# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_CMTD #TrackingRef '19601_web_deposit_cif_file_0_XitaoLiu_1366282003.CMTD.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H12 Cd Hg N4 O2 S6' _chemical_formula_sum 'C8 H12 Cd Hg N4 O2 S6' _chemical_formula_weight 701.57 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.52860(10) _cell_length_b 8.5521(2) _cell_length_c 28.2714(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2062.04(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2370 _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 26.83 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 9.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2192 _exptl_absorpt_correction_T_max 0.3848 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10216 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.37 _reflns_number_total 4592 _reflns_number_gt 3242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker,2005)' _computing_cell_refinement 'APEX2 Software Suite (Bruker,2005)' _computing_data_reduction 'APEX2 Software Suite (Bruker,2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'WINGX (Farrugia,1999)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00206(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(7) _refine_ls_number_reflns 4592 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _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 C1 C 0.8359(7) 0.5748(6) 0.8963(3) 0.0488(19) Uani 1 1 d . . . C2 C 0.9503(11) 0.3988(9) 1.0296(3) 0.111(3) Uani 1 1 d . . . H2A H 1.0338 0.3598 1.0491 0.166 Uiso 1 1 calc R . . H2B H 0.8582 0.4140 1.0486 0.166 Uiso 1 1 calc R . . H2C H 0.9810 0.4967 1.0158 0.166 Uiso 1 1 calc R . . C3 C 0.9258(11) 0.0953(8) 1.0187(4) 0.137(5) Uani 1 1 d . . . H3A H 0.8905 0.0080 1.0002 0.205 Uiso 1 1 calc R . . H3B H 0.8622 0.1045 1.0465 0.205 Uiso 1 1 calc R . . H3C H 1.0332 0.0795 1.0276 0.205 Uiso 1 1 calc R . . C4 C 1.1230(7) 0.2986(10) 0.7165(3) 0.090(3) Uani 1 1 d . . . H4A H 1.2285 0.3016 0.7283 0.135 Uiso 1 1 calc R . . H4B H 1.1109 0.3754 0.6920 0.135 Uiso 1 1 calc R . . H4C H 1.1014 0.1966 0.7038 0.135 Uiso 1 1 calc R . . C5 C 0.8173(7) 0.3213(13) 0.7315(3) 0.116(4) Uani 1 1 d . . . H5A H 0.8012 0.2139 0.7230 0.173 Uiso 1 1 calc R . . H5B H 0.8222 0.3841 0.7034 0.173 Uiso 1 1 calc R . . H5C H 0.7320 0.3562 0.7510 0.173 Uiso 1 1 calc R . . C6 C 1.3577(6) 0.4143(6) 0.8418(3) 0.0454(17) Uani 1 1 d . . . C7 C 0.6636(6) 0.0756(6) 0.8605(2) 0.0430(17) Uani 1 1 d . . . C8 C 1.1710(6) -0.1211(6) 0.9005(2) 0.0414(16) Uani 1 1 d . . . Cd1 Cd 1.01935(4) 0.23545(4) 0.874193(16) 0.03543(9) Uani 1 1 d . . . Hg1 Hg 0.50633(2) 0.73851(2) 0.875832(11) 0.05306(10) Uani 1 1 d . . . N1 N 0.8988(5) 0.4792(5) 0.8756(2) 0.0578(16) Uani 1 1 d . . . N2 N 0.7675(5) 0.1313(5) 0.8790(2) 0.0554(15) Uani 1 1 d . . . N3 N 1.1150(5) -0.0114(5) 0.8848(2) 0.0492(15) Uani 1 1 d . . . N4 N 1.2588(6) 0.3482(5) 0.8587(2) 