0.017(10) F2 0.103(10) 0.104(10) 0.103(10) -0.016(8) -0.012(8) 0.015(8) F3 0.107(10) 0.108(10) 0.069(7) 0.020(7) 0.014(7) 0.030(8) F4 0.142(13) 0.130(11) 0.089(9) 0.004(8) 0.073(9) 0.002(9) F5 0.092(9) 0.103(10) 0.084(8) 0.004(7) -0.001(7) -0.012(8) F6 0.087(9) 0.081(8) 0.087(8) 0.020(7) 0.010(6) -0.002(7) F7 0.26(3) 0.182(18) 0.151(16) 0.072(14) 0.122(17) 0.108(19) F8 0.26(3) 0.59(6) 0.16(2) -0.18(3) 0.12(2) -0.24(4) F9 0.23(2) 0.180(17) 0.142(14) 0.079(13) 0.115(15) 0.109(16) F10 0.052(5) 0.111(8) 0.032(4) -0.015(5) 0.025(4) -0.028(5) F11 0.051(5) 0.107(8) 0.033(4) -0.024(5) 0.024(4) -0.033(5) Cl1 0.195(11) 0.171(9) 0.174(9) -0.037(7) 0.077(8) -0.037(8) Cl2 0.169(10) 0.321(16) 0.149(9) -0.071(9) 0.080(8) -0.090(10) C1 0.066(12) 0.119(18) 0.050(10) -0.017(11) 0.022(9) -0.015(12) C4 0.13(2) 0.17(3) 0.098(17) -0.025(17) 0.099(17) -0.06(2) C6 0.12(2) 0.23(3) 0.040(10) -0.051(16) 0.034(12) -0.06(2) C7 0.040(8) 0.069(11) 0.045(8) -0.004(8) 0.019(7) -0.007(8) C8 0.036(8) 0.057(10) 0.030(7) -0.001(6) 0.009(6) -0.003(7) C9 0.046(9) 0.064(11) 0.031(7) 0.000(7) -0.003(7) -0.009(8) C10 0.042(8) 0.071(11) 0.022(6) 0.000(7) 0.014(6) -0.009(8) C11 0.036(8) 0.082(12) 0.026(6) -0.013(7) 0.014(6) -0.013(8) C12 0.050(9) 0.066(11) 0.032(7) 0.000(7) 0.022(7) -0.011(8) C13 0.064(12) 0.094(16) 0.055(10) 0.003(11) 0.019(9) 0.007(11) C14 0.13(2) 0.074(17) 0.067(13) 0.009(11) 0.029(14) 0.023(15) C15 0.11(2) 0.11(2) 0.12(2) 0.044(18) 0.044(18) -0.016(19) C16 0.093(18) 0.10(2) 0.107(18) 0.030(15) 0.044(15) -0.010(15) C17 0.071(13) 0.063(12) 0.048(9) 0.007(9) 0.027(9) 0.003(10) C18 0.076(13) 0.084(14) 0.042(9) -0.018(9) 0.033(9) -0.015(11) C19 0.069(15) 0.14(2) 0.064(12) -0.019(13) 0.027(11) -0.020(14) C20 0.062(15) 0.19(3) 0.072(15) -0.025(18) 0.020(12) 0.020(19) C21 0.054(13) 0.14(2) 0.091(16) -0.006(16) 0.026(12) 0.032(14) C22 0.067(14) 0.13(2) 0.061(11) -0.019(12) 0.020(10) 0.017(13) C28 0.080(14) 0.105(18) 0.081(14) -0.035(13) 0.061(12) -0.041(13) C29 0.088(18) 0.105(19) 0.104(19) -0.016(16) 0.042(15) 0.003(15) C30 0.072(16) 0.13(2) 0.083(16) -0.037(16) 0.035(13) -0.024(16) C31 0.055(12) 0.14(2) 0.039(10) 0.008(12) 0.007(9) -0.021(14) C32 0.058(12) 0.106(16) 0.066(12) 0.003(11) 0.027(10) -0.003(11) C33 0.27(5) 0.17(3) 0.087(19) -0.01(2) 0.09(3) -0.07(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.923(18) . ? Re1 