# 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_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_section_title ; Non-covalent interactions between anions and a cationic rhenium diamine complex: structural characterization of the supramolecular adducts ; _audit_creation_method SHELXL _publ_contact_author ; Julio Perez Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; _publ_contact_author_phone +34-85-102985 _publ_contact_author_fax +34-85-103446 _publ_contact_author_email japm@sauron.quimica.uniovi.es loop_ _publ_author_name _publ_author_address 'Sonia Nieto' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN' ; 'Julio Perez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Lucia Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Victor Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Daniel Miguel' ; Quimica Inorganica Facultad de Ciencias Universidad de Valladolid 47071 Valladolid SPAIN ; _publ_contact_author_name 'Julio Perez' #-------------------------- data section of block --------------------------- data_[Re(o-C6H4(NH2)2(NCtBu)(CO)3].NO3_(sn434am) _database_code_depnum_ccdc_archive 'CCDC 292720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Re(o-C6H4(NH2)2(NCtBu)(CO)3].NO3' _chemical_formula_sum 'C14 H17 N4 O6 Re' _chemical_formula_weight 523.52 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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.227(4) _cell_length_b 10.155(4) _cell_length_c 10.156(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.496(7) _cell_angle_gamma 90.00 _cell_volume 912.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 6.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731071 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4105 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 23.28 _reflns_number_total 1404 _reflns_number_gt 1273 _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^)+(0.0671P)^2^+5.5827P] 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 0.0049(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1404 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 O12 O -0.2789(18) 0.2500 -0.146(3) 0.209(15) Uani 1 2 d S . . N11 N -0.138(3) 0.2500 -0.0690(17) 0.104(8) Uani 1 2 d S . . O11 O -0.0907(13) 0.1468(10) -0.0335(14) 0.109(4) Uani 1 1 d . . . Re1 Re 0.33418(6) 0.2500 -0.03818(5) 0.0396(3) Uani 1 2 d S . . N1 N 0.2342(11) 0.1211(11) 0.0921(9) 0.061(3) Uani 1 1 d . . . H1A H 0.1345 0.1109 0.0523 0.073 Uiso 1 1 calc R . . H1B H 0.2780 0.0412 0.1015 0.073 Uiso 1 1 calc R . . N3 N 0.6466(14) 0.2500 0.2085(12) 0.043(3) Uani 1 2 d S . . C1 C 0.152(2) 0.2500 -0.191(2) 0.087(7) Uani 1 2 d S . . O1 O 0.0522(18) 0.2500 -0.2889(16) 