# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jie-Hui Yu' _publ_contact_author_email jiehuiyu@yahoo.com.c _publ_author_name 'Yu Hui' data_1 _database_code_depnum_ccdc_archive 'CCDC 790449' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H58 Br8 Cd3 N10 O13 S4' _chemical_formula_weight 1727.46 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 27.198(5) _cell_length_b 13.261(3) _cell_length_c 13.222(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4768.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description strip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 8.265 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.438 _exptl_absorpt_process_details ; Higashi, T.(1995).Program for Absorption Correction. Rigaku Corporation, Tokyo,Japan. ; _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40872 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5685 _reflns_number_gt 4582 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _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^)+(0.0528P)^2^+23.8430P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5685 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _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 0.36319(2) 0.2500 -0.23786(5) 0.02995(16) Uani 1 2 d S . . Cd2 Cd 0.37150(8) 0.2500 0.1500(6) 0.0213(6) Uani 0.86(2) 2 d SP . . Cd2' Cd 0.3761(4) 0.2500 0.190(3) 0.017(4) Uani 0.14(2) 2 d SP . . Cd3 Cd 0.40117(2) -0.2500 0.25349(4) 0.02201(14) Uani 1 2 d S . . Br1 Br 0.38271(4) 0.2500 -0.44125(8) 0.0414(2) Uani 1 2 d S . . Br2 Br 0.26660(3) 0.2500 -0.22949(6) 0.02845(19) Uani 1 2 d S . . Br3 Br 0.40575(16) 0.2500 -0.04009(12) 0.0347(7) Uani 0.830(14) 2 d SP . . Br3' Br 0.3791(11) 0.2500 -0.0202(11) 0.052(5) Uani 0.170(14) 2 d SP . . Br4 Br 0.27559(4) 0.2500 0.08054(8) 0.0340(3) Uani 0.881(3) 2 d SP . . Br4' Br 0.2870(4) 0.2500 0.2522(8) 0.061(3) Uani 0.119(3) 2 d SP . . Br5 Br 0.46168(4) 0.2500 0.24572(7) 0.0392(2) Uani 1 2 d S . . Br6 Br 0.49933(3) -0.2500 0.25076(7) 0.0322(2) Uani 1 2 d S . . Br7 Br 0.36649(3) -0.2500 0.07216(6) 0.02732(18) Uani 1 2 d S . . Br8 Br 0.36963(3) -0.2500 0.43688(6) 0.02939(19) Uani 1 2 d S . . S1 S 0.37190(4) 0.00361(9) 0.25186(9) 0.0143(2) Uani 1 1 d . . . S2 S 0.38378(8) -0.12353(14) -0.24906(17) 0.0532(5) Uani 1 1 d . . . N1 N 0.22292(16) 0.0645(3) 0.9396(3) 0.0228(10) Uani 1 1 d . . . H1A H 0.2020 0.0750 0.8879 0.080 Uiso 1 1 