# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1669 data_vk04 # compound 1 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H31 Cl4 N5 O2 Re' _chemical_formula_weight 677.48 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 'P 2(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 10.465(2) _cell_length_b 25.267(5) _cell_length_c 10.905(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.21(3) _cell_angle_gamma 90.00 _cell_volume 2669.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description prism _exptl_crystal_colour emerald _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 4.975 _exptl_absorpt_correction_type Numeric _exptl_absorpt_correction_T_min 0.091 _exptl_absorpt_correction_T_max 0.161 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_reflns_number 3620 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3430 _reflns_number_gt 3430 _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 w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+3.6176P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refined _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00276(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3430 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.701 _refine_ls_shift/su_mean 0.056 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.60416(2) 0.385058(7) 0.425003(19) 0.03963(10) Uani 1 d . . . Cl3 Cl 0.67463(16) 0.45561(6) 0.57385(15) 0.0594(4) Uani 1 d . . . Cl4 Cl 0.51613(18) 0.31972(6) 0.26469(15) 0.0603(4) Uani 1 d . . . Cl1 Cl 0.77521(16) 0.40482(7) 0.34373(16) 0.0579(4) Uani 1 d . . . Cl2 Cl 0.74332(16) 0.32523(6) 0.57942(15) 0.0601(4) Uani 1 d . . . O1 O 0.2847(4) 0.34071(15) 0.5694(4) 0.0546(10) Uani 1 d . . . O2 O 0.3046(4) 0.48635(15) 0.1312(4) 0.0511(9) Uani 1 d . . . N1 N 0.4473(5) 0.37442(19) 0.4974(5) 0.0439(10) Uani 1 d . . . N2 N 0.2432(5) 0.39605(19) 0.5704(5) 0.0533(12) Uani 1 d . . . N3 N 0.4798(5) 0.44051(18) 0.2883(4) 0.0437(10) Uani 1 d . . . N4 N 0.4167(5) 0.5187(2) 0.1234(5) 0.0569(12) Uani 1 d . . . C1 C 0.3845(6) 0.3353(2) 0.5223(6) 0.0496(13) Uani 1 d . . . C2 C 0.4117(13) 0.2786(3) 0.5083(14) 0.072(2) Uani 1 d . . . C3 C 0.1604(6) 0.3999(2) 0.6290(6) 0.0493(13) Uani 1 d . . . C4 C 0.1021(7) 0.4545(3) 0.6270(7) 0.0595(15) Uani 1 d . . . C5 C 0.1091(8) 0.4706(3) 0.7633(8) 0.0690(18) Uani 1 d . . . C6 