# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_(4) _database_code_depnum_ccdc_archive 'CCDC 902410' #TrackingRef '4.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-Poly-(bis(\m2-hexamathylenetetraamine)- tetra(\m2-thicyanato)-di(methanol)dicadium(II)) ; _chemical_name_common ; catena-Poly-(bis(mu2-hexamathylenetetraamine)-tetra(mu2- thicyanato)-di(methanol)dicadium(ii)) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cd N4 O S2' _chemical_formula_weight 330.73 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 8.8702(2) _cell_length_b 9.2216(3) _cell_length_c 13.7007(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.309(2) _cell_angle_gamma 90.00 _cell_volume 1069.93(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.989 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details CrysAlis _exptl_special_details ; CrysAlis RED Oxford Diffraction Ltd., version 1.171.13,1995-2003 ; _diffrn_ambient_temperature 100(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 'KM4 CCD kappa-geometry diffractometer' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13274 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.69 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3021 _reflns_number_gt 2746 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD Oxford Diffraction Ltd., version 1.171.13 ; _computing_cell_refinement ; CrysAlis RED Oxford Diffraction Ltd., version 1.171.13 ; _computing_data_reduction ; CrysAlis RED Oxford Diffraction Ltd., version 1.171.13 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1, Bruker AXS,1999' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^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_number_reflns 3021 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Cd2 Cd 0.0000 0.661776(15) 0.2500 0.01219(5) Uani 1 2 d S . . Cd1 Cd -0.5000 1.0000 0.0000 0.01053(5) Uani 1 2 d S . . S1 S -0.56394(4) 0.74789(4) 0.08055(3) 0.01355(7) Uani 1 1 d . . . S2 S 0.07373(4) 0.86953(4) 0.13398(3) 0.01569(8) Uani 1 1 d . . . N2 N -0.35565(14) 1.31805(13) 0.27827(8) 0.0120(2) Uani 1 1 d . . . N1 N -0.49968(13) 1.13105(13) 0.16046(8) 0.0109(2) Uani 1 1 d . . . C1 C -0.35721(16) 1.22507(16) 0.19074(10) 0.0122(3) Uani 1 1 d . . . H11 H -0.3564(18) 1.2823(19) 0.1355(12) 0.008(4) Uiso 1 1 d . . . H12 H -0.2674(19) 1.1620(16) 0.2100(13) 0.011(4) Uiso 1 1 d . . . C2 C -0.5000 1.4079(2) 0.2500 0.0137(4) Uani 1 2 d S . . H2 H -0.5007(17) 1.4690(17) 0.1967(11) 0.005(4) Uiso 