calc . . . H1BA H 0.2346 0.1247 0.9596 0.080 Uiso 1 1 calc . . . N2 N 0.27248(16) -0.0713(3) 1.0757(3) 0.0235(10) Uani 1 1 d . . . H2A H 0.2936 -0.0807 1.1272 0.080 Uiso 1 1 calc . . . H2BA H 0.2613 -0.1323 1.0564 0.080 Uiso 1 1 calc . . . N3 N 0.47251(17) -0.0652(4) 1.0666(3) 0.0247(10) Uani 1 1 d . . . H3A H 0.4811 -0.1269 1.0445 0.080 Uiso 1 1 calc . . . H3B H 0.4514 -0.0730 1.1184 0.080 Uiso 1 1 calc . . . N4 N 0.46561(16) 0.0645(4) 0.4482(3) 0.0246(10) Uani 1 1 d . . . H4A H 0.4393 0.0721 0.4076 0.080 Uiso 1 1 calc . . . H4B H 0.4759 0.1263 0.4667 0.080 Uiso 1 1 calc . . . N5 N 0.3761(2) 0.0835(4) -0.2326(4) 0.0402(14) Uani 1 1 d . . . O1 O 0.37073(14) 0.0722(3) 0.1644(3) 0.0245(8) Uani 1 1 d . . . O2 O 0.41433(13) -0.0658(3) 0.2412(3) 0.0227(8) Uani 1 1 d . . . O3 O 0.37687(13) 0.0604(3) 0.3480(3) 0.0219(8) Uani 1 1 d . . . O4 O 0.32610(13) -0.0562(3) 0.2549(3) 0.0240(8) Uani 1 1 d . . . OW1 O 0.3387(2) 0.2500 0.3113(5) 0.0354(14) Uani 1 2 d S . . OW2 O 0.2678(3) 0.2500 0.4932(6) 0.0497(19) Uani 1 2 d S . . OW3 O 0.5137(4) 0.2500 0.4998(9) 0.094(4) Uani 1 2 d S . . OW4 O 0.2254(3) 0.2500 0.3101(8) 0.102(4) Uani 1 2 d S . . OW5 O 0.4717(3) -0.2500 0.9527(7) 0.060(2) Uani 1 2 d S . . C1 C 0.1958(2) 0.0156(5) 1.0257(4) 0.0277(12) Uani 1 1 d . . . H1B H 0.1802 -0.0457 1.0020 0.033 Uiso 1 1 calc R . . H1C H 0.1703 0.0608 1.0495 0.033 Uiso 1 1 calc R . . C2 C 0.2300(2) -0.0091(4) 1.1118(4) 0.0245(12) Uani 1 1 d . . . H2B H 0.2422 0.0529 1.1417 0.029 Uiso 1 1 calc R . . H2C H 0.2122 -0.0459 1.1635 0.029 Uiso 1 1 calc R . . C3 C 0.2642(2) 0.0003(5) 0.9050(4) 0.0274(13) Uani 1 1 d . . . H3C H 0.2819 0.0349 0.8514 0.033 Uiso 1 1 calc R . . H3D H 0.2512 -0.0619 0.8772 0.033 Uiso 1 1 calc R . . C4 C 0.2993(2) -0.0241(5) 0.9893(4) 0.0278(12) Uani 1 1 d . . . H4C H 0.3244 -0.0701 0.9649 0.033 Uiso 1 1 calc R . . H4D H 0.3154 0.0371 1.0119 0.033 Uiso 1 1 calc R . . C5 C 0.4479(2) -0.0096(5) 0.9840(4) 0.0305(13) Uani 1 1 d . . . H5A H 0.4353 0.0538 1.0098 0.037 Uiso 1 1 calc R . . H5B H 0.4202 -0.0488 0.9596 0.037 Uiso 1 1 calc R . . C6 C 0.5173(2) -0.0110(5) 1.1031(4) 0.0313(13) Uani 1 1 d . . . H6A H 0.5338 -0.0516 1.1537 0.038 Uiso 1 1 calc R . . H6B H 0.5077 0.0522 1.1342 0.038 Uiso 1 1 calc R . . C7 C 0.5054(2) 0.0130(5) 0.3915(4) 0.0281(12) Uani 1 1 d . . . H7A H 0.5156 0.0547 0.3350 0.034 Uiso 1 1 calc R . . H7B H 0.4932 -0.0504 0.3647 0.034 Uiso 1 1 calc R . . C8 C 