Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' #================================================================= # 2. PROCESSING SUMMARY _journal_coden_Cambridge 0222 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Xiao-Ming Chen School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone 86-20-84113986 _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to Dalton. Oct 25, 2004 ; _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Homochiral crystallisation of helical coordination chains bridged by achiral ligands: can it be controlled by the ligand structure? ; loop_ _publ_author_name _publ_author_address 'Yong-Tao Wang' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Ming-Liang Tong' ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'Hai-Hua Fan' ; State Key Laboratory of Optoelcetronic Matrials and Technologies Sun Yat-Sen University Guangzhou 510275 P. R. China ; 'He-Zhou Wang' ; State Key Laboratory of Optoelcetronic Matrials and Technologies Sun Yat-Sen University Guangzhou 510275 P. R. China ; ; Xiao-Ming Chen ; ; School of Chemistry and Chemical Engineering State Key Laboratory of Optoelcetronic Matrials and Technologies Sun Yat-Sen University Guangzhou, 510275 P. R. China ; _publ_contact_author_name 'Xiao-Ming Chen' #====================================== data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 253093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Cd I2 N4 O' _chemical_formula_weight 590.42 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' Cd Cd -0.8075 1.2024 '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' _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 33.006(7) _cell_length_b 7.4118(15) _cell_length_c 13.816(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.460(3) _cell_angle_gamma 90.00 _cell_volume 3145.5(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 5.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1984 _exptl_absorpt_correction_T_max 0.7770 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 '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 12286 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.35 _reflns_number_total 3607 _reflns_number_gt 3173 _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^)+(0.0393P)^2^+13.5123P] 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_number_reflns 3607 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Cd1 Cd 0.123559(11) 0.55405(5) 0.25282(3) 0.04135(11) Uani 1 1 d . . . O1 O 0.15628(10) 0.8698(4) 0.0184(2) 0.0392(7) Uani 1 1 d . . . I1 I 0.078210(15) 0.66466(7) 0.37022(4) 0.07393(16) Uani 1 1 d . . . I2 I 0.128215(14) 0.20183(5) 0.19803(3) 0.06913(16) Uani 1 1 d . . . C1 C 0.02871(17) 0.6836(9) 0.0688(5) 0.0574(14) Uani 