# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Daofeng Sun' _publ_contact_author_email DFSUN@SDU.EDU.CN _publ_section_title ; 1D zigzag chain vs 1D helical chain: the role of the supramolecular interactions in the formation of chiral architecture ; loop_ _publ_author_name 'Daofeng Sun' 'Fangna Dai' 'Haiyan He' 'Yanxiong Ke' 'Guoqing Zhang' ; Xiaoliang Zhao ; # Attachment '1.cif' data_test _database_code_depnum_ccdc_archive 'CCDC 737145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H8 Cd I3 N5 O4' _chemical_formula_weight 803.35 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.701(2) _cell_length_b 24.227(5) _cell_length_c 9.861(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.821(4) _cell_angle_gamma 90.00 _cell_volume 2151.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2866 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 5.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6169 _exptl_absorpt_correction_T_max 0.6169 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _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 12343 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.59 _reflns_number_total 4889 _reflns_number_gt 3274 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1488P)^2^+62.8777P] 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 4889 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.1076 _refine_ls_wR_factor_ref 0.3150 _refine_ls_wR_factor_gt 0.2895 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Cd Cd 0.33707(13) 0.09021(5) 0.17989(15) 0.0437(4) Uani 1 1 d . . . C1 C 0.6170(19) 0.1358(8) 0.2600(19) 0.046(4) Uani 1 1 d . . . C2 C 0.7665(18) 0.1624(8) 0.3197(17) 0.042(4) Uani 1 1 d . . . C3 C 0.7836(16) 0.2127(7) 0.385(2) 0.044(4) Uani 1 1 d . . . C4 C 0.9191(19) 0.2405(8) 0.443(2) 0.049(4) Uani 1 1 d . . . C5 C 1.0412(17) 0.2119(7) 0.423(2) 0.043(4) Uani 1 1 d . . . C6 C 1.0266(19) 0.1628(7) 0.3637(19) 0.042(4) Uani 1 1 d . . . C7 C 1.1592(17) 0.1324(7) 0.3418(17) 0.035(3) Uani 1 1 d . . . C8 C 0.889(2) 0.1360(7) 0.310(2) 0.045(4) Uani 1 1 d . . . C9 C 0.367(3) -0.0440(12) 0.185(3) 0.087(8) Uani 1 1 d . . . H9 H 0.3720 -0.0443 0.0923 0.104 Uiso 1 1 calc R . . C10 C 0.379(4) -0.0872(12) 0.262(4) 0.097(9) Uani 1 1 d . . . H10 H 0.3947 -0.1231 0.2384 0.116 Uiso 1 1 calc R . . C11 C 0.331(3) -0.0128(10) 0.368(3) 0.070(6) Uani 1 1 d . . . H11 H 0.3039 0.0103 0.4294 0.084 Uiso 1 1 calc R . . C12 C 0.288(3) 0.0986(10) -0.160(2) 0.067(6) Uani 1 1 d . . . H12 H 0.3903 0.1026 -0.1331 0.081 Uiso 1 1 calc R . . C13 C 0.080(2) 0.0871(11) -0.142(3) 0.073(7) Uani 1 1 d . . . H13 H 0.0070 0.0790 -0.1049 0.088 Uiso 1 1 calc R . . C14 C 0.054(3) 0.0986(14) -0.288(3) 0.089(9) Uani 1 1 d . . . H14 H -0.0376 0.1036 -0.3635 0.107 Uiso 1 1 calc R . . O1 O 0.5314(18) 0.1433(8) 0.1298(19) 0.088(6) Uani 1 1 d . . . O2 O 0.5729(15) 0.1088(7) 0.3428(16) 0.064(4) Uani 1 1 d . . . O3 O 1.1701(14) 0.1398(5) 0.2233(14) 0.049(3) Uani 1 1 d . . . O4 O 1.2448(17) 0.1051(7) 0.4440(19) 0.072(4) Uani 1 1 d . . . I1 I 0.60308(16) 0.25146(7) 0.4143(2) 0.0768(6) Uani 1 1 d . . . I2 I 1.25165(15) 0.25033(7) 0.5061(2) 0.0775(6) Uani 1 1 d . . . I3 I 0.8710(2) 0.05510(7) 0.2271(3) 0.0951(7) Uani 1 1 d . . . N1 N 0.9357(17) 0.2898(8) 0.513(2) 0.068(5) Uani 1 1 d . . . N2 N 0.3459(19) 0.0020(7) 0.251(2) 0.056(4) Uani 1 1 d . . . N3 N 0.362(3) -0.0691(9) 0.392(3) 0.090(7) Uani 1 1 d . . . N4 N 0.2189(18) 0.0894(7) -0.0674(18) 0.056(4) Uani 1 1 d . . . N5 N 0.191(3) 0.1011(9) -0.295(2) 0.083(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 Cd 0.0273(6) 0.0521(7) 0.0559(8) -0.0008(6) 0.0204(5) 0.0001(5) C1 0.030(8) 0.064(11) 0.040(9) -0.002(8) 0.007(7) 0.001(8) C2 0.028(8) 0.069(11) 0.030(8) 0.005(8) 0.014(6) -0.003(7) C3 0.015(7) 0.057(10) 0.064(11) 0.005(9) 0.020(7) 0.010(6) C4 0.026(8) 0.053(10) 0.072(13) -0.012(9) 0.021(8) -0.002(7) C5 0.022(7) 0.051(10) 0.057(10) -0.011(8) 0.015(7) -0.008(6) C6 0.036(8) 0.051(10) 0.043(9) 0.001(8) 0.021(7) -0.003(7) C7 0.029(7) 0.043(8) 0.041(9) 0.000(7) 0.023(7) 0.000(6) C8 0.046(10) 0.047(9) 0.052(10) -0.003(8) 0.029(8) 0.005(7) C9 0.09(2) 0.09(2) 0.074(17) 0.000(15) 0.020(15) 0.004(15) C10 0.13(3) 0.062(15) 0.10(2) 0.008(15) 0.05(2) 0.017(16) C11 0.069(15) 0.073(15) 0.074(15) -0.007(12) 0.035(12) -0.020(11) C12 0.068(14) 0.088(16) 0.047(11) 0.017(11) 0.022(10) 0.011(12) C13 0.043(11) 0.093(17) 0.090(17) -0.006(14) 0.033(11) -0.019(11) C14 0.043(12) 0.17(3) 0.054(13) -0.021(16) 0.015(10) -0.025(15) O1 0.055(9) 0.121(15) 0.073(11) 0.029(10) 0.008(8) -0.035(10) O2 0.043(7) 0.088(10) 0.063(9) 0.017(8) 0.022(7) -0.021(7) O3 0.040(7) 0.067(8) 0.053(7) 0.004(6) 0.033(6) 0.010(6) O4 0.060(9) 0.084(10) 0.093(11) 0.031(9) 0.052(9) 0.031(8) I1 0.0340(7) 0.0969(12) 0.1108(14) -0.0134(9) 0.0400(8) 0.0109(6) I2 0.0299(7) 0.0886(11) 0.1206(14) -0.0390(9) 0.0358(8) -0.0175(6) I3 0.0805(12) 0.0649(10) 0.160(2) -0.0450(11) 0.0682(13) -0.0235(8) N1 0.035(8) 0.080(12) 0.103(14) -0.049(11) 0.043(9) -0.015(8) N2 0.051(10) 