C 0.0451(8) 0.4294(4) 0.8223(8) 0.074(2) Uani 1 d . . . C7 C 0.1153(9) 0.3756(4) 0.8297(8) 0.078(2) Uani 1 d . . . C8 C 0.1136(10) 0.3579(3) 0.6957(10) 0.070(2) Uani 1 d . . . C9 C 0.3524(6) 0.4463(2) 0.2165(5) 0.0470(12) Uani 1 d . . . C10 C 0.2380(8) 0.4117(3) 0.2179(9) 0.069(2) Uani 1 d . . . C11 C 0.3683(6) 0.5617(2) 0.0624(5) 0.0493(13) Uani 1 d . . . C12 C 0.2238(6) 0.5807(2) 0.0088(6) 0.0523(14) Uani 1 d . . . C13 C 0.2150(11) 0.6365(3) 0.0556(11) 0.076(2) Uani 1 d . . . C14 C 0.3170(11) 0.6733(3) 0.0298(11) 0.085(2) Uani 1 d . . . C15 C 0.4626(10) 0.6518(4) 0.0947(11) 0.091(3) Uani 1 d . . . C16 C 0.4731(8) 0.5971(3) 0.0424(9) 0.070(2) Uani 1 d . . . N5 N 0.9240(11) 0.7091(5) 0.7791(13) 0.154(4) Uani 1 d . . . C17 C 0.9900(11) 0.7176(4) 0.7166(11) 0.099(3) Uani 1 d . . . C18 C 1.0737(18) 0.7307(5) 0.6449(14) 0.108(3) Uani 1 d . . . H1N H 0.414(12) 0.399(4) 0.489(11) 0.12(5) Uiso 1 d . . . H3N H 0.523(8) 0.461(3) 0.270(8) 0.09(3) Uiso 1 d . . . H21 H 0.482(10) 0.270(4) 0.555(10) 0.10(4) Uiso 1 d . . . H22 H 0.414(16) 0.277(6) 0.459(14) 0.17(8) Uiso 1 d . . . H23 H 0.341(9) 0.254(4) 0.546(8) 0.10(3) Uiso 1 d . . . H41 H 0.162(6) 0.481(2) 0.591(6) 0.065(18) Uiso 1 d . . . H42 H 0.006(7) 0.453(3) 0.567(6) 0.07(2) Uiso 1 d . . . H51 H 0.206(8) 0.476(3) 0.819(8) 0.09(2) Uiso 1 d . . . H52 H 0.072(7) 0.503(3) 0.769(7) 0.07(2) Uiso 1 d . . . H61 H -0.052(7) 0.424(2) 0.760(6) 0.063(18) Uiso 1 d . . . H62 H 0.060(8) 0.436(3) 0.903(8) 0.10(3) Uiso 1 d . . . H71 H 0.215(9) 0.383(3) 0.890(8) 0.09(3) Uiso 1 d . . . H72 H 0.064(10) 0.348(4) 0.866(10) 0.14(3) Uiso 1 d . . . H81 H 0.167(6) 0.330(2) 0.703(6) 0.045(16) Uiso 1 d . . . H82 H 0.042(6) 0.351(2) 0.652(5) 0.036(17) Uiso 1 d . . . H101 H 0.245(11) 0.418(4) 0.315(12) 0.15(4) Uiso 1 d . . . H102 H 0.255(9) 0.377(3) 0.195(8) 0.09(3) Uiso 1 d . . . H103 H 0.187(8) 0.415(3) 0.147(8) 0.07(3) Uiso 1 d . . . H121 H 0.170(7) 0.558(3) 0.034(7) 0.07(2) Uiso 1 d . . . H122 H 0.193(6) 0.583(2) -0.092(6) 0.058(17) Uiso 1 d . . . H131 H 0.099(13) 0.644(5) -0.008(12) 0.17(4) Uiso 1 d . . . H132 H 0.211(10) 0.631(4) 0.113(9) 0.08(3) Uiso 1 d . . . H141 H 0.285(9) 0.674(3) -0.060(9) 0.11(3) Uiso 1 d . . . H142 H 0.302(6) 0.705(3) 0.059(6) 0.059(18) Uiso 1 d . . . H151 H 0.474(11) 0.654(4) 0.178(10) 0.12(4) Uiso 1 d . . . H152 H 0.531(8) 0.679(3) 0.060(7) 0.10(2) Uiso 