1 1 d . . . C3 C -0.35813(16) 1.22540(16) 0.36481(10) 0.0119(3) Uani 1 1 d . . . H31 H -0.2688(19) 1.1671(15) 0.3817(12) 0.009(4) Uiso 1 1 d . . . H32 H -0.3569(19) 1.2828(18) 0.4193(12) 0.008(4) Uiso 1 1 d . . . C4 C -0.5000 1.0404(2) 0.2500 0.0112(3) Uani 1 2 d S . . H4 H -0.598(2) 0.9834(19) 0.2318(13) 0.018(5) Uiso 1 1 d . . . N3 N -0.25519(14) 0.63871(14) 0.15228(10) 0.0175(3) Uani 1 1 d . . . N4 N -0.23584(14) 0.97654(14) 0.06778(9) 0.0153(2) Uani 1 1 d . . . C6 C -0.38199(16) 0.68677(15) 0.12292(10) 0.0131(3) Uani 1 1 d . . . C5 C -0.10787(16) 0.93337(15) 0.09539(10) 0.0124(3) Uani 1 1 d . . . C7 C -0.0299(2) 0.3741(2) 0.09386(14) 0.0299(4) Uani 1 1 d . . . H71 H -0.1350 0.4128 0.0706 0.032(5) Uiso 1 1 calc R . . H72 H -0.0301 0.2868 0.1319 0.044(6) Uiso 1 1 calc R . . H73 H 0.0065 0.3529 0.0361 0.045(7) Uiso 1 1 calc R . . O1 O 0.07210(13) 0.47744(13) 0.15749(9) 0.0213(2) Uani 1 1 d . . . H1 H 0.153(3) 0.447(2) 0.1759(15) 0.033(6) Uiso 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 Cd2 0.01000(7) 0.01160(9) 0.01339(7) 0.000 0.00106(5) 0.000 Cd1 0.01042(7) 0.01075(9) 0.00996(7) 0.00070(4) 0.00231(5) 0.00140(5) S1 0.01115(14) 0.01415(18) 0.01448(15) 0.00337(12) 0.00247(12) 0.00079(12) S2 0.01050(14) 0.0192(2) 0.01769(16) 0.00372(13) 0.00463(12) 0.00098(13) N2 0.0138(5) 0.0105(6) 0.0120(5) 0.0002(4) 0.0044(4) -0.0008(4) N1 0.0109(5) 0.0105(6) 0.0109(5) 0.0000(4) 0.0030(4) 0.0003(4) C1 0.0119(6) 0.0136(7) 0.0120(6) -0.0006(5) 0.0048(5) -0.0024(5) C2 0.0153(8) 0.0097(10) 0.0160(9) 0.000 0.0044(7) 0.000 C3 0.0122(6) 0.0126(7) 0.0109(6) -0.0010(5) 0.0031(5) -0.0012(5) C4 0.0134(8) 0.0095(9) 0.0112(8) 0.000 0.0042(7) 0.000 N3 0.0130(5) 0.0162(6) 0.0210(6) 0.0041(5) 0.0014(5) -0.0014(5) N4 0.0146(5) 0.0154(6) 0.0155(6) 0.0014(4) 0.0038(5) -0.0003(5) C6 0.0157(6) 0.0101(7) 0.0123(6) 0.0026(5) 0.0025(5) -0.0032(5) C5 0.0162(6) 0.0108(7) 0.0106(6) -0.0002(5) 0.0047(5) -0.0025(5) C7 0.0212(7) 0.0295(10) 0.0336(9) -0.0142(8) -0.0003(7) -0.0013(7) O1 0.0141(5) 0.0198(6) 0.0249(6) -0.0089(4) -0.0022(4) 0.0042(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 Cd2 N3 2.2712(12) . ? Cd2 N3 2.2712(12) 2 ? Cd2 O1 2.3211(12) . ? Cd2 O1 2.3211(12) 2 ? Cd2 S2 2.6913(4) 2 ? Cd2 S2 2.6913(4) . ? Cd1 N4 2.2594(12) . ? Cd1 N4 2.2594(12) 3_475 ? Cd1 N1 2.5079(11) . ? Cd1 N1 2.5079(11) 3_475 ? Cd1 S1 2.7049(4) 3_475 ? Cd1 S1 2.7050(4) . ? S1 C6 1.6438(14) . ? S2 C5 1.6474(14) . ? N2 C3 1.4670(18) . ? N2 C1 1.4710(17) . ? N2 