0.0594(17) Uani 1 1 d . . . O1 O 0.9999(5) 0.1958(4) 0.79428(14) 0.0560(10) Uani 1 1 d . . . O2 O 1.0537(4) 0.2656(5) 0.95379(13) 0.0520(10) Uani 1 1 d . . . S1 S 0.25252(16) 0.7211(2) 0.92334(7) 0.0640(6) Uani 1 1 d . . . S2 S 0.5092(2) 0.99916(15) 0.83293(7) 0.0607(5) Uani 1 1 d . . . S3 S 0.74804(18) 0.7134(3) 0.92752(8) 0.0713(6) Uani 1 1 d . . . S4 S 0.5042(2) 0.51119(18) 0.81728(8) 0.0765(6) Uani 1 1 d . . . S5 S 0.91030(15) 0.2657(2) 0.98532(6) 0.0548(4) Uani 1 1 d . . . S6 S 0.9921(2) 0.33893(16) 0.76257(6) 0.0571(4) 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 C1 0.045(3) 0.037(3) 0.064(6) 0.016(4) -0.013(3) 0.001(2) C2 0.130(8) 0.133(7) 0.069(7) -0.059(6) 0.004(6) 0.019(6) C3 0.149(9) 0.094(5) 0.167(11) 0.075(7) 0.098(8) 0.042(6) C4 0.095(5) 0.105(6) 0.071(7) 0.023(6) 0.035(4) -0.002(5) C5 0.065(4) 0.197(10) 0.085(7) 0.048(8) -0.009(5) 0.004(5) C6 0.043(3) 0.042(3) 0.051(5) -0.014(4) -0.010(3) -0.001(3) C7 0.036(3) 0.039(3) 0.054(5) 0.008(3) 0.014(3) -0.002(2) C8 0.034(3) 0.047(3) 0.043(5) -0.007(3) 0.008(3) -0.001(2) Cd1 0.03635(17) 0.03613(16) 0.0338(2) 0.0000(2) -0.00083(19) -0.0005(2) Hg1 0.03649(10) 0.03656(11) 0.0861(2) -0.00553(13) -0.00028(13) -0.00059(13) N1 0.053(3) 0.042(3) 0.078(5) 0.002(3) -0.015(3) 0.010(2) N2 0.043(3) 0.051(3) 0.073(5) 0.001(3) -0.003(3) -0.009(2) N3 0.046(3) 0.043(3) 0.059(4) 0.000(3) 0.001(3) 0.011(2) N4 0.048(3) 0.049(3) 0.081(5) -0.011(3) 0.012(3) -0.015(2) O1 0.082(3) 0.0491(18) 0.037(3) 0.002(2) -0.002(3) -0.002(3) O2 0.0467(17) 0.077(3) 0.033(3) -0.003(3) -0.0002(17) -0.008(2) S1 0.0549(8) 0.0494(10) 0.0877(16) 0.0230(12) 0.0197(9) 0.0133(8) S2 0.0510(10) 0.0532(7) 0.0779(14) 0.0108(9) -0.0176(10) -0.0101(8) S3 0.0615(8) 0.0713(13) 0.0811(17) -0.0241(13) -0.0219(10) 0.0190(9) S4 0.0727(13) 0.0708(9) 0.0861(16) -0.0298(11) 0.0358(13) -0.0274(10) S5 0.0545(7) 0.0690(10) 0.0409(11) -0.0024(11) 0.0053(7) 0.0062(9) S6 0.0817(11) 0.0530(7) 0.0365(10) 0.0035(8) -0.0012(11) 0.0030(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.140(7) . ? C1 S3 1.657(7) . ? C2 S5 1.727(7) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 S5 1.741(7) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 S6 1.751(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 S6 1.737(7) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N4 1.123(7) . ? C6 S4 1.651(6) 1_655 ? C7 N2 1.134(7) . ? C7 S2 1.664(7) 1_545 ? C8 N3 1.142(6) . ? C8 S1 1.650(6) 1_645 ? Cd1 N3 2.283(4) . ? Cd1 O2 2.284(4) . ? Cd1 O1 2.291(4) . ? Cd1 N4 2.300(5) . ? Cd1 N1 2.325(4) . ? Cd1 N2 2.330(5) . ? Hg1 S3 2.5359(16) . ? Hg1 S2 2.5379(15) . ? Hg1 S1 2.5520(15) . ? Hg1 S4 2.5534(17) . ? O1 S6 1.518(4) . ? O2 S5 1.514(4) . ? S1 C8 1.650(6) 1_465 ? S2 C7 1.664(7) 1_565 ? S4 C6 1.651(6) 1_455 ? 