# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm #TrackingRef 'CSLcompounds.CIF' _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sheng-Run, Zheng' _publ_contact_author_email zhengshengrun@gmail.com _publ_section_title ; Anion-dependent assembly and solvent-mediated structural transformations of three Cd(II) coordination polymers based on 1H-imidazole-4-carboxylic acid ; loop_ _publ_author_name G.Kole G.Tan J.Vittal data_cslCd1 _database_code_depnum_ccdc_archive 'CCDC 840721' #TrackingRef 'CSLcompounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 Cd N4 O5' _chemical_formula_weight 352.58 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc ' 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 6.7174(13) _cell_length_b 22.973(5) _cell_length_c 7.2182(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.255(2) _cell_angle_gamma 90.00 _cell_volume 1096.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2942 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.97 _exptl_crystal_description BLOCK _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 2.014 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5834 _exptl_absorpt_correction_T_max 0.6436 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 5554 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.24 _reflns_number_total 1971 _reflns_number_gt 1755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.5027P] 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 1971 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.18372(3) 0.638768(9) 0.84057(3) 0.02081(9) Uani 1 1 d . . . C1 C -0.1924(5) 0.55359(12) 0.7748(4) 0.0213(6) Uani 1 1 d . . . C2 C -0.1328(4) 0.56191(12) 0.5893(4) 0.0215(6) Uani 1 1 d . . . C3 C -0.2251(5) 0.54596(14) 0.4135(4) 0.0286(7) Uani 1 1 d . . . H3 H -0.3447 0.5250 0.3817 0.034 Uiso 1 1 calc R . . C4 C 0.0494(5) 0.59433(14) 0.3964(4) 0.0324(8) Uani 1 1 d . . . H4A H 0.1518 0.6126 0.3467 0.039 Uiso 1 1 calc R . . C5 C 0.1776(5) 0.76508(12) 0.6723(4) 0.0202(6) Uani 1 1 d . . . C6 C 0.3866(4) 0.75497(12) 0.7747(4) 0.0200(6) Uani 1 1 d . . . C7 C 0.5404(5) 0.79265(13) 0.8357(4) 0.0277(7) Uani 1 1 d . . . H7 H 0.5393 0.8328 0.8197 0.033 Uiso 1 1 calc R . . C8 C 0.6370(4) 0.70394(14) 0.9159(4) 0.0270(7) Uani 1 1 d . . . H8 H 0.7175 0.6728 0.9661 0.032 Uiso 1 1 calc R . . N1 N 0.0410(4) 0.59230(10) 0.5757(3) 0.0252(6) Uani 1 1 d . . . N2 N -0.1072(4) 0.56691(12) 0.2937(4) 0.0328(7) Uani 1 1 d . . . H2 H -0.1297 0.5631 0.1732 0.039 Uiso 1 1 calc R . . N3 N 0.4486(4) 0.69903(10) 0.8259(3) 0.0216(5) Uani 1 1 d . . . N4 N 0.6965(4) 0.75944(12) 0.9252(4) 0.0301(6) Uani 1 1 d . . . H4 H 0.8133 0.7721 0.9785 0.036 Uiso 1 1 calc R . . O1 O -0.0834(3) 0.57869(9) 0.9140(3) 0.0279(5) Uani 1 1 d . . . O1W O 0.4074(3) 0.57288(10) 1.0026(3) 0.0385(6) Uani 1 1 d . . . H1WA H 0.3517 0.5455 1.0531 0.046 Uiso 1 1 d R . . H1WB H 0.4877 0.5589 0.9352 0.046 Uiso 1 1 d R . . O2 O -0.3437(3) 0.52302(10) 0.7855(3) 0.0321(5) Uani 1 1 d . . . O3 O 