1 1 d . . . H1A H 0.0171 0.6292 0.1137 0.069 Uiso 1 1 calc R . . C2 C 0.00091(18) 0.7551(10) -0.0236(5) 0.0648(15) Uani 1 1 d . . . H2A H -0.0290 0.7488 -0.0404 0.078 Uiso 1 1 calc R . . C3 C 0.0170(2) 0.8349(10) -0.0904(5) 0.0685(17) Uani 1 1 d . . . H3A H -0.0017 0.8821 -0.1532 0.082 Uiso 1 1 calc R . . C4 C 0.06208(18) 0.8452(8) -0.0635(4) 0.0541(13) Uani 1 1 d . . . H4A H 0.0742 0.8993 -0.1072 0.065 Uiso 1 1 calc R . . C5 C 0.08754(15) 0.7724(6) 0.0300(4) 0.0417(10) Uani 1 1 d . . . C6 C 0.13486(15) 0.7840(6) 0.0711(4) 0.0399(10) Uani 1 1 d . . . C7 C 0.19836(14) 0.8623(6) 0.0862(3) 0.0372(9) Uani 1 1 d . . . C8 C 0.23192(15) 0.9431(6) 0.0550(4) 0.0372(9) Uani 1 1 d . . . C9 C 0.22427(16) 0.9911(7) -0.0466(4) 0.0439(10) Uani 1 1 d . . . H9A H 0.1969 0.9758 -0.0982 0.053 Uiso 1 1 calc R . . C11 C 0.29835(16) 1.0853(7) 0.0088(4) 0.0438(10) Uani 1 1 d . . . H11A H 0.3211 1.1337 -0.0075 0.053 Uiso 1 1 calc R . . C10 C 0.25827(17) 1.0627(7) -0.0696(4) 0.0449(11) Uani 1 1 d . . . H10A H 0.2542 1.0954 -0.1375 0.054 Uiso 1 1 calc R . . C12 C 0.27276(15) 0.9690(7) 0.1299(4) 0.0414(10) Uani 1 1 d . . . H12A H 0.2776 0.9361 0.1982 0.050 Uiso 1 1 calc R . . N1 N 0.07204(13) 0.6904(6) 0.0957(3) 0.0456(9) Uani 1 1 d . . . N2 N 0.16049(12) 0.7270(5) 0.1601(3) 0.0400(8) Uani 1 1 d . . . N3 N 0.20259(12) 0.7777(6) 0.1709(3) 0.0411(8) Uani 1 1 d . . . N4 N 0.30573(12) 1.0398(5) 0.1079(3) 0.0412(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 0.03674(18) 0.04354(19) 0.0439(2) -0.00192(14) 0.01493(14) 0.00336(13) O1 0.0334(15) 0.0440(17) 0.0363(16) 0.0006(14) 0.0082(13) -0.0018(13) I1 0.0680(3) 0.0940(3) 0.0744(3) -0.0047(2) 0.0434(2) 0.0166(2) I2 0.0718(3) 0.0476(2) 0.0603(3) -0.01492(16) -0.00868(19) 0.01545(17) C1 0.037(3) 0.072(4) 0.064(3) 0.000(3) 0.019(2) -0.002(2) C2 0.034(3) 0.081(4) 0.073(4) 0.001(3) 0.011(3) 0.000(3) C3 0.045(3) 0.089(4) 0.057(4) 0.006(3) 0.001(3) 0.007(3) C4 0.043(3) 0.063(3) 0.052(3) 0.003(3) 0.013(2) 0.000(2) C5 0.039(2) 0.039(2) 0.045(3) -0.002(2) 0.013(2) 0.0000(18) C6 0.041(2) 0.039(2) 0.039(2) -0.0044(19) 0.0141(19) -0.0021(18) C7 0.031(2) 0.038(2) 0.037(2) -0.0056(18) 0.0058(17) 0.0011(17) C8 0.036(2) 0.037(2) 0.037(2) -0.0031(18) 0.0117(18) 0.0020(17) C9 0.045(3) 0.047(2) 0.034(2) -0.003(2) 0.008(2) 0.002(2) C11 0.045(3) 0.048(2) 0.040(2) 0.005(2) 0.017(2) 0.004(2) C10 0.056(3) 0.048(3) 0.031(2) 0.003(2) 0.016(2) 0.006(2) C12 0.039(2) 0.049(3) 0.035(2) 0.003(2) 0.0130(19) 0.001(2) N1 0.034(2) 0.052(2) 0.048(2) 0.0000(18) 0.0107(17) 0.0015(17) N2 0.0350(19) 0.045(2) 0.038(2) 0.0025(17) 0.0105(16) 0.0006(16) N3 0.0342(19) 0.050(2) 0.038(2) 0.0019(17) 0.0112(16) -0.0016(16) N4 0.0345(19) 0.050(2) 0.039(2) 0.0045(17) 0.0126(16) 