C2 1.4765(16) . ? N1 C3 1.4859(17) 2_455 ? N1 C4 1.4851(16) . ? N1 C1 1.4863(17) . ? C1 H11 0.924(16) . ? C1 H12 0.958(16) . ? C2 N2 1.4766(16) 2_455 ? C2 H2 0.921(15) . ? C3 N1 1.4859(17) 2_455 ? C3 H31 0.928(15) . ? C3 H32 0.912(16) . ? C4 N1 1.4850(16) 2_455 ? C4 H4 0.983(17) . ? N3 C6 1.1636(18) . ? N4 C5 1.1553(18) . ? C7 O1 1.4204(19) . ? C7 H71 0.9600 . ? C7 H72 0.9600 . ? C7 H73 0.9600 . ? O1 H1 0.74(2) . ? 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 N3 Cd2 N3 169.25(7) . 2 ? N3 Cd2 O1 89.87(4) . . ? N3 Cd2 O1 82.25(4) 2 . ? N3 Cd2 O1 82.25(4) . 2 ? N3 Cd2 O1 89.87(4) 2 2 ? O1 Cd2 O1 85.83(7) . 2 ? N3 Cd2 S2 92.30(4) . 2 ? N3 Cd2 S2 95.35(3) 2 2 ? O1 Cd2 S2 177.08(3) . 2 ? O1 Cd2 S2 92.52(3) 2 2 ? N3 Cd2 S2 95.35(3) . . ? N3 Cd2 S2 92.30(4) 2 . ? O1 Cd2 S2 92.52(3) . . ? O1 Cd2 S2 177.08(3) 2 . ? S2 Cd2 S2 89.227(17) 2 . ? N4 Cd1 N4 180.0 . 3_475 ? N4 Cd1 N1 87.44(4) . . ? N4 Cd1 N1 92.56(4) 3_475 . ? N4 Cd1 N1 92.56(4) . 3_475 ? N4 Cd1 N1 87.44(4) 3_475 3_475 ? N1 Cd1 N1 180.00(5) . 3_475 ? N4 Cd1 S1 86.12(3) . 3_475 ? N4 Cd1 S1 93.88(3) 3_475 3_475 ? N1 Cd1 S1 89.87(3) . 3_475 ? N1 Cd1 S1 90.13(3) 3_475 3_475 ? N4 Cd1 S1 93.88(3) . . ? N4 Cd1 S1 86.12(3) 3_475 . ? N1 Cd1 S1 90.13(3) . . ? N1 Cd1 S1 89.87(3) 3_475 . ? S1 Cd1 S1 180.0 3_475 . ? C6 S1 Cd1 97.80(5) . . ? C5 S2 Cd2 93.31(5) . . ? C3 N2 C1 108.70(11) . . ? C3 N2 C2 108.56(10) . . ? C1 N2 C2 108.42(9) . . ? C3 N1 C4 108.16(10) 2_455 . ? C3 N1 C1 108.41(11) 2_455 . ? C4 N1 C1 107.94(9) . . ? C3 N1 Cd1 107.37(7) 2_455 . ? C4 N1 Cd1 116.95(9) . . ? C1 N1 Cd1 107.75(8) . . ? N2 C1 N1 111.63(11) . . ? N2 C1 H11 109.5(10) . . ? N1 C1 H11 108.5(10) . . ? N2 C1 H12 108.9(10) . . ? N1 C1 H12 106.9(9) . . ? H11 C1 H12 111.4(14) . . ? N2 C2 N2 111.76(16) . 2_455 ? N2 C2 H2 110.6(9) . . ? N2 C2 H2 109.6(9) 2_455 . ? N2 C3 N1 111.63(10) . 2_455 ? N2 C3 H31 108.8(10) . . ? N1 C3 H31 108.7(9) 2_455 . ? N2 C3 H32 108.9(10) . . ? N1 C3 H32 109.5(10) 2_455 . ? H31 C3 H32 109.3(14) . . ? N1 C4 N1 111.52(16) 2_455 . ? N1 C4 H4 106.9(11) 2_455 . ? N1 C4 H4 108.1(10) . . ? C6 N3 Cd2 149.25(12) . . ? C5 N4 Cd1 164.89(12) . . ? N3 C6 S1 177.67(14) . . ? N4 C5 S2 179.17(14) . . ? O1 C7 H71 109.5 . . ? O1 C7 H72 109.5 . . ? H71 C7 H72 109.5 . . ? O1 C7 H73 109.5 . . ? H71 C7 H73 109.5 . . ? H72 C7 H73 109.5 . . ? C7 O1 Cd2 126.72(10) . . ? C7 O1 H1 109.3(17) . . ? Cd2 O1 H1 119.1(16) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.626 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.079 data_(5) _database_code_depnum_ccdc_archive 'CCDC 902411' #TrackingRef '5.