0.0584(3) 0.72247(8) 0.6616(3) 0.0292(5) Uani 1 1 d . . . O4 O 0.1299(3) 0.81463(8) 0.6048(3) 0.0255(5) 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 0.02263(14) 0.01937(13) 0.01975(14) -0.00017(8) 0.00190(9) -0.00368(8) C1 0.0268(17) 0.0185(14) 0.0190(16) -0.0009(12) 0.0051(12) -0.0023(12) C2 0.0269(17) 0.0195(14) 0.0176(15) -0.0012(12) 0.0028(12) -0.0028(12) C3 0.0301(18) 0.0337(18) 0.0213(17) -0.0024(13) 0.0024(14) -0.0053(14) C4 0.042(2) 0.0326(18) 0.0250(18) 0.0041(14) 0.0130(15) -0.0088(15) C5 0.0230(16) 0.0230(15) 0.0143(15) 0.0005(12) 0.0026(12) 0.0020(12) C6 0.0189(15) 0.0213(14) 0.0197(16) 0.0021(12) 0.0037(12) -0.0023(12) C7 0.0288(18) 0.0245(16) 0.0294(18) 0.0001(13) 0.0039(14) -0.0040(13) C8 0.0176(16) 0.0328(17) 0.0295(18) 0.0033(14) 0.0012(13) 0.0008(13) N1 0.0348(15) 0.0257(13) 0.0162(14) -0.0006(10) 0.0073(11) -0.0092(11) N2 0.0486(18) 0.0372(15) 0.0122(14) -0.0002(11) 0.0043(12) -0.0028(13) N3 0.0187(13) 0.0220(12) 0.0230(14) 0.0020(10) 0.0007(10) 0.0009(10) N4 0.0168(14) 0.0424(16) 0.0288(15) -0.0022(12) -0.0026(11) -0.0066(12) O1 0.0345(13) 0.0336(12) 0.0162(11) -0.0042(9) 0.0061(9) -0.0117(10) O1W 0.0392(14) 0.0346(13) 0.0461(15) 0.0160(11) 0.0196(12) 0.0090(11) O2 0.0318(13) 0.0382(13) 0.0281(13) 0.0006(10) 0.0102(10) -0.0153(10) O3 0.0194(11) 0.0249(11) 0.0381(13) 0.0061(10) -0.0086(10) -0.0025(9) O4 0.0316(12) 0.0207(10) 0.0244(12) 0.0059(9) 0.0052(9) 0.0059(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 Cd1 N1 2.250(2) . ? Cd1 N3 2.272(2) . ? Cd1 O4 2.272(2) 4_576 ? Cd1 O1W 2.300(2) . ? Cd1 O3 2.385(2) . ? Cd1 O1 2.397(2) . ? C1 O2 1.249(4) . ? C1 O1 1.271(3) . ? C1 C2 1.477(4) . ? C2 C3 1.360(4) . ? C2 N1 1.379(4) . ? C3 N2 1.361(4) . ? C3 H3 0.9300 . ? C4 N1 1.307(4) . ? C4 N2 1.333(4) . ? C4 H4A 0.9300 . ? C5 O4 1.257(3) . ? C5 O3 1.258(3) . ? C5 C6 1.484(4) . ? C6 C7 1.360(4) . ? C6 N3 1.381(4) . ? C7 N4 1.363(4) . ? C7 H7 0.9300 . ? C8 N3 1.321(4) . ? C8 N4 1.334(4) . ? C8 H8 0.9300 . ? N2 H2 0.8600 . ? N4 H4 0.8600 . ? O1W H1WA 0.8467 . ? O1W H1WB 0.8509 . ? O4 Cd1 2.272(2) 4_575 ? 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 N3 117.93(9) . . ? N1 Cd1 O4 146.06(9) . 4_576 ? N3 Cd1 O4 89.72(8) . 4_576 ? N1 Cd1 O1W 105.11(9) . . ? N3 Cd1 O1W 88.78(8) . . ? O4 Cd1 O1W 94.04(8) 4_576 . ? N1 Cd1 O3 82.32(8) . . ? N3 Cd1 O3 71.77(8) . . ? O4 Cd1 O3 88.93(8) 4_576 . ? O1W Cd1 O3 160.32(8) . . ? N1 Cd1 O1 72.07(8) . . ? N3 Cd1 O1 169.96(8) . . ? O4 Cd1 O1 81.27(7) 4_576 . ? O1W Cd1 O1 87.46(8) . . ? O3 Cd1 O1 112.22(8) . . ? O2 C1 O1 124.5(3) . . ? O2 C1 C2 118.9(3) . . ? O1 C1 C2 116.6(3) . . ? C3 C2 N1 108.7(3) . . ? C3 C2 C1 131.2(3) . . ? N1 C2 C1 120.0(2) . . ? C2 C3 N2 106.1(3) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? N1 C4 N2 111.4(3) . . ? N1 C4 H4A 124.3 . . ? N2 C4 H4A 124.3 . . ? O4 C5 O3 124.4(3) . . ? O4 C5 C6 119.2(3) . . ? O3 C5 C6 116.4(2) . . ? C7 C6 N3 109.3(3) . . ? C7 C6 C5 131.2(3) . . ? N3 C6 C5 119.5(2) . . ? C6 C7 N4 105.9(3) . . ? C6 C7 H7 