0.054(9) 0.069(11) -0.002(8) 0.031(8) -0.007(7) N3 0.100(18) 0.070(13) 0.13(2) 0.010(13) 0.080(17) 0.006(12) N4 0.041(8) 0.078(11) 0.056(9) -0.008(8) 0.027(7) 0.001(8) N5 0.101(17) 0.102(16) 0.061(12) -0.008(11) 0.049(12) -0.020(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 Cd O3 2.182(11) 1_455 ? Cd N2 2.240(17) . ? Cd N4 2.277(17) . ? Cd O2 2.299(14) . ? Cd O1 2.480(15) . ? C1 O2 1.24(2) . ? C1 O1 1.26(2) . ? C1 C2 1.49(2) . ? C2 C3 1.36(3) . ? C2 C8 1.38(2) . ? C3 C4 1.40(2) . ? C3 I1 2.098(14) . ? C4 N1 1.36(2) . ? C4 C5 1.45(2) . ? C5 C6 1.31(2) . ? C5 I2 2.112(15) . ? C6 C8 1.40(2) . ? C6 C7 1.56(2) . ? C7 O3 1.225(19) . ? C7 O4 1.23(2) . ? C8 I3 2.107(17) . ? C9 C10 1.28(4) . ? C9 N2 1.35(3) . ? C9 H9 0.9300 . ? C10 N3 1.41(4) . ? C10 H10 0.9300 . ? C11 N2 1.27(3) . ? C11 N3 1.40(3) . ? C11 H11 0.9300 . ? C12 N5 1.32(3) . ? C12 N4 1.34(3) . ? C12 H12 0.9300 . ? C13 N4 1.28(3) . ? C13 C14 1.39(4) . ? C13 H13 0.9300 . ? C14 N5 1.36(3) . ? C14 H14 0.9300 . ? O3 Cd 2.182(11) 1_655 ? 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 O3 Cd N2 114.1(5) 1_455 . ? O3 Cd N4 95.7(5) 1_455 . ? N2 Cd N4 105.8(7) . . ? O3 Cd O2 111.9(6) 1_455 . ? N2 Cd O2 93.2(6) . . ? N4 Cd O2 136.4(5) . . ? O3 Cd O1 115.3(6) 1_455 . ? N2 Cd O1 127.9(6) . . ? N4 Cd O1 84.7(6) . . ? O2 Cd O1 53.5(5) . . ? O2 C1 O1 119.4(17) . . ? O2 C1 C2 119.3(15) . . ? O1 C1 C2 121.1(17) . . ? C3 C2 C8 119.4(15) . . ? C3 C2 C1 120.2(15) . . ? C8 C2 C1 120.5(17) . . ? C2 C3 C4 123.9(14) . . ? C2 C3 I1 120.3(11) . . ? C4 C3 I1 115.8(13) . . ? N1 C4 C3 123.3(15) . . ? N1 C4 C5 122.8(15) . . ? C3 C4 C5 113.9(15) . . ? C6 C5 C4 122.5(15) . . ? C6 C5 I2 120.2(12) . . ? C4 C5 I2 117.2(12) . . ? C5 C6 C8 121.2(16) . . ? C5 C6 C7 122.0(15) . . ? C8 C6 C7 116.7(15) . . ? O3 C7 O4 125.9(15) . . ? O3 C7 C6 115.5(14) . . ? O4 C7 C6 118.5(14) . . ? C2 C8 C6 119.0(16) . . ? C2 C8 I3 120.6(14) . . ? C6 C8 I3 120.4(12) . . ? C10 C9 N2 113(3) . . ? C10 C9 H9 123.7 . . ? N2 C9 H9 123.7 . . ? C9 C10 N3 106(3) . . ? C9 C10 H10 127.1 . . ? N3 C10 H10 127.1 . . ? N2 C11 N3 110(2) . . ? N2 C11 H11 125.2 . . ? N3 C11 H11 125.2 . . ? N5 C12 N4 110(2) . . ? N5 C12 H12 125.0 . . ? N4 C12 H12 125.0 . . ? N4 C13 C14 110(2) . . ? N4 C13 H13 125.2 . . ? C14 C13 H13 125.2 . . ? N5 C14 C13 105(2) . . ? N5 C14 H14 127.6 . . ? C13 C14 H14 127.6 . . ? C1 O1 Cd 89.0(11) . . ? C1 O2 Cd 98.1(11) . . ? C7 O3 Cd 116.2(11) . 