0.0009(16) _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 N4 2.424(4) 4_545 ? Cd1 N2 2.432(4) . ? Cd1 N1 2.434(4) . ? Cd1 I1 2.7055(6) . ? Cd1 I2 2.7380(7) . ? O1 C6 1.346(6) . ? O1 C7 1.363(5) . ? C1 N1 1.341(6) . ? C1 C2 1.377(9) . ? C2 C3 1.357(10) . ? C3 C4 1.396(8) . ? C4 C5 1.368(7) . ? C5 N1 1.340(6) . ? C5 C6 1.456(7) . ? C6 N2 1.282(6) . ? C7 N3 1.289(6) . ? C7 C8 1.456(7) . ? C8 C9 1.379(7) . ? C8 C12 1.380(7) . ? C9 C10 1.380(7) . ? C11 N4 1.343(6) . ? C11 C10 1.380(7) . ? C12 N4 1.339(6) . ? N2 N3 1.394(5) . ? N4 Cd1 2.424(4) 4 ? 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 N4 Cd1 N2 85.32(13) 4_545 . ? N4 Cd1 N1 151.84(14) 4_545 . ? N2 Cd1 N1 68.43(13) . . ? N4 Cd1 I1 96.93(9) 4_545 . ? N2 Cd1 I1 130.55(10) . . ? N1 Cd1 I1 92.85(10) . . ? N4 Cd1 I2 92.45(10) 4_545 . ? N2 Cd1 I2 105.50(10) . . ? N1 Cd1 I2 103.94(10) . . ? I1 Cd1 I2 123.64(2) . . ? C6 O1 C7 102.4(4) . . ? N1 C1 C2 121.6(6) . . ? C3 C2 C1 120.3(5) . . ? C2 C3 C4 119.1(6) . . ? C5 C4 C3 117.2(6) . . ? N1 C5 C4 124.3(5) . . ? N1 C5 C6 112.5(4) . . ? C4 C5 C6 123.1(5) . . ? N2 C6 O1 112.4(4) . . ? N2 C6 C5 126.3(4) . . ? O1 C6 C5 121.2(4) . . ? N3 C7 O1 112.8(4) . . ? N3 C7 C8 128.8(4) . . ? O1 C7 C8 118.3(4) . . ? C9 C8 C12 119.5(4) . . ? C9 C8 C7 122.1(4) . . ? C12 C8 C7 118.4(4) . . ? C8 C9 C10 118.2(4) . . ? N4 C11 C10 122.3(5) . . ? C9 C10 C11 119.5(4) . . ? N4 C12 C8 122.4(4) . . ? C5 N1 C1 117.6(5) . . ? C5 N1 Cd1 118.5(3) . . ? C1 N1 Cd1 123.9(4) . . ? C6 N2 N3 107.2(4) . . ? C6 N2 Cd1 113.4(3) . . ? N3 N2 Cd1 139.3(3) . . ? C7 N3 N2 105.1(4) . . ? C12 N4 C11 118.1(4) . . ? C12 N4 Cd1 117.6(3) . 4 ? C11 N4 Cd1 124.1(3) . 4 ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.157 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.133 #=======================================END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 253094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Cd I2 N4 O' _chemical_formula_weight 590.42 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.057(7) _cell_length_b 14.116(14) _cell_length_c 8.743(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.356(19) _cell_angle_gamma 90.00 _cell_volume 805.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 5.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5432 _exptl_absorpt_correction_T_max 0.6581 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 '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 1597 _diffrn_reflns_av_R_equivalents 0.0071 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 24.73 _reflns_number_total 1595 _reflns_number_gt 1548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0488P)^2^+4.5649P] 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 -0.03(6) _refine_ls_number_reflns 1595 _refine_ls_number_parameters 181 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.046 _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 -0.04970(12) -0.30239(6) -0.49138(11) 0.0376(2) Uani 1 1 d . . . O1 O -0.2289(11) -0.0352(6) -0.3190(10) 0.037(2) Uani 1 1 d . . . N1 N -0.2786(14) -0.1792(9) -0.6659(13) 0.037(2) Uani 1 1 d . . . N2 N -0.1077(14) -0.1769(9) -0.3275(13) 0.040(3) Uani 1 1 d . . . N3 N -0.0440(16) -0.1516(9) -0.1633(14) 0.045(3) Uani 1 1 d . . . N4 N -0.0159(16) 0.1022(9) 0.2508(13) 0.044(3) Uani 1 1 d . . . C1 C -0.3646(19) -0.1829(12) -0.8301(18) 0.051(4) Uani 1 1 d . . . H1A H -0.3482 -0.2369 -0.8846 0.061 Uiso 1 1 calc R . . C2 C -0.476(2) -0.1089(14) -0.9204(17) 0.054(4) Uani 1 1 d . . . H2A H -0.5340 -0.1134 -1.0351 0.065 Uiso 1 1 calc R . . C3 C -0.505(2) -0.0288(12) -0.8455(18) 0.051(4) Uani 1 1 d . . . H3A H -0.5798 0.0218 -0.9073 0.062 Uiso 1 1 calc R . . C4 C -0.4182(18) -0.0249(11) -0.6735(18) 0.047(4) Uani 1 1 d . . . H4A H -0.4342 0.0279 -0.6158 0.056 Uiso 1 1 calc R . . C5 C -0.3078(15) -0.1029(10) -0.5930(15) 0.033(3) Uani 1 1 d . . . C6 C -0.2138(15) -0.1059(9) -0.4157(15) 0.033(3) Uani 1 1 d . . . C7 C -0.1152(18) -0.0686(10) -0.1643(16) 0.039(3) Uani 1 1 d . . . C8 C -0.0868(16) -0.0082(10) -0.0212(15) 0.035(3) Uani 1 1 d . . . C9 C -0.1559(18) 0.0831(9) -0.0369(17) 0.040(3) Uani 1 1 d . . . H9A H -0.2262 0.1091 -0.1409 0.048 Uiso 1 1 calc R . . C10 C -0.120(2) 0.1359(11) 0.1031(16) 0.046(3) Uani 1 1 d . . . H10A H -0.1715 0.1972 0.0927 0.055 Uiso 1 1 calc R . . C11 C 0.0510(16) 0.0133(11) 0.2698(17) 0.039(3) Uani 1 1 d . . . H11A H 0.1210 -0.0105 0.3756 0.047 Uiso 1 1 calc R . . C12 C 0.0178(18) -0.0442(11) 0.1343(17) 0.043(3) Uani 1 1 d . . . H12A H 0.0655 -0.1062 0.1481 0.051 Uiso 1 1 calc R . . I1 I 0.32604(16) -0.24887(10) -0.4783(2) 0.0833(5) Uani 1 1 d . . . I2 I -0.25835(13) -0.43986(7) -0.71361(12) 0.0543(3) 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 0.0399(4) 0.0395(6) 0.0334(5) -0.0006(4) 0.0140(3) -0.0032(4) O1 0.032(4) 0.038(6) 0.039(5) -0.004(4) 0.011(4) 0.006(3) N1 0.035(4) 0.042(7) 0.030(6) 0.003(5) 0.009(4) -0.002(5) N2 0.038(5) 0.050(8) 0.029(6) -0.006(5) 0.010(4) 0.006(5) N3 0.047(6) 0.043(8) 0.042(7) -0.001(5) 0.014(5) 0.006(5) N4 0.052(6) 0.044(8) 0.032(6) -0.007(5) 0.012(5) 0.002(5) C1 0.048(7) 0.059(11) 0.042(9) -0.011(7) 0.013(6) -0.004(7) C2 0.046(7) 0.076(12) 0.033(8) 0.012(8) 0.005(6) -0.007(7) C3 0.048(7) 0.059(11) 0.045(9) 0.018(7) 0.015(6) 0.004(6) C4 0.039(6) 0.053(10) 0.052(9) -0.004(7) 0.021(6) 0.000(6) C5 0.026(5) 0.037(8) 0.038(7) 0.000(6) 0.015(5) -0.007(5) C6 0.026(5) 0.034(8) 0.042(7) 0.012(6) 0.016(5) 0.007(5) C7 0.040(6) 0.040(9) 0.035(7) 0.010(6) 0.011(5) 0.007(6) C8 0.033(5) 0.040(9) 