127.1 . . ? N4 C7 H7 127.1 . . ? N3 C8 N4 111.0(3) . . ? N3 C8 H8 124.5 . . ? N4 C8 H8 124.5 . . ? C4 N1 C2 106.0(2) . . ? C4 N1 Cd1 137.6(2) . . ? C2 N1 Cd1 114.71(19) . . ? C4 N2 C3 107.7(3) . . ? C4 N2 H2 126.1 . . ? C3 N2 H2 126.1 . . ? C8 N3 C6 105.6(2) . . ? C8 N3 Cd1 136.0(2) . . ? C6 N3 Cd1 112.25(18) . . ? C8 N4 C7 108.2(3) . . ? C8 N4 H4 125.9 . . ? C7 N4 H4 125.9 . . ? C1 O1 Cd1 115.76(18) . . ? Cd1 O1W H1WA 114.1 . . ? Cd1 O1W H1WB 112.4 . . ? H1WA O1W H1WB 109.8 . . ? C5 O3 Cd1 115.76(17) . . ? C5 O4 Cd1 133.2(2) . 4_575 ? 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 O1W H1WB O2 0.85 1.89 2.738(3) 176.2 1_655 O1W H1WA O2 0.85 1.96 2.759(3) 155.7 3_567 N2 H2 O1 0.86 1.98 2.786(3) 155.1 1_554 N4 H4 O3 0.86 1.92 2.742(3) 158.5 4_676 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.602 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.085 ##################################################################### data_cslCd2 _database_code_depnum_ccdc_archive 'CCDC 840722' #TrackingRef 'CSLcompounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Cd N4 O4' _chemical_formula_weight 334.57 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' 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 'Fdd2 ' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 11.2987(13) _cell_length_b 19.407(2) _cell_length_c 8.4415(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1851.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2125 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 27.86 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 2.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4824 _exptl_absorpt_correction_T_max 0.5566 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 2300 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.19 _reflns_number_total 785 _reflns_number_gt 767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+4.8530P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(8) _refine_ls_number_reflns 785 _refine_ls_number_parameters 78 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.2500 0.2500 1.13668(17) 0.01914(19) Uani 1 2 d S . . C1 C 0.3326(4) 0.3990(3) 1.0885(7) 0.0215(11) Uani 1 1 d . . . C2 C 0.2244(5) 0.3947(3) 0.9891(7) 0.0197(11) Uani 1 1 d . . . C3 C 0.0735(4) 0.4076(3) 0.8326(6) 0.0182(10) Uani 1 1 d U . . H3 H 0.0174 0.4268 0.7652 0.022 Uiso 1 1 calc R . . C4 C 0.0799(4) 0.3419(3) 0.8772(7) 0.0254(12) Uani 1 1 d . . . H4 H 0.0266 0.3081 0.8454 0.030 Uiso 1 1 calc R . . N1 N 0.1691(4) 0.3306(2) 0.9702(5) 0.0216(9) Uani 1 1 d . . . N2 N 0.1635(4) 0.4411(3) 0.9033(7) 0.0390(13) Uani 1 1 d U . . H2 H 0.1792 0.4843 0.8951 0.047 Uiso 1 1 calc R . . O1 O 0.3659(3) 0.34641(19) 1.1558(5) 0.0291(9) Uani 1 1 d . . . O2 O 0.3860(3) 0.45712(18) 1.0985(5) 0.0241(8) 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 0.0205(3) 0.0138(3) 0.0231(3) 0.000 0.000 -0.00029(19) C1 0.017(2) 0.026(3) 0.022(3) 0.002(2) -0.001(2) -0.0022(19) C2 0.020(2) 0.017(3) 0.022(3) 