Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peng Cheng' _publ_contact_author_address ; Department of Chemistry Nankai University Weijin Road Tianjin 300071 CHINA ; _publ_contact_author_email PCHENG@NANKAI.EDU.CN _publ_section_title ; Synthesis of a series of 4-pyridyl-1,2,4-triazole-containing cadmium(II) luminescent complexes ; loop_ _publ_author_name 'Peng Cheng' 'Bin Ding' 'Zong-Hui Jiang' 'Dai-Zheng Liao' 'Ying Wang' ; Shi-Ping Yan ; 'Long Yi' data_040310c _database_code_depnum_ccdc_archive 'CCDC 253304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Cd N14' _chemical_formula_weight 536.82 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' 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 Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.233(4) _cell_length_b 7.277(2) _cell_length_c 22.578(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2010.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 829 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 26.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.852761 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 '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 10596 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 26.42 _reflns_number_total 2056 _reflns_number_gt 1575 _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^)+(0.0270P)^2^+1.6184P] 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 2056 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.5000 0.14949(4) 0.7500 0.03024(10) Uani 1 2 d S . . N1 N 0.33666(18) 0.1594(3) 0.70040(10) 0.0323(5) Uani 1 1 d . . . N2 N 0.2381(2) 0.1308(4) 0.72871(11) 0.0384(6) Uani 1 1 d . . . N3 N 0.20754(17) 0.2040(3) 0.63593(10) 0.0289(5) Uani 1 1 d . . . N4 N 0.2219(2) 0.3180(4) 0.54090(11) 0.0449(7) Uani 1 1 d . . . N5 N 0.4333(2) 0.3756(4) 0.81750(12) 0.0475(7) Uani 1 1 d . . . N6 N 0.2507(2) 0.3906(4) 0.86102(11) 0.0513(8) Uani 1 1 d . . . N7 N 0.0720(2) 0.4303(4) 0.81469(12) 0.0476(7) Uani 1 1 d . . . C1 C 0.1628(2) 0.1575(5) 0.68896(12) 0.0366(7) Uani 1 1 d . . . H1 H 0.0882 0.1462 0.6959 0.044 Uiso 1 1 calc R . . C2 C 0.3165(2) 0.2035(5) 0.64606(12) 0.0363(7) Uani 1 1 d . . . H2 H 0.3695 0.2312 0.6179 0.044 Uiso 1 1 calc R . . C3 C 0.1561(2) 0.2406(4) 0.58010(12) 0.0318(6) Uani 1 1 d . . . C4 C 0.0487(3) 0.1941(4) 0.57028(13) 0.0400(7) Uani 1 1 d . . . H4 H 0.0059 0.1410 0.5998 0.048 Uiso 1 1 calc R . . C5 C 0.0071(3) 0.2301(6) 0.51440(15) 0.0504(8) Uani 1 1 d . . . H5 H -0.0649 0.2002 0.5053 0.060 Uiso 1 1 calc R . . C6 C 0.0731(3) 0.3101(5) 0.47271(14) 0.0548(10) Uani 1 1 d . . . H6 H 0.0464 0.3359 0.4350 0.066 Uiso 1 1 calc R . . C7 C 0.1785(3) 0.3513(6) 0.48723(14) 0.0549(9) Uani 1 1 d . . . H7 H 0.2226 0.4052 0.4585 0.066 Uiso 1 1 calc R . . C8 C 0.3444(3) 0.3840(4) 0.83494(13) 0.0362(7) Uani 1 1 d . . . C9 C 0.1591(3) 0.4135(4) 0.83306(12) 0.0370(7) 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 0.01951(14) 0.04132(17) 0.02989(15) 0.000 -0.00251(12) 0.000 N1 0.0222(11) 0.0434(14) 0.0315(12) 0.0012(11) -0.0020(9) -0.0015(11) N2 0.0273(12) 0.0562(17) 0.0316(11) 0.0073(11) -0.0007(10) -0.0017(12) N3 0.0244(11) 0.0350(14) 0.0274(11) 0.0007(10) -0.0021(9) -0.0004(10) N4 0.0407(15) 0.0604(19) 0.0334(13) 0.0084(13) -0.0027(11) -0.0044(13) N5 0.0342(15) 0.0589(19) 0.0495(16) -0.0143(14) -0.0051(13) 0.0096(13) N6 0.0384(14) 0.081(2) 0.0339(13) 0.0008(13) -0.0016(13) 0.0120(15) N7 0.0319(14) 0.0613(19) 0.0497(16) 0.0185(15) 0.0044(12) 0.0045(14) C1 0.0214(13) 0.058(2) 0.0306(14) 0.0059(14) 0.0006(11) -0.0016(14) C2 0.0218(13) 0.056(2) 0.0313(15) 0.0011(14) 0.0008(12) -0.0034(13) C3 0.0332(14) 0.0350(16) 0.0272(13) -0.0032(12) -0.0038(12) 0.0032(13) C4 0.0327(15) 0.049(2) 0.0383(16) -0.0010(14) -0.0045(14) 0.0000(14) C5 0.0402(17) 0.061(2) 0.0503(19) -0.0057(18) -0.0160(17) 0.0085(18) C6 0.060(2) 0.073(3) 0.0311(16) -0.0004(17) -0.0134(16) 0.011(2) C7 0.058(2) 0.075(3) 0.0326(16) 0.0119(18) 0.0000(15) -0.001(2) C8 0.0391(18) 0.0389(19) 0.0306(15) -0.0081(13) -0.0086(13) 0.0068(14) C9 0.0373(17) 0.0436(18) 0.0301(15) 0.0045(13) 0.0086(13) 0.0053(15) _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 2.292(2) 3_656 ? Cd1 N1 2.292(2) . ? Cd1 N7 2.335(3) 8_655 ? Cd1 N7 2.335(3) 6_657 ? Cd1 N5 2.386(3) 3_656 ? Cd1 N5 2.386(3) . ? N1 C2 1.292(3) . ? N1 N2 1.380(3) . ? N2 C1 1.301(4) . ? N3 C2 1.352(3) . ? N3 C1 1.359(3) . ? N3 C3 1.434(3) . ? N4 C3 1.322(4) . ? N4 C7 1.345(4) . ? N5 C8 1.158(4) . ? N6 C8 1.290(4) . ? N6 C9 1.297(4) . ? N7 C9 1.150(4) . ? N7 Cd1 2.335(3) 6_567 ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.376(4) . ? C4 C5 1.385(4) . ? C4 H4 0.9300 . ? C5 C6 1.370(5) . ? C5 H5 0.9300 . ? C6 C7 1.363(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? 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 N1 176.40(13) 3_656 . ? N1 Cd1 N7 92.57(9) 3_656 8_655 ? N1 Cd1 N7 89.90(9) . 8_655 ? N1 Cd1 N7 89.90(9) 3_656 6_657 ? N1 Cd1 N7 92.56(9) . 6_657 ? N7 Cd1 N7 93.83(16) 8_655 6_657 ? N1 Cd1 N5 89.56(9) 3_656 3_656 ? N1 Cd1 N5 87.95(9) . 3_656 ? N7 Cd1 N5 177.81(9) 8_655 3_656 ? N7 Cd1 N5 86.71(11) 6_657 3_656 ? N1 Cd1 N5 87.96(9) 3_656 . ? N1 Cd1 N5 89.57(9) . . ? N7 Cd1 N5 86.71(11) 8_655 . ? N7 Cd1 N5 177.81(9) 6_657 . ? N5 Cd1 N5 92.84(15) 3_656 . ? C2 N1 N2 108.1(2) . . ? C2 N1 Cd1 129.66(19) . . ? N2 N1 Cd1 122.04(17) . . ? C1 N2 N1 106.0(2) . . ? C2 N3 C1 104.3(2) . . ? C2 N3 C3 125.5(2) . . ? C1 N3 C3 130.1(2) . . ? C3 N4 C7 116.1(3) . . ? C8 N5 Cd1 125.1(2) . . ? C8 N6 C9 123.4(3) . . ? C9 N7 Cd1 130.4(3) . 6_567 ? N2 C1 N3 111.1(2) . . ? N2 C1 H1 124.5 . . ? N3 C1 H1 124.5 . . ? N1 C2 N3 110.4(3) . . ? N1 C2 H2 124.8 . . ? N3 C2 H2 124.8 . . ? N4 C3 C4 125.3(3) . . ? N4 C3 N3 113.7(2) . . ? C4 C3 N3 121.0(3) . . ? C3 C4 C5 116.8(3) . . ? C3 C4 H4 121.6 . . ? C5 C4 H4 121.6 . . ? C6 C5 C4 119.3(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C7 C6 C5 119.0(3) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? N4 C7 C6 123.4(3) . . ? N4 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? N5 C8 N6 172.7(3) . . ? N7 C9 N6 171.8(3) . . ? 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 N1 Cd1 N1 C2 72.7(3) 3_656 . . . ? N7 Cd1 N1 C2 -154.2(3) 8_655 . . . ? N7 Cd1 N1 C2 -60.3(3) 6_657 . . . ? N5 Cd1 N1 C2 26.3(3) 3_656 . . . ? N5 Cd1 N1 C2 119.1(3) . . . . ? N1 Cd1 N1 N2 -101.4(2) 3_656 . . . ? N7 Cd1 N1 N2 31.7(2) 8_655 . . . ? N7 Cd1 N1 N2 125.6(2) 6_657 . . . ? N5 Cd1 N1 N2 -147.8(2) 3_656 . . . ? N5 Cd1 N1 N2 -55.0(2) . . . . ? C2 N1 N2 C1 0.8(3) . . . . ? Cd1 N1 N2 C1 176.0(2) . . . . ? N1 Cd1 N5 C8 -145.2(3) 3_656 . . . ? N1 Cd1 N5 C8 37.4(3) . . . . ? N7 Cd1 N5 C8 -52.5(3) 8_655 . . . ? N7 Cd1 N5 C8 -157(3) 6_657 . . . ? N5 Cd1 N5 C8 125.4(3) 3_656 . . . ? N1 N2 C1 N3 -0.6(3) . . . . ? C2 N3 C1 N2 0.1(4) . . . . ? C3 N3 C1 N2 178.2(3) . . . . ? N2 N1 C2 N3 -0.8(4) . . . . ? Cd1 N1 C2 N3 -175.51(19) . . . . ? C1 N3 C2 N1 0.4(4) . . . . ? C3 N3 C2 N1 -177.8(3) . . . . ? C7 N4 C3 C4 -0.5(5) . . . . ? C7 N4 C3 N3 178.4(3) . . . . ? C2 N3 C3 N4 -15.4(4) . . . . ? C1 N3 C3 N4 166.9(3) . . . . ? C2 N3 C3 C4 163.7(3) . . . . ? C1 N3 C3 C4 -14.1(5) . . . . ? N4 C3 C4 C5 0.7(5) . . . . ? N3 C3 C4 C5 -178.2(3) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C4 C5 C6 C7 0.4(6) . . . . ? C3 N4 C7 C6 0.2(5) . . . . ? C5 C6 C7 N4 -0.2(6) . . . . ? Cd1 N5 C8 N6 119(3) . . . . ? C9 N6 C8 N5 180(100) . . . . ? Cd1 N7 C9 N6 135(3) 6_567 . . . ? C8 N6 C9 N7 174(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.514 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.066 data_dd _database_code_depnum_ccdc_archive 'CCDC 253305' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Cd N10 S2' _chemical_formula_weight 520.88 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8103(9) _cell_length_b 8.3849(13) _cell_length_c 10.2837(16) _cell_angle_alpha 84.804(2) _cell_angle_beta 81.042(2) _cell_angle_gamma 87.070(2) _cell_volume 492.52(13) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1080 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 22.