# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'En-Qing Gao' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University - Nonius B. V. Demo Lab For X-Ray Diffraction Department of Chemistry Peking University Beijing 100871 People's Republic of China Department of Chemistry Qufu Normal University Qufu 273165, Shandong People's Republic of China ; 'Zhe-Ming Wang' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University - Nonius B. V. Demo Lab For X-Ray Diffraction Department of Chemistry Peking University Beijing 100871 People's Republic of China ; 'Chun-Sheng Liao' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University - Nonius B. V. Demo Lab For X-Ray Diffraction Department of Chemistry Peking University Beijing 100871 People's Republic of China ; 'Chun-Hua Yan' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University - Nonius B. V. Demo Lab For X-Ray Diffraction Department of Chemistry Peking University Beijing 100871 People's Republic of China ; # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_contact_author_address ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University - Nonius B. V. Demo Lab For X-Ray Diffraction Department of Chemistry Peking University Beijing 100871 People's Republic of China ; _publ_contact_author_email chyan@chem.pku.edu.cn _publ_contact_author_phone '86-(10)-62754179' _publ_contact_author_fax '86-(10)-62754179' _publ_requested_journal 'New J. Chem.' _publ_requested_category FO _publ_contact_letter ; ? ; # TITLE AND AUTHOR LIST _publ_section_title ; A novel three-dimensional metal-organic polycatenane and topologic isomerism ; data_1 _database_code_CSD 185726 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Cd N8' _chemical_formula_weight 442.76 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 16.3548(5) _cell_length_b 10.4935(4) _cell_length_c 13.0115(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.0231(19) _cell_angle_gamma 90.00 _cell_volume 1893.23(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8226 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'column' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type ' empirical' _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 graphite _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 16206 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2132 _reflns_number_gt 1255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0334P)^2^+0.9242P] 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 SHELXL _refine_ls_extinction_coef 0.0027(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2132 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Cd1 Cd 0.2500 0.2500 0.0000 0.05122(18) Uani 1 2 d S . . N1 N 0.3179(2) 0.4482(3) 0.0758(3) 0.0595(8) Uani 1 1 d . . . N2 N 0.3198(2) 0.1706(4) 0.1959(3) 0.0745(10) Uani 1 1 d . . . N3 N 0.6147(2) 0.1908(4) 0.5049(3) 0.0716(9) Uani 1 1 d . . . N4 N 0.4477(2) 0.1255(5) 0.4009(3) 0.1032(15) Uani 1 1 d . . . C1 C 0.5000 0.8748(6) 0.2500 0.153(5) Uani 1 2 d S . . H1A H 0.4893 0.9310 0.3000 0.184 Uiso 1 1 d R . . C2 C 0.4089(3) 0.8383(4) 0.1701(6) 0.116(2) Uani 1 1 d . . . H2A H 0.3896 0.8796 0.0938 0.139 Uiso 1 1 calc R . . H2B H 0.3691 0.8743 0.1977 0.139 Uiso 1 1 calc R . . C3 C 0.3811(3) 0.6999(5) 0.1419(5) 0.0797(14) Uani 1 1 d . . . C4 C 0.3350(3) 0.6359(5) 0.1878(4) 0.0883(15) Uani 1 1 d . . . H4A H 0.3241 0.6761 0.2431 0.106 Uiso 1 1 calc R . . C5 C 0.3044(3) 0.5124(5) 0.1532(4) 0.0796(13) Uani 1 1 d . . . H5A H 0.2726 0.4720 0.1859 0.096 Uiso 1 1 calc R . . C6 C 0.3640(3) 0.5103(4) 0.0317(4) 0.0766(12) Uani 