0.4509(2) 0.0069(5) 0.5399(5) 0.0299(13) Uani 1 1 d . . . H8A H 0.4365 -0.0569 0.5196 0.036 Uiso 1 1 calc R . . H8B H 0.4262 0.0446 0.5768 0.036 Uiso 1 1 calc R . . C9 C 0.3785(2) -0.0023(5) -0.2383(4) 0.0285(13) 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 0.0338(3) 0.0185(3) 0.0375(4) 0.000 -0.0028(3) 0.000 Cd2 0.0262(5) 0.0189(4) 0.0188(18) 0.000 0.0029(6) 0.000 Cd2' 0.025(3) 0.012(2) 0.015(11) 0.000 0.001(3) 0.000 Cd3 0.0263(3) 0.0221(3) 0.0176(3) 0.000 0.0004(2) 0.000 Br1 0.0385(5) 0.0441(6) 0.0417(6) 0.000 0.0031(4) 0.000 Br2 0.0292(4) 0.0254(4) 0.0307(4) 0.000 0.0011(3) 0.000 Br3 0.0469(17) 0.0384(7) 0.0188(6) 0.000 0.0038(7) 0.000 Br3' 0.079(14) 0.043(4) 0.035(5) 0.000 -0.011(7) 0.000 Br4 0.0353(6) 0.0275(5) 0.0394(6) 0.000 -0.0124(4) 0.000 Br4' 0.061(7) 0.073(7) 0.048(6) 0.000 -0.009(4) 0.000 Br5 0.0305(5) 0.0461(6) 0.0410(5) 0.000 -0.0003(4) 0.000 Br6 0.0242(4) 0.0266(4) 0.0458(5) 0.000 0.0018(3) 0.000 Br7 0.0315(4) 0.0284(4) 0.0221(4) 0.000 -0.0051(3) 0.000 Br8 0.0329(4) 0.0322(5) 0.0231(4) 0.000 0.0044(3) 0.000 S1 0.0156(6) 0.0142(6) 0.0130(5) 0.0001(4) 0.0003(4) 0.0005(4) S2 0.0672(14) 0.0234(9) 0.0689(14) -0.0015(9) -0.0009(10) -0.0029(8) N1 0.026(2) 0.024(2) 0.018(2) 0.0059(19) -0.0066(17) 0.0005(19) N2 0.025(2) 0.024(2) 0.021(2) 0.0030(19) -0.0048(18) 0.0020(18) N3 0.024(2) 0.025(2) 0.026(2) 0.005(2) 0.0083(18) -0.0011(19) N4 0.020(2) 0.028(3) 0.026(2) -0.001(2) -0.0075(18) 0.0051(19) N5 0.050(4) 0.029(3) 0.042(3) -0.002(2) -0.014(3) 0.008(2) O1 0.041(2) 0.0180(19) 0.0149(18) 0.0031(15) -0.0003(15) 0.0013(16) O2 0.0157(17) 0.0217(19) 0.031(2) 0.0014(16) 0.0039(15) 0.0050(15) O3 0.0240(19) 0.025(2) 0.0165(18) -0.0050(15) -0.0060(14) 0.0014(15) O4 0.0165(18) 0.037(2) 0.0180(18) -0.0029(17) 0.0006(14) -0.0100(16) OW1 0.031(3) 0.038(4) 0.037(3) 0.000 0.001(3) 0.000 OW2 0.068(5) 0.036(4) 0.045(4) 0.000 0.015(4) 0.000 OW3 0.099(8) 0.032(4) 0.152(10) 0.000 -0.079(7) 0.000 OW4 0.053(6) 0.191(13) 0.062(6) 0.000 0.007(5) 0.000 OW5 0.063(5) 0.045(5) 0.071(6) 0.000 0.008(4) 0.000 C1 0.023(3) 0.033(3) 0.027(3) 0.006(3) -0.001(2) 0.003(2) C2 0.028(3) 0.027(3) 0.018(3) 0.003(2) 0.000(2) 0.005(2) C3 0.029(3) 0.034(3) 0.020(3) 0.003(2) -0.001(2) 0.006(2) C4 0.021(3) 0.034(3) 0.029(3) 0.010(3) 0.002(2) 0.003(2) C5 0.022(3) 0.037(3) 0.033(3) 0.011(3) 0.003(2) 0.001(2) C6 0.037(3) 0.038(3) 0.020(3) 0.007(3) -0.001(2) -0.003(3) C7 0.034(3) 0.032(3) 