1 d . . . H161 H 0.449(7) 0.598(3) -0.061(8) 0.08(2) Uiso 1 d . . . H162 H 0.558(8) 0.584(3) 0.086(7) 0.08(2) Uiso 1 d . . . H181 H 1.059(18) 0.752(7) 0.574(18) 0.21(8) Uiso 1 d . . . H182 H 1.04(2) 0.708(8) 0.591(19) 0.25(9) Uiso 1 d . . . H183 H 1.156(16) 0.710(6) 0.660(14) 0.19(6) Uiso 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 Re 0.04962(15) 0.03382(13) 0.03625(14) -0.00154(9) 0.01714(9) 0.00147(9) Cl3 0.0658(9) 0.0530(8) 0.0533(8) -0.0198(7) 0.0155(7) -0.0014(7) Cl4 0.0849(10) 0.0454(8) 0.0531(8) -0.0163(6) 0.0291(7) -0.0100(7) Cl1 0.0623(9) 0.0574(8) 0.0626(9) -0.0015(7) 0.0333(7) -0.0054(7) Cl2 0.0605(9) 0.0575(9) 0.0589(9) 0.0141(7) 0.0187(7) 0.0155(7) O1 0.071(3) 0.040(2) 0.065(2) 0.0074(19) 0.039(2) 0.0032(19) O2 0.052(2) 0.049(2) 0.049(2) 0.0156(18) 0.0156(17) -0.0023(17) N1 0.053(3) 0.039(3) 0.044(3) 0.005(2) 0.023(2) 0.004(2) N2 0.062(3) 0.044(3) 0.061(3) 0.007(2) 0.032(3) 0.003(2) N3 0.053(3) 0.038(2) 0.041(2) 0.0023(19) 0.018(2) -0.001(2) N4 0.052(3) 0.051(3) 0.066(3) 0.014(2) 0.021(2) -0.002(2) C1 0.058(3) 0.047(3) 0.046(3) 0.006(3) 0.022(3) 0.008(3) C2 0.092(7) 0.040(4) 0.100(7) 0.020(4) 0.053(6) 0.014(4) C3 0.048(3) 0.049(3) 0.049(3) -0.005(3) 0.016(3) -0.001(2) C4 0.060(4) 0.055(4) 0.068(4) 0.002(3) 0.029(3) 0.010(3) C5 0.063(4) 0.069(5) 0.076(5) -0.013(4) 0.027(4) 0.000(4) C6 0.061(4) 0.107(6) 0.059(4) -0.008(4) 0.028(4) 0.004(4) C7 0.073(5) 0.098(6) 0.075(5) 0.013(4) 0.042(4) -0.003(4) C8 0.063(5) 0.056(4) 0.105(6) -0.003(4) 0.047(5) -0.007(4) C9 0.058(3) 0.040(3) 0.044(3) 0.001(2) 0.020(3) -0.004(2) C10 0.057(4) 0.072(5) 0.062(5) 0.022(4) 0.003(4) -0.017(4) C11 0.049(3) 0.048(3) 0.051(3) 0.010(3) 0.019(3) 0.002(2) C12 0.050(3) 0.049(3) 0.059(4) 0.008(3) 0.023(3) 0.002(3) C13 0.104(7) 0.054(4) 0.094(6) 0.005(4) 0.064(6) 0.009(4) C14 0.118(7) 0.041(4) 0.102(7) -0.001(4) 0.048(6) 0.001(4) C15 0.096(6) 0.063(5) 0.100(7) 0.012(5) 0.023(5) -0.021(4) C16 0.052(4) 0.063(4) 0.094(6) 0.035(4) 0.025(4) 0.000(3) N5 0.136(9) 0.144(9) 0.180(11) 0.021(8) 0.059(8) -0.025(7) C17 0.090(6) 0.079(6) 0.119(8) 0.003(5) 0.028(6) -0.014(5) C18 0.148(11) 0.084(7) 0.099(8) -0.003(6) 0.053(7) 0.011(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 Re N1 2.091(5) . ? Re N3 2.100(5) . ? Re Cl2 2.3212(15) . ? Re Cl4 2.3265(15) . ? Re Cl1 2.3320(15) . ? Re Cl3 2.3349(14) . ? O1 C1 1.334(7) . ? O1 