# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name A.Bianchi 'Carla Bazzicalupi' 'Sixto Dominguez' 'Jorge S. Gancheff' 'Carlos Kremer' 'Alvaro Mombru' 'Leopoldo Suescun' 'Oscar N. Ventura' _publ_contact_author_name A.Bianchi _publ_contact_author_address ; Department of Chemistry University of Florence Via della Lastruccia 3 Florence 50019 ITALY ; _publ_contact_author_email ANTONIO.BIANCHI@UNIFI.IT _publ_section_title ; ReO2+ chelates with aliphatic diamines. Structural and proton transfer properties,ReO2+ chelates with aliphatic diamines. Structural and proton transfer properties ; # Attachment 'B606797Bcomp1.cif' data_jg01 _database_code_depnum_ccdc_archive 'CCDC 616325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 I N4 O4 Re' _chemical_formula_weight 613.56 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' I I -0.4742 1.8119 '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 'C 1 2/c 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' '-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 13.8941(17) _cell_length_b 19.078(4) _cell_length_c 10.2235(14) _cell_angle_alpha 90.00 _cell_angle_beta 128.293(5) _cell_angle_gamma 90.00 _cell_volume 2126.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.16 _cell_measurement_theta_max 14.75 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 7.184 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.2888 _exptl_absorpt_correction_T_max 0.6332 _exptl_absorpt_process_details 'MSC/AFC Diffractometer Software (1993)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2915 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2451 _reflns_number_gt 1909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Software, 1993' _computing_cell_refinement 'MSC/AFC Diffractometer Software, 1993' _computing_data_reduction 'MSC/AFC Diffractometer Software, 1993' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1995)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0709P)^2^+6.4164P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00073(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2451 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 C1 C 0.6771(9) 0.6874(5) 0.1807(12) 0.055(2) Uani 1 1 d . . . H1A H 0.7601 0.6851 0.2166 0.066 Uiso 1 1 calc R . . H1B H 0.6205 0.6826 0.0604 0.066 Uiso 1 1 calc R . . C2 C 0.6565(8) 0.6294(4) 0.2610(10) 0.0499(18) Uani 1 1 d . . . H2A H 0.5725 0.6307 0.2214 0.060 Uiso 1 1 calc R . . H2B H 0.6705 0.5843 0.2315 0.060 Uiso 1 1 calc R . . C3 C 0.6889(9) 0.8156(5) 0.1718(11) 0.053(2) Uani 1 1 d . . . H3A H 0.7759 0.8135 0.2259 0.064 Uiso 1 1 calc R . . H3B H 0.6738 0.8589 0.2062 0.064 Uiso 1 1 calc R . . C4 C 0.6192(10) 0.8179(6) -0.0142(12) 0.068(2) Uani 1 1 d . . . H4A H 0.6453 0.8578 -0.0423 0.101 Uiso 1 1 calc R . . H4B H 0.5330 0.8214 -0.0692 0.101 Uiso 1 1 calc R . . H4C H 0.6351 0.7758 -0.0496 0.101 Uiso 1 1 calc R . . C5 C 0.8616(8) 0.6038(5) 0.5223(13) 0.062(2) Uani 1 1 d . . . H5A H 0.9170 0.6171 0.6390 0.075 Uiso 1 1 calc R . . H5B H 0.8959 0.6214 0.4700 0.075 Uiso 1 1 calc R . . C6 C 0.8567(11) 0.5256(6) 0.511(2) 0.097(4) Uani 1 1 d . . . H6A H 0.9377 0.5076 0.5644 0.145 Uiso 1 1 calc R . . H6B H 0.8039 0.5117 0.3961 0.145 Uiso 1 1 calc R . . H6C H 0.8254 0.5074 0.5657 0.145 Uiso 1 1 calc R . . N1 N 0.6569(7) 0.7555(3) 0.2317(9) 0.0396(14) Uani 1 1 d . . . H1 H 0.5751 0.7587 0.1796 0.047 Uiso 1 1 calc R . . N2 N 0.7419(5) 0.6385(3) 0.4440(8) 0.0406(13) Uani 1 1 d . . . H2 H 0.7070 0.6166 0.4843 0.049 Uiso 1 1 calc R . . O1 O 0.8930(5) 0.7568(2) 0.5405(7) 0.0383(11) Uani 1 1 d . . . O1W O 0.6444(8) 0.5461(4) 0.5669(11) 0.077(2) Uani 1 1 d . . . I2 I 0.5000 0.58346(5) 0.7500 0.0645(3) Uani 1 2 d S . . Re1 Re 0.7500 0.7500 0.5000 0.03396(18) Uani 1 2 d S . . 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 C1 0.065(5) 0.059(5) 0.055(5) -0.006(4) 0.044(4) 0.003(4) C2 0.056(4) 0.045(4) 0.046(4) -0.016(3) 0.031(4) -0.010(3) C3 0.063(5) 0.059(5) 0.050(5) -0.003(4) 0.041(4) -0.010(4) C4 0.081(6) 0.079(7) 0.058(6) 0.005(5) 0.050(5) 0.005(5) C5 0.054(5) 0.054(5) 0.069(6) -0.009(4) 0.033(4) 0.008(4) C6 0.076(7) 0.057(6) 0.139(13) 0.002(7) 0.057(8) 0.017(5) N1 0.042(3) 0.048(4) 0.036(3) -0.005(2) 0.028(3) -0.003(2) N2 0.039(3) 0.047(3) 0.039(3) -0.004(3) 0.026(2) -0.001(2) O1 0.035(3) 0.049(3) 0.036(3) -0.0069(19) 0.025(2) -0.0041(18) O1W 0.101(5) 0.069(4) 0.088(5) -0.017(4) 0.073(5) -0.026(4) I2 0.0859(6) 0.0646(5) 0.0556(5) 0.000 0.0502(5) 0.000 Re1 0.0320(2) 0.0411(3) 0.0333(3) -0.00621(14) 0.02243(19) -0.00404(13) _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 C1 N1 1.491(10) . ? C1 C2 1.507(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.479(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.491(10) . ? C3 C4 1.508(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N2 1.482(10) . ? C5 C6 1.494(15) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N1 Re1 2.193(7) . ? N1 H1 0.9100 . ? N2 Re1 2.187(6) . ? N2 H2 0.9100 . ? O1 Re1 1.766(5) . ? Re1 O1 1.766(5) 7_666 ? Re1 N2 2.187(6) 7_666 ? Re1 N1 2.193(7) 7_666 ? 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 C1 C2 108.0(6) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 109.2(7) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? N1 C3 C4 114.7(8) . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 115.0(8) . . ? N2 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N2 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 N1 C3 111.0(7) . . ? C1 N1 Re1 107.6(5) . . ? C3 N1 Re1 117.1(5) . . ? C1 N1 H1 106.9 . . ? C3 N1 H1 106.9 . . ? Re1 N1 H1 106.9 . . ? C2 N2 C5 112.5(6) . . ? C2 N2 Re1 108.5(5) . . ? C5 N2 Re1 115.8(5) . . ? C2 N2 H2 106.5 . . ? C5 N2 H2 106.5 . . ? Re1 N2 H2 106.5 . . ? O1 Re1 O1 180.0(4) . 7_666 ? O1 Re1 N2 90.0(2) . 7_666 ? O1 Re1 N2 90.0(2) 7_666 7_666 ? O1 Re1 N2 90.0(2) . . ? O1 Re1 N2 90.0(2) 7_666 . ? N2 Re1 N2 180.000(1) 7_666 . ? O1 Re1 N1 90.3(3) . 7_666 ? O1 Re1 N1 89.7(3) 7_666 7_666 ? N2 Re1 N1 79.9(2) 7_666 7_666 ? N2 Re1 N1 100.1(2) . 