0.002(2) -0.003(2) -0.003(2) C3 0.018(2) 0.023(3) 0.013(3) 0.004(2) -0.0027(17) 0.0093(17) C4 0.020(3) 0.031(3) 0.025(3) -0.004(2) -0.002(2) -0.004(2) N1 0.024(2) 0.022(2) 0.019(2) -0.0014(17) -0.0060(18) -0.0031(19) N2 0.044(3) 0.033(3) 0.040(3) -0.003(2) -0.015(3) -0.002(2) O1 0.0264(19) 0.0196(18) 0.041(3) 0.0087(18) -0.0119(17) -0.0051(15) O2 0.0255(17) 0.0202(17) 0.027(2) 0.0013(16) -0.0007(16) -0.0093(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 O1 2.290(4) . ? Cd1 O1 2.290(4) 14 ? Cd1 N1 2.293(5) 14 ? Cd1 N1 2.293(5) . ? Cd1 O2 2.355(4) 16_545 ? Cd1 O2 2.355(4) 15_455 ? C1 O1 1.228(6) . ? C1 O2 1.281(6) . ? C1 C2 1.485(7) . ? C2 N2 1.344(8) . ? C2 N1 1.402(7) . ? C3 C4 1.332(7) . ? C3 N2 1.346(7) . ? C3 H3 0.9300 . ? C4 N1 1.296(7) . ? C4 H4 0.9300 . ? N2 H2 0.8600 . ? O2 Cd1 2.355(4) 7_554 ? 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 O1 Cd1 O1 171.9(2) . 14 ? O1 Cd1 N1 111.87(16) . 14 ? O1 Cd1 N1 73.37(15) 14 14 ? O1 Cd1 N1 73.37(15) . . ? O1 Cd1 N1 111.87(16) 14 . ? N1 Cd1 N1 104.4(2) 14 . ? O1 Cd1 O2 85.55(13) . 16_545 ? O1 Cd1 O2 88.32(15) 14 16_545 ? N1 Cd1 O2 90.35(14) 14 16_545 ? N1 Cd1 O2 157.56(14) . 16_545 ? O1 Cd1 O2 88.32(15) . 15_455 ? O1 Cd1 O2 85.55(13) 14 15_455 ? N1 Cd1 O2 157.56(14) 14 15_455 ? N1 Cd1 O2 90.35(14) . 15_455 ? O2 Cd1 O2 81.25(18) 16_545 15_455 ? O1 C1 O2 123.8(5) . . ? O1 C1 C2 117.8(5) . . ? O2 C1 C2 118.3(5) . . ? N2 C2 N1 107.7(5) . . ? N2 C2 C1 133.5(5) . . ? N1 C2 C1 118.8(5) . . ? C4 C3 N2 107.2(5) . . ? C4 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? N1 C4 C3 112.0(5) . . ? N1 C4 H4 124.0 . . ? C3 C4 H4 124.0 . . ? C4 N1 C2 105.4(5) . . ? C4 N1 Cd1 142.8(4) . . ? C2 N1 Cd1 111.0(3) . . ? C2 N2 C3 107.6(5) . . ? C2 N2 H2 126.2 . . ? C3 N2 H2 126.2 . . ? C1 O1 Cd1 118.1(3) . . ? C1 O2 Cd1 121.2(4) . 7_554 ? 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 O1 C1 C2 N2 178.7(6) . . . . ? O2 C1 C2 N2 -1.6(10) . . . . ? O1 C1 C2 N1 -3.2(8) . . . . ? O2 C1 C2 N1 176.4(5) . . . . ? N2 C3 C4 N1 -0.9(7) . . . . ? C3 C4 N1 C2 0.8(6) . . . . ? C3 C4 N1 Cd1 168.6(5) . . . . ? N2 C2 N1 C4 -0.4(6) . . . . ? C1 C2 N1 C4 -178.9(5) . . . . ? N2 C2 N1 Cd1 -172.5(4) . . . . ? C1 C2 N1 Cd1 9.0(6) . . . . ? O1 Cd1 N1 C4 -175.2(6) . . . . ? O1 Cd1 N1 C4 -1.8(7) 14 . . . ? N1 Cd1 N1 C4 75.8(6) 14 . . . ? O2 Cd1 N1 C4 -154.5(5) 16_545 . . . ? O2 Cd1 N1 C4 -87.1(6) 15_455 . . . ? O1 Cd1 N1 C2 -7.9(4) . . . . ? O1 Cd1 N1 C2 165.6(3) 14 . . . ? N1 Cd1 N1 C2 -116.9(4) 14 . . . ? O2 Cd1 N1 C2 12.8(7) 16_545 . . . ? O2 Cd1 N1 C2 80.2(4) 15_455 . . . ? N1 C2 N2 C3 -0.1(7) . . . . ? C1 C2 N2 C3 178.1(6) . . . . ? C4 C3 N2 C2 0.6(7) . . . . ? O2 C1 O1 Cd1 175.6(4) . . . . ? C2 C1 O1 Cd1 -4.7(7) . . . . ? O1 Cd1 O1 C1 -124.3(4) 14 . . . ? N1 Cd1 O1 C1 106.4(4) 14 . . . ? N1 Cd1 O1 C1 7.2(4) . . . . ? O2 Cd1 O1 C1 -165.1(4) 16_545 . . . ? O2 Cd1 O1 C1 -83.7(4) 15_455 . . . ? O1 C1 O2 Cd1 105.4(6) . . . 7_554 ? C2 C1 O2 Cd1 -74.2(5) . . . 