N2 1.466(6) . ? O2 C9 1.337(6) . ? O2 N4 1.459(6) . ? N1 C1 1.271(7) . ? N2 C3 1.260(7) . ? N3 C9 1.274(7) . ? N4 C11 1.275(7) . ? C1 C2 1.481(10) . ? C3 C8 1.470(9) . ? C3 C4 1.504(8) . ? C4 C5 1.516(10) . ? C5 C6 1.508(11) . ? C6 C7 1.531(12) . ? C7 C8 1.522(11) . ? C9 C10 1.488(9) . ? C11 C12 1.479(8) . ? C11 C16 1.494(8) . ? C12 C13 1.515(10) . ? C13 C14 1.520(12) . ? C14 C15 1.517(14) . ? C15 C16 1.515(13) . ? N5 C17 1.160(13) . ? C17 C18 1.416(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re N3 89.40(19) . . ? N1 Re Cl2 90.53(14) . . ? N3 Re Cl2 178.76(13) . . ? N1 Re Cl4 92.75(14) . . ? N3 Re Cl4 88.68(13) . . ? Cl2 Re Cl4 92.56(7) . . ? N1 Re Cl1 175.00(14) . . ? N3 Re Cl1 86.91(14) . . ? Cl2 Re Cl1 93.09(6) . . ? Cl4 Re Cl1 90.53(6) . . ? N1 Re Cl3 85.55(14) . . ? N3 Re Cl3 86.11(13) . . ? Cl2 Re Cl3 92.65(6) . . ? Cl4 Re Cl3 174.54(6) . . ? Cl1 Re Cl3 90.84(6) . . ? C1 O1 N2 112.2(4) . . ? C9 O2 N4 111.5(4) . . ? C1 N1 Re 136.3(4) . . ? C3 N2 O1 109.9(4) . . ? C9 N3 Re 137.4(4) . . ? C11 N4 O2 109.8(4) . . ? N1 C1 O1 123.1(5) . . ? N1 C1 C2 126.6(6) . . ? O1 C1 C2 110.3(6) . . ? N2 C3 C8 128.0(6) . . ? N2 C3 C4 114.6(5) . . ? C8 C3 C4 117.3(6) . . ? C3 C4 C5 111.3(6) . . ? C4 C5 C6 111.6(6) . . ? C5 C6 C7 110.7(6) . . ? C8 C7 C6 112.3(7) . . ? C3 C8 C7 112.2(6) . . ? N3 C9 O2 123.0(5) . . ? N3 C9 C10 125.8(6) . . ? O2 C9 C10 111.2(5) . . ? N4 C11 C12 128.9(5) . . ? N4 C11 C16 114.7(5) . . ? C12 C11 C16 116.5(5) . . ? C11 C12 C13 110.6(6) . . ? C12 C13 C14 111.8(6) . . ? C15 C14 C13 110.3(7) . . ? C16 C15 C14 110.7(7) . . ? C11 C16 C15 109.2(7) . . ? N5 C17 C18 176.5(13) . . ? _diffrn_measured_fraction_theta_max 0.715 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.715 _refine_diff_density_max 1.448 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.102 #===END data_vk16 # compound 2 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Cl4 N4 O2 Re' _chemical_formula_weight 748.63 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.890(2) _cell_length_b 16.460(3) _cell_length_c 19.921(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3242.