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 258 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732248 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2618 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.08 _reflns_number_total 1725 _reflns_number_gt 1613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0476P)^2^+1.9927P] 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 1725 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1120 _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 0.5000 1.0000 0.5000 0.0368(2) Uani 1 2 d S . . N1 N 0.5533(9) 0.7270(6) 0.5744(5) 0.0444(12) Uani 1 1 d . . . N2 N 0.7509(10) 0.6324(7) 0.5345(6) 0.0655(18) Uani 1 1 d . . . N3 N 0.5543(8) 0.5124(5) 0.7132(4) 0.0388(11) Uani 1 1 d . . . N4 N 0.2766(9) 0.4242(6) 0.8882(5) 0.0455(12) Uani 1 1 d . . . C1 C 0.4404(10) 0.6504(7) 0.6788(6) 0.0420(13) Uani 1 1 d . . . H1 H 0.2988 0.6862 0.7241 0.050 Uiso 1 1 calc R . . C2 C 0.7458(13) 0.5079(8) 0.6182(7) 0.0612(19) Uani 1 1 d . . . H2 H 0.8590 0.4252 0.6142 0.073 Uiso 1 1 calc R . . C3 C 0.4940(10) 0.4059(6) 0.8285(5) 0.0376(12) Uani 1 1 d . . . C4 C 0.6581(11) 0.2972(7) 0.8713(6) 0.0445(14) Uani 1 1 d . . . H4 H 0.8090 0.2892 0.8257 0.053 Uiso 1 1 calc R . . C5 C 0.5874(13) 0.2009(7) 0.9851(7) 0.0536(16) Uani 1 1 d . . . H5 H 0.6909 0.1248 1.0176 0.064 Uiso 1 1 calc R . . C6 C 0.3629(13) 0.2179(8) 1.0504(7) 0.0566(17) Uani 1 1 d . . . H6 H 0.3132 0.1544 1.1277 0.068 Uiso 1 1 calc R . . C7 C 0.2146(12) 0.3299(8) 0.9994(6) 0.0522(16) Uani 1 1 d . . . H7 H 0.0634 0.3413 1.0439 0.063 Uiso 1 1 calc R . . C8 C 1.0444(9) 0.9537(7) 0.3388(5) 0.0348(12) Uani 1 1 d . . . N5 N 1.2170(8) 0.9474(7) 0.3825(5) 0.0509(13) Uani 1 1 d . . . S1 S 0.8040(2) 0.95817(19) 0.27315(14) 0.0424(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 Cd1 0.0280(3) 0.0427(4) 0.0380(3) 0.0035(2) -0.0048(2) 0.0005(2) N1 0.044(3) 0.040(3) 0.043(3) 0.005(2) 0.003(2) 0.008(2) N2 0.059(4) 0.057(4) 0.064(4) 0.017(3) 0.025(3) 0.019(3) N3 0.044(3) 0.032(2) 0.036(2) 0.0018(19) 0.002(2) 0.004(2) N4 0.047(3) 0.042(3) 0.044(3) 0.003(2) 0.003(2) 0.001(2) C1 0.035(3) 0.038(3) 0.048(3) 0.005(3) 0.002(2) 0.007(2) C2 0.057(4) 0.053(4) 0.058(4) 0.012(3) 0.023(3) 0.021(3) C3 0.042(3) 0.031(3) 0.039(3) -0.004(2) -0.005(2) 0.001(2) C4 0.053(4) 0.036(3) 0.043(3) -0.002(2) -0.007(3) 0.006(3) C5 0.074(5) 0.037(3) 0.051(4) 0.003(3) -0.020(3) 0.008(3) C6 0.080(5) 0.046(4) 0.041(3) 0.005(3) -0.003(3) -0.010(3) C7 0.057(4) 0.051(4) 0.044(3) -0.004(3) 0.009(3) -0.008(3) C8 0.029(3) 0.047(3) 0.027(3) -0.003(2) 0.001(2) 0.002(2) N5 0.024(2) 0.084(4) 0.044(3) -0.009(3) -0.003(2) -0.004(2) S1 0.0290(7) 0.0630(10) 0.0343(7) -0.0030(7) -0.0059(6) 0.0063(6) _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 2.269(5) 2_776 ? Cd1 N5 2.269(5) 1_455 ? Cd1 N1 2.368(5) . ? Cd1 N1 2.368(5) 2_676 ? Cd1 S1 2.7362(14) . ? Cd1 S1 2.7362(14) 2_676 ? N1 C1 1.302(7) . ? N1 N2 1.391(7) . ? N2 C2 1.290(8) . ? N3 C1 1.349(7) . ? N3 C2 1.363(8) . ? N3 C3 1.427(7) . ? N4 C3 1.324(7) . ? N4 C7 1.341(8) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.380(8) . ? C4 C5 1.379(9) . ? C4 H4 0.9300 . ? C5 C6 1.378(10) . ? C5 H5 0.9300 . ? C6 C7 1.367(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N5 1.158(7) . ? C8 S1 1.640(5) . ? N5 Cd1 2.269(5) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cd1 N5 180.000(1) 2_776 1_455 ? N5 Cd1 N1 87.1(2) 2_776 . ? N5 Cd1 N1 92.9(2) 1_455 . ? N5 Cd1 N1 92.9(2) 2_776 2_676 ? N5 Cd1 N1 87.1(2) 1_455 2_676 ? N1 Cd1 N1 180.0(2) . 2_676 ? N5 Cd1 S1 94.22(13) 2_776 . ? N5 Cd1 S1 85.78(13) 1_455 . ? N1 Cd1 S1 90.80(12) . . ? N1 Cd1 S1 89.20(12) 2_676 . ? N5 Cd1 S1 85.78(13) 2_776 2_676 ? N5 Cd1 S1 94.22(13) 1_455 2_676 ? N1 Cd1 S1 89.20(12) . 2_676 ? N1 Cd1 S1 90.80(12) 2_676 2_676 ? S1 Cd1 S1 180.0 . 2_676 ? C1 N1 N2 106.5(5) . . ? C1 N1 Cd1 127.2(4) . . ? N2 N1 Cd1 124.3(4) . . ? C2 N2 N1 106.6(5) . . ? C1 N3 C2 103.5(5) . . ? C1 N3 C3 127.0(5) . . ? C2 N3 C3 129.2(5) . . ? C3 N4 C7 116.7(5) . . ? N1 C1 N3 111.6(5) . . ? N1 C1 H1 124.2 . . ? N3 C1 H1 124.2 . . ? N2 C2 N3 111.7(6) . . ? N2 C2 H2 124.1 . . ? N3 C2 H2 124.1 . . ? N4 C3 C4 125.0(5) . . ? N4 C3 N3 114.7(5) . . ? C4 C3 N3 120.3(5) . . ? C5 C4 C3 116.7(6) . . ? C5 C4 H4 121.6 . . ? C3 C4 H4 121.6 . . ? C6 C5 C4 119.7(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 118.6(6) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? N4 C7 C6 123.2(6) . . ? N4 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? N5 C8 S1 178.0(5) . . ? C8 N5 Cd1 162.3(5) . 1_655 ? C8 S1 Cd1 96.93(18) . . ? 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 N5 Cd1 N1 C1 92.4(5) 2_776 . . . ? N5 Cd1 N1 C1 -87.6(5) 1_455 . . . ? N1 Cd1 N1 C1 -102(51) 2_676 . . . ? S1 Cd1 N1 C1 -173.4(5) . . . . ? S1 Cd1 N1 C1 6.6(5) 2_676 . . . ? N5 Cd1 N1 N2 -69.3(5) 2_776 . . . ? N5 Cd1 N1 N2 110.7(5) 1_455 . . . ? N1 Cd1 N1 N2 96(51) 2_676 . . . ? S1 Cd1 N1 N2 24.9(5) . . . . ? S1 Cd1 N1 N2 -155.1(5) 2_676 . . . ? C1 N1 N2 C2 -1.1(8) . . . . ? Cd1 N1 N2 C2 163.8(5) . . . . ? N2 N1 C1 N3 1.7(7) . . . . ? Cd1 N1 C1 N3 -162.6(4) . . . . ? C2 N3 C1 N1 -1.6(7) . . . . ? C3 N3 C1 N1 173.7(5) . . . . ? N1 N2 C2 N3 0.2(9) . . . . ? C1 N3 C2 N2 0.8(9) . . . . ? C3 N3 C2 N2 -174.4(6) . . . . ? C7 N4 C3 C4 0.7(9) . . . . ? C7 N4 C3 N3 -177.9(5) . . . . ? C1 N3 C3 N4 18.1(8) . . . . ? C2 N3 C3 N4 -167.8(7) . . . . ? C1 N3 C3 C4 -160.6(6) . . . . ? C2 N3 C3 C4 13.5(10) . . . . ? N4 C3 C4 C5 0.1(9) . . . . ? N3 C3 C4 C5 178.6(5) . . . . ? C3 C4 C5 C6 -0.7(9) . . . . ? C4 C5 C6 C7 0.6(10) . . . . ? C3 N4 C7 C6 -0.9(9) . . . . ? C5 C6 C7 N4 0.3(11) . . . . ? S1 C8 N5 Cd1 168(15) . . . 1_655 ? N5 C8 S1 Cd1 148(16) . . . . ? N5 Cd1 S1 C8 11.2(3) 2_776 . . . ? N5 Cd1 S1 C8 -168.8(3) 1_455 . . . ? N1 Cd1 S1 C8 -76.0(2) . . . . ? N1 Cd1 S1 C8 104.0(2) 2_676 . . . ? S1 Cd1 S1 C8 66(73) 2_676 . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.563 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.119 data_040220b _database_code_depnum_ccdc_archive 'CCDC 253306' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H33.50 Cd2 N24 O15.75' _chemical_formula_weight 1267.16 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.642(6) _cell_length_b 12.611(6) _cell_length_c 19.317(9) _cell_angle_alpha 92.038(7) _cell_angle_beta 105.963(6) _cell_angle_gamma 116.004(7) _cell_volume 2410(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 935 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 26.39 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1267 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.855796 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 '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 13987 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 26.46 _reflns_number_total 9803 _reflns_number_gt 7585 _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^)+(0.0425P)^2^+1.6511P] 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 9803 _refine_ls_number_parameters 731 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.066 _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 0.61824(3) 0.65175(3) 0.187593(14) 0.03255(8) Uani 1 1 d . . . Cd2 Cd 0.37987(3) 0.57927(2) 0.325200(14) 0.02883(8) Uani 1 1 d . . . O1 O 0.1878(3) 0.6026(3) 0.28852(18) 0.0552(8) Uani 1 1 d . . . O2 O 0.8265(3) 0.8223(3) 0.2389(2) 0.0686(10) Uani 1 1 d . . . O3 O 0.7499(4) 0.5615(3) 0.16715(17) 0.0606(9) Uani 1 1 d . . . O4 O 0.5705(4) 0.4600(4) 0.0779(3) 0.1113(18) Uani 1 1 d . . . O5 O 0.7267(4) 0.4084(3) 0.1010(2) 0.0633(9) Uani 1 1 d . . . O6 O 0.4862(4) 0.6150(3) 0.4667(2) 0.0706(10) Uani 1 1 d . . . O7 O 0.4215(4) 0.7407(4) 0.4286(2) 0.0858(13) Uani 1 1 d . . . O8 O 0.5074(3) 0.7534(3) 0.54364(16) 0.0601(9) Uani 1 1 d . . . N1 N 0.6489(3) 0.5709(3) 0.29345(16) 0.0333(7) Uani 1 1 d . . . N2 N 0.5680(3) 0.5462(3) 0.33813(16) 0.0325(7) Uani 1 1 d . . . N3 N 0.7147(3) 0.4810(3) 0.37853(16) 0.0308(7) Uani 1 1 d . . . N4 N 0.7932(3) 0.4346(3) 0.48995(17) 0.0379(8) Uani 1 1 d . . . N5 N 0.5487(4) 0.7815(3) 0.23623(19) 0.0421(8) Uani 1 1 d . . . N6 N 0.4903(3) 0.7652(3) 0.29112(18) 0.0364(7) Uani 1 1 d . . . N7 N 0.5258(3) 0.9397(3) 0.26123(17) 0.0345(7) Uani 1 1 d . . . N8 N 0.5681(4) 1.1000(3) 0.2014(2) 0.0503(9) Uani 1 1 d . . . N9 N 0.3865(3) 0.5209(3) 0.14990(17) 0.0387(8) Uani 1 1 d . . . N10 N 0.3082(3) 0.4929(3) 0.19575(17) 0.0400(8) Uani 1 1 d . . . N11 N 0.1751(3) 0.4242(3) 0.08238(16) 0.0338(7) Uani 1 1 d . . . N12 N 0.0827(3) 0.3722(3) -0.04370(18) 0.0424(8) Uani 1 1 d . . . N13 N 0.6175(4) 0.7347(3) 0.08518(18) 0.0449(8) Uani 1 1 d . . . N14 N 0.5362(4) 0.7876(4) 0.0596(2) 0.0579(11) Uani 1 1 d . . . N15 N 0.6879(4) 0.8337(3) 0.00323(18) 0.0430(8) Uani 1 1 d . . . N16 N 0.8379(5) 0.8328(4) -0.0538(2) 0.0653(12) Uani 1 1 d . . . N17 N 0.2583(3) 0.3919(3) 0.34848(17) 0.0344(7) Uani 1 1 d . . . N18 N 0.2310(4) 0.2906(3) 0.30296(19) 0.0485(9) Uani 1 1 d . . . N19 N 0.1989(3) 0.2427(3) 0.40657(17) 0.0334(7) Uani 1 1 d . . . N20 N 0.1500(4) 0.2227(3) 0.51545(19) 0.0436(8) Uani 1 1 d . . . N21 N 0.6807(4) 0.4743(4) 0.1149(2) 0.0491(9) Uani 1 1 d . . . N22 N 0.4730(3) 0.7056(3) 0.48108(18) 0.0392(8) Uani 1 1 d . . . C1 C 0.7347(4) 0.5313(4) 0.3191(2) 0.0351(8) Uani 1 1 d . . . H1 H 0.8012 0.5366 0.2994 0.042 Uiso 1 1 calc R . . C2 C 0.6102(4) 0.4932(3) 0.3881(2) 0.0327(8) Uani 1 1 d . . . H2 H 0.5735 0.4673 0.4252 0.039 Uiso 1 1 calc R . . C3 C 0.7829(4) 0.4217(3) 0.4205(2) 0.0316(8) Uani 1 1 d . . . C4 C 0.8287(4) 0.3577(4) 0.3872(2) 0.0449(10) Uani 1 1 d . . . H4 H 0.8170 0.3513 0.3374 0.054 Uiso 1 1 calc R . . C5 C 0.8933(5) 0.3029(4) 0.4315(3) 0.0522(12) Uani 1 1 d . . . H5 H 0.9275 0.2591 0.4122 0.063 