0.019(3) -0.002(2) 0.001(2) 0.008(2) C8 0.020(3) 0.034(3) 0.035(3) 0.004(3) 0.003(2) 0.004(2) C9 0.022(3) 0.034(4) 0.030(3) 0.002(3) 0.000(2) 0.002(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 N5 2.237(6) 7_565 ? Cd1 N5 2.237(6) . ? Cd1 Br2 2.6294(12) . ? Cd1 Br1 2.7412(13) . ? Cd1 Br3 2.8596(16) . ? Cd1 Br3' 2.911(11) . ? Cd2 Cd2' 0.54(4) . ? Cd2 Br3' 2.259(18) . ? Cd2 OW1 2.313(9) . ? Cd2 O1 2.366(4) 7_565 ? Cd2 O1 2.366(4) . ? Cd2 Br4' 2.667(12) . ? Cd2 Br3 2.680(7) . ? Cd2 Br5 2.760(5) . ? Cd2 Br4 2.765(5) . ? Cd2' OW1 1.90(3) . ? Cd2' O1 2.387(8) . ? Cd2' O1 2.387(8) 7_565 ? Cd2' Br5 2.44(2) . ? Cd2' Br4' 2.561(15) . ? Cd2' Br3' 2.78(5) . ? Cd2' Br4 3.09(3) . ? Cd3 O2 2.474(4) . ? Cd3 O2 2.474(4) 7 ? Cd3 Br8 2.5720(11) . ? Cd3 Br7 2.5764(10) . ? Cd3 Br6 2.6700(11) . ? Br3 Br3' 0.77(3) . ? Br4 Br4' 2.290(10) . ? Br4' OW1 1.609(12) . ? Br4' OW4 1.842(15) . ? S1 O1 1.472(4) . ? S1 O4 1.477(4) . ? S1 O2 1.483(4) . ? S1 O3 1.484(4) . ? S2 C9 1.620(7) . ? N1 C3 1.482(7) . ? N1 C1 1.503(7) . ? N2 C4 1.493(7) . ? N2 C2 1.498(7) . ? N3 C5 1.479(7) . ? N3 C6 1.493(7) . ? N4 C7 1.483(7) . ? N4 C8 1.487(7) . ? N5 C9 1.142(8) . ? C1 C2 1.506(7) . ? C3 C4 1.503(8) . ? C5 C6 1.516(8) 5_657 ? C6 C5 1.516(8) 5_657 ? C7 C8 1.518(8) 5_656 ? C8 C7 1.518(8) 5_656 ? 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 N5 Cd1 N5 161.6(3) 7_565 . ? N5 Cd1 Br2 98.92(16) 7_565 . ? N5 Cd1 Br2 98.92(16) . . ? N5 Cd1 Br1 90.01(15) 7_565 . ? N5 Cd1 Br1 90.01(15) . . ? Br2 Cd1 Br1 103.58(4) . . ? N5 Cd1 Br3 84.73(14) 7_565 . ? N5 Cd1 Br3 84.73(14) . . ? Br2 Cd1 Br3 111.47(9) . . ? Br1 Cd1 Br3 144.95(9) . . ? N5 Cd1 Br3' 86.90(17) 7_565 . ? N5 Cd1 Br3' 86.90(17) . . ? Br2 Cd1 Br3' 96.1(6) . . ? Br1 Cd1 Br3' 160.3(6) . . ? Br3 Cd1 Br3' 15.3(5) . . ? Cd2' Cd2 Br3' 161.3(12) . . ? Cd2' Cd2 OW1 36.2(9) . . ? Br3' Cd2 OW1 162.5(8) . . ? Cd2' Cd2 O1 85.6(2) . 7_565 ? Br3' Cd2 O1 94.6(2) . 7_565 ? OW1 Cd2 O1 85.55(18) . 7_565 ? Cd2' Cd2 O1 85.6(2) . . ? Br3' Cd2 O1 94.6(2) . . ? OW1 Cd2 O1 85.55(18) . . ? O1 Cd2 O1 170.7(4) 7_565 . ? Cd2' Cd2 Br4' 73.0(9) . . ? Br3' Cd2 Br4' 125.7(8) . . ? OW1 Cd2 Br4' 36.8(3) . . ? O1 Cd2 Br4' 87.23(12) 7_565 . ? O1 Cd2 Br4' 87.23(12) . . ? Cd2' Cd2 Br3 146.2(9) . . ? Br3' Cd2 Br3 15.1(7) . . ? OW1 Cd2 Br3 177.6(3) . . ? O1 Cd2 Br3 94.50(17) 7_565 . ? O1 Cd2 Br3 94.50(17) . . ? Br4' Cd2 Br3 140.8(3) . . ? Cd2' Cd2 Br5 49.2(9) . . ? Br3' Cd2 Br5 112.0(7) . . ? OW1 