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description prism _exptl_crystal_colour blueish(?) _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 4.102 _exptl_absorpt_correction_type numeric _exptl_absorpt_correction_T_min 0.2841 _exptl_absorpt_correction_T_max 0.6388 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 1662 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1662 _reflns_number_gt 1662 _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 w=1/[\s^2^(Fo^2^)+(0.0702P)^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 -0.038(19) _refine_ls_number_reflns 1662 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.47327(5) 0.50288(5) 0.467126(18) 0.05231(18) Uani 1 d . . . Cl1 Cl 0.3736(4) 0.6089(3) 0.5277(2) 0.0802(12) Uani 1 d . . . Cl2 Cl 0.4727(5) 0.5781(3) 0.36883(17) 0.0892(14) Uani 1 d . . . Cl3 Cl 0.5946(6) 0.3991(2) 0.4168(2) 0.0944(15) Uani 1 d . . . Cl4 Cl 0.2653(5) 0.4439(3) 0.4446(2) 0.1066(18) Uani 1 d . . . O1 O 0.4559(12) 0.3520(5) 0.6479(4) 0.066(3) Uani 1 d . . . O2 O 0.8472(9) 0.6224(5) 0.5274(4) 0.054(2) Uani 1 d . . . N1 N 0.4773(12) 0.4437(7) 0.5617(4) 0.060(3) Uani 1 d . . . N2 N 0.4839(12) 0.4220(6) 0.6914(4) 0.049(3) Uani 1 d . . . N3 N 0.6637(10) 0.5474(7) 0.4973(5) 0.048(2) Uani 1 d . . . N4 N 0.8985(12) 0.5443(6) 0.5524(5) 0.052(3) Uani 1 d . . . C1 C 0.4373(13) 0.4089(8) 0.7505(6) 0.053(4) Uani 1 d . . . C2 C 0.4609(16) 0.4716(9) 0.8041(6) 0.060(4) Uani 1 d . . . C3 C 0.529(2) 0.4260(10) 0.8648(7) 0.078(5) Uani 1 d . . . C4 C 0.449(2) 0.3543(9) 0.8869(6) 0.082(5) Uani 1 d . . . C5 C 0.4238(16) 0.2940(9) 0.8312(6) 0.072(4) Uani 1 d . . . C6 C 0.3549(16) 0.3361(9) 0.7722(6) 0.062(4) Uani 1 d . . . C7 C 0.5406(18) 0.5461(10) 0.7800(7) 0.069(4) Uani 1 d . . . C8 C 0.523(3) 0.6153(10) 0.8297(9) 0.106(7) Uani 1 d . . . C9 C 0.6913(16) 0.5309(10) 0.7668(8) 0.078(5) Uani 1 d . . . C10 C 0.340(2) 0.2203(11) 0.8536(7) 0.102(7) Uani 1 d . . . C11 C 0.4629(17) 0.3718(8) 0.5822(6) 0.059(3) Uani 1 d . . . C12 C 0.4447(17) 0.2968(8) 0.5413(6) 0.069(4) Uani 1 d . . . C13 C 0.9921(15) 0.5532(8) 0.5954(7) 0.047(4) Uani 1 d . . . C14 C 1.0564(14) 0.4785(7) 0.6213(7) 0.054(4) Uani 1 d . . . C15 C 1.0713(18) 0.4831(8) 0.6999(7) 0.069(5) Uani 1 d . . . C16 C 1.1382(17) 0.5597(10) 0.7219(7) 0.066(4) Uani 1 d . . . C17 C 1.0606(16) 0.6357(9) 0.6957(7) 0.065(4) Uani 1 d . . . C18 C 1.0481(16) 0.6336(8) 0.6201(7) 0.056(4) Uani 1 d . . . C19 C 0.9949(19) 0.4003(10) 0.5969(9) 0.068(5) Uani 1 d . . . C20 C 0.855(2) 0.3799(10) 0.6240(10) 0.099(7) Uani 1 d . . . C21 C 1.090(3) 0.3281(11) 