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(tris(3,5-dimethylpyrazol-1-ylmethyl)amine)-bis(thiocyanato)cadmium(II)] ; _chemical_name_common ;((tris(3,5-dimethylpyrazol-1-ylmethyl)amine)- bis(thiocyanato)cadmium(ii)) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 Cd N9 S2' _chemical_formula_weight 569.05 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' Cd Cd -0.8075 1.2024 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.274(2) _cell_length_b 8.407(2) _cell_length_c 17.567(3) _cell_angle_alpha 79.22(2) _cell_angle_beta 89.42(2) _cell_angle_gamma 84.370(10) _cell_volume 1194.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.995 _cell_measurement_theta_max 28.50 _exptl_crystal_description column _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 1.116 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details CrysAlis _exptl_special_details ; CrysAlis RED Oxford Diffraction Ltd., version 1.171.13,1995-2003 ; _diffrn_ambient_temperature 100(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 'KM4 CCD kappa-geometry diffractometer' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17515 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.73 _diffrn_reflns_theta_max 28.50 _reflns_number_total 6021 _reflns_number_gt 5085 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD Oxford Diffraction Ltd., version 1.171.13 ; _computing_cell_refinement ; CrysAlis RED Oxford Diffraction Ltd., version 1.171.13 ; _computing_data_reduction ; CrysAlis RED Oxford Diffraction Ltd., version 1.171.13 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V5.1, Bruker AXS,1999' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0998P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6021 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 0.04516(2) 0.37753(2) 0.251147(11) 0.02214(9) Uani 1 1 d . . . S1 S -0.33571(12) 0.77303(11) 0.09327(5) 0.0372(2) Uani 1 1 d . . . S2 S -0.31720(10) 0.04530(10) 0.44470(4) 0.02765(17) Uani 1 1 d . . . N4 N -0.1488(4) 0.5068(4) 0.17422(18) 0.0345(6) Uani 1 1 d . . . N5 N -0.1086(3) 0.2257(3) 0.34523(16) 0.0297(6) Uani 1 1 d . . . C11 C -0.2265(4) 0.6185(4) 0.14020(18) 0.0278(6) Uani 1 1 d . . . C12 C -0.1942(4) 0.1501(4) 0.38674(17) 0.0232(6) Uani 1 1 d . . . N1 N 0.1413(3) 0.1310(3) 0.21590(14) 0.0208(5) Uani 1 1 d . . . N2 N 0.2516(3) 0.0369(3) 