7_554 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.649 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.108 ########################################################################## data_cslCd3 _database_code_depnum_ccdc_archive 'CCDC 840723' #TrackingRef 'CSLcompounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 Cd2 N4 O10 S' _chemical_formula_weight 579.06 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' 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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3478(17) _cell_length_b 7.609(2) _cell_length_c 17.406(5) _cell_angle_alpha 84.001(3) _cell_angle_beta 89.051(3) _cell_angle_gamma 66.246(3) _cell_volume 765.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2792 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 27.90 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 2.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3974 _exptl_absorpt_correction_T_max 0.4491 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 3886 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.25 _reflns_number_total 2683 _reflns_number_gt 2438 _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^)+(0.0907P)^2^+18.3555P] 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 2683 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1877 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.14378(13) 0.00219(11) 0.19315(4) 0.0184(3) Uani 1 1 d . . . Cd2 Cd -0.30847(13) 0.88626(11) 0.32127(4) 0.0177(3) Uani 1 1 d . . . C1 C 0.6035(19) 0.0526(16) 0.1454(7) 0.021(2) Uani 1 1 d . . . C2 C 0.4335(19) 0.1456(16) 0.0809(6) 0.019(2) Uani 1 1 d . . . C3 C 0.455(2) 0.2440(17) 0.0118(7) 0.024(2) Uani 1 1 d . . . H3 H 0.5802 0.2706 -0.0043 0.028 Uiso 1 1 calc R . . C4 C 0.119(2) 0.2266(19) 0.0158(7) 0.029(3) Uani 1 1 d . . . H4 H -0.0273 0.2399 0.0007 0.035 Uiso 1 1 calc R . . C5 C 0.188(2) -0.1533(17) 0.3688(7) 0.023(2) Uani 1 1 d . . . C6 C 0.0873(19) -0.2086(17) 0.4401(6) 0.020(2) Uani 1 1 d . . . C7 C 0.181(2) -0.283(2) 0.5128(7) 0.037(3) Uani 1 1 d . . . H7 H 0.3306 -0.3122 0.5297 0.044 Uiso 1 1 calc R . . C8 C -0.177(2) -0.243(2) 0.5108(7) 0.033(3) Uani 1 1 d . . . H8 H -0.3169 -0.2426 0.5274 0.039 Uiso 1 1 calc R . . N1 N 0.2190(16) 0.1404(14) 0.0821(5) 0.022(2) Uani 1 1 d . . . N2 N 0.2509(17) 0.2934(15) -0.0276(6) 0.026(2) Uani 1 1 d . . . H2 H 0.2143 0.3568 -0.0727 0.031 Uiso 1 1 calc R . . N3 N -0.1416(17) -0.1810(14) 0.4408(6) 0.024(2) Uani 1 1 d . . . N4 N 0.012(2) -0.306(2) 0.5547(6) 0.042(3) Uani 1 1 d . . . H4A H 0.0248 -0.3538 0.6023 0.050 Uiso 1 1 calc R . . O1 O 0.5342(13) -0.0297(12) 0.2027(5) 0.0238(17) Uani 1 1 d . . . O1W O 0.2818(16) -0.3030(13) 0.1541(5) 0.033(2) Uani 1 1 d . . . H1WA H 0.4114 -0.3986 0.1606 0.040 Uiso 1 1 d R . . H1WB H 0.1803 -0.3467 0.1475 0.040 Uiso 1 1 d R . . O2W O -0.4983(15) 1.2230(12) 0.3289(5) 0.032(2) Uani 1 1 d . . . H2WA H -0.4614 1.3109 0.3065 0.038 Uiso 1 1 d R . . H2WB H -0.6404 1.2548 0.3190 0.038 Uiso 1 1 d R . . O2 O 0.7961(14) 0.0571(14) 