0.6098(11) 0.116(8) Uani 1 d . . . C22 C 1.135(2) 0.7140(11) 0.7175(8) 0.106(7) Uani 1 d . . . C23 C 0.7264(13) 0.6138(7) 0.4973(6) 0.042(3) Uani 1 d . . . C24 C 0.6797(14) 0.6898(8) 0.4686(7) 0.063(3) Uani 1 d . . . H1N H 0.5175 0.4804 0.5910 0.080 Uiso 1 d . . . H2 H 0.3448 0.4987 0.8196 0.080 Uiso 1 d . . . H3N H 0.7181 0.5130 0.5119 0.080 Uiso 1 d . . . H31 H 0.5294 0.4835 0.9074 0.080 Uiso 1 d . . . H32 H 0.6260 0.4114 0.8542 0.080 Uiso 1 d . . . H41 H 0.3764 0.3762 0.8968 0.080 Uiso 1 d . . . H42 H 0.4981 0.3006 0.9222 0.080 Uiso 1 d . . . H5 H 0.5331 0.2704 0.8167 0.080 Uiso 1 d . . . H61 H 0.3405 0.2984 0.7361 0.080 Uiso 1 d . . . H62 H 0.2630 0.3538 0.7864 0.080 Uiso 1 d . . . H7 H 0.4981 0.5652 0.7382 0.080 Uiso 1 d . . . H81 H 0.4753 0.6477 0.8349 0.080 Uiso 1 d . . . H82 H 0.6127 0.6457 0.8260 0.080 Uiso 1 d . . . H83 H 0.5355 0.5893 0.8738 0.080 Uiso 1 d . . . H91 H 0.7461 0.5794 0.7579 0.080 Uiso 1 d . . . H92 H 0.7099 0.4933 0.7282 0.080 Uiso 1 d . . . H93 H 0.7119 0.5061 0.8079 0.080 Uiso 1 d . . . H101 H 0.3003 0.1785 0.8245 0.080 Uiso 1 d . . . H102 H 0.2632 0.2444 0.8798 0.080 Uiso 1 d . . . H103 H 0.3924 0.1935 0.8887 0.080 Uiso 1 d . . . H121 H 0.5477 0.2734 0.5287 0.080 Uiso 1 d . . . H122 H 0.3977 0.2560 0.5655 0.080 Uiso 1 d . . . H123 H 0.3960 0.3160 0.5012 0.080 Uiso 1 d . . . H14 H 1.1541 0.4631 0.6078 0.080 Uiso 1 d . . . H151 H 1.0053 0.4870 0.7126 0.080 Uiso 1 d . . . H152 H 1.1013 0.4134 0.7085 0.080 Uiso 1 d . . . H161 H 1.2435 0.5581 0.7064 0.080 Uiso 1 d . . . H162 H 1.1515 0.5415 0.7882 0.080 Uiso 1 d . . . H17 H 0.9764 0.6342 0.7167 0.080 Uiso 1 d . . . H181 H 0.9997 0.6808 0.6003 0.080 Uiso 1 d . . . H182 H 1.1422 0.6393 0.6030 0.080 Uiso 1 d . . . H19 H 0.9650 0.3920 0.5411 0.080 Uiso 1 d . . . H201 H 0.7943 0.4317 0.6231 0.080 Uiso 1 d . . . H202 H 0.8665 0.3579 0.6691 0.080 Uiso 1 d . . . H203 H 0.8190 0.3358 0.5969 0.080 Uiso 1 d . . . H211 H 1.0205 0.2671 0.6108 0.080 Uiso 1 d . . . H212 H 1.1549 0.3364 0.6488 0.080 Uiso 1 d . . . H213 H 1.1664 0.3253 0.5707 0.080 Uiso 1 d . . . H221 H 1.0914 0.7606 0.7007 0.080 Uiso 1 d . . . H222 H 1.1439 0.7157 0.7650 0.080 Uiso 1 d . . . H223 H 1.2271 0.7114 0.6981 0.080 Uiso 1 d . . . H241 H 0.5545 0.7000 0.4696 0.080 Uiso 1 d . . . H242 H 0.7376 0.7216 0.4740 0.080 Uiso 1 d . . . H243 H 0.6928 0.6800 0.4207 0.080 Uiso 