1_655 ? C11 N2 C9 107(2) . . ? C11 N2 Cd 123.5(16) . . ? C9 N2 Cd 129.2(17) . . ? C11 N3 C10 104(2) . . ? C13 N4 C12 108(2) . . ? C13 N4 Cd 128.5(15) . . ? C12 N4 Cd 123.3(14) . . ? C12 N5 C14 107(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.690 _refine_diff_density_min -2.618 _refine_diff_density_rms 0.327 # Attachment '2.cif' data_e _database_code_depnum_ccdc_archive 'CCDC 737146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cd I3 N3 O5' _chemical_formula_weight 795.37 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 tetragonal _symmetry_space_group_name_H-M P43212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 11.3689(3) _cell_length_b 11.3689(3) _cell_length_c 16.5658(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2141.16(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4101 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 22.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 5.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4996 _exptl_absorpt_correction_T_max 0.6156 _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 ? _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 14175 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 26.38 _reflns_number_total 2194 _reflns_number_gt 1796 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+4.5691P] 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 0.01(7) _refine_ls_number_reflns 2194 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Cd Cd 0.63502(6) 0.63502(6) 0.5000 0.0627(3) Uani 1 2 d S . . I2 I 0.53163(5) 0.46837(5) 0.2500 0.0826(3) Uani 1 2 d S . . I1 I 0.28595(6) 0.87126(7) 0.41591(4) 0.0800(2) Uani 1 1 d . . . N1 N 0.1397(6) 0.8603(6) 0.2500 0.074(3) Uani 1 2 d S . . C1 C 0.4756(9) 0.6655(8) 0.3850(6) 0.065(2) Uani 1 1 d . . . C2 C 0.3901(7) 0.6763(7) 0.3150(5) 0.055(2) Uani 1 1 d . . . C3 C 0.3029(7) 0.7606(7) 0.3151(5) 0.056(2) Uani 1 1 d . . . C4 C 0.2252(6) 0.7748(6) 0.2500 0.055(3) Uani 1 2 d S . . C5 C 0.4012(6) 0.5988(6) 0.2500 0.054(3) Uani 1 2 d S . . O1 O 0.5683(6) 0.7187(8) 0.3802(4) 0.086(2) Uani 1 1 d . . . N3 N 0.6121(10) 0.8692(8) 0.6633(6) 0.094(3) Uani 1 1 d . . . C6 C 0.7163(12) 0.8493(13) 0.6260(9) 0.106(5) Uani 1 1 d . . . C7 C 0.5126(12) 0.8258(14) 0.6136(13) 0.155(9) Uani 1 1 d . . . H7A H 0.4399 0.8412 0.6411 0.232 Uiso 1 1 calc R . . H7B H 0.5209 0.7427 0.6052 0.232 Uiso 1 1 calc R . . H7C H 0.5126 0.8654 0.5625 0.232 Uiso 1 1 calc R . . C8 C 0.6007(17) 0.9223(16) 0.7429(11) 0.147(7) Uani 1 1 d . . . H8A H 0.6409 0.8745 0.7819 0.220 Uiso 1 1 calc R . . H8B H 0.5190 0.9277 0.7570 0.220 Uiso 1 1 calc R . . H8C H 0.6347 0.9995 0.7423 0.220 Uiso 1 1 calc R . . O3B O 0.7164(14) 0.8022(11) 0.5508(8) 0.074(4) Uani 0.50 1 d P . . O2A O 0.4498(16) 0.5845(16) 0.4321(11) 0.054(5) Uiso 0.40 1 d P . . O2B O 0.4470(12) 0.6115(11) 0.4500(7) 0.061(4) Uiso 0.60 1 d P . . 