7_666 ? O1 Re1 N1 89.7(3) . . ? O1 Re1 N1 90.3(3) 7_666 . ? N2 Re1 N1 100.1(2) 7_666 . ? N2 Re1 N1 79.9(2) . . ? N1 Re1 N1 180.000(1) 7_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -58.5(9) . . . . ? C2 C1 N1 C3 173.9(7) . . . . ? C2 C1 N1 Re1 44.5(8) . . . . ? C4 C3 N1 C1 57.7(11) . . . . ? C4 C3 N1 Re1 -178.2(6) . . . . ? C1 C2 N2 C5 -87.9(8) . . . . ? C1 C2 N2 Re1 41.4(7) . . . . ? C6 C5 N2 C2 -66.1(12) . . . . ? C6 C5 N2 Re1 168.4(9) . . . . ? C2 N2 Re1 O1 -102.7(5) . . . . ? C5 N2 Re1 O1 24.8(6) . . . . ? C2 N2 Re1 O1 77.3(5) . . . 7_666 ? C5 N2 Re1 O1 -155.2(6) . . . 7_666 ? C2 N2 Re1 N2 68(100) . . . 7_666 ? C5 N2 Re1 N2 -164(100) . . . 7_666 ? C2 N2 Re1 N1 167.0(5) . . . 7_666 ? C5 N2 Re1 N1 -65.5(6) . . . 7_666 ? C2 N2 Re1 N1 -13.0(5) . . . . ? C5 N2 Re1 N1 114.5(6) . . . . ? C1 N1 Re1 O1 72.8(5) . . . . ? C3 N1 Re1 O1 -52.9(6) . . . . ? C1 N1 Re1 O1 -107.2(5) . . . 7_666 ? C3 N1 Re1 O1 127.1(6) . . . 7_666 ? C1 N1 Re1 N2 162.7(5) . . . 7_666 ? C3 N1 Re1 N2 37.0(6) . . . 7_666 ? C1 N1 Re1 N2 -17.3(5) . . . . ? C3 N1 Re1 N2 -143.0(6) . . . . ? C1 N1 Re1 N1 5(100) . . . 7_666 ? C3 N1 Re1 N1 -121(100) . . . 7_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.161 _refine_diff_density_min -2.359 _refine_diff_density_rms 0.196 # Attachment 'B606797Bcomp3.cif' data_redeten _database_code_depnum_ccdc_archive 'CCDC 616326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H33 Cl2 N4 O10 Re' _chemical_formula_weight 650.6 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 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.513(5) _cell_length_b 15.322(5) _cell_length_c 16.926(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 2207.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 5.801 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8468 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.31 _diffrn_reflns_theta_max 25.85 _reflns_number_total 1789 _reflns_number_gt 1192 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0324P)^2^+19.8789P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1789 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.0000 0.0000 0.0000 0.02688(18) Uani 1 2 d S . . Cl2 Cl 0.0987(3) -0.28304(16) 0.13778(15) 0.0466(6) Uani 1 1 d . . . C5 C -0.0948(11) -0.0701(6) 0.1651(5) 0.035(2) Uani 1 1 d . . . H5A H 0.0183 -0.0723 0.1717 0.042 Uiso 1 1 calc R . . H5B H -0.1262 -0.1230 0.1380 0.042 Uiso 1 1 calc R . . N2 N -0.1336(7) 0.0063(4) 0.1130(4) 0.0248(16) Uani 1 1 d . . . C8 C -0.3870(12) -0.0689(7) 0.0714(6) 0.055(3) Uani 1 1 d . . . H11A H -0.3507 -0.0799 0.0187 0.082 Uiso 1 1 calc R . . H11B H -0.4989 -0.0612 0.0710 0.082 Uiso 1 1 calc R . . H11C H -0.3604 -0.1174 0.1047 0.082 Uiso 1 1 calc R . . C1 C -0.0621(12) 0.1612(6) 0.0956(5) 0.041(2) Uani 1 1 d . . . H13A H -0.1637 0.1754 0.0729 0.050 Uiso 1 1 calc R . . H13B H -0.0217 0.2128 0.1219 0.050 Uiso 1 1 calc R . . C6 C -0.1695(13) -0.0698(7) 0.2458(6) 0.057(3) Uani 1 1 d . . . H14A H -0.1557 -0.0135 0.2698 0.086 Uiso 1 1 calc R . . H14B H -0.1207 -0.1136 0.2782 0.086 Uiso 1 1 calc R . . H14C H -0.2796 -0.0822 0.2410 0.086 Uiso 1 1 calc R . . C7 C -0.3107(10) 0.0118(6) 0.1024(6) 0.045(3) Uani 