Cd2 Br5 85.4(3) . . ? O1 Cd2 Br5 88.33(17) 7_565 . ? O1 Cd2 Br5 88.33(17) . . ? Br4' Cd2 Br5 122.3(4) . . ? Br3 Cd2 Br5 96.96(9) . . ? Cd2' Cd2 Br4 122.8(9) . . ? Br3' Cd2 Br4 75.9(8) . . ? OW1 Cd2 Br4 86.68(16) . . ? O1 Cd2 Br4 91.05(14) 7_565 . ? O1 Cd2 Br4 91.05(14) . . ? Br4' Cd2 Br4 49.8(2) . . ? Br3 Cd2 Br4 90.9(2) . . ? Br5 Cd2 Br4 172.1(3) . . ? Cd2 Cd2' OW1 134.1(13) . . ? Cd2 Cd2' O1 81.3(11) . . ? OW1 Cd2' O1 95.0(7) . . ? Cd2 Cd2' O1 81.3(11) . 7_565 ? OW1 Cd2' O1 95.0(7) . 7_565 ? O1 Cd2' O1 162(2) . 7_565 ? Cd2 Cd2' Br5 121.1(14) . . ? OW1 Cd2' Br5 104.8(19) . . ? O1 Cd2' Br5 95.8(4) . . ? O1 Cd2' Br5 95.8(4) 7_565 . ? Cd2 Cd2' Br4' 95.3(12) . . ? OW1 Cd2' Br4' 38.8(3) . . ? O1 Cd2' Br4' 89.3(2) . . ? O1 Cd2' Br4' 89.3(2) 7_565 . ? Br5 Cd2' Br4' 143.7(19) . . ? Cd2 Cd2' Br3' 15.1(10) . . ? OW1 Cd2' Br3' 149.3(13) . . ? O1 Cd2' Br3' 82.0(10) . . ? O1 Cd2' Br3' 82.0(10) 7_565 . ? Br5 Cd2' Br3' 105.9(10) . . ? Br4' Cd2' Br3' 110.4(14) . . ? Cd2 Cd2' Br4 48.7(9) . . ? OW1 Cd2' Br4 85.5(4) . . ? O1 Cd2' Br4 83.1(7) . . ? O1 Cd2' Br4 83.1(7) 7_565 . ? Br5 Cd2' Br4 169.7(15) . . ? Br4' Cd2' Br4 46.6(4) . . ? Br3' Cd2' Br4 63.8(10) . . ? O2 Cd3 O2 161.70(17) . 7 ? O2 Cd3 Br8 96.33(9) . . ? O2 Cd3 Br8 96.33(9) 7 . ? O2 Cd3 Br7 89.53(9) . . ? O2 Cd3 Br7 89.53(9) 7 . ? Br8 Cd3 Br7 139.05(4) . . ? O2 Cd3 Br6 81.63(8) . . ? O2 Cd3 Br6 81.63(8) 7 . ? Br8 Cd3 Br6 110.26(3) . . ? Br7 Cd3 Br6 110.70(3) . . ? Br3' Br3 Cd2 49.7(6) . . ? Br3' Br3 Cd1 86.1(6) . . ? Cd2 Br3 Cd1 135.78(19) . . ? Br3 Br3' Cd2 115.2(9) . . ? Br3 Br3' Cd2' 111.6(8) . . ? Cd2 Br3' Cd2' 3.6(3) . . ? Br3 Br3' Cd1 78.6(9) . . ? Cd2 Br3' Cd1 166.2(14) . . ? Cd2' Br3' Cd1 169.8(13) . . ? Br4' Br4 Cd2 62.9(3) . . ? Br4' Br4 Cd2' 54.4(7) . . ? Cd2 Br4 Cd2' 8.5(5) . . ? OW1 Br4' OW4 126.3(7) . . ? OW1 Br4' Br4 126.9(7) . . ? OW4 Br4' Br4 106.8(6) . . ? OW1 Br4' Cd2' 47.8(11) . . ? OW4 Br4' Cd2' 174.2(12) . . ? Br4 Br4' Cd2' 79.0(10) . . ? OW1 Br4' Cd2 59.5(5) . . ? OW4 Br4' Cd2 174.1(6) . . ? Br4 Br4' Cd2 67.3(3) . . ? Cd2' Br4' Cd2 11.7(8) . . ? Cd2' Br5 Cd2 9.7(8) . . ? O1 S1 O4 109.6(2) . . ? O1 S1 O2 109.0(2) . . ? O4 S1 O2 109.0(2) . . ? O1 S1 O3 111.2(2) . . ? O4 S1 O3 109.0(2) . . ? O2 S1 O3 109.0(2) . . ? C3 N1 C1 111.0(4) . . ? C4 N2 C2 113.0(4) . . ? C5 N3 C6 111.6(4) . . ? C7 N4 C8 111.8(4) . . ? C9 N5 Cd1 172.1(5) . . ? S1 O1 Cd2 132.7(3) . . ? S1 O1 Cd2' 119.9(11) . . ? Cd2 O1 Cd2' 13.1(9) . . ? S1 O2 Cd3 119.6(2) . . ? Br4' OW1 Cd2' 93.3(11) . . ? Br4' OW1 Cd2 83.6(5) . . ? Cd2' OW1 Cd2 9.7(8) . . ? N1 C1 C2 111.4(4) . . ? N2 C2 C1 110.8(4) . . ? N1 C3 C4 112.1(5) . . ? N2 C4 C3 110.3(4) . . ? N3 C5 C6 111.5(4) . 