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 Cd 0.0664(4) 0.0664(4) 0.0551(4) -0.0034(3) 0.0034(3) -0.0023(5) I2 0.0688(4) 0.0688(4) 0.1102(7) 0.0247(4) 0.0247(4) 0.0331(4) I1 0.0785(5) 0.0831(5) 0.0783(4) -0.0106(4) -0.0031(4) 0.0264(4) N1 0.062(4) 0.062(4) 0.099(8) -0.011(5) -0.011(5) 0.033(6) C1 0.068(6) 0.062(6) 0.065(5) 0.023(4) 0.011(4) 0.013(5) C2 0.047(5) 0.051(4) 0.068(5) 0.026(4) 0.019(4) 0.009(3) C3 0.051(5) 0.048(4) 0.068(5) 0.011(4) 0.012(4) 0.008(3) C4 0.050(4) 0.050(4) 0.063(6) 0.013(4) 0.013(4) 0.017(5) C5 0.048(4) 0.048(4) 0.067(7) 0.017(4) 0.017(4) 0.012(5) O1 0.050(4) 0.109(6) 0.099(5) 0.035(5) 0.006(4) -0.016(4) N3 0.113(8) 0.076(6) 0.093(6) 0.010(6) 0.020(6) -0.001(6) C6 0.089(8) 0.111(10) 0.116(10) 0.036(8) 0.042(8) 0.033(7) C7 0.077(8) 0.115(11) 0.27(2) 0.107(13) -0.086(11) -0.039(8) C8 0.159(15) 0.144(14) 0.137(13) -0.072(11) 0.037(12) -0.052(12) O3B 0.105(11) 0.054(7) 0.061(7) -0.008(6) 0.007(7) 0.001(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 Cd O3B 2.276(13) 7_556 ? Cd O3B 2.276(13) . ? Cd O2B 2.308(13) . ? Cd O2B 2.308(13) 7_556 ? Cd O1 2.328(7) 7_556 ? Cd O1 2.328(7) . ? Cd O2A 2.456(18) . ? Cd O2A 2.456(18) 7_556 ? Cd C1 2.653(10) . ? Cd C1 2.653(10) 7_556 ? I2 C5 2.097(10) . ? I1 C3 2.100(9) . ? N1 C4 1.375(14) . ? C1 O1 1.217(12) . ? C1 O2A 1.242(19) . ? C1 O2B 1.281(14) . ? C1 C2 1.517(13) . ? C2 C3 1.379(11) . ? C2 C5 1.397(11) . ? C3 C4 1.403(10) . ? C4 C3 1.403(10) 8_665 ? C5 C2 1.397(11) 8_665 ? N3 C6 1.355(15) . ? N3 C8 1.456(17) . ? N3 C7 1.483(17) . ? C6 O3B 1.355(18) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 O3B Cd O3B 57.2(7) 7_556 . ? O3B Cd O2B 133.4(4) 7_556 . ? O3B Cd O2B 127.3(5) . . ? O3B Cd O2B 127.3(5) 7_556 7_556 ? O3B Cd O2B 133.4(4) . 7_556 ? O2B Cd O2B 85.1(6) . 7_556 ? O3B Cd O1 96.1(4) 7_556 7_556 ? O3B Cd O1 77.9(4) . 7_556 ? O2B Cd O1 130.3(4) . 7_556 ? O2B Cd O1 55.9(3) 7_556 7_556 ? O3B Cd O1 77.9(4) 7_556 . ? O3B Cd O1 96.1(4) . . ? O2B Cd O1 55.9(3) . . ? O2B Cd O1 130.3(4) 7_556 . ? O1 Cd O1 173.3(4) 7_556 . ? O3B Cd O2A 129.9(5) 7_556 . ? O3B Cd O2A 135.5(6) . . ? O2B Cd O2A 9.7(5) . . ? O2B Cd O2A 81.3(4) 7_556 . ? O1 Cd O2A 131.7(5) 7_556 . ? O1 Cd O2A 54.9(4) . . ? O3B Cd O2A 135.5(6) 7_556 7_556 ? O3B Cd O2A 129.9(5) . 