0.036(7) -0.004(6) 0.017(5) -0.007(5) C9 0.048(6) 0.021(7) 0.042(7) 0.001(5) 0.006(6) -0.006(5) C10 0.062(7) 0.035(9) 0.035(8) 0.002(6) 0.011(6) 0.011(6) C11 0.033(5) 0.049(10) 0.036(7) -0.006(6) 0.014(5) -0.006(6) C12 0.037(6) 0.049(10) 0.044(8) 0.004(6) 0.016(6) 0.010(6) I1 0.0552(5) 0.0685(9) 0.1408(12) 0.0134(8) 0.0538(7) -0.0092(5) I2 0.0551(5) 0.0552(7) 0.0427(5) -0.0131(5) 0.0076(4) -0.0012(5) _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 N4 2.390(11) 2_545 ? Cd1 N2 2.409(11) . ? Cd1 N1 2.467(11) . ? Cd1 I1 2.717(3) . ? Cd1 I2 2.744(2) . ? O1 C6 1.338(15) . ? O1 C7 1.368(15) . ? N1 C5 1.307(18) . ? N1 C1 1.330(18) . ? N2 C6 1.311(16) . ? N2 N3 1.379(15) . ? N3 C7 1.273(19) . ? N4 C10 1.308(17) . ? N4 C11 1.329(19) . ? N4 Cd1 2.390(11) 2 ? C1 C2 1.36(2) . ? C2 C3 1.36(2) . ? C3 C4 1.39(2) . ? C4 C5 1.38(2) . ? C5 C6 1.436(17) . ? C7 C8 1.463(19) . ? C8 C9 1.366(19) . ? C8 C12 1.374(18) . ? C9 C10 1.371(19) . ? C11 C12 1.379(19) . ? 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 N4 Cd1 N2 84.9(4) 2_545 . ? N4 Cd1 N1 143.5(4) 2_545 . ? N2 Cd1 N1 68.3(4) . . ? N4 Cd1 I1 105.1(3) 2_545 . ? N2 Cd1 I1 98.9(3) . . ? N1 Cd1 I1 103.2(2) . . ? N4 Cd1 I2 95.6(3) 2_545 . ? N2 Cd1 I2 140.7(2) . . ? N1 Cd1 I2 90.7(3) . . ? I1 Cd1 I2 118.60(6) . . ? C6 O1 C7 102.2(10) . . ? C5 N1 C1 117.8(12) . . ? C5 N1 Cd1 117.8(8) . . ? C1 N1 Cd1 124.3(10) . . ? C6 N2 N3 107.5(11) . . ? C6 N2 Cd1 113.6(8) . . ? N3 N2 Cd1 138.4(8) . . ? C7 N3 N2 105.1(11) . . ? C10 N4 C11 120.4(13) . . ? C10 N4 Cd1 120.8(10) . 2 ? C11 N4 Cd1 118.8(9) . 2 ? N1 C1 C2 121.4(15) . . ? C3 C2 C1 121.1(14) . . ? C2 C3 C4 118.0(14) . . ? C5 C4 C3 116.8(13) . . ? N1 C5 C4 125.0(12) . . ? N1 C5 C6 114.1(12) . . ? C4 C5 C6 120.9(12) . . ? N2 C6 O1 111.3(10) . . ? N2 C6 C5 125.7(12) . . ? O1 C6 C5 123.0(11) . . ? N3 C7 O1 113.9(12) . . ? N3 C7 C8 127.2(12) . . ? O1 C7 C8 118.9(12) . . ? C9 C8 C12 119.0(13) . . ? C9 C8 C7 122.4(12) . . ? C12 C8 C7 118.6(13) . . ? C8 C9 C10 119.1(12) . . ? N4 C10 C9 121.8(14) . . ? N4 C11 C12 120.8(13) . . ? C8 C12 C11 119.0(14) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.837 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.129 #=======================================END data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 253095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cd I2 N6 O4' _chemical_formula_weight 754.63 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' Cd Cd -0.8075 1.2024 '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' _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 8.2949(9) _cell_length_b 14.7244(17) _cell_length_c 21.236(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2593.8(5) _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 plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 3.