1 1 d . . . H6A H 0.3756 0.4677 -0.0220 0.092 Uiso 1 1 calc R . . C7 C 0.3951(3) 0.6337(4) 0.0617(4) 0.0854(14) Uani 1 1 d . . . H7A H 0.4260 0.6729 0.0273 0.102 Uiso 1 1 calc R . . C8 C 0.3828(2) 0.1548(4) 0.2913(3) 0.0556(9) Uani 1 1 d . . . C9 C 0.5364(3) 0.1638(4) 0.4507(3) 0.0583(9) 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 Cd1 0.0349(2) 0.0465(2) 0.0490(2) -0.00179(18) 0.00646(15) -0.00208(19) N1 0.0495(17) 0.0523(19) 0.0613(19) -0.0107(15) 0.0190(16) -0.0075(15) N2 0.0543(19) 0.087(3) 0.054(2) 0.0092(18) 0.0102(17) 0.0000(19) N3 0.0452(18) 0.081(2) 0.070(2) 0.0076(18) 0.0174(17) -0.0075(17) N4 0.052(2) 0.161(4) 0.062(2) 0.036(2) 0.0064(18) -0.023(2) C1 0.078(5) 0.028(4) 0.214(9) 0.000 -0.016(5) 0.000 C2 0.078(3) 0.045(3) 0.171(5) -0.021(3) 0.029(3) 0.001(3) C3 0.051(2) 0.049(2) 0.104(4) -0.016(3) 0.017(2) -0.003(2) C4 0.068(3) 0.079(3) 0.112(4) -0.042(3) 0.043(3) -0.012(3) C5 0.071(3) 0.075(3) 0.096(3) -0.026(3) 0.046(3) -0.019(2) C6 0.086(3) 0.063(3) 0.084(3) -0.016(2) 0.047(3) -0.018(2) C7 0.092(3) 0.057(3) 0.105(3) -0.008(3) 0.051(3) -0.024(2) C8 0.0438(19) 0.059(3) 0.054(2) 0.0010(17) 0.0189(19) -0.0029(17) C9 0.054(2) 0.063(3) 0.049(2) 0.0030(18) 0.0207(18) 0.003(2) _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 Cd1 N1 2.317(3) . ? Cd1 N1 2.317(3) 7 ? Cd1 N2 2.325(3) 7 ? Cd1 N2 2.325(3) . ? Cd1 N3 2.331(3) 8_455 ? Cd1 N3 2.331(3) 2_655 ? N1 C5 1.323(5) . ? N1 C6 1.335(5) . ? N2 C8 1.129(4) . ? N3 C9 1.123(4) . ? N3 Cd1 2.331(3) 2_655 ? N4 C8 1.284(4) . ? N4 C9 1.300(5) . ? C1 C2 1.343(5) . ? C1 C2 1.343(5) 2_655 ? C2 C3 1.509(7) . ? C3 C4 1.361(7) . ? C3 C7 1.370(7) . ? C4 C5 1.376(6) . ? C6 C7 1.370(6) . ? 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 Cd1 N1 180.0 . 7 ? N1 Cd1 N2 89.50(12) . 7 ? N1 Cd1 N2 90.50(12) 7 7 ? N1 Cd1 N2 90.50(12) . . ? N1 Cd1 N2 89.50(12) 7 . ? N2 Cd1 N2 180.0(2) 7 . ? N1 Cd1 N3 89.78(12) . 8_455 ? N1 Cd1 N3 90.22(12) 7 8_455 ? N2 Cd1 N3 90.73(12) 7 8_455 ? N2 Cd1 N3 89.27(12) . 8_455 ? N1 Cd1 N3 90.22(12) . 2_655 ? N1 Cd1 N3 89.78(12) 7 2_655 ? N2 Cd1 N3 89.27(12) 7 2_655 ? N2 Cd1 N3 90.73(12) . 2_655 ? N3 Cd1 N3 180.00(14) 8_455 2_655 ? C5 N1 C6 116.0(4) . . ? C5 N1 Cd1 123.1(3) . . ? C6 N1 Cd1 120.5(3) . . ? C8 N2 Cd1 152.9(3) . . ? C9 N3 Cd1 146.5(3) . 2_655 ? C8 N4 C9 121.7(4) . . ? C2 C1 C2 146.9(6) . 2_655 ? C1 C2 C3 122.0(5) . . ? C4 C3 C7 116.1(4) . . ? C4 C3 C2 122.3(5) . . ? C7 C3 C2 121.5(5) . . ? C3 C4 C5 120.7(5) . . ? N1 C5 C4 123.4(4) . . ? N1 C6 C7 123.3(4) . . ? C6 C7 C3 120.6(5) . . ? N2 C8 N4 172.5(4) . . ? N3 C9 N4 172.5(4) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.510 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.071 #===END data_2 _database_code_CSD 185727 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Cd N8' _chemical_formula_weight 442.76 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 13.2140(2) _cell_length_b 21.7332(4) _cell_length_c 28.7125(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8245.7(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20254 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 graphite _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 36198 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2346 _reflns_number_gt 1692 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0925P)^2^+10.3993P] 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 SHELXL _refine_ls_extinction_coef 0.00037(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2346 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Cd1 Cd 0.3750 0.3750 0.074184(15) 