7_556 ? O2B Cd O2A 81.3(4) . 7_556 ? O2B Cd O2A 9.7(5) 7_556 7_556 ? O1 Cd O2A 54.9(4) 7_556 7_556 ? O1 Cd O2A 131.7(5) . 7_556 ? O2A Cd O2A 79.0(8) . 7_556 ? O3B Cd C1 104.6(4) 7_556 . ? O3B Cd C1 115.8(4) . . ? O2B Cd C1 28.9(4) . . ? O2B Cd C1 107.5(4) 7_556 . ? O1 Cd C1 159.1(3) 7_556 . ? O1 Cd C1 27.3(3) . . ? O2A Cd C1 27.8(5) . . ? O2A Cd C1 106.3(4) 7_556 . ? O3B Cd C1 115.8(4) 7_556 7_556 ? O3B Cd C1 104.6(4) . 7_556 ? O2B Cd C1 107.5(4) . 7_556 ? O2B Cd C1 28.9(4) 7_556 7_556 ? O1 Cd C1 27.3(3) 7_556 7_556 ? O1 Cd C1 159.1(3) . 7_556 ? O2A Cd C1 106.3(4) . 7_556 ? O2A Cd C1 27.8(5) 7_556 7_556 ? C1 Cd C1 134.0(4) . 7_556 ? O1 C1 O2A 127.8(12) . . ? O1 C1 O2B 120.8(10) . . ? O2A C1 O2B 19.5(10) . . ? O1 C1 C2 117.7(8) . . ? O2A C1 C2 112.9(12) . . ? O2B C1 C2 121.2(10) . . ? O1 C1 Cd 61.3(5) . . ? O2A C1 Cd 67.2(9) . . ? O2B C1 Cd 60.5(7) . . ? C2 C1 Cd 175.4(6) . . ? C3 C2 C5 120.2(8) . . ? C3 C2 C1 121.1(8) . . ? C5 C2 C1 118.7(7) . . ? C2 C3 C4 122.2(8) . . ? C2 C3 I1 118.9(7) . . ? C4 C3 I1 119.0(6) . . ? N1 C4 C3 121.8(5) . . ? N1 C4 C3 121.8(5) . 8_665 ? C3 C4 C3 116.4(10) . 8_665 ? C2 C5 C2 118.7(10) . 8_665 ? C2 C5 I2 120.6(5) . . ? C2 C5 I2 120.6(5) 8_665 . ? C1 O1 Cd 91.4(6) . . ? C6 N3 C8 124.0(14) . . ? C6 N3 C7 111.0(13) . . ? C8 N3 C7 124.9(14) . . ? O3B C6 N3 119.1(15) . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 O3B Cd 132.1(10) . . ? C1 O2A Cd 84.9(10) . . ? C1 O2B Cd 90.7(8) . . ? 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 O3B Cd C1 O1 -12.8(8) 7_556 . . . ? O3B Cd C1 O1 47.4(8) . . . . ? O2B Cd C1 O1 168.7(12) . . . . ? O2B Cd C1 O1 -150.4(7) 7_556 . . . ? O1 Cd C1 O1 175.2(3) 7_556 . . . ? O2A Cd C1 O1 -170.9(13) . . . . ? O2A Cd C1 O1 -160.4(7) 7_556 . . . ? C1 Cd C1 O1 -163.9(7) 7_556 . . . ? O3B Cd C1 O2A 158.2(11) 7_556 . . . ? O3B Cd C1 O2A -141.6(10) . . . . ? O2B Cd C1 O2A -20.4(11) . . . . ? O2B Cd C1 O2A 20.6(11) 7_556 . . . ? O1 Cd C1 O2A -13.9(14) 7_556 . . . ? O1 Cd C1 O2A 170.9(13) . . . . ? O2A Cd C1 O2A 10.5(14) 7_556 . . . ? C1 Cd C1 O2A 7.1(10) 7_556 . . . ? O3B Cd C1 O2B 178.5(9) 7_556 . . . ? O3B Cd C1 O2B -121.3(8) . . . . ? O2B Cd C1 O2B 40.9(11) 7_556 . . . ? O1 Cd C1 O2B 6.5(13) 7_556 . . . ? O1 Cd C1 O2B -168.7(12) . . . . ? O2A Cd C1 O2B 20.4(11) . . . . ? O2A Cd C1 O2B 30.9(9) 7_556 . . . ? C1 Cd C1 O2B 27.4(8) 7_556 . . . ? O3B Cd C1 C2 66(8) 7_556 . . . ? O3B Cd C1 C2 126(8) . . . . ? O2B Cd C1 C2 -113(8) . . . . ? O2B Cd C1 C2 -72(8) 7_556 . . . ? O1 Cd C1 C2 -106(8) 7_556 . . . ? O1 Cd C1 C2 79(8) . . . . ? O2A Cd C1 C2 -92(8) . . . . ? O2A Cd C1 C2 -82(8) 7_556 . . . ? C1 Cd C1 C2 -85(8) 7_556 . . . ? O1 C1 C2 C3 -92.8(11) . . . . ? O2A C1 C2 C3 100.6(13) . . . . ? O2B C1 C2 C3 80.8(13) . . . . ? Cd C1 C2 C3 -169(8) . . . . ? O1 C1 C2 C5 87.2(10) . . . . ? O2A C1 C2 C5 -79.4(13) . . . . ? O2B C1 C2 C5 -99.2(11) . . . . ? Cd C1 C2 C5 11(8) . . . . ? C5 C2 C3 C4 -2.1(11) . . . . ? C1 C2 C3 C4 177.9(7) . . . . ? C5 C2 C3 I1 177.9(4) . . . . ? C1 C2 C3 I1 -2.1(10) . . . . ? C2 C3 C4 N1 -178.9(6) . . . . ? I1 C3 C4 N1 1.1(6) . . . . ? C2 C3 C4 C3 1.1(6) . . . 8_665 ? I1 C3 C4 C3 -178.9(6) . . . 8_665 ? C3 C2 C5 C2 1.0(5) . . . 8_665 ? C1 C2 C5 C2 -179.0(8) . . . 8_665 ? C3 C2 C5 I2 -179.0(5) . . . . ? C1 C2 C5 I2 1.0(8) . . . . ? O2A C1 O1 Cd -10.6(16) . . . . ? O2B C1 O1 Cd 11.5(12) . . . . ? C2 C1 O1 Cd -174.9(7) . . . . ? O3B Cd O1 C1 167.4(8) 7_556 . . . ? O3B Cd O1 C1 -138.2(7) . . . . ? O2B Cd O1 C1 -6.6(7) . . . . ? O2B Cd O1 C1 38.2(8) 7_556 . . . ? O1 Cd O1 C1 -165.2(6) 7_556 . . . ? O2A Cd O1 C1 5.2(8) . . . . ? O2A Cd O1 C1 25.5(9) 7_556 . . . ? C1 Cd O1 C1 34.1(14) 7_556 . . . ? C8 N3 C6 O3B -178.3(14) . . . . ? C7 N3 C6 O3B 3.8(16) . . . . ? N3 C6 O3B Cd -54.9(19) . . . . ? O3B Cd O3B C6 -151(2) 7_556 . . . ? O2B Cd O3B C6 86.9(15) . . . . ? O2B Cd O3B C6 -38.1(18) 7_556 . . . ? O1 Cd O3B C6 -45.0(14) 7_556 . . . ? O1 Cd O3B C6 138.1(15) . . . . ? O2A Cd O3B C6 93.8(16) . . . . ? O2A Cd O3B C6 -26.0(18) 7_556 . . . ? C1 Cd O3B C6 118.2(14) . . . . ? C1 Cd O3B C6 -39.1(15) 7_556 . . . ? O1 C1 O2A Cd 10.1(15) . . . . ? O2B C1 O2A Cd -65(4) . . . . ? C2 C1 O2A Cd 175.0(7) . . . . ? O3B Cd O2A C1 -28.0(14) 7_556 . . . ? O3B Cd O2A C1 53.0(13) . . . . ? O2B Cd O2A C1 87(4) . . . . ? O2B Cd O2A C1 -160.2(10) 7_556 . . . ? O1 Cd O2A C1 173.4(7) 7_556 . . . ? O1 Cd O2A C1 -5.1(7) . . . . ? O2A Cd O2A C1 -169.7(14) 7_556 . . . ? C1 Cd O2A C1 -174.7(7) 7_556 . . . ? O1 C1 O2B Cd -11.6(12) . . . . ? O2A C1 O2B Cd 106(4) . . . . ? C2 C1 O2B Cd 175.1(8) . . . . ? O3B Cd O2B C1 -2.0(12) 7_556 . . . ? O3B Cd O2B C1 75.5(9) . . . . ? O2B Cd O2B C1 -141.1(10) 7_556 . . . ? O1 Cd O2B C1 -177.0(6) 7_556 . . . ? O1 Cd O2B C1 6.2(6) . . . . ? O2A Cd O2B C1 -75(4) . . . . ? O2A Cd O2B C1 -150.1(9) 7_556 . . . ? C1 Cd O2B C1 -159.7(6) 7_556 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.017 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.114