5_657 ? N3 C6 C5 110.6(5) . 5_657 ? N4 C7 C8 110.4(4) . 5_656 ? N4 C8 C7 111.5(5) . 5_656 ? N5 C9 S2 177.8(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.125 _refine_diff_density_min -2.269 _refine_diff_density_rms 0.305 # Attachment '- 3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 790450' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H7 Cd I N2 O S2' _chemical_formula_weight 402.54 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' S S 0.1246 0.1234 '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 4.2002(8) _cell_length_b 20.158(4) _cell_length_c 12.441(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.58(3) _cell_angle_gamma 90.00 _cell_volume 1046.4(4) _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 strip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 5.388 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.578 _exptl_absorpt_correction_T_max 0.583 _exptl_absorpt_process_details ; Higashi, T.(1995).Program for Absorption Correction. Rigaku Corporation, Tokyo,Japan. ; _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9972 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2410 _reflns_number_gt 2123 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _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^)+(0.0114P)^2^+0.5756P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2410 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0423 _refine_ls_wR_factor_gt 0.0412 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.21870(4) 0.382467(8) 0.861929(16) 0.03319(6) Uani 1 1 d . . . I1 I 0.65701(4) 0.382006(8) 0.698166(13) 0.03315(6) Uani 1 1 d . . . S1 S 0.24882(17) 0.62203(3) 0.97063(6) 0.03543(15) Uani 1 1 d . . . S2 S 0.19507(19) 0.25779(3) 0.91995(5) 0.04014(16) Uani 1 1 d . . . N1 N 0.2120(5) 0.49165(9) 0.89103(19) 0.0375(5) Uani 1 1 d . . . N2 N 0.2419(7) 0.22188(12) 0.7171(2) 0.0651(8) Uani 1 1 d . . . H2A H 0.2206 0.1930 0.6659 0.078 Uiso 1 1 calc R . . H2B H 0.3171 0.2606 0.7057 0.078 Uiso 1 1 calc R . . O1 O 0.0500(5) 0.14585(8) 0.81581(15) 0.0462(5) Uani 1 1 d . . . C1 C 0.2265(6) 0.54497(11) 0.9236(2) 0.0308(5) Uani 1 1 d . . . C2 C 0.1603(6) 0.20693(11) 