Uiso 1 1 calc R . . C6 C 0.9058(4) 0.3145(4) 0.5047(3) 0.0501(11) Uani 1 1 d . . . H6 H 0.9482 0.2781 0.5354 0.060 Uiso 1 1 calc R . . C7 C 0.8552(4) 0.3803(4) 0.5317(2) 0.0463(10) Uani 1 1 d . . . H7 H 0.8643 0.3876 0.5812 0.056 Uiso 1 1 calc R . . C8 C 0.5680(5) 0.8857(4) 0.2198(2) 0.0458(10) Uani 1 1 d . . . H8 H 0.6058 0.9186 0.1842 0.055 Uiso 1 1 calc R . . C9 C 0.4790(4) 0.8614(4) 0.3050(2) 0.0379(9) Uani 1 1 d . . . H9 H 0.4436 0.8744 0.3402 0.046 Uiso 1 1 calc R . . C10 C 0.5218(4) 1.0502(3) 0.2538(2) 0.0378(9) Uani 1 1 d . . . C11 C 0.4707(5) 1.0945(4) 0.2968(3) 0.0546(12) Uani 1 1 d . . . H11 H 0.4426 1.0568 0.3339 0.066 Uiso 1 1 calc R . . C12 C 0.4631(5) 1.1986(4) 0.2820(3) 0.0641(14) Uani 1 1 d . . . H12 H 0.4287 1.2321 0.3093 0.077 Uiso 1 1 calc R . . C13 C 0.5065(5) 1.2519(4) 0.2270(3) 0.0637(14) Uani 1 1 d . . . H13 H 0.5003 1.3207 0.2157 0.076 Uiso 1 1 calc R . . C14 C 0.5592(6) 1.2010(4) 0.1893(3) 0.0611(13) Uani 1 1 d . . . H14 H 0.5908 1.2386 0.1530 0.073 Uiso 1 1 calc R . . C15 C 0.3045(4) 0.4791(4) 0.0833(2) 0.0402(9) Uani 1 1 d . . . H15 H 0.3312 0.4859 0.0418 0.048 Uiso 1 1 calc R . . C16 C 0.1830(4) 0.4347(4) 0.1535(2) 0.0423(10) Uani 1 1 d . . . H16 H 0.1090 0.4044 0.1702 0.051 Uiso 1 1 calc R . . C17 C 0.0564(4) 0.3770(3) 0.0185(2) 0.0361(9) Uani 1 1 d . . . C18 C -0.0680(4) 0.3479(4) 0.0244(2) 0.0479(11) Uani 1 1 d . . . H18 H -0.0802 0.3522 0.0698 0.057 Uiso 1 1 calc R . . C19 C -0.1745(5) 0.3119(4) -0.0397(3) 0.0558(12) Uani 1 1 d . . . H19 H -0.2613 0.2899 -0.0385 0.067 Uiso 1 1 calc R . . C20 C -0.1504(5) 0.3092(4) -0.1050(3) 0.0547(12) Uani 1 1 d . . . H20 H -0.2203 0.2873 -0.1490 0.066 Uiso 1 1 calc R . . C21 C -0.0220(5) 0.3391(4) -0.1050(2) 0.0511(11) Uani 1 1 d . . . H21 H -0.0071 0.3363 -0.1498 0.061 Uiso 1 1 calc R . . C22 C 0.7053(5) 0.7625(4) 0.0511(2) 0.0443(10) Uani 1 1 d . . . H22 H 0.7709 0.7370 0.0585 0.053 Uiso 1 1 calc R . . C23 C 0.5807(5) 0.8454(5) 0.0112(2) 0.0577(13) Uani 1 1 d . . . H23 H 0.5442 0.8900 -0.0152 0.069 Uiso 1 1 calc R . . C24 C 0.7647(5) 0.8842(4) -0.0443(2) 0.0442(10) Uani 1 1 d . . . C25 C 0.7589(5) 0.9771(4) -0.0762(3) 0.0587(13) Uani 1 1 d . . . H25 H 0.7078 1.0117 -0.0663 0.070 Uiso 1 1 calc R . . C26 C 0.8320(6) 1.0182(5) -0.1240(3) 0.0689(15) Uani 1 1 d . . . H26 H 0.8278 1.0791 -0.1485 0.083 Uiso 1 1 calc R . . C27 C 0.9100(6) 0.9681(5) -0.1344(3) 0.0690(15) Uani 1 1 d . . . H27 H 0.9606 0.9948 -0.1658 0.083 Uiso 1 1 calc R . . C28 C 0.9124(6) 0.8782(5) -0.0981(3) 0.0744(17) Uani 1 1 d . . . H28 H 0.9683 0.8464 -0.1041 0.089 Uiso 1 1 calc R . . C29 C 0.1960(5) 0.2042(4) 0.3393(2) 0.0477(11) Uani 1 1 d . . . H29 H 0.1718 0.1253 0.3215 0.057 Uiso 1 1 calc R . . C30 C 0.2381(4) 0.3612(3) 0.4091(2) 0.0359(9) Uani 1 1 d . . . H30 H 0.2490 0.4131 0.4486 0.043 Uiso 1 1 calc R . . C31 C 0.1846(4) 0.1786(3) 0.4660(2) 0.0354(9) Uani 1 1 d . . . C32 C 0.2098(4) 0.0821(4) 0.4699(3) 0.0476(11) Uani 1 1 d . . . H32 H 0.2336 0.0548 0.4334 0.057 Uiso 1 1 calc R . . C33 C 0.1985(5) 0.0268(4) 0.5300(3) 0.0585(13) Uani 1 1 d . . . H33 H 0.2150 -0.0388 0.5349 0.070 Uiso 1 1 calc R . . C34 C 0.1630(5) 0.0696(5) 0.5818(3) 0.0586(13) Uani 1 1 d . . . H34 H 0.1545 0.0334 0.6226 0.070 Uiso 1 1 calc R . . C35 C 0.1399(5) 0.1669(4) 0.5732(2) 0.0525(12) Uani 1 1 d . . . H35 H 0.1161 0.1957 0.6090 0.063 Uiso 1 1 calc R . . N23 N 0.1227(4) 0.8334(4) 0.3082(3) 0.0630(11) Uani 1 1 d . . . O9 O 0.2341(8) 0.8391(9) 0.3509(9) 0.086(5) Uani 0.482(18) 1 d P A 1 O1O O 0.024(3) 0.7410(18) 0.3004(18) 0.107(9) Uani 0.482(18) 1 d P A 1 O11 O 0.121(3) 0.921(2) 0.2902(17) 0.083(7) Uani 0.482(18) 1 d P A 1 O9' O 0.2101(8) 0.8213(7) 0.2845(8) 0.076(4) Uani 0.518(18) 1 d P A 2 O10' O 0.028(3) 0.743(2) 0.3148(14) 0.085(7) Uani 0.518(18) 1 d P A 2 O11' O 0.108(3) 0.926(2) 0.3057(16) 0.087(8) Uani 0.518(18) 1 d P A 2 N24 N 0.8754(4) 0.1274(5) 0.2194(4) 0.0725(14) Uani 1 1 d . . . O12 O 0.8401(5) 0.0301(5) 0.1823(3) 0.1076(16) Uani 1 1 d . . . O13 O 0.8992(5) 0.2126(4) 0.1843(3) 0.1054(15) Uani 1 1 d . . . O14 O 0.8849(5) 0.1416(7) 0.2803(3) 0.150(3) Uani 1 1 d . . . O15 O 0.9294(4) 0.4303(3) 0.2363(2) 0.0766(11) Uani 1 1 d . . . O16 O 0.6666(8) 0.1081(8) 0.0557(5) 0.089(3) Uani 0.50 1 d P . . O17 O 0.518(2) 0.0134(16) 0.4663(9) 0.096(5) Uani 0.25 1 d PU . . 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 0.03520(16) 0.03726(16) 0.03298(15) 0.01232(12) 0.01787(12) 0.01914(13) Cd2 0.03190(15) 0.03045(15) 0.03202(15) 0.01201(11) 0.01501(11) 0.01808(12) O1 0.0436(17) 0.056(2) 0.073(2) 0.0094(17) 0.0156(16) 0.0313(16) O2 0.0427(19) 0.062(2) 0.081(2) 0.0194(19) 0.0087(17) 0.0134(17) O3 0.073(2) 0.076(2) 0.0452(18) 0.0015(18) 0.0218(17) 0.044(2) O4 0.066(3) 0.096(3) 0.152(4) -0.016(3) -0.010(3) 0.051(3) O5 0.082(2) 0.052(2) 0.081(2) 0.0186(18) 0.047(2) 0.0413(19) O6 0.074(2) 0.047(2) 0.099(3) -0.0009(19) 0.050(2) 0.0229(18) O7 0.078(3) 0.138(4) 0.062(2) 0.065(3) 0.031(2) 0.060(3) O8 0.058(2) 0.069(2) 0.0354(17) -0.0089(16) 0.0153(15) 0.0155(17) N1 0.0352(17) 0.0389(18) 0.0343(17) 0.0135(14) 0.0166(14) 0.0207(15) N2 0.0359(17) 0.0372(18) 0.0347(16) 0.0144(14) 0.0173(14) 0.0219(15) N3 0.0332(16) 0.0353(17) 0.0310(16) 0.0111(13) 0.0124(13) 0.0205(14) N4 0.0405(18) 0.046(2) 0.0345(18) 0.0142(15) 0.0140(14) 0.0253(16) N5 0.050(2) 0.0352(19) 0.051(2) 0.0127(16) 0.0307(17) 0.0202(16) N6 0.0401(18) 0.0331(18) 0.0425(18) 0.0118(15) 0.0218(15) 0.0173(15) N7 0.0400(18) 0.0295(17) 0.0413(18) 0.0107(14) 0.0217(15) 0.0173(14) N8 0.074(3) 0.0332(19) 0.052(2) 0.0173(17) 0.034(2) 0.0242(19) N9 0.0367(18) 0.045(2) 0.0317(17) 0.0061(15) 0.0145(14) 0.0149(16) N10 0.0407(19) 0.047(2) 0.0307(17) 0.0090(15) 0.0160(15) 0.0166(17) N11 0.0355(17) 0.0332(17) 0.0297(16) 0.0034(13) 0.0095(13) 0.0143(14) N12 0.044(2) 0.043(2) 0.0349(18) 0.0032(15) 0.0094(15) 0.0181(17) N13 0.051(2) 0.057(2) 0.0370(18) 0.0152(17) 0.0202(16) 0.0297(19) N14 0.058(2) 0.092(3) 0.042(2) 0.021(2) 0.0229(19) 0.046(2) N15 0.057(2) 0.053(2) 0.0338(18) 0.0164(16) 0.0207(16) 0.0342(19) N16 0.094(3) 0.065(3) 0.080(3) 0.038(2) 0.060(3) 0.054(3) N17 0.0410(18) 0.0284(17) 0.0387(18) 0.0081(14) 0.0178(15) 0.0173(15) N18 0.069(3) 0.037(2) 0.045(2) 0.0088(16) 0.0267(19) 0.0244(19) N19 0.0353(17) 0.0279(16) 0.0395(18) 0.0094(14) 0.0153(14) 0.0146(14) N20 0.046(2) 0.040(2) 0.044(2) 0.0150(16) 0.0193(16) 0.0167(17) N21 0.056(2) 0.053(2) 0.057(2) 0.022(2) 0.031(2) 0.033(2) N22 0.0337(18) 0.045(2) 0.0364(19) 0.0098(16) 0.0162(15) 0.0135(16) C1 0.035(2) 0.041(2) 0.036(2) 0.0119(17) 0.0181(17) 0.0199(18) C2 0.037(2) 0.039(2) 0.0328(19) 0.0127(16) 0.0165(16) 0.0242(18) C3 0.0279(19) 0.033(2) 0.037(2) 0.0090(16) 0.0097(16) 0.0170(16) C4 0.052(3) 0.056(3) 0.041(2) 0.010(2) 0.017(2) 0.036(2) C5 0.052(3) 0.055(3) 0.067(3) 0.015(2) 0.018(2) 0.039(2) C6 0.049(3) 0.057(3) 0.058(3) 0.026(2) 0.016(2) 0.036(2) C7 0.048(3) 0.059(3) 0.043(2) 0.020(2) 0.017(2) 0.032(2) C8 0.061(3) 0.037(2) 0.055(3) 0.015(2) 0.039(2) 0.024(2) C9 0.048(2) 0.035(2) 0.042(2) 0.0130(18) 0.0268(19) 0.0215(19) C10 0.040(2) 0.028(2) 0.044(2) 0.0063(17) 0.0154(18) 0.0134(17) C11 0.067(3) 0.034(2) 0.069(3) 0.011(2) 0.034(3) 0.022(2) C12 0.066(3) 0.040(3) 0.092(4) 0.005(3) 0.034(3) 0.025(3) C13 0.070(3) 0.029(2) 0.077(4) 0.005(2) 0.002(3) 0.023(2) C14 0.084(4) 0.038(3) 0.057(3) 0.017(2) 0.022(3) 0.024(3) C15 0.040(2) 0.047(2) 0.032(2) 0.0063(18) 0.0170(18) 0.0171(19) C16 0.040(2) 0.047(2) 0.035(2) 0.0086(19) 0.0171(18) 0.013(2) C17 0.036(2) 0.033(2) 0.033(2) 0.0042(16) 0.0055(16) 0.0151(18) C18 0.043(2) 0.056(3) 0.044(2) 0.004(2) 0.014(2) 0.024(2) C19 0.040(3) 0.059(3) 0.066(3) 0.007(2) 0.010(2) 0.025(2) C20 0.053(3) 0.047(3) 0.048(3) 0.004(2) -0.004(2) 0.022(2) C21 0.058(3) 0.054(3) 0.035(2) 0.006(2) 0.007(2) 0.025(2) C22 0.053(3) 0.053(3) 0.041(2) 0.018(2) 0.022(2) 0.033(2) C23 0.073(3) 0.085(4) 0.046(3) 0.026(3) 0.026(2) 0.058(3) C24 0.060(3) 0.044(2) 0.035(2) 0.0118(19) 0.021(2) 0.026(2) C25 0.078(3) 0.049(3) 0.065(3) 0.021(2) 0.035(3) 0.035(3) C26 0.096(4) 0.051(3) 0.068(3) 0.032(3) 0.035(3) 0.035(3) C27 0.090(4) 0.056(3) 0.068(3) 0.026(3) 0.048(3) 0.026(3) C28 0.106(5) 0.073(4) 0.091(4) 0.041(3) 0.069(4) 0.057(4) C29 0.068(3) 0.030(2) 0.047(2) 0.0055(19) 0.024(2) 0.021(2) C30 0.042(2) 0.028(2) 0.041(2) 0.0077(17) 0.0189(18) 0.0160(17) C31 0.0281(19) 0.0284(19) 0.045(2) 0.0119(17) 0.0115(17) 0.0093(16) C32 0.050(3) 0.037(2) 0.059(3) 0.016(2) 0.019(2) 0.021(2) C33 0.061(3) 0.040(3) 0.072(3) 0.028(2) 0.017(3) 0.023(2) C34 0.053(3) 0.059(3) 0.050(3) 0.026(2) 0.010(2) 0.018(2) C35 0.056(3) 0.054(3) 0.044(2) 0.015(2) 0.017(2) 0.021(2) N23 0.055(3) 0.053(3) 0.093(3) 0.019(3) 0.022(3) 0.036(2) O9 0.046(5) 0.092(7) 0.125(13) 0.030(7) 0.021(5) 0.039(5) O1O 0.062(13) 0.037(9) 0.19(2) -0.001(10) 0.004(11) 0.015(9) O11 0.132(13) 0.067(11) 0.104(12) 0.047(10) 0.061(9) 0.076(9) O9' 0.060(5) 0.070(5) 0.123(12) 0.031(5) 0.046(6) 0.042(4) O10' 