0.139(8) Uani 1 2 d S . . C2 C 0.4176(12) 0.1205(11) -0.1327(10) 0.049(3) Uani 1 1 d . . . O2 O 0.4685(11) 0.0436(8) -0.1903(8) 0.071(2) Uani 1 1 d . . . C3 C 0.5372(16) 0.2500 0.1233(15) 0.040(3) Uani 1 2 d S . . C4 C 0.7777(16) 0.2500 0.3303(16) 0.055(4) Uani 1 2 d S . . C5 C 0.717(3) 0.2500 0.4538(19) 0.119(10) Uani 1 2 d S . . H5A H 0.6572 0.1721 0.4524 0.179 Uiso 0.50 1 d PR . . H5B H 0.6546 0.3265 0.4509 0.179 Uiso 0.50 1 d PR . . H5C H 0.7992 0.2500 0.5363 0.179 Uiso 1 2 d SR . . C6 C 0.8701(15) 0.1290(15) 0.3233(17) 0.094(5) Uani 1 1 d . . . H6A H 0.8081 0.0520 0.3167 0.141 Uiso 1 1 calc R . . H6B H 0.9540 0.1237 0.4046 0.141 Uiso 1 1 calc R . . H6C H 0.9069 0.1343 0.2440 0.141 Uiso 1 1 calc R . . C11 C 0.2592(12) 0.1821(11) 0.2241(10) 0.053(3) Uani 1 1 d . . . C12 C 0.2863(14) 0.1132(15) 0.3442(12) 0.069(3) Uani 1 1 d . . . H12 H 0.2847 0.0216 0.3439 0.082 Uiso 1 1 calc R . . C13 C 0.3164(15) 0.1826(16) 0.4665(11) 0.079(4) Uani 1 1 d . . . H13 H 0.3368 0.1372 0.5493 0.095 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 O12 0.031(8) 0.25(3) 0.28(3) 0.000 -0.061(13) 0.000 N11 0.26(3) 0.020(7) 0.072(10) 0.000 0.106(15) 0.000 O11 0.093(7) 0.055(6) 0.182(13) 0.025(7) 0.046(7) 0.002(5) Re1 0.0316(4) 0.0562(4) 0.0257(4) 0.000 -0.0004(2) 0.000 N1 0.054(5) 0.085(7) 0.046(5) -0.008(5) 0.016(4) -0.024(5) N3 0.042(7) 0.050(7) 0.031(6) 0.000 -0.001(6) 0.000 C1 0.045(10) 0.16(2) 0.050(11) 0.000 0.000(9) 0.000 O1 0.066(10) 0.26(3) 0.065(10) 0.000 -0.020(9) 0.000 C2 0.058(6) 0.049(6) 0.037(5) 0.003(5) 0.007(5) -0.021(5) O2 0.113(7) 0.048(5) 0.060(5) -0.017(4) 0.037(5) -0.009(5) C3 0.038(8) 0.030(7) 0.051(9) 0.000 0.011(8) 0.000 C4 0.040(8) 0.058(9) 0.050(9) 0.000 -0.015(7) 0.000 C5 0.086(15) 0.22(3) 0.033(10) 0.000 -0.010(10) 0.000 C6 0.053(8) 0.088(10) 0.113(12) -0.006(9) -0.020(8) 0.020(7) C11 0.042(5) 0.076(7) 0.043(6) 0.000(5) 0.013(5) -0.012(5) C12 0.072(8) 0.088(9) 0.051(7) 0.006(7) 0.025(6) -0.006(7) C13 0.086(9) 0.115(11) 0.039(7) 0.021(6) 0.022(6) 0.005(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 O12 N11 1.31(3) . ? N11 O11 1.153(14) . ? N11 O11 1.153(14) 4_565 ? Re1 C2 1.914(12) . ? Re1 C2 1.914(12) 4_565 ? Re1 C1 1.938(18) . ? Re1 C3 2.110(15) . ? Re1 N1 2.238(9) . ? Re1 N1 2.238(9) 4_565 ? N1 C11 1.435(14) . ? N3 C3 1.128(18) . ? N3 C4 1.464(18) . ? C1 O1 1.15(2) . ? C2 O2 1.153(13) . ? C4 C6 1.509(16) . ? C4 C6 1.509(16) 4_565 ? C4 C5 1.51(3) . ? C11 C12 1.366(16) . ? C11 C11 1.38(2) 4_565 ? C12 C13 1.386(18) . ? C13 C13 1.37(3) 4_565 ? 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 N11 O11 131(3) . 4_565 ? O11 N11 O12 114.1(14) . . ? O11 N11 O12 114.1(14) 4_565 . ? C2 Re1 C2 86.8(6) . 