0.8121(2) 0.0347(6) Uani 1 1 d . . . C3 C -0.0667(7) 0.12092(11) 0.9137(2) 0.0410(6) Uani 1 1 d . . . H3A H -0.2235 0.1511 0.9379 0.049 Uiso 1 1 calc R . . H3B H 0.1088 0.1161 0.9710 0.049 Uiso 1 1 calc R . . C4 C -0.2169(8) 0.05475(13) 0.8850(3) 0.0549(8) Uani 1 1 d . . . H4A H -0.2979 0.0361 0.9475 0.082 Uiso 1 1 calc R . . H4B H -0.0591 0.0255 0.8609 0.082 Uiso 1 1 calc R . . H4C H -0.3897 0.0603 0.8282 0.082 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 0.03621(11) 0.02343(9) 0.03958(12) -0.00341(7) 0.00283(9) -0.00110(7) I1 0.02909(9) 0.04213(10) 0.02802(9) 0.00092(6) 0.00237(7) -0.00298(6) S1 0.0469(4) 0.0238(3) 0.0337(3) -0.0040(2) -0.0035(3) 0.0014(2) S2 0.0664(5) 0.0257(3) 0.0284(3) -0.0056(2) 0.0059(3) -0.0052(3) N1 0.0446(13) 0.0306(10) 0.0364(12) -0.0091(9) 0.0007(10) 0.0002(9) N2 0.124(3) 0.0369(12) 0.0400(15) -0.0131(11) 0.0351(16) -0.0280(15) O1 0.0785(14) 0.0278(8) 0.0341(10) -0.0069(8) 0.0140(10) -0.0153(9) C1 0.0347(13) 0.0307(12) 0.0259(12) -0.0029(10) -0.0010(10) -0.0007(10) C2 0.0467(15) 0.0257(11) 0.0319(14) -0.0036(10) 0.0055(12) -0.0023(10) C3 0.0559(17) 0.0337(12) 0.0344(15) 0.0017(11) 0.0099(13) -0.0074(12) C4 0.071(2) 0.0356(14) 0.060(2) -0.0002(13) 0.0143(17) -0.0140(14) _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 2.231(2) . ? Cd1 S2 2.6199(8) . ? Cd1 S1 2.8779(11) 3_667 ? Cd1 I1 2.8982(8) . ? Cd1 I1 2.9352(10) 1_455 ? I1 Cd1 2.9352(10) 1_655 ? S1 C1 1.659(2) . ? S1 Cd1 2.8779(11) 3_667 ? S2 C2 1.682(2) . ? N1 C1 1.148(3) . ? N2 C2 1.303(3) . ? O1 C2 1.318(3) . ? O1 C3 1.453(3) . ? C3 C4 1.501(3) . ? 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 S2 154.16(6) . . ? N1 Cd1 S1 86.38(6) . 3_667 ? S2 Cd1 S1 79.70(2) . 3_667 ? N1 Cd1 I1 97.94(6) . . ? S2 Cd1 I1 103.754(18) . . ? S1 Cd1 I1 90.30(2) 3_667 . ? N1 Cd1 I1 95.26(6) . 1_455 ? S2 Cd1 I1 97.782(18) . 1_455 ? S1 Cd1 I1 176.875(15) 3_667 1_455 ? I1 Cd1 I1 92.111(18) . 1_455 ? Cd1 I1 Cd1 92.111(18) . 1_655 ? C1 S1 Cd1 103.51(9) . 3_667 ? C2 S2 Cd1 111.56(9) . . ? C1 N1 Cd1 168.5(2) . . ? C2 O1 C3 120.4(2) . . ? N1 C1 S1 179.8(3) . . ? N2 C2 O1 112.2(2) . . ? N2 C2 S2 125.09(19) . . ? O1 C2 S2 122.7(2) . . ? O1 C3 C4 106.3(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A S1 0.86 2.84 3.557(3) 142.3 2_546 N2 H2B I1 0.86 2.84 3.689(2) 169.4 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.600 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.094