0.066(12) 0.098(14) 0.105(9) 0.052(9) 0.050(9) 0.034(10) O11' 0.090(10) 0.052(8) 0.115(15) -0.011(8) 0.005(11) 0.047(8) N24 0.050(3) 0.056(3) 0.118(5) 0.019(3) 0.038(3) 0.024(2) O12 0.109(4) 0.075(3) 0.153(5) 0.019(3) 0.079(3) 0.034(3) O13 0.103(4) 0.081(3) 0.148(4) 0.047(3) 0.062(3) 0.041(3) O14 0.099(4) 0.253(9) 0.077(3) 0.012(4) 0.031(3) 0.064(5) O15 0.056(2) 0.066(2) 0.096(3) 0.018(2) 0.015(2) 0.0233(19) O16 0.074(5) 0.103(7) 0.095(6) -0.003(5) 0.021(5) 0.051(5) O17 0.155(10) 0.082(8) 0.085(8) -0.004(6) 0.036(7) 0.088(8) _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 N13 2.271(3) . ? Cd1 N1 2.327(3) . ? Cd1 O2 2.333(3) . ? Cd1 N9 2.337(3) . ? Cd1 O3 2.373(3) . ? Cd1 N5 2.385(3) . ? Cd2 N17 2.298(3) . ? Cd2 O1 2.305(3) . ? Cd2 N6 2.348(3) . ? Cd2 N2 2.354(3) . ? Cd2 N10 2.449(3) . ? Cd2 O7 2.585(5) . ? Cd2 O6 2.602(4) . ? O3 N21 1.255(5) . ? O4 N21 1.213(5) . ? O5 N21 1.227(5) . ? O6 N22 1.248(5) . ? O7 N22 1.231(5) . ? O8 N22 1.206(4) . ? N1 C1 1.294(5) . ? N1 N2 1.392(4) . ? N2 C2 1.301(5) . ? N3 C2 1.351(5) . ? N3 C1 1.359(5) . ? N3 C3 1.434(5) . ? N4 C3 1.311(5) . ? N4 C7 1.339(5) . ? N5 C8 1.299(5) . ? N5 N6 1.385(4) . ? N6 C9 1.304(5) . ? N7 C8 1.348(5) . ? N7 C9 1.352(5) . ? N7 C10 1.425(5) . ? N8 C10 1.327(5) . ? N8 C14 1.345(6) . ? N9 C15 1.297(5) . ? N9 N10 1.387(4) . ? N10 C16 1.301(5) . ? N11 C15 1.349(5) . ? N11 C16 1.350(5) . ? N11 C17 1.441(5) . ? N12 C17 1.325(5) . ? N12 C21 1.337(5) . ? N13 C22 1.294(5) . ? N13 N14 1.380(5) . ? N14 C23 1.287(6) . ? N15 C22 1.347(5) . ? N15 C23 1.368(6) . ? N15 C24 1.428(5) . ? N16 C24 1.320(6) . ? N16 C28 1.350(6) . ? N17 C30 1.297(5) . ? N17 N18 1.384(4) . ? N18 C29 1.291(5) . ? N19 C30 1.353(5) . ? N19 C29 1.357(5) . ? N19 C31 1.433(5) . ? N20 C31 1.324(5) . ? N20 C35 1.345(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.371(5) . ? C4 C5 1.385(6) . ? C4 H4 0.9300 . ? C5 C6 1.376(6) . ? C5 H5 0.9300 . ? C6 C7 1.369(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.374(6) . ? C11 C12 1.387(7) . ? C11 H11 0.9300 . ? C12 C13 1.372(7) . ? C12 H12 0.9300 . ? C13 C14 1.371(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.368(6) . ? C18 C19 1.377(6) . ? C18 H18 0.9300 . ? C19 C20 1.369(7) . ? C19 H19 0.9300 . ? C20 C21 1.372(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.362(6) . ? C25 C26 1.387(7) . ? C25 H25 0.9300 . ? C26 C27 1.365(8) . ? C26 H26 0.9300 . ? C27 C28 1.361(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.371(6) . ? C32 C33 1.383(6) . ? C32 H32 0.9300 . ? C33 C34 1.360(7) . ? C33 H33 0.9300 . ? C34 C35 1.373(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? N23 O11 1.18(3) . ? N23 O1O 1.19(2) . ? N23 O10' 1.23(2) . ? N23 O11' 1.25(3) . ? N23 O9' 1.288(9) . ? N23 O9 1.301(10) . ? N24 O14 1.151(7) . ? N24 O12 1.233(6) . ? N24 O13 1.260(6) . ? O17 O17 1.48(3) 2_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 N13 Cd1 N1 172.02(12) . . ? N13 Cd1 O2 83.47(13) . . ? N1 Cd1 O2 91.44(12) . . ? N13 Cd1 N9 96.39(12) . . ? N1 Cd1 N9 90.36(11) . . ? O2 Cd1 N9 161.84(13) . . ? N13 Cd1 O3 93.86(12) . . ? N1 Cd1 O3 79.47(11) . . ? O2 Cd1 O3 84.22(14) . . ? N9 Cd1 O3 113.87(13) . . ? N13 Cd1 N5 91.27(13) . . ? N1 Cd1 N5 93.90(12) . . ? O2 Cd1 N5 79.90(13) . . ? N9 Cd1 N5 81.94(12) . . ? O3 Cd1 N5 162.64(12) . . ? N17 Cd2 O1 90.51(12) . . ? N17 Cd2 N6 175.02(11) . . ? O1 Cd2 N6 86.56(12) . . ? N17 Cd2 N2 91.46(11) . . ? O1 Cd2 N2 168.85(11) . . ? N6 Cd2 N2 90.65(11) . . ? N17 Cd2 N10 89.72(11) . . ? O1 Cd2 N10 83.35(12) . . ? N6 Cd2 N10 85.94(12) . . ? N2 Cd2 N10 85.69(11) . . ? N17 Cd2 O7 109.46(12) . . ? O1 Cd2 O7 76.53(12) . . ? N6 Cd2 O7 73.77(12) . . ? N2 Cd2 O7 113.02(12) . . ? N10 Cd2 O7 152.03(12) . . ? N17 Cd2 O6 79.33(11) . . ? O1 Cd2 O6 113.45(11) . . ? N6 Cd2 O6 105.54(11) . . ? N2 Cd2 O6 77.70(11) . . ? N10 Cd2 O6 159.75(12) . . ? O7 Cd2 O6 47.97(11) . . ? N21 O3 Cd1 110.3(3) . . ? N22 O6 Cd2 97.1(3) . . ? N22 O7 Cd2 98.4(3) . . ? C1 N1 N2 106.7(3) . . ? C1 N1 Cd1 127.8(2) . . ? N2 N1 Cd1 125.3(2) . . ? C2 N2 N1 107.1(3) . . ? C2 N2 Cd2 124.4(2) . . ? N1 N2 Cd2 128.3(2) . . ? C2 N3 C1 104.8(3) . . ? C2 N3 C3 126.5(3) . . ? C1 N3 C3 128.6(3) . . ? C3 N4 C7 116.3(4) . . ? C8 N5 N6 107.0(3) . . ? C8 N5 Cd1 126.0(3) . . ? N6 N5 Cd1 126.8(2) . . ? C9 N6 N5 106.7(3) . . ? C9 N6 Cd2 126.9(3) . . ? N5 N6 Cd2 124.3(2) . . ? C8 N7 C9 104.7(3) . . ? C8 N7 C10 125.9(3) . . ? C9 N7 C10 129.2(3) . . ? C10 N8 C14 115.4(4) . . ? C15 N9 N10 107.2(3) . . ? C15 N9 Cd1 127.2(3) . . ? N10 N9 Cd1 124.5(2) . . ? C16 N10 N9 106.4(3) . . ? C16 N10 Cd2 124.4(3) . . ? N9 N10 Cd2 127.2(2) . . ? C15 N11 C16 104.8(3) . . ? C15 N11 C17 126.4(3) . . ? C16 N11 C17 128.4(3) . . ? C17 N12 C21 116.0(4) . . ? C22 N13 N14 108.7(4) . . ? C22 N13 Cd1 127.7(3) . . ? N14 N13 Cd1 122.2(3) . . ? C23 N14 N13 105.4(4) . . ? C22 N15 C23 103.8(4) . . ? C22 N15 C24 127.5(4) . . ? C23 N15 C24 128.8(4) . . ? C24 N16 C28 116.2(4) . . ? C30 N17 N18 108.2(3) . . ? C30 N17 Cd2 129.1(3) . . ? N18 N17 Cd2 120.1(2) . . ? C29 N18 N17 105.8(3) . . ? C30 N19 C29 104.3(3) . . ? C30 N19 C31 126.7(3) . . ? C29 N19 C31 128.4(3) . . ? C31 N20 C35 116.0(4) . . ? O4 N21 O5 121.8(5) . . ? O4 N21 O3 118.3(4) . . ? O5 N21 O3 119.8(4) . . ? O8 N22 O7 122.8(4) . . ? O8 N22 O6 120.7(4) . . ? O7 N22 O6 116.5(4) . . ? N1 C1 N3 110.9(3) . . ? N1 C1 H1 124.5 . . ? N3 C1 H1 124.5 . . ? N2 C2 N3 110.5(3) . . ? N2 C2 H2 124.8 . . ? N3 C2 H2 124.8 . . ? N4 C3 C4 126.1(4) . . ? N4 C3 N3 113.7(3) . . ? C4 C3 N3 120.2(3) . . ? C3 C4 C5 116.7(4) . . ? C3 C4 H4 121.7 . . ? C5 C4 H4 121.7 . . ? C6 C5 C4 118.8(4) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? N4 C7 C6 122.9(4) . . ? N4 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? N5 C8 N7 110.9(4) . . ? N5 C8 H8 124.6 . . ? N7 C8 H8 124.6 . . ? N6 C9 N7 110.7(3) . . ? N6 C9 H9 124.6 . . ? N7 C9 H9 124.6 . . ? N8 C10 C11 125.8(4) . . ? N8 C10 N7 113.1(3) . . ? C11 C10 N7 121.1(4) . . ? C10 C11 C12 116.6(5) . . ? C10 C11 H11 121.7 . . ? C12 C11 H11 121.7 . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 118.1(5) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N8 C14 C13 124.2(5) . . ? N8 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? N9 C15 N11 110.7(3) . . ? N9 C15 H15 124.7 . . ? N11 C15 H15 124.7 . . ? N10 C16 N11 110.9(3) . . ? N10 C16 H16 124.6 . . ? N11 C16 H16 124.6 . . ? N12 C17 C18 125.4(4) . . ? N12 C17 N11 113.4(3) . . ? C18 C17 N11 121.1(4) . . ? C17 C18 C19 117.3(4) . . ? C17 C18 H18 121.3 . . ? C19 C18 H18 121.3 . . ? C20 C19 C18 118.9(4) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C19 C20 C21 119.2(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N12 C21 C20 123.1(4) . . ? N12 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? N13 C22 N15 110.2(4) . . ? N13 C22 H22 124.9 . . ? N15 C22 H22 124.9 . . ? N14 C23 N15 112.0(4) . . ? N14 C23 H23 124.0 . . ? N15 C23 H23 124.0 . . ? N16 C24 C25 124.8(4) . . ? N16 C24 N15 114.3(4) . . ? C25 C24 N15 120.9(4) . . ? C24 C25 C26 117.5(5) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 118.7(5) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? N16 C28 C27 123.4(5) . . ? N16 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? N18 C29 N19 111.8(4) . . ? N18 C29 H29 124.1 . . ? N19 C29 H29 124.1 . . ? N17 C30 N19 110.0(3) . . ? N17 C30 H30 125.0 . . ? N19 C30 H30 125.0 . . ? N20 C31 C32 124.9(4) . . ? N20 C31 N19 114.5(3) . . ? C32 C31 N19 120.5(4) . . ? C31 C32 C33 117.5(4) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C34 C33 C32 119.2(5) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.0(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N20 C35 C34 123.3(5) . . ? N20 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? O11 N23 O1O 124(2) . . ? O11 N23 O10' 128(2) . . ? O1O N23 O10' 13(3) . . ? O11 N23 O11' 18(3) . . ? O1O N23 O11' 116.7(19) . . ? O10' N23 O11' 116.5(19) . . ? O11 N23 O9' 105.6(17) . . ? O1O N23 O9' 113.0(14) . . ? O10' N23 O9' 118.5(13) . . ? O11' N23 O9' 122.1(15) . . ? O11 N23 O9 119.7(17) . . ? O1O N23 O9 114.8(16) . . ? O10' N23 O9 107.4(15) . . ? O11' N23 O9 120.1(13) . . ? O9' N23 O9 56.6(5) . . ? O14 N24 O12 124.6(7) . . ? O14 N24 O13 121.5(7) . . ? O12 N24 O13 113.8(6) . . ? 