C3 1.99(2) . ? Re1 C2 2.00(3) . ? Re1 N1 2.122(11) . ? Re1 N2 2.178(15) . ? Re1 N3 2.195(13) . ? Re2 C6 1.92(2) . ? Re2 C5 1.95(3) . ? Re2 C4 1.962(18) . ? Re2 N4 2.128(12) . ? Re2 N5 2.153(18) . ? Re2 N6 2.158(12) . ? N1 C7 1.131(18) . ? N2 C13 1.34(2) . ? N2 C17 1.37(2) . ? N3 C18 1.33(2) . ? N3 C22 1.35(3) . ? N4 C9 1.11(2) . ? N5 C27 1.28(2) . ? N5 C23 1.40(3) . ? N6 C32 1.30(2) . ? N6 C28 1.40(3) . ? O1 C1 1.16(2) . ? O2 C2 1.10(3) . ? O3 C3 1.11(2) . ? O4 C4 1.13(2) . ? O5 C5 1.18(3) . ? O6 C6 1.15(2) . ? P1 F4 1.581(12) . ? P1 F5 1.585(13) . ? P1 F2 1.592(14) . ? P1 F6 1.596(13) . ? P1 F1 1.605(14) . ? P1 F3 1.637(14) . ? P2 F8 1.47(2) 3_656 ? P2 F8 1.47(2) . ? P2 F7 1.530(18) . ? P2 F7 1.530(18) 3_656 ? P2 F9 1.556(15) 3_656 ? P2 F9 1.556(15) . ? F10 C11 1.354(14) . ? F11 C12 1.359(16) . ? Cl1 C33 1.77(4) . ? Cl2 C33 1.73(4) . ? C7 C8 1.443(19) . ? C8 C10 1.40(2) . ? C8 C9 1.44(2) . ? C10 C12 1.437(18) . ? C10 C11 1.440(19) . ? C11 C12 1.31(2) 3_666 ? C12 C11 1.31(2) 3_666 ? C13 C14 1.38(3) . ? C14 C15 1.38(4) . ? C15 C16 1.36(4) . ? C16 C17 1.32(3) . ? C17 C18 1.48(3) . ? C18 C19 1.45(3) . ? C19 C20 1.39(3) . ? C20 C21 1.38(4) . ? C21 C22 1.38(3) . ? C23 C24 1.30(4) . ? C24 C25 1.38(4) . ? C25 C26 1.43(5) . ? C26 C27 1.42(4) . ? C27 C28 1.53(3) . ? C28 C29 1.32(3) . ? C29 C30 1.35(3) . ? C30 C31 1.32(3) . ? C31 C32 1.41(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C3 89.3(8) . . ? C1 Re1 C2 88.2(10) . . ? C3 Re1 C2 85.2(9) . . ? C1 Re1 N1 177.3(8) . . ? C3 Re1 N1 90.8(6) . . ? C2 Re1 N1 94.5(8) . . ? C1 Re1 N2 93.4(8) . . ? C3 Re1 N2 100.2(7) . . ? C2 Re1 N2 174.4(8) . . ? N1 Re1 N2 83.9(5) . . ? C1 Re1 N3 93.5(7) . . ? C3 Re1 N3 174.7(7) . . ? C2 Re1 N3 99.5(8) . . ? N1 Re1 N3 86.1(5) . . ? N2 Re1 N3 75.1(6) . . ? C6 Re2 C5 83.4(12) . . ? C6 Re2 C4 87.9(11) . . ? C5 Re2 C4 89.1(12) . . ? C6 Re2 N4 93.2(8) . . ? C5 Re2 N4 94.1(9) . . ? C4 Re2 N4 176.7(11) . . ? C6 Re2 N5 101.4(12) . . ? C5 Re2 N5 174.5(8) . . ? C4 Re2 N5 93.7(11) . . ? N4 Re2 N5 83.0(7) . . ? C6 Re2 N6 176.6(11) . . ? C5 Re2 N6 99.7(8) . . ? C4 Re2 N6 93.4(8) . . ? N4 Re2 N6 85.4(5) . . ? N5 Re2 N6 75.4(6) . . ? C7 N1 Re1 171.5(13) . . ? C13 N2 C17 118.5(16) . . ? C13 N2 Re1 123.7(13) . . ? C17 N2 Re1 117.6(12) . . ? C18 N3 C22 122.3(18) . . ? C18 N3 Re1 115.2(12) . . ? C22 N3 Re1 