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 Re 0.0655(3) 0.0589(3) 0.0326(2) 0.0053(3) -0.0049(2) -0.0071(5) Cl1 0.077(3) 0.076(3) 0.087(3) 0.014(2) 0.017(2) 0.025(2) Cl2 0.124(4) 0.098(3) 0.0457(17) 0.026(2) -0.023(2) -0.031(3) Cl3 0.154(4) 0.062(2) 0.067(2) -0.0158(19) 0.042(3) -0.010(3) Cl4 0.102(4) 0.123(4) 0.094(3) 0.036(3) -0.046(3) -0.050(3) O1 0.107(8) 0.057(5) 0.035(4) 0.005(4) -0.002(5) -0.004(6) O2 0.059(6) 0.046(5) 0.057(5) 0.007(4) -0.010(5) 0.004(4) N1 0.067(8) 0.091(9) 0.023(4) 0.010(5) -0.012(5) -0.010(7) N2 0.072(8) 0.045(6) 0.031(4) 0.002(4) -0.001(5) -0.007(6) N3 0.044(6) 0.054(7) 0.046(5) -0.004(5) -0.004(5) 0.005(6) N4 0.060(7) 0.040(6) 0.057(6) 0.008(5) -0.003(6) 0.008(6) C1 0.057(10) 0.060(9) 0.042(6) 0.006(6) -0.006(6) 0.001(7) C2 0.060(9) 0.081(10) 0.037(6) 0.002(6) -0.003(6) 0.005(9) C3 0.104(13) 0.080(11) 0.050(7) 0.017(8) -0.016(9) -0.009(12) C4 0.145(16) 0.070(10) 0.030(6) 0.016(6) -0.015(8) 0.000(12) C5 0.082(11) 0.076(10) 0.057(8) 0.013(7) -0.002(8) -0.012(9) C6 0.074(10) 0.067(9) 0.045(7) 0.003(6) -0.014(7) -0.017(8) C7 0.083(12) 0.074(10) 0.050(8) -0.006(7) 0.004(8) -0.005(10) C8 0.15(2) 0.047(9) 0.122(15) -0.017(10) 0.041(16) -0.014(13) C9 0.060(10) 0.097(14) 0.075(10) -0.006(9) 0.014(8) -0.017(8) C10 0.156(18) 0.088(13) 0.061(9) 0.010(9) -0.003(10) -0.052(14) C11 0.085(10) 0.054(8) 0.038(6) 0.004(6) 0.014(7) 0.007(8) C12 0.110(13) 0.051(7) 0.048(7) -0.009(6) 0.004(8) -0.016(8) C13 0.045(11) 0.043(8) 0.055(7) 0.000(6) 0.013(7) -0.002(8) C14 0.052(9) 0.047(10) 0.063(7) 0.002(6) -0.006(6) 0.015(7) C15 0.091(11) 0.049(10) 0.067(8) -0.009(7) -0.007(7) 0.016(9) C16 0.072(11) 0.066(10) 0.059(8) 0.004(7) -0.022(8) -0.016(9) C17 0.066(12) 0.064(9) 0.065(8) 0.001(7) -0.007(7) -0.009(9) C18 0.048(11) 0.045(8) 0.074(9) 0.021(7) 0.007(8) 0.003(8) C19 0.074(15) 0.042(8) 0.087(10) -0.001(8) -0.012(10) 0.015(10) C20 0.129(18) 0.049(10) 0.121(15) 0.024(10) -0.040(13) -0.008(11) C21 0.14(2) 0.077(13) 0.128(17) -0.008(12) -0.018(16) 0.035(14) C22 0.15(2) 0.073(12) 0.093(12) -0.007(10) -0.037(13) -0.014(13) C23 0.044(8) 0.038(7) 0.043(6) 0.000(5) 0.000(6) 0.009(6) C24 0.067(9) 0.055(8) 0.066(8) 0.005(8) -0.012(8) 0.009(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 Re N3 2.109(10) . ? Re N1 2.121(9) . ? Re Cl3 2.316(4) . ? Re Cl4 2.319(5) . ? Re Cl2 2.317(3) . ? Re Cl1 