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 N13 Cd1 O3 N21 -72.4(3) . . . . ? N1 Cd1 O3 N21 112.0(3) . . . . ? O2 Cd1 O3 N21 -155.4(3) . . . . ? N9 Cd1 O3 N21 26.4(3) . . . . ? N5 Cd1 O3 N21 -179.3(3) . . . . ? N17 Cd2 O6 N22 -128.4(2) . . . . ? O1 Cd2 O6 N22 -42.5(3) . . . . ? N6 Cd2 O6 N22 50.5(2) . . . . ? N2 Cd2 O6 N22 137.7(2) . . . . ? N10 Cd2 O6 N22 173.3(3) . . . . ? O7 Cd2 O6 N22 0.3(2) . . . . ? N17 Cd2 O7 N22 54.0(3) . . . . ? O1 Cd2 O7 N22 139.7(3) . . . . ? N6 Cd2 O7 N22 -130.0(3) . . . . ? N2 Cd2 O7 N22 -46.4(3) . . . . ? N10 Cd2 O7 N22 -175.1(2) . . . . ? O6 Cd2 O7 N22 -0.4(2) . . . . ? N13 Cd1 N1 C1 -18.8(11) . . . . ? O2 Cd1 N1 C1 -69.0(3) . . . . ? N9 Cd1 N1 C1 129.0(3) . . . . ? O3 Cd1 N1 C1 14.8(3) . . . . ? N5 Cd1 N1 C1 -149.0(3) . . . . ? N13 Cd1 N1 N2 167.3(8) . . . . ? O2 Cd1 N1 N2 117.1(3) . . . . ? N9 Cd1 N1 N2 -44.9(3) . . . . ? O3 Cd1 N1 N2 -159.1(3) . . . . ? N5 Cd1 N1 N2 37.1(3) . . . . ? C1 N1 N2 C2 0.0(4) . . . . ? Cd1 N1 N2 C2 175.0(3) . . . . ? C1 N1 N2 Cd2 -176.2(3) . . . . ? Cd1 N1 N2 Cd2 -1.2(4) . . . . ? N17 Cd2 N2 C2 -40.9(3) . . . . ? O1 Cd2 N2 C2 -141.0(5) . . . . ? N6 Cd2 N2 C2 143.6(3) . . . . ? N10 Cd2 N2 C2 -130.5(3) . . . . ? O7 Cd2 N2 C2 71.0(3) . . . . ? O6 Cd2 N2 C2 37.9(3) . . . . ? N17 Cd2 N2 N1 134.7(3) . . . . ? O1 Cd2 N2 N1 34.6(7) . . . . ? N6 Cd2 N2 N1 -40.8(3) . . . . ? N10 Cd2 N2 N1 45.1(3) . . . . ? O7 Cd2 N2 N1 -113.4(3) . . . . ? O6 Cd2 N2 N1 -146.5(3) . . . . ? N13 Cd1 N5 C8 -24.7(4) . . . . ? N1 Cd1 N5 C8 149.2(4) . . . . ? O2 Cd1 N5 C8 58.4(4) . . . . ? N9 Cd1 N5 C8 -121.0(4) . . . . ? O3 Cd1 N5 C8 82.6(6) . . . . ? N13 Cd1 N5 N6 160.8(3) . . . . ? N1 Cd1 N5 N6 -25.2(3) . . . . ? O2 Cd1 N5 N6 -116.0(3) . . . . ? N9 Cd1 N5 N6 64.6(3) . . . . ? O3 Cd1 N5 N6 -91.9(5) . . . . ? C8 N5 N6 C9 -0.6(5) . . . . ? Cd1 N5 N6 C9 174.7(3) . . . . ? C8 N5 N6 Cd2 163.8(3) . . . . ? Cd1 N5 N6 Cd2 -20.9(4) . . . . ? N17 Cd2 N6 C9 98.0(13) . . . . ? O1 Cd2 N6 C9 43.9(3) . . . . ? N2 Cd2 N6 C9 -146.9(3) . . . . ? N10 Cd2 N6 C9 127.5(4) . . . . ? O7 Cd2 N6 C9 -33.1(3) . . . . ? O6 Cd2 N6 C9 -69.5(4) . . . . ? N17 Cd2 N6 N5 -63.1(13) . . . . ? O1 Cd2 N6 N5 -117.2(3) . . . . ? N2 Cd2 N6 N5 52.0(3) . . . . ? N10 Cd2 N6 N5 -33.7(3) . . . . ? O7 Cd2 N6 N5 165.8(3) . . . . ? O6 Cd2 N6 N5 129.4(3) . . . . ? N13 Cd1 N9 C15 24.1(4) . . . . ? N1 Cd1 N9 C15 -151.6(4) . . . . ? O2 Cd1 N9 C15 112.7(5) . . . . ? O3 Cd1 N9 C15 -73.0(4) . . . . ? N5 Cd1 N9 C15 114.5(4) . . . . ? N13 Cd1 N9 N10 -142.7(3) . . . . ? N1 Cd1 N9 N10 41.6(3) . . . . ? O2 Cd1 N9 N10 -54.1(6) . . . . ? O3 Cd1 N9 N10 120.2(3) . . . . ? N5 Cd1 N9 N10 -52.3(3) . . . . ? C15 N9 N10 C16 0.5(5) . . . . ? Cd1 N9 N10 C16 169.5(3) . . . . ? C15 N9 N10 Cd2 -164.2(3) . . . . ? Cd1 N9 N10 Cd2 4.8(5) . . . . ? N17 Cd2 N10 C16 59.2(4) . . . . ? O1 Cd2 N10 C16 -31.3(4) . . . . ? N6 Cd2 N10 C16 -118.3(4) . . . . ? N2 Cd2 N10 C16 150.7(4) . . . . ? O7 Cd2 N10 C16 -75.3(4) . . . . ? O6 Cd2 N10 C16 116.0(4) . . . . ? N17 Cd2 N10 N9 -138.7(3) . . . . ? O1 Cd2 N10 N9 130.8(3) . . . . ? N6 Cd2 N10 N9 43.8(3) . . . . ? N2 Cd2 N10 N9 -47.2(3) . . . . ? O7 Cd2 N10 N9 86.8(4) . . . . ? O6 Cd2 N10 N9 -81.9(5) . . . . ? N1 Cd1 N13 C22 8.1(11) . . . . ? O2 Cd1 N13 C22 58.7(4) . . . . ? N9 Cd1 N13 C22 -139.6(4) . . . . ? O3 Cd1 N13 C22 -25.0(4) . . . . ? N5 Cd1 N13 C22 138.4(4) . . . . ? N1 Cd1 N13 N14 -157.0(8) . . . . ? O2 Cd1 N13 N14 -106.3(3) . . . . ? N9 Cd1 N13 N14 55.4(3) . . . . ? O3 Cd1 N13 N14 169.9(3) . . . . ? N5 Cd1 N13 N14 -26.6(3) . . . . ? C22 N13 N14 C23 -0.3(5) . . . . ? Cd1 N13 N14 C23 167.2(3) . . . . ? O1 Cd2 N17 C30 -92.4(3) . . . . ? N6 Cd2 N17 C30 -146.4(11) . . . . ? N2 Cd2 N17 C30 98.6(3) . . . . ? N10 Cd2 N17 C30 -175.7(3) . . . . ? O7 Cd2 N17 C30 -16.5(4) . . . . ? O6 Cd2 N17 C30 21.4(3) . . . . ? O1 Cd2 N17 N18 108.2(3) . . . . ? N6 Cd2 N17 N18 54.3(13) . . . . ? N2 Cd2 N17 N18 -60.8(3) . . . . ? N10 Cd2 N17 N18 24.9(3) . . . . ? O7 Cd2 N17 N18 -175.9(3) . . . . ? O6 Cd2 N17 N18 -138.0(3) . . . . ? C30 N17 N18 C29 -0.2(5) . . . . ? Cd2 N17 N18 C29 163.1(3) . . . . ? Cd1 O3 N21 O4 9.9(5) . . . . ? Cd1 O3 N21 O5 -172.2(3) . . . . ? Cd2 O7 N22 O8 -178.0(3) . . . . ? Cd2 O7 N22 O6 0.6(4) . . . . ? Cd2 O6 N22 O8 178.1(3) . . . . ? Cd2 O6 N22 O7 -0.6(4) . . . . ? N2 N1 C1 N3 0.3(4) . . . . ? Cd1 N1 C1 N3 -174.5(2) . . . . ? C2 N3 C1 N1 -0.4(4) . . . . ? C3 N3 C1 N1 176.6(3) . . . . ? N1 N2 C2 N3 -0.3(4) . . . . ? Cd2 N2 C2 N3 176.1(2) . . . . ? C1 N3 C2 N2 0.4(4) . . . . ? C3 N3 C2 N2 -176.7(3) . . . . ? C7 N4 C3 C4 0.4(6) . . . . ? C7 N4 C3 N3 179.6(3) . . . . ? C2 N3 C3 N4 -35.3(5) . . . . ? C1 N3 C3 N4 148.3(4) . . . . ? C2 N3 C3 C4 143.8(4) . . . . ? C1 N3 C3 C4 -32.5(6) . . . . ? N4 C3 C4 C5 -0.8(7) . . . . ? N3 C3 C4 C5 -179.9(4) . . . . ? C3 C4 C5 C6 0.8(7) . . . . ? C4 C5 C6 C7 -0.5(7) . . . . ? C3 N4 C7 C6 0.0(6) . . . . ? C5 C6 C7 N4 0.0(7) . . . . ? N6 N5 C8 N7 0.2(5) . . . . ? Cd1 N5 C8 N7 -175.1(3) . . . . ? C9 N7 C8 N5 0.2(5) . . . . ? C10 N7 C8 N5 -174.7(4) . . . . ? N5 N6 C9 N7 0.7(5) . . . . ? Cd2 N6 C9 N7 -163.1(3) . . . . ? C8 N7 C9 N6 -0.6(5) . . . . ? C10 N7 C9 N6 174.1(4) . . . . ? C14 N8 C10 C11 -2.0(7) . . . . ? C14 N8 C10 N7 176.2(4) . . . . ? C8 N7 C10 N8 -1.5(6) . . . . ? C9 N7 C10 N8 -175.1(4) . . . . ? C8 N7 C10 C11 176.8(4) . . . . ? C9 N7 C10 C11 3.2(7) . . . . ? N8 C10 C11 C12 2.2(7) . . . . ? N7 C10 C11 C12 -175.8(4) . . . . ? C10 C11 C12 C13 -0.4(8) . . . . ? C11 C12 C13 C14 -1.4(8) . . . . ? C10 N8 C14 C13 -0.1(8) . . . . ? C12 C13 C14 N8 1.8(8) . . . . ? N10 N9 C15 N11 -0.1(5) . . . . ? Cd1 N9 C15 N11 -168.7(3) . . . . ? C16 N11 C15 N9 -0.3(5) . . . . ? C17 N11 C15 N9 173.8(4) . . . . ? N9 N10 C16 N11 -0.6(5) . . . . ? Cd2 N10 C16 N11 164.6(3) . . . . ? C15 N11 C16 N10 0.6(5) . . . . ? C17 N11 C16 N10 -173.4(4) . . . . ? C21 N12 C17 C18 2.0(6) . . . . ? C21 N12 C17 N11 -174.3(4) . . . . ? C15 N11 C17 N12 11.4(6) . . . . ? C16 N11 C17 N12 -175.9(4) . . . . ? C15 N11 C17 C18 -165.1(4) . . . . ? C16 N11 C17 C18 7.6(6) . . . . ? N12 C17 C18 C19 -0.9(7) . . . . ? N11 C17 C18 C19 175.2(4) . . . . ? C17 C18 C19 C20 -1.1(7) . . . . ? C18 C19 C20 C21 1.8(7) . . . . ? C17 N12 C21 C20 -1.3(7) . . . . ? C19 C20 C21 N12 -0.5(7) . . . . ? N14 N13 C22 N15 0.5(5) . . . . ? Cd1 N13 C22 N15 -166.1(3) . . . . ? C23 N15 C22 N13 -0.5(5) . . . . ? C24 N15 C22 N13 179.5(4) . . . . ? N13 N14 C23 N15 0.0(6) . . . . ? C22 N15 C23 N14 0.3(6) . . . . ? C24 N15 C23 N14 -179.7(4) . . . . ? C28 N16 C24 C25 0.6(8) . . . . ? C28 N16 C24 N15 -179.8(5) . . . . ? C22 N15 C24 N16 16.9(7) . . . . ? C23 N15 C24 N16 -163.2(5) . . . . ? C22 N15 C24 C25 -163.5(5) . . . . ? C23 N15 C24 C25 16.4(7) . . . . ? N16 C24 C25 C26 2.1(8) . . . . ? N15 C24 C25 C26 -177.4(4) . . . . ? C24 C25 C26 C27 -2.7(8) . . . . ? C25 C26 C27 C28 0.7(9) . . . . ? C24 N16 C28 C27 -2.9(9) . . . . ? C26 C27 C28 N16 2.3(10) . . . . ? N17 N18 C29 N19 -0.1(5) . . . . ? C30 N19 C29 N18 0.4(5) . . . . ? C31 N19 C29 N18 -171.0(4) . . . . ? N18 N17 C30 N19 0.5(5) . . . . ? Cd2 N17 C30 N19 -160.8(2) . . . . ? C29 N19 C30 N17 -0.5(5) . . . . ? C31 N19 C30 N17 171.0(3) . . . . ? C35 N20 C31 C32 0.1(6) . . . . ? C35 N20 C31 N19 -178.0(3) . . . . ? C30 N19 C31 N20 30.4(5) . . . . ? C29 N19 C31 N20 -160.0(4) . . . . ? C30 N19 C31 C32 -147.7(4) . . . . ? C29 N19 C31 C32 21.8(6) . . . . ? N20 C31 C32 C33 -0.1(7) . . . . ? N19 C31 C32 C33 177.8(4) . . . . ? C31 C32 C33 C34 0.2(7) . . . . ? C32 C33 C34 C35 -0.3(7) . . . . ? C31 N20 C35 C34 -0.2(7) . . . . ? C33 C34 C35 N20 0.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.944 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.081 data_041003b _database_code_depnum_ccdc_archive 'CCDC 253308' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H8 Cd N4 O5 S' _chemical_formula_weight 372.63 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.4376(15) _cell_length_b 18.426(5) _cell_length_c 5.5827(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.483(4) _cell_angle_gamma 90.00 _cell_volume 541.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 911 _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 26.26 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 2.230 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.641867 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 '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 3125 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.26 _reflns_number_total 1785 _reflns_number_gt 1759 _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^)+(0.0280P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 1785 _refine_ls_number_parameters 163 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0485 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _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 0.69614(4) -0.165307(15) 0.26168(4) 0.01619(8) Uani 1 1 d . . . S1 S 1.29475(15) -0.12997(5) 0.67975(17) 0.01610(18) Uani 1 1 d . . . O1 O 1.0965(5) -0.17550(19) 0.5155(4) 0.0246(7) Uani 1 1 d . . . O2 O 1.2222(6) -0.05448(18) 0.6770(6) 0.0318(7) Uani 1 1 d . . . O3 O 1.3394(4) -0.1616(3) 0.9328(4) 0.0282(6) Uani 1 1 d . . . O4 O 1.5369(5) -0.13774(16) 0.6024(5) 0.0229(6) Uani 1 1 d . . . O5 O 0.8815(6) -0.21333(18) -0.0256(5) 0.0294(7) Uani 1 1 d . . . H5A H 0.7806 -0.1952 -0.1641 0.035 Uiso 1 1 d R . . H5B H 1.0108 -0.2407 -0.0061 0.035 Uiso 1 1 d R . . N1 N 0.7378(6) -0.0406(2) 0.2048(6) 0.0215(7) Uani 1 1 d . . . N2 N 0.5067(6) 0.12361(19) 0.4523(6) 0.0220(7) Uani 1 1 d . . . N3 N 0.2340(8) 0.1596(2) 0.6599(8) 