0.26642(14) 0.0199(5) Uani 1 1 d . . . C3 C 0.3195(4) -0.0916(3) 0.23717(17) 0.0232(6) Uani 1 1 d . . . C4 C 0.2540(4) -0.0774(4) 0.16483(17) 0.0255(6) Uani 1 1 d . . . H4 H 0.2771 -0.1473 0.1300 0.031 Uiso 1 1 calc R . . C5 C 0.1448(4) 0.0638(4) 0.15354(17) 0.0233(6) Uani 1 1 d . . . C23 C 0.4382(4) -0.2191(4) 0.28157(19) 0.0279(6) Uani 1 1 d . . . H231 H 0.5235 -0.1684 0.3015 0.042 Uiso 1 1 calc R . . H232 H 0.4835 -0.2896 0.2480 0.042 Uiso 1 1 calc R . . H233 H 0.3840 -0.2815 0.3238 0.042 Uiso 1 1 calc R . . C25 C 0.0416(4) 0.1373(4) 0.08462(18) 0.0314(7) Uani 1 1 d . . . H251 H -0.0225 0.2324 0.0948 0.047 Uiso 1 1 calc R . . H252 H -0.0288 0.0598 0.0739 0.047 Uiso 1 1 calc R . . H253 H 0.1096 0.1671 0.0407 0.047 Uiso 1 1 calc R . . N3 N 0.2777(3) 0.2475(3) 0.33756(13) 0.0190(5) Uani 1 1 d . . . N23 N 0.1890(3) 0.4627(3) 0.40366(14) 0.0208(5) Uani 1 1 d . . . N13 N 0.0877(3) 0.5340(3) 0.34334(14) 0.0220(5) Uani 1 1 d . . . C53 C 0.1933(4) 0.5591(4) 0.45752(16) 0.0219(6) Uani 1 1 d . . . C43 C 0.0975(4) 0.6996(4) 0.42882(18) 0.0247(6) Uani 1 1 d . . . H43 H 0.0783 0.7903 0.4521 0.030 Uiso 1 1 calc R . . C33 C 0.0342(4) 0.6808(3) 0.35792(17) 0.0225(6) Uani 1 1 d . . . C35 C 0.2846(4) 0.5065(4) 0.53192(18) 0.0287(6) Uani 1 1 d . . . H351 H 0.2112 0.4685 0.5724 0.043 Uiso 1 1 calc R . . H352 H 0.3346 0.5968 0.5444 0.043 Uiso 1 1 calc R . . H353 H 0.3668 0.4203 0.5270 0.043 Uiso 1 1 calc R . . C331 C -0.0765(4) 0.7946(4) 0.30261(19) 0.0279(6) Uani 1 1 d . . . H133 H -0.0242 0.8907 0.2827 0.042 Uiso 1 1 calc R . . H333 H -0.1027 0.7429 0.2606 0.042 Uiso 1 1 calc R . . C16 C 0.2718(4) 0.0721(3) 0.34272(16) 0.0216(5) Uani 1 1 d . . . H161 H 0.3715 0.0140 0.3661 0.026 Uiso 1 1 calc R . . H162 H 0.1819 0.0361 0.3752 0.026 Uiso 1 1 calc R . . C17 C 0.2468(4) 0.2914(3) 0.41290(16) 0.0221(6) Uani 1 1 d . . . H171 H 0.3459 0.2695 0.4437 0.027 Uiso 1 1 calc R . . H172 H 0.1661 0.2261 0.4400 0.027 Uiso 1 1 calc R . . N11 N 0.2858(3) 0.4586(3) 0.18340(15) 0.0249(5) Uani 1 1 d . . . N12 N 0.4095(3) 0.3470(3) 0.21769(14) 0.0242(5) Uani 1 1 d . . . C13 C 0.3049(4) 0.4640(4) 0.10791(18) 0.0289(6) Uani 1 1 d . . . C14 C 0.4383(4) 0.3591(4) 0.09377(19) 0.0306(7) Uani 1 1 d . . . H14 H 0.4765 0.3428 0.0456 0.037 Uiso 1 1 calc R . . C15 C 0.5019(4) 0.2849(4) 0.16427(18) 0.0267(6) Uani 1 1 d . . . C31 C 0.1954(4) 0.5730(4) 0.0511(2) 0.0357(7) Uani 1 1 d . . . H311 H 0.1019 0.6129 0.0772 0.054 Uiso 1 1 calc R . . H312 H 0.1615 0.5141 