4_565 ? C2 Re1 C1 88.7(5) . . ? C2 Re1 C1 88.7(5) 4_565 . ? C2 Re1 C3 89.7(4) . . ? C2 Re1 C3 89.7(4) 4_565 . ? C1 Re1 C3 177.8(7) . . ? C2 Re1 N1 100.8(4) . . ? C2 Re1 N1 172.1(4) 4_565 . ? C1 Re1 N1 93.8(5) . . ? C3 Re1 N1 88.0(4) . . ? C2 Re1 N1 172.1(4) . 4_565 ? C2 Re1 N1 100.8(4) 4_565 4_565 ? C1 Re1 N1 93.8(5) . 4_565 ? C3 Re1 N1 88.0(4) . 4_565 ? N1 Re1 N1 71.6(5) . 4_565 ? C11 N1 Re1 108.5(7) . . ? C3 N3 C4 173.3(15) . . ? O1 C1 Re1 174.3(19) . . ? O2 C2 Re1 179.2(9) . . ? N3 C3 Re1 179.2(12) . . ? N3 C4 C6 107.6(9) . . ? N3 C4 C6 107.6(9) . 4_565 ? C6 C4 C6 109.1(16) . 4_565 ? N3 C4 C5 106.7(14) . . ? C6 C4 C5 112.8(11) . . ? C6 C4 C5 112.8(11) 4_565 . ? C12 C11 C11 120.8(8) . 4_565 ? C12 C11 N1 123.6(11) . . ? C11 C11 N1 115.6(6) 4_565 . ? C11 C12 C13 118.6(13) . . ? C13 C13 C12 120.6(8) 4_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.862 _refine_diff_density_min -1.386 _refine_diff_density_rms 0.183 #===END data_[Re(o-C6H4(NH2)2(NCtBu)(CO)3].ClO4_(sn504b) _database_code_depnum_ccdc_archive 'CCDC 292721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Re(o-C6H4(NH2)2(NCtBu)(CO)3].ClO4' _chemical_formula_sum 'C14 H17 Cl N3 O7 Re' _chemical_formula_weight 560.96 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 10.160(7) _cell_length_b 12.354(9) _cell_length_c 15.993(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2007(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description NEEDDLE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 6.225 _exptl_absorpt_correction_type multi_scan _exptl_absorpt_correction_T_min 0.246677 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17956 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.31 _reflns_number_total 2893 _reflns_number_gt 2680 _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^)+(0.0843P)^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 constr _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 -0.03(2) _refine_ls_number_reflns 2893 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.80353(4) 0.82739(4) 0.31913(3) 0.04472(19) Uani 1 1 d . . . N1 N 0.7111(10) 0.8000(8) 0.4457(5) 0.045(2) Uani 1 1 d . . . H1A H 0.6993 0.7288 0.4547 0.055 Uiso 1 1 calc R . . H1B H 0.7637 0.8263 0.4862 0.055 Uiso 1 1 calc R . . N2 N 0.5858(7) 0.8297(7) 0.2987(5) 0.0385(18) Uani 1 1 d . . . H2A H 0.5666 0.8724 0.2548 0.046 Uiso 1 1 calc R . . H2B H 0.5574 0.7624 0.2871 0.046 Uiso 1 1 calc R . . N3 N 0.7719(9) 1.0820(8) 0.3635(6) 0.047(2) Uani 1 1 d . . . C1 C 0.8185(12) 0.6719(10) 0.2909(8) 0.059(3) Uani 1 1 d . . . O1 O 0.8397(15) 0.5874(10) 0.2666(9) 0.113(5) Uani 1 1 d . . . C2 C 0.8574(13) 0.8657(13) 0.2066(8) 0.068(4) Uani 1 1 d . . . O2 O 0.8927(13) 0.8834(12) 