0.0316(8) Uani 1 1 d . . . N4 N 0.3886(7) 0.2175(2) 0.6352(7) 0.0262(8) Uani 1 1 d . . . C1 C 0.8598(8) -0.0117(3) 0.0505(8) 0.0281(9) Uani 1 1 d . . . H1 H 0.9390 -0.0426 -0.0389 0.034 Uiso 1 1 calc R . . C2 C 0.8745(9) 0.0619(3) 0.0168(8) 0.0317(11) Uani 1 1 d . . . H2 H 0.9646 0.0799 -0.0917 0.038 Uiso 1 1 calc R . . C3 C 0.7549(8) 0.1097(3) 0.1446(8) 0.0275(9) Uani 1 1 d . . . H3 H 0.7570 0.1596 0.1204 0.033 Uiso 1 1 calc R . . C4 C 0.6319(8) 0.0787(2) 0.3108(8) 0.0208(8) Uani 1 1 d . . . C5 C 0.6262(8) 0.0049(3) 0.3367(8) 0.0228(9) Uani 1 1 d . . . H5 H 0.5430 -0.0147 0.4485 0.027 Uiso 1 1 calc R . . C6 C 0.3083(8) 0.1049(3) 0.5516(9) 0.0291(10) Uani 1 1 d . . . H6 H 0.2368 0.0588 0.5420 0.035 Uiso 1 1 calc R . . C7 C 0.5486(8) 0.1940(2) 0.5129(9) 0.0260(9) Uani 1 1 d . . . H7 H 0.6746 0.2222 0.4731 0.031 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 0.01642(12) 0.01707(13) 0.01559(11) 0.00075(14) 0.00495(8) 0.00019(14) S1 0.0147(4) 0.0196(5) 0.0145(4) 0.0002(4) 0.0046(3) 0.0001(3) O1 0.0212(11) 0.019(2) 0.0288(12) -0.0042(13) -0.0024(9) 0.0025(12) O2 0.0354(17) 0.0215(17) 0.0434(17) 0.0009(15) 0.0192(14) 0.0047(14) O3 0.0171(10) 0.0481(18) 0.0195(11) 0.009(2) 0.0045(8) -0.003(2) O4 0.0180(12) 0.0335(16) 0.0195(12) 0.0008(11) 0.0091(10) 0.0023(11) O5 0.0246(14) 0.042(2) 0.0229(14) 0.0023(13) 0.0090(11) 0.0029(13) N1 0.0227(16) 0.0209(19) 0.0214(16) -0.0029(14) 0.0061(13) 0.0006(14) N2 0.0256(16) 0.0159(18) 0.0279(18) -0.0012(14) 0.0129(14) -0.0011(14) N3 0.033(2) 0.026(2) 0.041(2) -0.0019(18) 0.0205(18) 0.0008(18) N4 0.0274(18) 0.019(2) 0.0361(19) 0.0001(15) 0.0152(16) 0.0032(14) C1 0.030(2) 0.032(3) 0.025(2) -0.0027(18) 0.0125(17) 0.0039(18) C2 0.040(3) 0.029(3) 0.032(2) 0.0009(18) 0.021(2) -0.0008(19) C3 0.038(2) 0.016(2) 0.032(2) 0.0022(19) 0.0151(17) -0.0036(19) C4 0.022(2) 0.020(2) 0.022(2) -0.0008(18) 0.0090(16) 0.0005(16) C5 0.022(2) 0.025(2) 0.024(2) 0.0029(17) 0.0112(17) 0.0045(18) C6 0.031(2) 0.024(2) 0.039(3) -0.003(2) 0.0196(19) -0.007(2) C7 0.029(2) 0.014(2) 0.037(2) -0.0013(18) 0.0132(19) -0.0017(16) _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 O5 2.276(3) . ? Cd1 O1 2.289(2) . ? Cd1 N4 2.310(4) 2_646 ? Cd1 O3 2.314(2) 1_454 ? Cd1 O4 2.334(2) 1_455 ? Cd1 N1 2.338(4) . ? S1 O2 1.445(3) . ? S1 O1 1.487(3) . ? S1 O3 1.491(3) . ? S1 O4 1.492(3) . ? O3 Cd1 2.314(2) 1_656 ? O4 Cd1 2.334(2) 1_655 ? O5 H5A 0.8931 . ? O5 H5B 0.8502 . ? N1 C1 1.323(6) . ? N1 C5 1.356(6) . ? N2 C7 1.346(5) . ? N2 C6 1.375(5) . ? N2 C4 1.429(5) . ? N3 C6 1.291(6) . ? N3 N4 1.386(5) . ? N4 C7 1.307(6) . ? N4 Cd1 2.310(4) 2_656 ? C1 C2 1.376(7) . ? C1 H1 0.9300 . ? C2 C3 1.392(7) . ? C2 H2 0.9300 . ? C3 C4 1.395(6) . ? C3 H3 0.9300 . ? C4 C5 1.368(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? 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 O5 Cd1 O1 83.34(10) . . ? O5 Cd1 N4 87.89(12) . 2_646 ? O1 Cd1 N4 89.27(12) . 2_646 ? O5 Cd1 O3 83.31(11) . 1_454 ? O1 Cd1 O3 166.44(9) . 1_454 ? N4 Cd1 O3 92.62(15) 2_646 1_454 ? O5 Cd1 O4 168.15(11) . 1_455 ? O1 Cd1 O4 90.16(9) . 1_455 ? N4 Cd1 O4 82.11(11) 2_646 1_455 ? O3 Cd1 O4 103.41(9) 1_454 1_455 ? O5 Cd1 N1 102.20(12) . . ? O1 Cd1 N1 93.16(12) . . ? N4 Cd1 N1 169.82(11) 2_646 . ? O3 Cd1 N1 87.34(15) 1_454 . ? O4 Cd1 N1 88.00(11) 1_455 . ? O2 S1 O1 112.50(19) . . ? O2 S1 O3 111.4(2) . . ? O1 S1 O3 106.6(2) . . ? O2 S1 O4 110.35(18) . . ? O1 S1 O4 108.87(16) . . ? O3 S1 O4 106.89(15) . . ? S1 O1 Cd1 140.0(2) . . ? S1 O3 Cd1 132.00(16) . 1_656 ? S1 O4 Cd1 142.27(16) . 1_655 ? Cd1 O5 H5A 100.4 . . ? Cd1 O5 H5B 129.7 . . ? H5A O5 H5B 129.9 . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Cd1 124.4(3) . . ? C5 N1 Cd1 117.5(3) . . ? C7 N2 C6 103.9(4) . . ? C7 N2 C4 128.6(4) . . ? C6 N2 C4 127.5(4) . . ? C6 N3 N4 106.6(3) . . ? C7 N4 N3 107.2(4) . . ? C7 N4 Cd1 129.8(3) . 2_656 ? N3 N4 Cd1 122.1(3) . 2_656 ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 120.2(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 116.4(4) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 N2 119.4(4) . . ? C3 C4 N2 120.3(4) . . ? N1 C5 C4 122.1(4) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N3 C6 N2 111.2(4) . . ? N3 C6 H6 124.4 . . ? N2 C6 H6 124.4 . . ? N4 C7 N2 111.0(4) . . ? N4 C7 H7 124.5 . . ? N2 C7 H7 124.5 . . ? 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 S1 O1 Cd1 -2.8(3) . . . . ? O3 S1 O1 Cd1 119.6(3) . . . . ? O4 S1 O1 Cd1 -125.4(2) . . . . ? O5 Cd1 O1 S1 124.6(3) . . . . ? N4 Cd1 O1 S1 -147.5(3) 2_646 . . . ? O3 Cd1 O1 S1 114.4(7) 1_454 . . . ? O4 Cd1 O1 S1 -65.4(3) 1_455 . . . ? N1 Cd1 O1 S1 22.6(3) . . . . ? O2 S1 O3 Cd1 -87.1(3) . . . 1_656 ? O1 S1 O3 Cd1 149.8(3) . . . 1_656 ? O4 S1 O3 Cd1 33.5(4) . . . 1_656 ? O2 S1 O4 Cd1 -98.2(3) . . . 1_655 ? O1 S1 O4 Cd1 25.7(4) . . . 1_655 ? O3 S1 O4 Cd1 140.5(3) . . . 1_655 ? O5 Cd1 N1 C1 -4.3(4) . . . . ? O1 Cd1 N1 C1 79.6(3) . . . . ? N4 Cd1 N1 C1 -176.8(6) 2_646 . . . ? O3 Cd1 N1 C1 -86.9(3) 1_454 . . . ? O4 Cd1 N1 C1 169.6(3) 1_455 . . . ? O5 Cd1 N1 C5 174.7(3) . . . . ? O1 Cd1 N1 C5 -101.4(3) . . . . ? N4 Cd1 N1 C5 2.2(8) 2_646 . . . ? O3 Cd1 N1 C5 92.2(3) 1_454 . . . ? O4 Cd1 N1 C5 -11.4(3) 1_455 . . . ? C6 N3 N4 C7 -0.1(5) . . . . ? C6 N3 N4 Cd1 170.0(3) . . . 2_656 ? C5 N1 C1 C2 -0.9(6) . . . . ? Cd1 N1 C1 C2 178.1(3) . . . . ? N1 C1 C2 C3 -1.0(7) . . . . ? C1 C2 C3 C4 2.4(7) . . . . ? C2 C3 C4 C5 -1.9(7) . . . . ? C2 C3 C4 N2 179.2(4) . . . . ? C7 N2 C4 C5 158.1(4) . . . . ? C6 N2 C4 C5 -24.2(6) . . . . ? C7 N2 C4 C3 -23.0(7) . . . . ? C6 N2 C4 C3 154.7(5) . . . . ? C1 N1 C5 C4 1.4(6) . . . . ? Cd1 N1 C5 C4 -177.7(3) . . . . ? C3 C4 C5 N1 0.0(7) . . . . ? N2 C4 C5 N1 178.9(4) . . . . ? N4 N3 C6 N2 -0.5(5) . . . . ? C7 N2 C6 N3 0.9(5) . . . . ? C4 N2 C6 N3 -177.3(5) . . . . ? N3 N4 C7 N2 0.7(5) . . . . ? Cd1 N4 C7 N2 -168.4(3) 2_656 . . . ? C6 N2 C7 N4 -1.0(5) . . . . ? C4 N2 C7 N4 177.2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.330 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.129 data_41030a _database_code_depnum_ccdc_archive 'CCDC 266097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 Cd2 N28' _chemical_formula_weight 1073.63 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7470(10) _cell_length_b 7.4296(8) _cell_length_c 14.2432(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.1910(10) _cell_angle_gamma 90.00 _cell_volume 1028.68(19) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2566 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 27.02 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.778329 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 '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 5369 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1809 _reflns_number_gt 1528 _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^)+(0.0348P)^2^+0.1366P] 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 1809 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.0000 1.0000 0.03340(10) Uani 1 2 d S . . N1 N 0.4212(2) 0.1217(3) 0.61293(13) 0.0505(5) Uani 1 1 d . . . N2 N 0.58617(17) 0.1135(2) 0.85417(11) 0.0354(4) Uani 1 1 d . . . N3 N 0.68470(18) 0.1592(3) 0.99554(13) 0.0462(5) Uani 1 1 d . . . N4 N 0.77809(18) 0.0768(3) 0.94043(13) 0.0400(4) Uani 1 1 d . . . N5 N 0.9747(2) 0.1833(3) 1.12919(14) 0.0477(5) Uani 1 1 d . . . N6 N 0.8660(3) 0.4731(3) 1.15661(18) 0.0532(6) Uani 1 1 d . . . N7 N 0.9164(2) 0.7561(3) 1.08071(16) 0.0590(6) Uani 1 1 d . . . C1 C 0.3492(2) 0.0607(4) 0.79550(17) 0.0468(6) Uani 1 1 d . . . H1 H 0.3252 0.0407 0.8566 0.056 Uiso 1 1 calc R . . C2 C 0.2522(3) 0.0496(4) 0.72019(19) 0.0541(7) Uani 1 1 d . . . H2 H 0.1612 0.0216 0.7293 0.065 Uiso 1 1 calc R . . C3 C 0.2932(2) 0.0806(4) 0.63153(17) 0.0521(6) Uani 1 1 d . . . H3 H 0.2272 0.0725 0.5812 0.062 Uiso 1 1 calc R . . C4 C 0.5144(2) 0.1319(3) 0.68639(14) 0.0411(5) Uani 1 1 d . . . H4 H 0.6048 0.1601 0.6754 0.049 Uiso 1 1 calc R . . C5 C 0.4821(2) 0.1024(3) 0.77763(14) 0.0348(5) Uani 1 1 d . . . C6 C 0.7173(2) 0.0514(3) 0.85716(16) 0.0385(5) Uani 1 1 d . . . H6 H 0.7579 -0.0017 0.8069 0.046 Uiso 1 1 calc R . . C7 C 0.5722(2) 0.1787(3) 0.94204(15) 0.0437(6) Uani 1 1 d . . . H7 H 0.4922 0.2308 0.9614 0.052 Uiso 1 1 calc R . . C8 C 0.9266(2) 0.3219(3) 1.13882(15) 0.0382(5) Uani 1 1 d . . . C9 C 0.8982(2) 0.6200(3) 1.11396(16) 0.0386(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 0.03251(14) 0.03195(14) 0.03540(14) 0.00344(9) 0.00014(9) 0.00243(8) N1 0.0451(11) 0.0729(15) 0.0332(10) 0.0034(10) 0.0015(9) 0.0002(10) N2 0.0327(9) 0.0451(11) 0.0285(9) 0.0021(8) 0.0037(7) 0.0057(8) N3 0.0412(10) 0.0637(13) 0.0335(10) -0.0014(9) 0.0026(8) 0.0077(9) N4 0.0361(10) 0.0468(11) 0.0368(10) 0.0020(9) 0.0016(8) 0.0056(9) N5 0.0526(11) 0.0444(12) 0.0458(12) -0.0056(10) 0.0019(9) -0.0005(10) N6 0.0657(15) 0.0416(13) 0.0559(14) 0.0043(9) 0.0301(12) -0.0002(9) N7 0.0704(15) 0.0463(13) 0.0623(14) 0.0112(12) 0.0173(12) -0.0032(11) C1 0.0373(12) 0.0667(15) 0.0369(13) 0.0133(12) 0.0055(10) 0.0059(11) C2 0.0313(12) 0.0751(17) 0.0556(16) 0.0175(14) 0.0015(11) 0.0026(12) C3 0.0432(13) 0.0688(16) 0.0423(14) 0.0052(13) -0.0096(11) 0.0024(13) C4 0.0346(11) 0.0526(14) 0.0365(12) 0.0021(10) 0.0052(9) 0.0001(10) C5 0.0336(11) 0.0395(12) 0.0309(11) 0.0035(10) 0.0000(9) 0.0058(9) C6 0.0355(12) 0.0456(12) 0.0346(12) -0.0003(10) 0.0039(10) 0.0067(10) C7 0.0385(11) 0.0591(15) 0.0341(12) -0.0021(11) 0.0072(10) 0.0099(11) C8 0.0395(11) 0.0455(15) 0.0299(11) 0.0010(10) 0.0052(9) -0.0097(11) C9 0.0395(12) 0.0410(14) 0.0357(12) -0.0003(11) 0.0066(9) -0.0022(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 N5 2.317(2) . ? Cd1 N5 2.317(2) 3_757 ? Cd1 N7 2.325(2) 3_767 ? Cd1 N7 2.325(2) 1_545 ? Cd1 N4 2.3358(17) 3_757 ? Cd1 N4 2.3358(17) . ? N1 C3 1.330(3) . ? N1 C4 1.337(3) . ? N2 C6 1.356(3) . ? N2 C7 1.358(3) . ? N2 C5 1.436(2) . ? N3 C7 1.297(3) . ? N3 N4 1.387(2) . ? N4 C6 1.300(3) . ? N5 C8 1.144(3) . ? N6 C9 1.299(3) . ? N6 C8 1.302(3) . ? N7 C9 1.136(3) . ? N7 Cd1 2.325(2) 1_565 ? C1 C5 1.374(3) . ? C1 C2 1.379(3) . ? C1 H1 0.9300 . ? C2 C3 1.371(4) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? 