0.0132 0.054 Uiso 1 1 calc R . . H313 H 0.2514 0.6628 0.0259 0.054 Uiso 1 1 calc R . . C51 C 0.6425(4) 0.1610(4) 0.1851(2) 0.0319(7) Uani 1 1 d . . . H511 H 0.7274 0.2088 0.2071 0.048 Uiso 1 1 calc R . . H512 H 0.6817 0.1227 0.1395 0.048 Uiso 1 1 calc R . . H513 H 0.6094 0.0715 0.2223 0.048 Uiso 1 1 calc R . . C18 C 0.4244(4) 0.3122(4) 0.30093(17) 0.0252(6) Uani 1 1 d . . . H181 H 0.4427 0.4110 0.3192 0.030 Uiso 1 1 calc R . . H182 H 0.5175 0.2334 0.3160 0.030 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 Cd 0.02343(13) 0.02219(13) 0.02074(13) -0.00377(8) 0.00064(8) -0.00245(8) S1 0.0411(5) 0.0355(4) 0.0309(4) -0.0017(4) -0.0013(3) 0.0076(4) S2 0.0307(4) 0.0296(4) 0.0206(4) 0.0030(3) 0.0007(3) -0.0076(3) N4 0.0343(16) 0.0353(15) 0.0342(16) -0.0066(13) -0.0031(12) -0.0041(12) N5 0.0290(14) 0.0329(14) 0.0297(14) -0.0102(12) 0.0067(11) -0.0079(11) C11 0.0275(16) 0.0338(16) 0.0238(15) -0.0097(13) 0.0021(11) -0.0031(12) C12 0.0241(14) 0.0231(14) 0.0235(14) -0.0070(12) -0.0012(11) -0.0030(11) N1 0.0206(12) 0.0230(12) 0.0179(11) -0.0012(9) 0.0003(8) -0.0021(9) N2 0.0222(12) 0.0183(11) 0.0184(11) -0.0023(9) -0.0019(8) -0.0003(9) C3 0.0229(14) 0.0216(13) 0.0254(14) -0.0042(11) 0.0041(10) -0.0046(10) C4 0.0300(16) 0.0258(14) 0.0229(14) -0.0105(12) 0.0045(11) -0.0031(11) C5 0.0211(14) 0.0290(15) 0.0201(14) -0.0039(12) 0.0005(10) -0.0062(11) C23 0.0274(16) 0.0239(14) 0.0307(16) -0.0018(13) 0.0041(12) -0.0006(11) C25 0.0302(17) 0.0422(18) 0.0212(15) -0.0043(14) -0.0027(12) -0.0036(13) N3 0.0254(12) 0.0157(10) 0.0154(11) -0.0013(9) 0.0001(8) -0.0022(8) N23 0.0284(13) 0.0172(11) 0.0166(11) -0.0023(9) 0.0010(9) -0.0028(9) N13 0.0242(12) 0.0220(12) 0.0192(12) -0.0022(9) -0.0005(9) -0.0028(9) C53 0.0244(14) 0.0264(14) 0.0166(13) -0.0055(11) 0.0049(10) -0.0084(11) C43 0.0258(15) 0.0214(13) 0.0283(15) -0.0073(12) 0.0064(11) -0.0052(11) C33 0.0233(14) 0.0197(13) 0.0242(14) -0.0028(11) 0.0044(11) -0.0028(10) C35 0.0315(16) 0.0354(16) 0.0198(14) -0.0057(13) 0.0005(11) -0.0057(13) C331 0.0256(15) 0.0252(14) 0.0304(16) -0.0009(13) -0.0015(12) 0.0018(11) C16 0.0284(15) 0.0175(13) 0.0186(13) -0.0023(11) -0.0029(10) -0.0021(10) C17 0.0306(15) 0.0184(13) 0.0163(13) -0.0012(10) -0.0008(10) -0.0009(10) N11 0.0272(13) 0.0259(12) 0.0204(12) -0.0009(10) 0.0008(9) -0.0030(10) N12 0.0265(13) 0.0242(12) 0.0206(12) -0.0019(10) -0.0005(9) -0.0006(9) C13 0.0326(17) 0.0305(16) 0.0233(15) -0.0015(13) 0.0005(12) -0.0089(12) C14 0.0319(17) 0.0369(17) 