122.4(15) . . ? C9 N4 Re2 173.8(16) . . ? C27 N5 C23 122(2) . . ? C27 N5 Re2 119.3(15) . . ? C23 N5 Re2 118.3(16) . . ? C32 N6 C28 116.5(17) . . ? C32 N6 Re2 126.9(15) . . ? C28 N6 Re2 116.6(12) . . ? F4 P1 F5 92.8(8) . . ? F4 P1 F2 94.0(9) . . ? F5 P1 F2 173.1(9) . . ? F4 P1 F6 90.9(8) . . ? F5 P1 F6 91.9(7) . . ? F2 P1 F6 88.9(7) . . ? F4 P1 F1 175.0(9) . . ? F5 P1 F1 85.4(8) . . ? F2 P1 F1 87.7(9) . . ? F6 P1 F1 93.8(8) . . ? F4 P1 F3 86.7(8) . . ? F5 P1 F3 87.2(7) . . ? F2 P1 F3 92.3(7) . . ? F6 P1 F3 177.5(8) . . ? F1 P1 F3 88.5(9) . . ? F8 P2 F8 180(3) 3_656 . ? F8 P2 F7 85.0(17) 3_656 . ? F8 P2 F7 95.0(17) . . ? F8 P2 F7 95.0(17) 3_656 3_656 ? F8 P2 F7 85.0(17) . 3_656 ? F7 P2 F7 180.0(12) . 3_656 ? F8 P2 F9 93.6(17) 3_656 3_656 ? F8 P2 F9 86.4(17) . 3_656 ? F7 P2 F9 84.2(8) . 3_656 ? F7 P2 F9 95.8(8) 3_656 3_656 ? F8 P2 F9 86.4(17) 3_656 . ? F8 P2 F9 93.6(17) . . ? F7 P2 F9 95.8(8) . . ? F7 P2 F9 84.2(8) 3_656 . ? F9 P2 F9 180.000(6) 3_656 . ? O1 C1 Re1 179(2) . . ? O2 C2 Re1 178(2) . . ? O3 C3 Re1 177(2) . . ? O4 C4 Re2 174(3) . . ? O5 C5 Re2 175(2) . . ? O6 C6 Re2 174(3) . . ? N1 C7 C8 177.8(16) . . ? C10 C8 C9 123.1(12) . . ? C10 C8 C7 121.8(12) . . ? C9 C8 C7 115.1(12) . . ? N4 C9 C8 175(2) . . ? C8 C10 C12 124.4(13) . . ? C8 C10 C11 124.7(12) . . ? C12 C10 C11 110.9(12) . . ? C12 C11 F10 119.0(12) 3_666 . ? C12 C11 C10 124.1(12) 3_666 . ? F10 C11 C10 116.9(12) . . ? C11 C12 F11 118.5(12) 3_666 . ? C11 C12 C10 125.0(13) 3_666 . ? F11 C12 C10 116.3(13) . . ? N2 C13 C14 119(2) . . ? C13 C14 C15 123(2) . . ? C16 C15 C14 113(2) . . ? C17 C16 C15 125(3) . . ? C16 C17 N2 121(2) . . ? C16 C17 C18 126(2) . . ? N2 C17 C18 113.2(15) . . ? N3 C18 C19 118(2) . . ? N3 C18 C17 118.9(16) . . ? C19 C18 C17 123(2) . . ? C20 C19 C18 119(2) . . ? C21 C20 C19 121(3) . . ? C22 C21 C20 117(2) . . ? N3 C22 C21 122(2) . . ? C24 C23 N5 110(3) . . ? C23 C24 C25 135(4) . . ? C24 C25 C26 112(3) . . ? C27 C26 C25 114(3) . . ? N5 C27 C26 126(3) . . ? N5 C27 C28 116.5(19) . . ? C26 C27 C28 117(2) . . ? C29 C28 N6 120(2) . . ? C29 C28 C27 128(2) . . ? N6 C28 C27 112.2(16) . . ? C28 C29 C30 122(3) . . ? C31 C30 C29 121(2) . . ? C30 C31 C32 116(2) . . ? N6 C32 C31 124(2) . . ? Cl2 C33 Cl1 106(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 6.033 _refine_diff_density_min -2.783 _refine_diff_density_rms 0.319