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 180.00(8) . 3_757 ? N5 Cd1 N7 89.78(8) . 3_767 ? N5 Cd1 N7 90.22(8) 3_757 3_767 ? N5 Cd1 N7 90.22(8) . 1_545 ? N5 Cd1 N7 89.78(8) 3_757 1_545 ? N7 Cd1 N7 180.0 3_767 1_545 ? N5 Cd1 N4 90.26(7) . 3_757 ? N5 Cd1 N4 89.74(7) 3_757 3_757 ? N7 Cd1 N4 91.22(7) 3_767 3_757 ? N7 Cd1 N4 88.78(7) 1_545 3_757 ? N5 Cd1 N4 89.74(7) . . ? N5 Cd1 N4 90.26(7) 3_757 . ? N7 Cd1 N4 88.78(7) 3_767 . ? N7 Cd1 N4 91.22(7) 1_545 . ? N4 Cd1 N4 180.0 3_757 . ? C3 N1 C4 116.8(2) . . ? C6 N2 C7 104.47(18) . . ? C6 N2 C5 128.03(18) . . ? C7 N2 C5 127.38(17) . . ? C7 N3 N4 106.17(17) . . ? C6 N4 N3 107.83(17) . . ? C6 N4 Cd1 130.09(15) . . ? N3 N4 Cd1 122.07(13) . . ? C8 N5 Cd1 133.84(18) . . ? C9 N6 C8 120.4(2) . . ? C9 N7 Cd1 166.1(2) . 1_565 ? C5 C1 C2 118.1(2) . . ? C5 C1 H1 120.9 . . ? C2 C1 H1 120.9 . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? N1 C3 C2 124.2(2) . . ? N1 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? N1 C4 C5 122.7(2) . . ? N1 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C1 C5 C4 119.6(2) . . ? C1 C5 N2 119.72(19) . . ? C4 C5 N2 120.63(18) . . ? N4 C6 N2 110.2(2) . . ? N4 C6 H6 124.9 . . ? N2 C6 H6 124.9 . . ? N3 C7 N2 111.37(19) . . ? N3 C7 H7 124.3 . . ? N2 C7 H7 124.3 . . ? N5 C8 N6 174.4(2) . . ? N7 C9 N6 173.4(3) . . ? 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 C7 N3 N4 C6 0.0(3) . . . . ? C7 N3 N4 Cd1 -178.51(15) . . . . ? N5 Cd1 N4 C6 166.9(2) . . . . ? N5 Cd1 N4 C6 -13.1(2) 3_757 . . . ? N7 Cd1 N4 C6 77.1(2) 3_767 . . . ? N7 Cd1 N4 C6 -102.9(2) 1_545 . . . ? N4 Cd1 N4 C6 -151(3) 3_757 . . . ? N5 Cd1 N4 N3 -14.98(17) . . . . ? N5 Cd1 N4 N3 165.02(17) 3_757 . . . ? N7 Cd1 N4 N3 -104.77(17) 3_767 . . . ? N7 Cd1 N4 N3 75.23(17) 1_545 . . . ? N4 Cd1 N4 N3 27(3) 3_757 . . . ? N5 Cd1 N5 C8 -93(18) 3_757 . . . ? N7 Cd1 N5 C8 48.5(2) 3_767 . . . ? N7 Cd1 N5 C8 -131.5(2) 1_545 . . . ? N4 Cd1 N5 C8 139.7(2) 3_757 . . . ? N4 Cd1 N5 C8 -40.3(2) . . . . ? C5 C1 C2 C3 -0.1(4) . . . . ? C4 N1 C3 C2 0.3(4) . . . . ? C1 C2 C3 N1 -0.2(5) . . . . ? C3 N1 C4 C5 -0.2(4) . . . . ? C2 C1 C5 C4 0.2(4) . . . . ? C2 C1 C5 N2 -179.4(2) . . . . ? N1 C4 C5 C1 -0.1(4) . . . . ? N1 C4 C5 N2 179.5(2) . . . . ? C6 N2 C5 C1 138.4(2) . . . . ? C7 N2 C5 C1 -37.1(3) . . . . ? C6 N2 C5 C4 -41.2(3) . . . . ? C7 N2 C5 C4 143.4(2) . . . . ? N3 N4 C6 N2 -0.1(3) . . . . ? Cd1 N4 C6 N2 178.30(14) . . . . ? C7 N2 C6 N4 0.1(3) . . . . ? C5 N2 C6 N4 -176.2(2) . . . . ? N4 N3 C7 N2 0.0(3) . . . . ? C6 N2 C7 N3 -0.1(3) . . . . ? C5 N2 C7 N3 176.2(2) . . . . ? Cd1 N5 C8 N6 133(3) . . . . ? C9 N6 C8 N5 171(3) . . . . ? Cd1 N7 C9 N6 173.1(18) 1_565 . . . ? C8 N6 C9 N7 174(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.248 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.048 data_041020b _database_code_depnum_ccdc_archive 'CCDC 266224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Cd N8 O2 S2' _chemical_formula_weight 552.91 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9290(17) _cell_length_b 10.0981(18) _cell_length_c 10.9452(19) _cell_angle_alpha 87.578(3) _cell_angle_beta 74.968(2) _cell_angle_gamma 85.958(3) _cell_volume 1056.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2807 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 26.43 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.792133 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 '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 5567 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3708 _reflns_number_gt 3130 _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^)+(0.0602P)^2^+0.3128P] 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 3708 _refine_ls_number_parameters 280 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.24737(3) 0.26329(3) 0.76970(3) 0.03553(14) Uani 1 1 d . . . S1 S -0.14262(12) 0.28961(14) 0.56085(13) 0.0540(3) Uani 1 1 d . . . S2 S 0.60900(15) 0.20080(16) 0.99923(14) 0.0659(4) Uani 1 1 d . . . O1 O 0.1822(3) 0.4802(3) 0.8349(3) 0.0444(7) Uani 1 1 d . . . H1A H 0.1829 0.4844 0.9139 0.053 Uiso 1 1 d R . . H1B H 0.0961 0.4895 0.8373 0.053 Uiso 1 1 d R . . O2 O 0.3263(3) 0.0500(3) 0.6887(3) 0.0399(7) Uani 1 1 d D . . H2A H 0.4154 0.0339 0.6703 0.048 Uiso 1 1 d RD . . H2B H 0.2922 0.0579 0.6244 0.048 Uiso 1 1 d RD . . N1 N 0.0502(4) 0.2438(4) 0.7048(4) 0.0487(10) Uani 1 1 d . . . N2 N 0.4455(4) 0.2773(4) 0.8340(4) 0.0503(10) Uani 1 1 d . . . N3 N 0.1249(3) 0.1821(3) 0.9745(3) 0.0339(8) Uani 1 1 d . . . N4 N 0.3814(4) 0.0121(4) 1.3528(4) 0.0451(9) Uani 1 1 d . . . N5 N 0.2668(4) 0.0418(4) 1.4503(3) 0.0416(9) Uani 1 1 d . . . N6 N 0.3636(3) 0.3350(3) 0.5604(3) 0.0347(8) Uani 1 1 d . . . N7 N 0.2116(4) 0.4793(4) 0.0883(4) 0.0527(11) Uani 1 1 d . . . N8 N 0.0941(4) 0.4503(4) 0.1790(4) 0.0448(9) Uani 1 1 d . . . C1 C -0.0320(4) 0.2631(4) 0.6466(4) 0.0358(9) Uani 1 1 d . . . C2 C 0.5152(4) 0.2459(5) 0.9020(4) 0.0411(10) Uani 1 1 d . . . C3 C -0.0136(4) 0.1830(4) 1.0078(4) 0.0386(10) Uani 1 1 d . . . H3 H -0.0624 0.2118 0.9486 0.046 Uiso 1 1 calc R . . C4 C -0.0881(4) 0.1426(5) 1.1272(4) 0.0465(11) Uani 1 1 d . . . H4 H -0.1851 0.1439 1.1470 0.056 Uiso 1 1 calc R . . C5 C -0.0183(4) 0.1007(5) 1.2164(4) 0.0407(10) Uani 1 1 d . . . H5 H -0.0663 0.0720 1.2968 0.049 Uiso 1 1 calc R . . C6 C 0.1260(4) 0.1027(4) 1.1824(4) 0.0307(8) Uani 1 1 d . . . C7 C 0.1942(4) 0.1424(4) 1.0612(4) 0.0325(9) Uani 1 1 d . . . H7 H 0.2912 0.1417 1.0390 0.039 Uiso 1 1 calc R . . C8 C 0.2052(3) 0.0664(3) 1.2721(3) 0.0196(7) Uani 1 1 d . . . C9 C 0.1641(4) 0.0751(4) 1.3991(4) 0.0404(10) Uani 1 1 d . . . H9 H 0.0740 0.1015 1.4444 0.048 Uiso 1 1 calc R . . C10 C 0.3423(4) 0.0274(5) 1.2488(4) 0.0459(11) Uani 1 1 d . . . H10 H 0.4010 0.0133 1.1685 0.055 Uiso 1 1 calc R . . C11 C 0.5027(4) 0.3173(4) 0.5209(4) 0.0395(10) Uani 1 1 d . . . H11 H 0.5530 0.2906 0.5794 0.047 Uiso 1 1 calc R . . C12 C 0.5735(5) 0.3370(5) 0.3973(4) 0.0488(12) Uani 1 1 d . . . H12 H 0.6705 0.3267 0.3731 0.059 Uiso 1 1 calc R . . C13 C 0.4997(4) 0.3726(5) 0.3082(4) 0.0429(11) Uani 1 1 d . . . H13 H 0.5460 0.3855 0.2235 0.052 Uiso 1 1 calc R . . C14 C 0.3583(4) 0.3881(4) 0.3477(4) 0.0316(9) Uani 1 1 d . . . C15 C 0.2930(4) 0.3717(4) 0.4751(4) 0.0342(9) Uani 1 1 d . . . H15 H 0.1965 0.3869 0.5020 0.041 Uiso 1 1 calc R . . C16 C 0.2736(4) 0.4202(3) 0.2615(3) 0.0219(7) Uani 1 1 d . . . C17 C 0.3160(5) 0.4620(5) 0.1394(5) 0.0551(13) Uani 1 1 d . . . H17 H 0.4082 0.4764 0.0973 0.066 Uiso 1 1 calc R . . C18 C 0.1349(5) 0.4156(4) 0.2812(4) 0.0429(11) Uani 1 1 d . . . H18 H 0.0750 0.3908 0.3579 0.052 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 0.02801(18) 0.0536(2) 0.02591(19) 0.00152(13) -0.01046(12) 0.00313(13) S1 0.0398(6) 0.0703(8) 0.0609(8) -0.0144(6) -0.0308(6) 0.0101(6) S2 0.0622(8) 0.0844(10) 0.0664(9) -0.0037(8) -0.0461(7) 0.0053(7) O1 0.0432(17) 0.0605(19) 0.0301(16) -0.0022(14) -0.0132(13) 0.0067(15) O2 0.0324(15) 0.0581(19) 0.0292(15) -0.0018(13) -0.0100(12) 0.0060(13) N1 0.035(2) 0.074(3) 0.040(2) -0.001(2) -0.0166(17) 0.0003(19) N2 0.033(2) 0.076(3) 0.045(2) -0.001(2) -0.0190(18) 0.0018(19) N3 0.0291(17) 0.046(2) 0.0279(18) -0.0016(15) -0.0107(14) -0.0001(15) N4 0.038(2) 0.059(2) 0.041(2) -0.0024(18) -0.0178(17) 0.0102(18) N5 0.045(2) 0.050(2) 0.032(2) -0.0036(17) -0.0168(16) 0.0058(17) N6 0.0325(18) 0.045(2) 0.0270(18) 0.0019(15) -0.0095(14) -0.0023(15) N7 0.063(3) 0.063(3) 0.040(2) 0.006(2) -0.028(2) -0.004(2) N8 0.046(2) 0.051(2) 0.043(2) -0.0091(18) -0.0240(19) 0.0101(18) C1 0.027(2) 0.045(2) 0.033(2) -0.0010(19) -0.0058(18) 0.0009(18) C2 0.030(2) 0.058(3) 0.037(2) -0.007(2) -0.0111(19) 0.000(2) C3 0.031(2) 0.057(3) 