0.1401(5) 0.031(2) Uani 1 1 d . . . O3 O 0.0603(14) -0.1049(13) 0.3086(4) 0.0258(18) Uani 1 1 d . . . O4 O 0.3836(15) -0.1589(16) 0.3737(6) 0.039(2) Uani 1 1 d . . . O5 O 0.0826(15) 0.2688(12) 0.2589(5) 0.0300(19) Uani 1 1 d . . . O6 O -0.0598(16) 0.5624(14) 0.1714(5) 0.035(2) Uani 1 1 d . . . O7 O -0.1286(19) 0.5656(12) 0.3077(5) 0.040(2) Uani 1 1 d . . . O8 O -0.3196(16) 0.4334(15) 0.2271(6) 0.043(2) Uani 1 1 d . . . S1 S -0.1092(5) 0.4594(4) 0.23982(16) 0.0182(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 Cd1 0.0166(4) 0.0260(5) 0.0142(4) 0.0011(3) 0.0016(3) -0.0110(3) Cd2 0.0159(4) 0.0225(5) 0.0148(4) 0.0013(3) -0.0007(3) -0.0084(3) C1 0.018(5) 0.022(6) 0.023(6) -0.006(5) 0.000(4) -0.008(4) C2 0.024(6) 0.026(6) 0.012(5) -0.001(4) 0.006(4) -0.016(5) C3 0.020(6) 0.029(6) 0.023(6) 0.003(5) 0.004(4) -0.012(5) C4 0.016(5) 0.039(7) 0.028(7) 0.004(5) -0.004(5) -0.008(5) C5 0.023(6) 0.031(6) 0.020(6) 0.000(5) 0.010(5) -0.016(5) C6 0.024(6) 0.031(6) 0.010(5) 0.001(4) -0.001(4) -0.018(5) C7 0.027(7) 0.064(9) 0.023(7) 0.014(6) -0.010(5) -0.025(7) C8 0.031(7) 0.058(9) 0.020(6) -0.004(6) 0.005(5) -0.029(6) N1 0.018(5) 0.027(5) 0.020(5) 0.003(4) 0.002(4) -0.008(4) N2 0.027(5) 0.029(5) 0.019(5) 0.014(4) -0.010(4) -0.010(4) N3 0.023(5) 0.028(5) 0.022(5) 0.002(4) 0.001(4) -0.012(4) N4 0.051(7) 0.076(9) 0.015(5) 0.009(5) -0.004(5) -0.046(7) O1 0.017(4) 0.029(4) 0.019(4) 0.003(3) -0.002(3) -0.004(3) O1W 0.027(5) 0.029(5) 0.043(5) -0.007(4) 0.003(4) -0.010(4) O2W 0.028(5) 0.027(4) 0.036(5) 0.001(4) -0.004(4) -0.007(4) O2 0.018(4) 0.047(5) 0.035(5) 0.005(4) -0.005(4) -0.021(4) O3 0.027(4) 0.040(5) 0.014(4) 0.006(3) 0.004(3) -0.021(4) O4 0.022(5) 0.069(7) 0.037(5) 0.007(5) 0.001(4) -0.031(5) O5 0.027(4) 0.024(4) 0.030(5) -0.005(4) -0.005(4) 0.001(4) O6 0.038(5) 0.045(5) 0.021(4) 0.010(4) -0.005(4) -0.020(4) O7 0.068(7) 0.015(4) 0.023(5) 0.002(3) -0.010(4) -0.002(4) O8 0.024(5) 0.050(6) 0.058(7) 0.014(5) -0.007(4) -0.022(4) S1 0.0194(13) 0.0154(12) 0.0175(13) 0.0017(10) -0.0026(10) -0.0054(10) _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 O3 2.227(7) . ? Cd1 N1 2.240(9) . ? Cd1 O2 2.268(8) 1_455 ? Cd1 O1W 2.300(9) . ? Cd1 O5 2.326(8) . ? Cd1 O1 2.398(8) . ? Cd2 O1 2.223(8) 1_465 ? Cd2 N3 2.264(10) 1_565 ? Cd2 O7 2.276(9) . ? Cd2 O4 2.278(8) 1_465 ? Cd2 O2W 2.369(9) . ? Cd2 O3 2.374(8) 1_565 ? C1 O2 1.239(14) . ? C1 O1 1.287(14) . ? C1 C2 1.478(16) . ? C2 N1 1.378(14) . ? C2 C3 1.383(16) . ? C3 N2 1.367(15) . ? C3 H3 0.9300 . ? C4 N1 1.303(16) . ? C4 N2 1.333(16) . ? C4 H4 0.9300 . ? C5 O4 1.232(14) . ? C5 O3 1.262(15) . ? C5 C6 1.484(15) . ? C6 C7 1.370(16) . ? C6 N3 1.382(15) . ? C7 N4 1.345(17) . ? C7 H7 0.9300 . ? C8 N3 1.308(16) . ? C8 N4 1.319(18) . ? C8 H8 0.9300 . ? N2 H2 0.8600 . ? N3 Cd2 2.264(10) 1_545 ? N4 H4A 0.8600 . ? O1 Cd2 2.223(8) 1_645 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8499 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O2 Cd1 2.268(8) 1_655 ? O3 Cd2 2.374(8) 1_545 ? O4 Cd2 2.278(8) 1_645 ? O5 S1 1.479(8) . ? O6 S1 1.456(9) . ? O7 S1 1.476(9) . ? O8 S1 1.450(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 N1 173.8(3) . . ? O3 Cd1 O2 93.3(3) . 