0.1414(7) 0.105(4) Uani 1 1 d . . . C3 C 0.9870(15) 0.8281(12) 0.3570(7) 0.066(3) Uani 1 1 d . . . O3 O 1.0934(9) 0.8309(11) 0.3765(7) 0.089(3) Uani 1 1 d . . . C4 C 0.7860(11) 0.9945(9) 0.3478(7) 0.048(3) Uani 1 1 d . . . C5 C 0.7448(14) 1.1955(9) 0.3868(9) 0.062(3) Uani 1 1 d . . . C6 C 0.600(2) 1.1946(15) 0.4078(14) 0.102(6) Uani 1 1 d . . . H6A H 0.5498 1.1802 0.3581 0.153 Uiso 1 1 calc R . . H6B H 0.5749 1.2638 0.4301 0.153 Uiso 1 1 calc R . . H6C H 0.5827 1.1393 0.4485 0.153 Uiso 1 1 calc R . . C7 C 0.833(3) 1.2212(14) 0.4614(12) 0.143(11) Uani 1 1 d . . . H7A H 0.8107 1.1741 0.5071 0.215 Uiso 1 1 calc R . . H7B H 0.8196 1.2951 0.4780 0.215 Uiso 1 1 calc R . . H7C H 0.9232 1.2105 0.4461 0.215 Uiso 1 1 calc R . . C8 C 0.7766(18) 1.2628(12) 0.3105(10) 0.087(5) Uani 1 1 d . . . H8A H 0.8654 1.2485 0.2931 0.130 Uiso 1 1 calc R . . H8B H 0.7677 1.3382 0.3239 0.130 Uiso 1 1 calc R . . H8C H 0.7171 1.2446 0.2661 0.130 Uiso 1 1 calc R . . C11 C 0.5847(12) 0.8560(9) 0.4466(7) 0.050(3) Uani 1 1 d . . . C12 C 0.5314(13) 0.8995(9) 0.5206(7) 0.054(3) Uani 1 1 d . . . H12 H 0.5759 0.8919 0.5710 0.065 Uiso 1 1 calc R . . C13 C 0.4088(13) 0.9552(11) 0.5176(9) 0.064(3) Uani 1 1 d . . . H13 H 0.3722 0.9840 0.5661 0.076 Uiso 1 1 calc R . . C14 C 0.3462(13) 0.9657(12) 0.4428(10) 0.070(4) Uani 1 1 d . . . H14 H 0.2646 0.9997 0.4410 0.084 Uiso 1 1 calc R . . C15 C 0.4013(13) 0.9267(10) 0.3690(8) 0.057(3) Uani 1 1 d . . . H15 H 0.3595 0.9386 0.3181 0.069 Uiso 1 1 calc R . . C16 C 0.5203(10) 0.8694(10) 0.3720(7) 0.045(3) Uani 1 1 d . . . Cl1 Cl 0.4687(3) 0.5535(2) 0.3804(2) 0.0577(8) Uani 1 1 d . . . O12 O 0.479(2) 0.6020(14) 0.2993(11) 0.156(7) Uani 1 1 d . . . O11 O 0.586(2) 0.5805(19) 0.4177(16) 0.195(10) Uani 1 1 d . . . O13 O 0.373(3) 0.599(2) 0.4219(18) 0.245(14) Uani 1 1 d . . . O14 O 0.4531(19) 0.4445(10) 0.3670(9) 0.128(6) 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 0.0446(3) 0.0494(3) 0.0401(3) 0.0000(2) 0.0015(2) 0.0011(2) N1 0.050(5) 0.050(5) 0.036(4) 0.004(4) -0.003(4) -0.002(4) N2 0.028(4) 0.043(4) 0.045(5) -0.010(4) -0.007(3) -0.002(4) N3 0.050(6) 0.046(6) 0.045(5) 0.005(4) -0.001(4) -0.005(4) C1 0.068(7) 0.042(6) 0.065(7) -0.005(5) -0.002(5) 0.019(7) O1 0.141(12) 0.080(8) 0.116(10) -0.033(7) -0.018(8) 0.027(7) C2 0.060(7) 0.093(10) 0.052(8) 0.010(7) 0.011(6) 0.015(7) O2 0.107(9) 0.146(11) 0.061(6) 0.039(7) 0.023(6) 0.011(8) C3 0.080(9) 0.077(9) 0.040(6) -0.016(7) 0.019(6) 0.009(8) O3 0.032(4) 0.133(9) 0.103(8) -0.007(7) -0.013(5) -0.012(6) C4 0.052(6) 0.035(6) 0.058(6) 0.012(5) -0.004(5) -0.017(5) C5 0.081(8) 0.038(7) 0.066(8) -0.002(6) -0.008(6) -0.010(6) C6 0.111(13) 0.072(11) 0.123(15) 0.000(10) 0.044(12) 0.011(10) C7 