0.0630(2) Uani 1 2 d S . . N1 N 0.4278(3) 0.30524(15) 0.13099(12) 0.0636(8) Uani 1 1 d . . . N2 N 0.2166(3) 0.32710(19) 0.07226(15) 0.0817(10) Uani 1 1 d . . . N3 N 0.0693(4) 0.1942(2) -0.01741(18) 0.1041(15) Uani 1 1 d . . . N4 N 0.0766(5) 0.2833(4) 0.0309(4) 0.186(4) Uani 1 1 d . . . C1 C 0.6250 0.1250 0.1895(2) 0.0797(18) Uani 1 2 d S . . H1A H 0.6713 0.1471 0.1699 0.096 Uiso 1 1 d R . . C2 C 0.5660(4) 0.1709(2) 0.22038(15) 0.0777(12) Uani 1 1 d . . . H2A H 0.5154 0.1490 0.2384 0.093 Uiso 1 1 calc R . . H2B H 0.6121 0.1908 0.2419 0.093 Uiso 1 1 calc R . . C3 C 0.5157(3) 0.21834(18) 0.19075(15) 0.0660(10) Uani 1 1 d . . . C4 C 0.5584(3) 0.2749(2) 0.18328(15) 0.0736(11) Uani 1 1 d . . . H4A H 0.6189 0.2851 0.1980 0.088 Uiso 1 1 calc R . . C5 C 0.5131(3) 0.31660(19) 0.15442(14) 0.0684(10) Uani 1 1 d . . . H5A H 0.5433 0.3550 0.1509 0.082 Uiso 1 1 calc R . . C6 C 0.3851(4) 0.2510(2) 0.1383(2) 0.0852(15) Uani 1 1 d . . . H6A H 0.3248 0.2419 0.1231 0.102 Uiso 1 1 calc R . . C7 C 0.4266(4) 0.2072(2) 0.1678(2) 0.0920(15) Uani 1 1 d . . . H7A H 0.3937 0.1698 0.1721 0.110 Uiso 1 1 calc R . . C8 C 0.0805(4) 0.2346(3) 0.0057(2) 0.0941(16) Uani 1 1 d . . . C9 C 0.1561(4) 0.3030(2) 0.0527(2) 0.0881(15) 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 Cd1 0.0660(3) 0.0506(3) 0.0723(4) 0.000 0.000 -0.00096(15) N1 0.0633(19) 0.0502(17) 0.077(2) 0.0016(14) 0.0025(15) 0.0000(14) N2 0.074(2) 0.072(2) 0.099(3) -0.0094(19) -0.005(2) -0.0038(19) N3 0.098(3) 0.108(3) 0.106(3) -0.044(3) 0.000(3) -0.003(3) N4 0.090(4) 0.181(6) 0.287(10) -0.143(7) -0.042(5) 0.024(4) C1 0.098(5) 0.079(4) 0.062(4) 0.000 0.000 0.027(3) C2 0.093(3) 0.071(2) 0.069(3) 0.002(2) 0.009(2) 0.024(2) C3 0.067(2) 0.060(2) 0.071(2) -0.0017(18) 0.0122(18) 0.0147(17) C4 0.071(2) 0.078(3) 0.071(3) 0.003(2) 0.0011(19) 0.002(2) C5 0.076(2) 0.062(2) 0.067(3) 0.0021(18) -0.0014(19) -0.0116(18) C6 0.075(3) 0.054(2) 0.127(4) 0.017(3) -0.020(3) -0.0103(19) C7 0.094(3) 0.052(2) 0.131(4) 0.018(2) -0.014(3) -0.008(2) C8 0.064(3) 0.107(4) 0.110(4) -0.042(3) -0.008(3) 0.005(3) C9 0.058(2) 0.087(3) 0.120(4) -0.040(3) -0.003(3) 0.006(2) _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 Cd1 N1 2.333(3) 2 ? Cd1 N1 2.333(3) . ? Cd1 N3 2.337(4) 29 ? Cd1 N3 2.337(4) 18_665 ? Cd1 N2 2.339(4) 2 ? Cd1 N2 2.339(4) . ? N1 C6 1.324(5) . ? N1 C5 1.336(5) . ? N2 C9 1.109(6) . ? N3 C8 1.110(6) . ? N3 Cd1 2.337(4) 29 ? N4 C8 1.283(7) . ? N4 C9 1.295(8) . ? C1 C2 1.546(6) 14_545 ? C1 C2 1.546(6) . ? C2 C3 1.492(6) . ? C3 C7 1.370(7) . ? C3 C4 1.371(6) . ? C4 C5 1.366(6) . ? C6 C7 1.388(7) . ? 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 Cd1 N1 91.31(16) 2 . ? N1 Cd1 N3 179.01(14) 2 29 ? N1 Cd1 N3 88.58(17) . 29 ? N1 Cd1 N3 88.58(17) 2 18_665 ? N1 Cd1 N3 179.01(14) . 18_665 ? N3 Cd1 N3 91.5(3) 29 18_665 ? N1 Cd1 N2 89.70(13) 2 2 ? N1 Cd1 N2 92.19(13) . 2 ? N3 Cd1 N2 89.33(16) 29 2 ? N3 Cd1 N2 88.79(16) 18_665 2 ? N1 Cd1 N2 92.19(13) 2 . ? N1 Cd1 N2 89.70(13) . . ? N3 Cd1 N2 88.79(16) 29 . ? N3 Cd1 N2 89.33(16) 18_665 . ? N2 Cd1 N2 177.3(2) 2 . ? C6 N1 C5 116.4(4) . . ? C6 N1 Cd1 124.2(3) . . ? C5 N1 Cd1 118.9(3) . . ? C9 N2 Cd1 150.2(4) . . ? C8 N3 Cd1 152.2(5) . 29 ? C8 N4 C9 120.8(6) . . ? C2 C1 C2 110.1(5) 14_545 . ? C3 C2 C1 110.1(4) . . ? C7 C3 C4 116.0(4) . . ? C7 C3 C2 122.3(4) . . ? C4 C3 C2 121.7(4) . . ? C5 C4 C3 120.6(4) . . ? N1 C5 C4 123.6(4) . . ? N1 C6 C7 122.6(4) . . ? C3 C7 C6 120.8(4) . . ? N3 C8 N4 169.7(6) . . ? N2 C9 N4 170.2(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.884 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.091 #===END