2.340(4) . ? O1 C11 1.350(13) . ? O1 N2 1.467(12) . ? O2 C23 1.344(15) . ? O2 N4 1.469(12) . ? N1 C11 1.259(15) . ? N2 C1 1.283(14) . ? N3 C23 1.257(15) . ? N4 C13 1.271(17) . ? C1 C2 1.503(18) . ? C1 C6 1.512(18) . ? C2 C7 1.54(2) . ? C2 C3 1.575(18) . ? C3 C4 1.49(2) . ? C4 C5 1.510(19) . ? C5 C6 1.525(18) . ? C5 C10 1.53(2) . ? C7 C8 1.52(2) . ? C7 C9 1.53(2) . ? C11 C12 1.491(17) . ? C13 C14 1.476(18) . ? C13 C18 1.516(19) . ? C14 C19 1.505(19) . ? C14 C15 1.576(19) . ? C15 C16 1.491(19) . ? C16 C17 1.56(2) . ? C17 C18 1.513(19) . ? C17 C22 1.55(2) . ? C19 C20 1.52(3) . ? C19 C21 1.54(2) . ? C23 C24 1.450(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Re N1 83.7(4) . . ? N3 Re Cl3 85.3(3) . . ? N1 Re Cl3 92.0(4) . . ? N3 Re Cl4 173.3(3) . . ? N1 Re Cl4 89.8(3) . . ? Cl3 Re Cl4 93.8(2) . . ? N3 Re Cl2 93.3(3) . . ? N1 Re Cl2 174.9(3) . . ? Cl3 Re Cl2 91.72(16) . . ? Cl4 Re Cl2 93.34(16) . . ? N3 Re Cl1 88.3(3) . . ? N1 Re Cl1 83.8(3) . . ? Cl3 Re Cl1 172.67(18) . . ? Cl4 Re Cl1 92.19(19) . . ? Cl2 Re Cl1 92.07(16) . . ? C11 O1 N2 111.9(9) . . ? C23 O2 N4 111.5(9) . . ? C11 N1 Re 135.8(9) . . ? C1 N2 O1 110.1(10) . . ? C23 N3 Re 138.0(9) . . ? C13 N4 O2 112.3(11) . . ? N2 C1 C2 118.8(12) . . ? N2 C1 C6 126.1(12) . . ? C2 C1 C6 115.1(10) . . ? C1 C2 C7 113.9(11) . . ? C1 C2 C3 106.6(11) . . ? C7 C2 C3 113.5(13) . . ? C4 C3 C2 111.9(14) . . ? C3 C4 C5 113.0(12) . . ? C4 C5 C6 109.9(12) . . ? C4 C5 C10 113.2(12) . . ? C6 C5 C10 110.1(13) . . ? C1 C6 C5 109.9(11) . . ? C8 C7 C2 109.6(12) . . ? C8 C7 C9 110.3(15) . . ? C2 C7 C9 115.0(14) . . ? N1 C11 O1 123.2(12) . . ? N1 C11 C12 127.9(11) . . ? O1 C11 C12 108.9(11) . . ? N4 C13 C14 116.9(13) . . ? N4 C13 C18 125.8(13) . . ? C14 C13 C18 117.2(11) . . ? C13 C14 C19 115.2(13) . . ? C13 C14 C15 110.3(11) . . ? C19 C14 C15 113.5(11) . . ? C16 C15 C14 112.0(11) . . ? C15 C16 C17 111.3(11) . . ? C18 C17 C22 109.7(13) . . ? C18 C17 C16 110.9(12) . . ? C22 C17 C16 109.8(12) . . ? C17 C18 C13 111.8(11) . . ? C14 C19 C20 116.2(15) . . ? C14 C19 C21 111.1(14) . . ? C20 C19 C21 109.1(15) . . ? N3 C23 O2 122.0(11) . . ? N3 C23 C24 126.4(12) . . ? O2 C23 C24 111.6(11) . . ? _diffrn_measured_fraction_theta_max 0.518 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.518 _refine_diff_density_max 1.140 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.098