1_455 ? N1 Cd1 O2 87.8(3) . 1_455 ? O3 Cd1 O1W 91.4(3) . . ? N1 Cd1 O1W 94.7(3) . . ? O2 Cd1 O1W 88.5(3) 1_455 . ? O3 Cd1 O5 80.5(3) . . ? N1 Cd1 O5 93.3(3) . . ? O2 Cd1 O5 105.4(3) 1_455 . ? O1W Cd1 O5 164.2(3) . . ? O3 Cd1 O1 106.6(3) . . ? N1 Cd1 O1 72.7(3) . . ? O2 Cd1 O1 159.9(3) 1_455 . ? O1W Cd1 O1 88.2(3) . . ? O5 Cd1 O1 81.2(3) . . ? O1 Cd2 N3 175.9(3) 1_465 1_565 ? O1 Cd2 O7 95.2(3) 1_465 . ? N3 Cd2 O7 87.7(3) 1_565 . ? O1 Cd2 O4 93.7(3) 1_465 1_465 ? N3 Cd2 O4 89.0(3) 1_565 1_465 ? O7 Cd2 O4 90.5(4) . 1_465 ? O1 Cd2 O2W 82.1(3) 1_465 . ? N3 Cd2 O2W 94.9(3) 1_565 . ? O7 Cd2 O2W 177.2(3) . . ? O4 Cd2 O2W 90.4(4) 1_465 . ? O1 Cd2 O3 105.0(3) 1_465 1_565 ? N3 Cd2 O3 72.3(3) 1_565 1_565 ? O7 Cd2 O3 86.5(4) . 1_565 ? O4 Cd2 O3 161.2(3) 1_465 1_565 ? O2W Cd2 O3 93.5(3) . 1_565 ? O2 C1 O1 126.0(11) . . ? O2 C1 C2 119.0(10) . . ? O1 C1 C2 115.0(9) . . ? N1 C2 C3 108.9(10) . . ? N1 C2 C1 122.0(9) . . ? C3 C2 C1 129.1(10) . . ? N2 C3 C2 104.9(10) . . ? N2 C3 H3 127.6 . . ? C2 C3 H3 127.6 . . ? N1 C4 N2 111.6(10) . . ? N1 C4 H4 124.2 . . ? N2 C4 H4 124.2 . . ? O4 C5 O3 126.6(10) . . ? O4 C5 C6 117.8(11) . . ? O3 C5 C6 115.6(10) . . ? C7 C6 N3 108.1(10) . . ? C7 C6 C5 131.4(11) . . ? N3 C6 C5 120.5(10) . . ? N4 C7 C6 106.0(11) . . ? N4 C7 H7 127.0 . . ? C6 C7 H7 127.0 . . ? N3 C8 N4 111.3(11) . . ? N3 C8 H8 124.3 . . ? N4 C8 H8 124.3 . . ? C4 N1 C2 106.2(10) . . ? C4 N1 Cd1 139.6(8) . . ? C2 N1 Cd1 114.1(7) . . ? C4 N2 C3 108.4(9) . . ? C4 N2 H2 125.8 . . ? C3 N2 H2 125.8 . . ? C8 N3 C6 105.9(10) . . ? C8 N3 Cd2 138.8(8) . 1_545 ? C6 N3 Cd2 113.3(7) . 1_545 ? C8 N4 C7 108.7(11) . . ? C8 N4 H4A 125.6 . . ? C7 N4 H4A 125.6 . . ? C1 O1 Cd2 126.0(7) . 1_645 ? C1 O1 Cd1 115.9(7) . . ? Cd2 O1 Cd1 115.1(3) 1_645 . ? Cd1 O1W H1WA 132.7 . . ? Cd1 O1W H1WB 115.1 . . ? H1WA O1W H1WB 107.7 . . ? Cd2 O2W H2WA 126.9 . . ? Cd2 O2W H2WB 107.2 . . ? H2WA O2W H2WB 107.7 . . ? C1 O2 Cd1 150.5(8) . 1_655 ? C5 O3 Cd1 125.8(7) . . ? C5 O3 Cd2 117.1(7) . 1_545 ? Cd1 O3 Cd2 117.1(3) . 1_545 ? C5 O4 Cd2 151.7(8) . 1_645 ? S1 O5 Cd1 123.4(5) . . ? S1 O7 Cd2 130.9(5) . . ? O8 S1 O6 110.1(6) . . ? O8 S1 O7 110.5(7) . . ? O6 S1 O7 110.3(6) . . ? O8 S1 O5 109.5(6) . . ? O6 S1 O5 110.8(6) . . ? O7 S1 O5 105.7(5) . . ? 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 C1 C2 N1 177.9(11) . . . . ? O1 C1 C2 N1 -1.2(16) . . . . ? O2 C1 C2 C3 -0.6(19) . . . . ? O1 C1 C2 C3 -179.7(11) . . . . ? N1 C2 C3 N2 -0.8(13) . . . . ? C1 C2 C3 N2 177.8(11) . . . . ? O4 C5 C6 C7 -6(2) . . . . ? O3 C5 C6 C7 173.6(14) . . . . ? O4 C5 C6 N3 171.4(11) . . . . ? O3 C5 C6 N3 -8.7(17) . . . . ? N3 C6 C7 N4 2.3(16) . . . . ? C5 C6 C7 N4 -179.8(13) . . . . ? N2 C4 N1 C2 -2.0(15) . . . . ? N2 C4 N1 Cd1 175.3(9) . . . . ? C3 C2 N1 C4 1.8(14) . . . . ? C1 C2 N1 C4 -177.0(11) . . . . ? C3 C2 N1 Cd1 -176.4(8) . . . . ? C1 