0.0243(15) -0.0053(13) 0.0055(12) -0.0110(13) C15 0.0245(15) 0.0291(15) 0.0288(16) -0.0083(13) 0.0055(11) -0.0093(12) C31 0.0390(19) 0.0396(18) 0.0256(16) 0.0026(14) -0.0024(13) -0.0057(15) C51 0.0294(17) 0.0317(16) 0.0368(18) -0.0111(14) 0.0035(13) -0.0048(13) C18 0.0260(15) 0.0263(14) 0.0221(14) -0.0020(12) -0.0035(11) -0.0019(11) _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 N4 2.176(3) . ? Cd N13 2.319(2) . ? Cd N5 2.338(3) . ? Cd N1 2.336(2) . ? Cd N11 2.400(3) . ? Cd N3 2.495(2) . ? S1 C11 1.603(3) . ? S2 C12 1.633(3) . ? N4 C11 1.154(5) . ? N5 C12 1.158(4) . ? N1 C5 1.322(4) . ? N1 N2 1.363(3) . ? N2 C3 1.353(4) . ? N2 C16 1.440(3) . ? C3 C4 1.366(4) . ? C3 C23 1.489(4) . ? C4 C5 1.403(4) . ? C4 H4 0.9300 . ? C5 C25 1.488(4) . ? C23 H231 0.9600 . ? C23 H232 0.9600 . ? C23 H233 0.9600 . ? C25 H251 0.9600 . ? C25 H252 0.9600 . ? C25 H253 0.9600 . ? N3 C17 1.453(3) . ? N3 C16 1.466(3) . ? N3 C18 1.472(4) . ? N23 N13 1.366(3) . ? N23 C53 1.359(4) . ? N23 C17 1.452(4) . ? N13 C33 1.339(4) . ? C53 C43 1.371(4) . ? C53 C35 1.487(4) . ? C43 C33 1.398(4) . ? C43 H43 0.9300 . ? C33 C331 1.482(4) . ? C35 H351 0.9600 . ? C35 H352 0.9600 . ? C35 H353 0.9600 . ? C331 H133 0.9600 . ? C331 H333 0.9600 . ? C16 H161 0.9700 . ? C16 H162 0.9700 . ? C17 H171 0.9700 . ? C17 H172 0.9700 . ? N11 C13 1.327(4) . ? N11 N12 1.380(3) . ? N12 C15 1.352(4) . ? N12 C18 1.441(4) . ? C13 C14 1.394(5) . ? C13 C31 1.473(5) . ? C14 C15 1.364(5) . ? C14 H14 0.9300 . ? C15 C51 1.483(5) . ? C31 H311 0.9600 . ? C31 H312 0.9600 . ? C31 H313 0.9600 . ? C51 H511 0.9600 . ? C51 H512 0.9600 . ? C51 H513 0.9600 . ? C18 H181 0.9700 . ? C18 H182 0.9700 . ? 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 Cd N13 107.63(10) . . ? N4 Cd N5 99.78(11) . . ? N13 Cd N5 86.34(9) . . ? N4 Cd N1 111.75(10) . . ? N13 Cd N1 140.62(9) . . ? N5 Cd N1 86.88(9) . . ? N4 Cd N11 102.87(10) . . ? N13 Cd N11 91.10(9) . . ? N5 Cd N11 156.89(10) . . ? N1 Cd N11 80.59(9) . . ? N4 Cd N3 175.89(9) . . ? N13 Cd N3 69.91(8) . . ? N5 Cd N3 83.46(9) . . ? N1 Cd N3 70.79(8) . . ? N11 Cd N3 74.12(8) . . ? C11 N4 Cd 156.5(3) . . ? C12 N5 Cd 174.1(3) . . ? N4 C11 S1 179.5(4) . . ? N5 C12 S2 179.2(3) . . ? C5 N1 N2 105.9(2) . . ? C5 N1 Cd 138.2(2) . . ? N2 N1 Cd 114.45(17) . . ? C3 N2 N1 111.2(2) . . ? C3 N2 C16 128.3(2) . . ? N1 N2 C16 120.1(2) . . ? N2 C3 C4 106.5(3) . . ? N2 C3 C23 122.8(3) . . ? C4 C3 C23 130.7(3) . . ? C3 C4 C5 106.2(3) . . ? C3 C4 H4 126.9 . . ? C5 C4 