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.8286 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 '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 15753 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5995 _reflns_number_gt 5294 _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^)+(0.0425P)^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 0.02(3) _refine_ls_number_reflns 5995 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Cd1 Cd -0.51908(5) -1.07063(3) -0.20036(2) 0.03143(12) Uani 1 1 d . . . I1 I -0.32408(5) -0.93918(3) -0.14425(2) 0.04007(13) Uani 1 1 d . . . I2 I -0.39586(6) -1.11140(3) -0.32386(2) 0.04409(13) Uani 1 1 d . . . N1 N -0.3892(6) -1.2066(3) -0.1595(2) 0.0263(11) Uani 1 1 d . . . N2 N -0.6937(6) -1.2055(3) -0.2136(3) 0.0317(12) Uani 1 1 d . . . N3 N -0.8447(6) -1.2295(3) -0.2362(3) 0.0360(13) Uani 1 1 d . . . N4 N -1.2607(6) -1.4777(3) -0.2714(3) 0.0311(12) Uani 1 1 d . . . N5 N -0.6198(10) -0.8157(5) 0.0286(4) 0.065(2) Uani 1 1 d . . . N6 N -0.6813(7) -0.3885(4) -0.0193(3) 0.0429(14) Uani 1 1 d . . . O1 O -0.7275(5) -1.3516(3) -0.1964(2) 0.0292(10) Uani 1 1 d . . . O1W O -0.6673(7) -1.0842(3) -0.1003(3) 0.0597(16) Uani 1 1 d . . . H1WA H -0.7254 -1.1307 -0.0933 0.072 Uiso 1 1 d R . . H1WB H -0.6604 -1.0425 -0.0728 0.072 Uiso 1 1 d R . . O2 O -0.6802(9) -0.9600(5) 0.0001(4) 0.083(2) Uani 1 1 d . . . O3 O -0.7791(7) -0.2547(4) -0.0562(3) 0.0538(15) Uani 1 1 d . . . C1 C -0.2424(8) -1.2081(5) -0.1350(4) 0.0387(16) Uani 1 1 d . . . H1A H -0.1839 -1.1542 -0.1344 0.046 Uiso 1 1 calc R . . C2 C -0.1713(9) -1.2851(5) -0.1103(3) 0.0413(16) Uani 1 1 d . . . H2A H -0.0689 -1.2828 -0.0925 0.050 Uiso 1 1 calc R . . C3 C -0.2565(8) -1.3655(5) -0.1129(4) 0.0385(16) Uani 1 1 d . . . H3A H -0.2123 -1.4186 -0.0967 0.046 Uiso 1 1 calc R . . C4 C -0.4083(8) -1.3661(4) -0.1398(3) 0.0318(14) Uani 1 1 d . . . H4A H -0.4682 -1.4194 -0.1423 0.038 Uiso 1 1 calc R . . C5 C -0.4680(7) -1.2852(4) -0.1628(3) 0.0253(13) Uani 1 1 d . . . C6 C -0.6284(7) -1.2784(4) -0.1910(3) 0.0252(13) Uani 1 1 d . . . C7 C -0.8602(7) -1.3152(4) -0.2256(3) 0.0265(13) Uani 1 1 d . . . C8 C -0.9953(7) -1.3727(4) -0.2409(3) 0.0274(13) Uani 1 1 d . . . C9 C -1.0005(8) -1.4633(4) -0.2253(3) 0.0341(15) Uani 1 1 d . . . H9A H -0.9149 -1.4904 -0.2041 0.041 Uiso 1 1 calc R . . C10 C -1.1345(8) -1.5131(4) -0.2416(3) 0.0376(16) Uani 1 1 d . . . H10A H -1.1369 -1.5745 -0.2313 0.045 Uiso 1 1 calc R . . C11 C -1.2558(8) -1.3902(5) -0.2869(3) 0.0346(15) Uani 1 1 d . . . H11A H -1.3430 -1.3653 -0.3084 0.041 Uiso 1 1 calc R . . C12 C -1.1274(8) -1.3352(4) -0.2726(3) 0.0333(15) Uani 1 1 d . . . H12A H -1.1282 -1.2741 -0.2837 0.040 Uiso 1 1 calc R . . C13 C -0.580(2) -0.7225(8) 0.0108(8) 0.148(7) Uani 1 1 d . . . H13A H -0.5660 -0.7191 -0.0340 0.222 Uiso 1 1 calc R . . H13B H -0.4816 -0.7045 0.0312 0.222 Uiso 1 1 calc R . . H13C H -0.6654 -0.6826 0.0234 0.222 Uiso 1 1 calc R . . C14 C -0.643(2) -0.8323(9) 0.0934(5) 0.115(5) Uani 1 1 d . . . H14A H -0.6691 -0.8951 0.0997 0.173 Uiso 1 1 calc R . . H14B H -0.7297 -0.7951 0.1086 0.173 Uiso 1 1 calc R . . H14C H -0.5460 -0.8178 0.1159 0.173 Uiso 1 1 calc R . . C15 C -0.6430(12) -0.8823(7) -0.0118(5) 0.069(3) Uani 1 1 d . . . H16A H -0.6293 -0.8681 -0.0542 0.083 Uiso 1 1 calc R . . C16 C -0.5457(9) -0.4367(7) 0.0064(4) 0.065(3) Uani 1 1 d . . . H17A H -0.4584 -0.3950 0.0134 0.097 Uiso 1 1 calc R . . H17B H -0.5121 -0.4829 -0.0226 0.097 Uiso 1 1 calc R . . H17C H -0.5760 -0.4642 0.0456 0.097 Uiso 1 1 calc R . . C17 C -0.8290(10) -0.4392(6) -0.0332(5) 0.064(2) Uani 1 1 d . . . H18A H -0.9091 -0.3985 -0.0496 0.097 Uiso 1 1 calc R . . H18B H -0.8685 -0.4668 0.0047 0.097 Uiso 1 1 calc R . . H18C H -0.8063 -0.4855 -0.0638 0.097 Uiso 1 1 calc R . . C18 C -0.6739(10) -0.3001(5) -0.0327(3) 0.0435(18) Uani 1 1 d . . . H20A H -0.5781 -0.2704 -0.0229 0.052 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 Cd1 0.0270(2) 0.02259(19) 0.0447(3) 0.0029(2) -0.0055(2) -0.00067(18) I1 0.0388(2) 0.0388(2) 0.0426(3) -0.0012(2) -0.0041(2) -0.0109(2) I2 0.0515(3) 0.0370(2) 0.0438(3) -0.0013(2) 0.0019(2) 0.0017(2) N1 0.024(2) 0.023(2) 0.032(3) -0.002(2) -0.005(2) -0.002(2) N2 0.024(2) 0.021(2) 0.050(4) -0.002(2) -0.005(3) -0.008(2) N3 0.029(3) 0.024(2) 0.055(4) 0.003(3) -0.010(3) -0.002(2) N4 0.031(3) 0.024(3) 0.039(3) -0.004(2) -0.006(3) -0.011(2) N5 0.086(5) 0.049(4) 0.061(5) -0.008(4) 0.011(4) -0.005(4) N6 0.036(3) 0.054(3) 0.038(3) 0.002(3) 0.006(3) -0.002(3) O1 0.028(2) 0.0214(19) 0.038(3) -0.002(2) -0.0059(19) -0.0022(16) O1W 0.084(4) 0.038(3) 0.057(4) -0.012(3) 0.032(3) -0.018(3) O2 0.094(5) 0.065(4) 0.090(5) -0.026(4) 0.029(4) -0.017(4) O3 0.054(3) 0.045(3) 0.062(4) 0.007(3) 0.006(3) 0.005(3) C1 0.036(4) 0.036(4) 0.044(4) -0.009(3) -0.004(3) -0.002(3) C2 0.036(4) 0.049(4) 0.039(4) -0.006(4) -0.005(3) 0.006(3) C3 0.039(4) 0.035(4) 0.042(4) 0.001(3) -0.006(3) 0.007(3) C4 0.033(3) 0.023(3) 0.040(4) 0.002(3) 0.002(3) 0.004(3) C5 0.026(3) 0.023(3) 0.027(3) -0.007(2) 0.003(2) -0.004(2) C6 0.027(3) 0.018(2) 0.030(3) -0.002(2) 0.000(3) -0.007(2) C7 0.020(3) 0.023(3) 0.037(3) -0.002(3) -0.005(3) 0.000(2) C8 0.024(3) 0.024(3) 0.035(4) -0.001(3) 0.002(3) -0.005(2) C9 0.032(3) 0.023(3) 0.047(4) -0.001(3) -0.011(3) 0.003(3) C10 0.044(4) 0.021(3) 0.048(4) -0.003(3) -0.007(3) -0.001(3) C11 0.031(3) 0.031(3) 0.041(4) 0.002(3) -0.006(3) -0.005(3) C12 0.036(4) 0.026(3) 0.038(4) 