1 1 d . . . H15A H -0.3576 0.0259 0.1531 0.054 Uiso 1 1 calc R . . H15B H -0.3338 0.0595 0.0666 0.054 Uiso 1 1 calc R . . C2 C -0.0784(12) 0.0883(6) 0.1531(5) 0.037(2) Uani 1 1 d . . . H16A H -0.1529 0.1047 0.1939 0.045 Uiso 1 1 calc R . . H16B H 0.0222 0.0776 0.1782 0.045 Uiso 1 1 calc R . . O17 O 0.1600(9) -0.3703(4) 0.1385(4) 0.063(2) Uani 1 1 d . . . O19 O 0.2099(10) -0.2257(5) 0.1003(5) 0.081(3) Uani 1 1 d . . . O21 O 0.0744(13) -0.2541(6) 0.2146(5) 0.102(3) Uani 1 1 d . . . O22 O -0.0407(9) -0.2787(5) 0.0919(6) 0.083(3) Uani 1 1 d . . . N1 N 0.0477(9) 0.1331(5) 0.0327(5) 0.0375(19) Uani 1 1 d . . . H1A H 0.1472 0.1378 0.0501 0.045 Uiso 1 1 calc R . . H1B H 0.0367 0.1679 -0.0098 0.045 Uiso 1 1 calc R . . O1 O 0.1674(7) -0.0355(4) 0.0543(3) 0.0405(16) 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 0.0310(3) 0.0238(3) 0.0258(3) 0.0000(2) 0.0031(2) 0.0005(2) Cl2 0.0507(15) 0.0433(15) 0.0457(14) 0.0061(13) 0.0054(13) 0.0146(13) C5 0.038(6) 0.039(6) 0.028(5) 0.006(4) 0.004(4) -0.004(5) N2 0.028(3) 0.031(4) 0.016(3) -0.001(3) 0.008(3) 0.001(3) C8 0.034(6) 0.079(8) 0.052(7) -0.001(6) -0.007(5) -0.026(6) C1 0.044(6) 0.037(6) 0.044(6) -0.010(5) 0.010(5) 0.009(5) C6 0.072(8) 0.065(7) 0.035(6) 0.006(6) 0.009(5) -0.009(6) C7 0.034(5) 0.057(7) 0.044(6) 0.008(5) 0.010(4) 0.006(5) C2 0.047(6) 0.043(6) 0.023(5) -0.005(4) 0.009(4) -0.006(5) O17 0.076(5) 0.043(4) 0.070(5) 0.007(4) 0.014(4) 0.022(4) O19 0.075(6) 0.070(5) 0.099(7) 0.031(5) 0.009(5) -0.002(5) O21 0.171(10) 0.083(6) 0.053(5) 0.002(4) 0.017(6) 0.050(7) O22 0.065(6) 0.056(5) 0.127(8) 0.011(5) -0.035(5) 0.004(4) N1 0.038(5) 0.033(5) 0.041(4) -0.002(4) 0.001(4) -0.007(3) O1 0.025(3) 0.070(4) 0.026(3) 0.004(3) -0.001(3) 0.007(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 O1 1.780(6) . ? Re1 O1 1.780(6) 5 ? Re1 N1 2.152(7) . ? Re1 N1 2.152(7) 5 ? Re1 N2 2.228(6) 5 ? Re1 N2 2.228(6) . ? Cl2 O21 1.390(8) . ? Cl2 O22 1.420(8) . ? Cl2 O17 1.435(7) . ? Cl2 O19 1.438(8) . ? C5 N2 1.502(10) . ? C5 C6 1.508(12) . ? N2 C2 1.503(10) . ? N2 C7 1.520(10) . ? C8 C7 1.491(13) . ? C1 N1 1.481(11) . ? C1 C2 1.488(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O1 180.0(5) . 5 ? O1 Re1 N1 90.3(3) . . ? O1 Re1 N1 89.7(3) 5 . ? O1 Re1 N1 89.7(3) . 5 ? O1 Re1 N1 90.3(3) 5 5 ? N1 Re1 N1 180.0(4) . 5 ? O1 Re1 N2 91.2(2) . 5 ? O1 Re1 N2 88.8(2) 5 5 ? N1 Re1 N2 99.5(3) . 5 ? N1 Re1 N2 80.5(3) 5 5 ? O1 Re1 N2 88.8(2) . . ? O1 Re1 N2 91.2(2) 5 . ? N1 Re1 N2 80.5(3) . . ? N1 Re1 N2 99.5(3) 5 . ? N2 Re1 N2 180.0(3) 5 . ? O21 Cl2 O22 111.9(6) . . ? O21 Cl2 O17 110.1(5) . . ? O22 Cl2 O17 110.6(5) . . ? O21 Cl2 O19 108.4(6) . . ? O22 Cl2 O19 106.3(5) . . ? O17 Cl2 O19 109.5(5) . . ? N2 C5 C6 115.9(8) . . ? C5 N2 C2 108.5(6) . . ? C5 N2 C7 109.3(6) . . ? C2 N2 C7 108.5(7) . . ? C5 N2 Re1 110.9(5) . . ? C2 N2 Re1 105.3(5) . . ? C7 N2 Re1 114.1(5) . . ? N1 C1 C2 108.1(7) . . ? C8 C7 N2 115.3(8) . . ? C1 C2 N2 111.2(7) . . ? C1 N1 Re1 110.0(5) . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 0.657 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.118