C2 N1 Cd1 4.9(13) . . . . ? O3 Cd1 N1 C4 -97(3) . . . . ? O2 Cd1 N1 C4 3.5(14) 1_455 . . . ? O1W Cd1 N1 C4 91.7(14) . . . . ? O5 Cd1 N1 C4 -101.9(14) . . . . ? O1 Cd1 N1 C4 178.4(14) . . . . ? O3 Cd1 N1 C2 80(3) . . . . ? O2 Cd1 N1 C2 -179.3(8) 1_455 . . . ? O1W Cd1 N1 C2 -91.0(8) . . . . ? O5 Cd1 N1 C2 75.4(8) . . . . ? O1 Cd1 N1 C2 -4.3(7) . . . . ? N1 C4 N2 C3 1.6(15) . . . . ? C2 C3 N2 C4 -0.4(14) . . . . ? N4 C8 N3 C6 0.6(16) . . . . ? N4 C8 N3 Cd2 162.3(10) . . . 1_545 ? C7 C6 N3 C8 -1.8(15) . . . . ? C5 C6 N3 C8 -180.0(11) . . . . ? C7 C6 N3 Cd2 -168.8(9) . . . 1_545 ? C5 C6 N3 Cd2 13.0(13) . . . 1_545 ? N3 C8 N4 C7 0.8(19) . . . . ? C6 C7 N4 C8 -1.9(18) . . . . ? O2 C1 O1 Cd2 18.7(16) . . . 1_645 ? C2 C1 O1 Cd2 -162.3(7) . . . 1_645 ? O2 C1 O1 Cd1 178.1(9) . . . . ? C2 C1 O1 Cd1 -2.9(12) . . . . ? O3 Cd1 O1 C1 -169.5(7) . . . . ? N1 Cd1 O1 C1 4.0(8) . . . . ? O2 Cd1 O1 C1 18.9(14) 1_455 . . . ? O1W Cd1 O1 C1 99.6(8) . . . . ? O5 Cd1 O1 C1 -92.2(8) . . . . ? O3 Cd1 O1 Cd2 -7.8(5) . . . 1_645 ? N1 Cd1 O1 Cd2 165.7(5) . . . 1_645 ? O2 Cd1 O1 Cd2 -179.4(7) 1_455 . . 1_645 ? O1W Cd1 O1 Cd2 -98.7(4) . . . 1_645 ? O5 Cd1 O1 Cd2 69.5(4) . . . 1_645 ? O1 C1 O2 Cd1 -9(3) . . . 1_655 ? C2 C1 O2 Cd1 171.8(12) . . . 1_655 ? O4 C5 O3 Cd1 -3.7(19) . . . . ? C6 C5 O3 Cd1 176.3(7) . . . . ? O4 C5 O3 Cd2 179.6(11) . . . 1_545 ? C6 C5 O3 Cd2 -0.3(14) . . . 1_545 ? N1 Cd1 O3 C5 -76(3) . . . . ? O2 Cd1 O3 C5 -176.2(10) 1_455 . . . ? O1W Cd1 O3 C5 95.2(10) . . . . ? O5 Cd1 O3 C5 -71.1(10) . . . . ? O1 Cd1 O3 C5 6.7(10) . . . . ? N1 Cd1 O3 Cd2 101(3) . . . 1_545 ? O2 Cd1 O3 Cd2 0.4(4) 1_455 . . 1_545 ? O1W Cd1 O3 Cd2 -88.1(4) . . . 1_545 ? O5 Cd1 O3 Cd2 105.5(4) . . . 1_545 ? O1 Cd1 O3 Cd2 -176.7(3) . . . 1_545 ? O3 C5 O4 Cd2 2(3) . . . 1_645 ? C6 C5 O4 Cd2 -177.6(14) . . . 1_645 ? O3 Cd1 O5 S1 -114.4(6) . . . . ? N1 Cd1 O5 S1 65.1(6) . . . . ? O2 Cd1 O5 S1 -23.5(7) 1_455 . . . ? O1W Cd1 O5 S1 -174.3(9) . . . . ? O1 Cd1 O5 S1 137.0(6) . . . . ? O1 Cd2 O7 S1 5.2(9) 1_465 . . . ? N3 Cd2 O7 S1 -172.0(9) 1_565 . . . ? O4 Cd2 O7 S1 99.0(9) 1_465 . . . ? O2W Cd2 O7 S1 -10(8) . . . . ? O3 Cd2 O7 S1 -99.6(9) 1_565 . . . ? Cd2 O7 S1 O8 -78.6(9) . . . . ? Cd2 O7 S1 O6 43.4(10) . . . . ? Cd2 O7 S1 O5 163.1(8) . . . . ? Cd1 O5 S1 O8 44.0(8) . . . . ? Cd1 O5 S1 O6 -77.6(7) . . . . ? Cd1 O5 S1 O7 163.0(6) . . . . ? 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 N4 H4A S1 0.86 2.78 3.627(11) 168.6 2_556 N4 H4A O5 0.86 2.58 3.310(14) 143.8 2_556 N4 H4A O7 0.86 2.03 2.842(14) 156.2 2_556 N2 H2 O6 0.86 1.91 2.720(12) 156.7 2_565 O1W H1WB O6 0.85 1.94 2.747(13) 159.5 1_545 O1W H1WA O8 0.85 1.97 2.743(13) 150.3 1_645 O2W H2WB S1 0.85 3.02 3.831(9) 159.6 1_465 O2W H2WB O5 0.85 2.02 2.820(13) 156.3 1_465 O2W H2WA O8 0.85 1.99 2.791(13) 157.1 1_565 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.529 _refine_diff_density_min -1.964 _refine_diff_density_rms 0.335 ##############################################################################