0.26(3) 0.062(10) 0.106(15) -0.016(10) -0.106(19) 0.004(14) C8 0.105(12) 0.073(9) 0.083(10) 0.019(8) -0.017(10) -0.022(8) C11 0.063(7) 0.043(6) 0.044(6) 0.007(5) 0.005(5) -0.006(5) C12 0.076(8) 0.047(7) 0.041(6) -0.006(5) 0.008(6) -0.010(6) C13 0.061(8) 0.062(8) 0.067(9) -0.011(6) 0.024(7) -0.004(6) C14 0.057(7) 0.064(8) 0.089(11) -0.009(8) 0.006(7) -0.010(6) C15 0.053(7) 0.057(7) 0.061(7) -0.011(6) -0.006(6) -0.007(6) C16 0.027(5) 0.061(7) 0.046(6) -0.004(5) 0.002(5) -0.010(5) Cl1 0.0621(18) 0.0516(17) 0.0593(18) -0.0098(14) 0.0007(14) -0.0080(14) O12 0.211(18) 0.137(13) 0.120(11) 0.057(10) -0.042(12) -0.040(12) O11 0.152(16) 0.20(2) 0.23(2) -0.049(18) -0.068(16) -0.050(15) O13 0.24(2) 0.20(2) 0.30(3) -0.11(2) 0.16(2) 0.035(18) O14 0.214(18) 0.074(8) 0.095(9) -0.011(7) -0.016(10) -0.021(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 C2 1.940(13) . ? Re1 C3 1.960(16) . ? Re1 C1 1.979(12) . ? Re1 C4 2.121(12) . ? Re1 N2 2.236(8) . ? Re1 N1 2.257(9) . ? N1 C11 1.458(16) . ? N2 C16 1.434(13) . ? N3 C4 1.119(14) . ? N3 C5 1.477(16) . ? C1 O1 1.134(15) . ? C2 O2 1.124(15) . ? C3 O3 1.126(17) . ? C5 C6 1.51(2) . ? C5 C8 1.511(19) . ? C5 C7 1.52(2) . ? C11 C16 1.371(17) . ? C11 C12 1.408(17) . ? C12 C13 1.423(19) . ? C13 C14 1.36(2) . ? C14 C15 1.393(19) . ? C15 C16 1.402(18) . ? Cl1 O13 1.306(17) . ? Cl1 O14 1.373(13) . ? Cl1 O11 1.377(18) . ? Cl1 O12 1.432(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 91.0(5) . . ? C2 Re1 C1 90.2(6) . . ? C3 Re1 C1 90.1(6) . . ? C2 Re1 C4 89.2(6) . . ? C3 Re1 C4 90.5(5) . . ? C1 Re1 C4 179.2(5) . . ? C2 Re1 N2 98.1(5) . . ? C3 Re1 N2 170.4(4) . . ? C1 Re1 N2 93.2(4) . . ? C4 Re1 N2 86.3(4) . . ? C2 Re1 N1 170.4(5) . . ? C3 Re1 N1 96.9(4) . . ? C1 Re1 N1 95.2(5) . . ? C4 Re1 N1 85.3(4) . . ? N2 Re1 N1 73.8(3) . . ? C11 N1 Re1 107.7(6) . . ? C16 N2 Re1 110.2(6) . . ? C4 N3 C5 176.2(12) . . ? O1 C1 Re1 170.3(14) . . ? O2 C2 Re1 176.4(14) . . ? O3 C3 Re1 177.6(13) . . ? N3 C4 Re1 177.4(10) . . ? N3 C5 C6 103.3(12) . . ? N3 C5 C8 106.2(12) . . ? C6 C5 C8 113.1(14) . . ? N3 C5 C7 106.6(12) . . ? C6 C5 C7 113.5(18) . . ? C8 C5 C7 113.1(14) . . ? C16 C11 C12 120.1(12) . . ? C16 C11 N1 118.0(10) . . ? C12 C11 N1 121.9(11) . . ? C11 C12 C13 119.6(12) . . ? C14 C13 C12 118.9(12) . . ? C13 C14 C15 121.6(13) . . ? C14 C15 C16 119.5(12) . . ? C11 C16 C15 120.2(11) . . ? C11 C16 N2 116.6(10) . . ? C15 C16 N2 123.0(10) . . ? O13 Cl1 O14 114.8(15) . . ? O13 Cl1 O11 108.6(17) . . ? O14 Cl1 O11 113.9(13) . . ? O13 Cl1 O12 109.5(18) . . ? O14 Cl1 O12 106.2(10) . . ? O11 Cl1 O12 103.1(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.606 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.169 #===END