H4 126.9 . . ? N1 C5 C4 110.2(3) . . ? N1 C5 C25 120.9(3) . . ? C4 C5 C25 128.9(3) . . ? C3 C23 H231 109.5 . . ? C3 C23 H232 109.5 . . ? H231 C23 H232 109.5 . . ? C3 C23 H233 109.5 . . ? H231 C23 H233 109.5 . . ? H232 C23 H233 109.5 . . ? C5 C25 H251 109.5 . . ? C5 C25 H252 109.5 . . ? H251 C25 H252 109.5 . . ? C5 C25 H253 109.5 . . ? H251 C25 H253 109.5 . . ? H252 C25 H253 109.5 . . ? C17 N3 C16 110.2(2) . . ? C17 N3 C18 112.6(2) . . ? C16 N3 C18 114.9(2) . . ? C17 N3 Cd 107.13(17) . . ? C16 N3 Cd 105.00(17) . . ? C18 N3 Cd 106.27(16) . . ? N13 N23 C53 111.3(2) . . ? N13 N23 C17 120.0(2) . . ? C53 N23 C17 127.1(2) . . ? C33 N13 N23 105.8(2) . . ? C33 N13 Cd 137.8(2) . . ? N23 N13 Cd 116.35(17) . . ? N23 C53 C43 106.1(3) . . ? N23 C53 C35 122.7(3) . . ? C43 C53 C35 131.2(3) . . ? C53 C43 C33 107.0(3) . . ? C53 C43 H43 126.5 . . ? C33 C43 H43 126.5 . . ? N13 C33 C43 109.7(3) . . ? N13 C33 C331 120.5(3) . . ? C43 C33 C331 129.8(3) . . ? C53 C35 H351 109.5 . . ? C53 C35 H352 109.5 . . ? H351 C35 H352 109.5 . . ? C53 C35 H353 109.5 . . ? H351 C35 H353 109.5 . . ? H352 C35 H353 109.5 . . ? C33 C331 H133 109.5 . . ? C33 C331 H333 109.5 . . ? H133 C331 H333 109.5 . . ? N2 C16 N3 109.8(2) . . ? N2 C16 H161 109.7 . . ? N3 C16 H161 109.7 . . ? N2 C16 H162 109.7 . . ? N3 C16 H162 109.7 . . ? H161 C16 H162 108.2 . . ? N3 C17 N23 110.1(2) . . ? N3 C17 H171 109.6 . . ? N23 C17 H171 109.6 . . ? N3 C17 H172 109.6 . . ? N23 C17 H172 109.6 . . ? H171 C17 H172 108.2 . . ? C13 N11 N12 104.7(3) . . ? C13 N11 Cd 123.0(2) . . ? N12 N11 Cd 104.90(17) . . ? C15 N12 N11 111.6(2) . . ? C15 N12 C18 129.4(3) . . ? N11 N12 C18 119.1(2) . . ? N11 C13 C14 110.8(3) . . ? N11 C13 C31 121.0(3) . . ? C14 C13 C31 128.2(3) . . ? C15 C14 C13 106.7(3) . . ? C15 C14 H14 126.6 . . ? C13 C14 H14 126.6 . . ? N12 C15 C14 106.2(3) . . ? N12 C15 C51 122.9(3) . . ? C14 C15 C51 130.9(3) . . ? C13 C31 H311 109.5 . . ? C13 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C13 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C15 C51 H511 109.5 . . ? C15 C51 H512 109.5 . . ? H511 C51 H512 109.5 . . ? C15 C51 H513 109.5 . . ? H511 C51 H513 109.5 . . ? H512 C51 H513 109.5 . . ? N12 C18 N3 111.5(2) . . ? N12 C18 H181 109.3 . . ? N3 C18 H181 109.3 . . ? N12 C18 H182 109.3 . . ? N3 C18 H182 109.3 . . ? H181 C18 H182 108.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.748 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.048 ###############END OF CIF FILE