0.006(3) -0.006(3) -0.004(3) C13 0.211(18) 0.083(9) 0.149(14) -0.005(10) 0.074(14) -0.030(11) C14 0.196(16) 0.085(8) 0.065(8) -0.013(7) 0.004(10) -0.021(9) C15 0.077(7) 0.076(7) 0.053(6) -0.010(5) 0.023(5) 0.017(6) C16 0.049(4) 0.079(6) 0.068(6) 0.030(6) 0.005(4) 0.018(5) C17 0.063(5) 0.051(5) 0.080(7) 0.020(5) 0.008(5) -0.004(5) C18 0.046(4) 0.046(4) 0.038(4) -0.014(4) 0.012(4) -0.015(4) _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 N4 2.360(5) 3_354 ? Cd1 N1 2.434(5) . ? Cd1 O1W 2.463(5) . ? Cd1 N2 2.474(5) . ? Cd1 I1 2.7897(7) . ? Cd1 I2 2.8781(8) . ? N1 C1 1.324(8) . ? N1 C5 1.331(7) . ? N2 C6 1.295(7) . ? N2 N3 1.387(7) . ? N3 C7 1.288(8) . ? N4 C10 1.330(8) . ? N4 C11 1.331(8) . ? N4 Cd1 2.360(5) 3_344 ? N5 C15 1.318(12) . ? N5 C14 1.409(13) . ? N5 C13 1.462(13) . ? N6 C18 1.333(9) . ? N6 C16 1.438(9) . ? N6 C17 1.465(10) . ? O1 C6 1.360(6) . ? O1 C7 1.372(7) . ? O2 C15 1.211(11) . ? O3 C18 1.207(9) . ? C1 C2 1.382(10) . ? C2 C3 1.379(10) . ? C3 C4 1.383(10) . ? C4 C5 1.380(8) . ? C5 C6 1.462(8) . ? C7 C8 1.441(8) . ? C8 C9 1.375(8) . ? C8 C12 1.399(9) . ? C9 C10 1.377(9) . ? C11 C12 1.372(9) . ? 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 N4 Cd1 N1 155.54(18) 3_354 . ? N4 Cd1 O1W 83.1(2) 3_354 . ? N1 Cd1 O1W 81.15(18) . . ? N4 Cd1 N2 89.03(18) 3_354 . ? N1 Cd1 N2 68.87(17) . . ? O1W Cd1 N2 74.96(18) . . ? N4 Cd1 I1 98.93(13) 3_354 . ? N1 Cd1 I1 99.30(11) . . ? O1W Cd1 I1 88.70(13) . . ? N2 Cd1 I1 160.89(14) . . ? N4 Cd1 I2 99.46(14) 3_354 . ? N1 Cd1 I2 89.79(12) . . ? O1W Cd1 I2 161.16(12) . . ? N2 Cd1 I2 86.39(14) . . ? I1 Cd1 I2 109.15(2) . . ? C1 N1 C5 117.3(5) . . ? C1 N1 Cd1 124.1(4) . . ? C5 N1 Cd1 118.6(4) . . ? C6 N2 N3 107.1(5) . . ? C6 N2 Cd1 112.3(4) . . ? N3 N2 Cd1 140.6(4) . . ? C7 N3 N2 106.2(5) . . ? C10 N4 C11 118.3(6) . . ? C10 N4 Cd1 120.2(4) . 3_344 ? C11 N4 Cd1 121.5(5) . 3_344 ? C15 N5 C14 119.2(9) . . ? C15 N5 C13 124.2(10) . . ? C14 N5 C13 116.5(10) . . ? C18 N6 C16 121.8(7) . . ? C18 N6 C17 119.6(7) . . ? C16 N6 C17 118.6(7) . . ? C6 O1 C7 102.3(4) . . ? N1 C1 C2 123.7(6) . . ? C3 C2 C1 118.0(7) . . ? C2 C3 C4 119.3(6) . . ? C5 C4 C3 117.9(6) . . ? N1 C5 C4 123.7(6) . . ? N1 C5 C6 114.2(5) . . ? C4 C5 C6 122.1(5) . . ? N2 C6 O1 111.9(5) . . ? N2 C6 C5 126.1(5) . . ? O1 C6 C5 122.0(5) . . ? N3 C7 O1 112.4(5) . . ? N3 C7 C8 127.8(6) . . ? O1 C7 C8 119.8(5) . . ? C9 C8 C12 118.3(6) . . ? C9 C8 C7 122.6(6) . . ? C12 C8 C7 119.1(5) . . ? C8 C9 C10 118.8(6) . . ? N4 C10 C9 123.1(6) . . ? N4 C11 C12 122.6(6) . . ? C11 C12 C8 118.8(6) . . ? O2 C15 N5 127.1(10) . . ? O3 C18 N6 126.5(7) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.159 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.155 #End of Crystallographic Information File