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 C1 S3 178.5(6) . . ? S5 C2 H2A 109.5 . . ? S5 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S5 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S5 C3 H3A 109.5 . . ? S5 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S5 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S6 C4 H4A 109.5 . . ? S6 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S6 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S6 C5 H5A 109.5 . . ? S6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 S4 179.5(7) . 1_655 ? N2 C7 S2 178.3(6) . 1_545 ? N3 C8 S1 179.7(7) . 1_645 ? N3 Cd1 O2 85.92(18) . . ? N3 Cd1 O1 91.09(17) . . ? O2 Cd1 O1 176.22(12) . . ? N3 Cd1 N4 95.49(17) . . ? O2 Cd1 N4 91.51(18) . . ? O1 Cd1 N4 86.47(19) . . ? N3 Cd1 N1 170.0(2) . . ? O2 Cd1 N1 86.49(19) . . ? O1 Cd1 N1 96.74(19) . . ? N4 Cd1 N1 91.15(17) . . ? N3 Cd1 N2 88.17(16) . . ? O2 Cd1 N2 95.94(18) . . ? O1 Cd1 N2 86.26(19) . . ? N4 Cd1 N2 171.9(2) . . ? N1 Cd1 N2 86.21(16) . . ? S3 Hg1 S2 110.00(7) . . ? S3 Hg1 S1 112.41(6) . . ? S2 Hg1 S1 108.12(6) . . ? S3 Hg1 S4 108.36(7) . . ? S2 Hg1 S4 111.04(7) . . ? S1 Hg1 S4 106.90(6) . . ? C1 N1 Cd1 149.3(6) . . ? C7 N2 Cd1 148.6(5) . . ? C8 N3 Cd1 163.7(5) . . ? C6 N4 Cd1 163.6(6) . . ? S6 O1 Cd1 117.79(19) . . ? S5 O2 Cd1 118.46(18) . . ? C8 S1 Hg1 96.0(2) 1_465 . ? C7 S2 Hg1 97.4(2) 1_565 . ? C1 S3 Hg1 97.0(2) . . ? C6 S4 Hg1 96.6(2) 1_455 . ? O2 S5 C2 105.6(4) . . ? O2 S5 C3 104.9(3) . . ? C2 S5 C3 98.3(5) . . ? O1 S6 C5 105.4(4) . . ? O1 S6 C4 104.7(3) . . ? C5 S6 C4 98.8(4) . . ? 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 O2 Cd1 N1 C1 -21.3(9) . . . . ? O1 Cd1 N1 C1 160.7(9) . . . . ? N4 Cd1 N1 C1 -112.8(9) . . . . ? N2 Cd1 N1 C1 74.9(9) . . . . ? N3 Cd1 N2 C7 -87.6(9) . . . . ? O2 Cd1 N2 C7 -173.3(9) . . . . ? O1 Cd1 N2 C7 3.6(9) . . . . ? N1 Cd1 N2 C7 100.6(9) . . . . ? O2 Cd1 N3 C8 -10.4(16) . . . . ? O1 Cd1 N3 C8 167.3(16) . . . . ? N4 Cd1 N3 C8 80.8(16) . . . . ? N2 Cd1 N3 C8 -106.5(16) . . . . ? N3 Cd1 N4 C6 125.1(17) . . . . ? O2 Cd1 N4 C6 -148.9(17) . . . . ? O1 Cd1 N4 C6 34.3(17) . . . . ? N1 Cd1 N4 C6 -62.3(17) . . . . ? N3 Cd1 O1 S6 -159.7(3) . . . . ? N4 Cd1 O1 S6 -64.3(3) . . . . ? N1 Cd1 O1 S6 26.5(3) . . . . ? N2 Cd1 O1 S6 112.2(3) . . . . ? N3 Cd1 O2 S5 -106.3(3) . . . . ? N4 Cd1 O2 S5 158.3(3) . . . . ? N1 Cd1 O2 S5 67.3(3) . . . . ? N2 Cd1 O2 S5 -18.5(3) . . . . ? S3 Hg1 S1 C8 130.5(2) . . . 1_465 ? S2 Hg1 S1 C8 8.9(2) . . . 1_465 ? S4 Hg1 S1 C8 -110.7(2) . . . 1_465 ? S3 Hg1 S2 C7 -7.5(2) . . . 1_565 ? S1 Hg1 S2 C7 115.6(2) . . . 1_565 ? S4 Hg1 S2 C7 -127.4(2) . . . 1_565 ? S2 Hg1 S3 C1 -110.6(2) . . . . ? S1 Hg1 S3 C1 128.9(2) . . . . ? S4 Hg1 S3 C1 11.0(2) . . . . ? S3 Hg1 S4 C6 108.2(2) . . . 1_455 ? S2 Hg1 S4 C6 -130.9(2) . . . 1_455 ? S1 Hg1 S4 C6 -13.2(2) . . . 1_455 ? Cd1 O2 S5 C2 -144.2(4) . . . . ? Cd1 O2 S5 C3 112.6(4) . . . . ? Cd1 O1 S6 C5 -121.8(4) . . . . ? Cd1 O1 S6 C4 134.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.742 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 934757'