0.030(2) 0.000(2) -0.0125(17) 0.0018(19) C4 0.027(2) 0.073(3) 0.041(3) 0.002(2) -0.0121(19) -0.003(2) C5 0.033(2) 0.057(3) 0.031(2) 0.003(2) -0.0072(18) -0.005(2) C6 0.031(2) 0.034(2) 0.028(2) -0.0030(17) -0.0104(16) 0.0028(17) C7 0.028(2) 0.041(2) 0.028(2) 0.0002(17) -0.0088(16) 0.0024(17) C8 0.0206(17) 0.0254(18) 0.0149(17) -0.0016(14) -0.0090(13) 0.0028(14) C9 0.039(2) 0.048(3) 0.032(2) -0.0027(19) -0.0054(18) 0.002(2) C10 0.037(2) 0.068(3) 0.031(2) -0.006(2) -0.0106(19) 0.017(2) C11 0.032(2) 0.057(3) 0.033(2) 0.003(2) -0.0146(18) 0.000(2) C12 0.031(2) 0.074(3) 0.041(3) -0.004(2) -0.011(2) 0.000(2) C13 0.035(2) 0.067(3) 0.027(2) -0.001(2) -0.0078(18) -0.001(2) C14 0.032(2) 0.035(2) 0.030(2) -0.0029(17) -0.0130(17) 0.0009(17) C15 0.028(2) 0.045(2) 0.028(2) 0.0009(18) -0.0061(16) 0.0017(18) C16 0.0263(18) 0.0284(19) 0.0145(17) -0.0020(14) -0.0115(14) 0.0000(15) C17 0.050(3) 0.075(4) 0.044(3) 0.015(3) -0.018(2) -0.015(3) C18 0.043(3) 0.052(3) 0.035(2) -0.003(2) -0.016(2) 0.005(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 N2 2.270(3) . ? Cd1 N1 2.272(4) . ? Cd1 O1 2.328(3) . ? Cd1 O2 2.366(3) . ? Cd1 N6 2.390(3) . ? Cd1 N3 2.397(3) . ? S1 C1 1.622(4) . ? S2 C2 1.619(4) . ? O1 H1A 0.8688 . ? O1 H1B 0.8465 . ? O2 H2A 0.8607 . ? O2 H2B 0.8555 . ? N1 C1 1.161(5) . ? N2 C2 1.162(5) . ? N3 C3 1.328(5) . ? N3 C7 1.342(5) . ? N4 C10 1.295(5) . ? N4 N5 1.368(5) . ? N5 C9 1.303(5) . ? N6 C15 1.332(5) . ? N6 C11 1.337(5) . ? N7 C17 1.298(6) . ? N7 N8 1.361(5) . ? N8 C18 1.311(5) . ? C3 C4 1.385(6) . ? C3 H3 0.9300 . ? C4 C5 1.374(6) . ? C4 H4 0.9300 . ? C5 C6 1.385(6) . ? C5 H5 0.9300 . ? C6 C7 1.381(5) . ? C6 C8 1.430(5) . ? C7 H7 0.9300 . ? C8 C9 1.349(5) . ? C8 C10 1.351(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.366(6) . ? C11 H11 0.9300 . ? C12 C13 1.386(6) . ? C12 H12 0.9300 . ? C13 C14 1.357(6) . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C14 C16 1.432(5) . ? C15 H15 0.9300 . ? C16 C18 1.341(6) . ? C16 C17 1.352(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 N2 Cd1 N1 178.60(14) . . ? N2 Cd1 O1 88.36(13) . . ? N1 Cd1 O1 93.01(13) . . ? N2 Cd1 O2 90.60(13) . . ? N1 Cd1 O2 88.05(12) . . ? O1 Cd1 O2 175.36(9) . . ? N2 Cd1 N6 90.82(13) . . ? N1 Cd1 N6 89.40(12) . . ? O1 Cd1 N6 92.50(11) . . ? O2 Cd1 N6 82.99(11) . . ? N2 Cd1 N3 91.52(12) . . ? N1 Cd1 N3 88.21(12) . . ? O1 Cd1 N3 89.77(11) . . ? O2 Cd1 N3 94.77(11) . . ? N6 Cd1 N3 176.78(10) . . ? Cd1 O1 H1A 108.4 . . ? Cd1 O1 H1B 104.2 . . ? H1A O1 H1B 103.4 . . ? Cd1 O2 H2A 115.0 . . ? Cd1 O2 H2B 96.8 . . ? H2A O2 H2B 114.2 . . ? C1 N1 Cd1 159.5(4) . . ? C2 N2 Cd1 150.9(4) . . ? C3 N3 C7 118.3(3) . . ? C3 N3 Cd1 120.9(3) . . ? C7 N3 Cd1 120.7(3) . . ? C10 N4 N5 107.3(3) . . ? C9 N5 N4 106.5(3) . . ? C15 N6 C11 118.2(3) . . ? C15 N6 Cd1 121.5(3) . . ? C11 N6 Cd1 119.3(3) . . ? C17 N7 N8 107.4(4) . . ? C18 N8 N7 106.2(4) . . ? N1 C1 S1 178.1(4) . . ? N2 C2 S2 178.6(4) . . ? N3 C3 C4 122.5(4) . . ? N3 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 117.6(4) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C7 C6 C5 119.7(4) . . ? C7 C6 C8 119.5(3) . . ? C5 C6 C8 120.8(4) . . ? N3 C7 C6 122.1(4) . . ? N3 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C9 C8 C10 103.7(3) . . ? C9 C8 C6 128.0(3) . . ? C10 C8 C6 128.0(3) . . ? N5 C9 C8 111.4(4) . . ? N5 C9 H9 124.3 . . ? C8 C9 H9 124.3 . . ? N4 C10 C8 111.2(4) . . ? N4 C10 H10 124.4 . . ? C8 C10 H10 124.4 . . ? N6 C11 C12 122.2(4) . . ? N6 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 118.3(4) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 119.4(4) . . ? C13 C14 C16 122.1(4) . . ? C15 C14 C16 118.5(3) . . ? N6 C15 C14 122.3(4) . . ? N6 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C18 C16 C17 103.5(4) . . ? C18 C16 C14 128.9(4) . . ? C17 C16 C14 127.6(4) . . ? N7 C17 C16 111.3(4) . . ? N7 C17 H17 124.4 . . ? C16 C17 H17 124.4 . . ? N8 C18 C16 111.7(4) . . ? N8 C18 H18 124.2 . . ? C16 C18 H18 124.2 . . ? 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 N2 Cd1 N1 C1 -127(5) . . . . ? O1 Cd1 N1 C1 65.0(10) . . . . ? O2 Cd1 N1 C1 -110.5(10) . . . . ? N6 Cd1 N1 C1 -27.5(10) . . . . ? N3 Cd1 N1 C1 154.7(10) . . . . ? N1 Cd1 N2 C2 -56(5) . . . . ? O1 Cd1 N2 C2 112.2(8) . . . . ? O2 Cd1 N2 C2 -72.3(8) . . . . ? N6 Cd1 N2 C2 -155.3(8) . . . . ? N3 Cd1 N2 C2 22.4(8) . . . . ? N2 Cd1 N3 C3 163.8(3) . . . . ? N1 Cd1 N3 C3 -17.6(3) . . . . ? O1 Cd1 N3 C3 75.4(3) . . . . ? O2 Cd1 N3 C3 -105.5(3) . . . . ? N6 Cd1 N3 C3 -59.6(19) . . . . ? N2 Cd1 N3 C7 -12.0(3) . . . . ? N1 Cd1 N3 C7 166.6(3) . . . . ? O1 Cd1 N3 C7 -100.4(3) . . . . ? O2 Cd1 N3 C7 78.7(3) . . . . ? N6 Cd1 N3 C7 124.7(17) . . . . ? C10 N4 N5 C9 -0.7(5) . . . . ? N2 Cd1 N6 C15 -167.5(3) . . . . ? N1 Cd1 N6 C15 13.8(3) . . . . ? O1 Cd1 N6 C15 -79.1(3) . . . . ? O2 Cd1 N6 C15 102.0(3) . . . . ? N3 Cd1 N6 C15 55.8(19) . . . . ? N2 Cd1 N6 C11 23.8(3) . . . . ? N1 Cd1 N6 C11 -154.8(3) . . . . ? O1 Cd1 N6 C11 112.2(3) . . . . ? O2 Cd1 N6 C11 -66.7(3) . . . . ? N3 Cd1 N6 C11 -112.9(18) . . . . ? C17 N7 N8 C18 -0.5(5) . . . . ? Cd1 N1 C1 S1 49(14) . . . . ? Cd1 N2 C2 S2 -20(19) . . . . ? C7 N3 C3 C4 -1.1(6) . . . . ? Cd1 N3 C3 C4 -176.9(3) . . . . ? N3 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C4 C5 C6 C7 -1.8(6) . . . . ? C4 C5 C6 C8 177.1(4) . . . . ? C3 N3 C7 C6 0.2(6) . . . . ? Cd1 N3 C7 C6 176.1(3) . . . . ? C5 C6 C7 N3 1.3(6) . . . . ? C8 C6 C7 N3 -177.6(4) . . . . ? C7 C6 C8 C9 151.8(4) . . . . ? C5 C6 C8 C9 -27.1(6) . . . . ? C7 C6 C8 C10 -21.3(6) . . . . ? C5 C6 C8 C10 159.9(4) . . . . ? N4 N5 C9 C8 1.1(5) . . . . ? C10 C8 C9 N5 -1.1(5) . . . . ? C6 C8 C9 N5 -175.5(4) . . . . ? N5 N4 C10 C8 0.0(5) . . . . ? C9 C8 C10 N4 0.7(5) . . . . ? C6 C8 C10 N4 175.0(4) . . . . ? C15 N6 C11 C12 0.8(7) . . . . ? Cd1 N6 C11 C12 169.8(4) . . . . ? N6 C11 C12 C13 -2.1(7) . . . . ? C11 C12 C13 C14 0.7(7) . . . . ? C12 C13 C14 C15 1.8(7) . . . . ? C12 C13 C14 C16 -177.8(4) . . . . ? C11 N6 C15 C14 1.9(6) . . . . ? Cd1 N6 C15 C14 -166.9(3) . . . . ? C13 C14 C15 N6 -3.2(6) . . . . ? C16 C14 C15 N6 176.4(4) . . . . ? C13 C14 C16 C18 166.9(4) . . . . ? C15 C14 C16 C18 -12.8(6) . . . . ? C13 C14 C16 C17 -12.6(7) . . . . ? C15 C14 C16 C17 167.8(4) . . . . ? N8 N7 C17 C16 0.9(6) . . . . ? C18 C16 C17 N7 -1.0(6) . . . . ? C14 C16 C17 N7 178.6(4) . . . . ? N7 N8 C18 C16 -0.1(5) . . . . ? C17 C16 C18 N8 0.6(5) . . . . ? C14 C16 C18 N8 -178.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.841 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.094 data_50317d _database_code_depnum_ccdc_archive 'CCDC 266847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H13 Cd2 N20 O0.50' _chemical_formula_weight 790.32 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7347(10) _cell_length_b 13.7682(17) _cell_length_c 14.1403(18) _cell_angle_alpha 111.1800(10) _cell_angle_beta 93.100(2) _cell_angle_gamma 96.835(2) _cell_volume 1386.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4790 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.89 _exptl_crystal_description BLOCK _exptl_crystal_colour PALE-RED _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 770 _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.757266 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'APEX II 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 7588 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4858 _reflns_number_gt 4306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _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^)+(0.0286P)^2^+0.6473P] 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 4858 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.0000 0.0000 0.0000 0.02520(7) Uani 1 2 d S . . Cd2 Cd 0.13255(2) 0.511342(14) 0.706330(14) 0.02790(7) Uani 1 1 d . . . Cd3 Cd 0.5000 0.0000 0.5000 0.04515(9) Uani 1 2 d S . . N1 N -0.1265(3) 0.11125(17) 0.93355(17) 0.0335(5) Uani 1 1 d . . . N2 N -0.3043(3) 0.09591(19) 0.9068(2) 0.0462(6) Uani 1 1 d . . . N3 N -0.1882(3) 0.24521(16) 0.89780(17) 0.0320(5) Uani 1 1 d . . . N4 N -0.0495(3) 0.46569(16) 0.81757(16) 0.0308(5) Uani 1 1 d . . . N5 N 0.0552(3) 0.35078(17) 0.57541(16) 0.0329(5) Uani 1 1 d . . . N6 N 0.1703(3) 0.27784(19) 0.55419(19) 0.0479(6) Uani 1 1 d . . . N7 N -0.0305(3) 0.23269(16) 0.42386(15) 0.0291(5) Uani 1 1 d . . . N8 N -0.1366(3) 0.07527(16) 0.15050(16) 0.0309(5) Uani 1 1 d . . . N9 N -0.2729(4) -0.0346(2) 0.3972(3) 0.0653(8) Uani 1 1 d . . . N10 N -0.0259(4) -0.1038(3) 0.3120(2) 0.0727(9) Uani 1 1 d . . . N11 N 0.2837(5) -0.0273(3) 0.3635(2) 0.0681(8) Uani 1 1 d . . . N12 N 0.5548(4) 0.1791(2) 0.5411(2) 0.0558(7) Uani 1 1 d . . . N13 N 0.5752(4) 0.3506(3) 0.6736(3) 0.1120(17) Uani 1 1 d . . . N14 N 0.3519(4) 0.4396(2) 0.7709(2) 0.0527(7) Uani 1 1 d . . . N15 N 0.2361(3) 0.67133(18) 0.84255(19) 0.0443(6) Uani 1 1 d . . . N16 N 0.5426(3) 0.7174(2) 0.9129(2) 0.0579(8) Uani 1 1 d . . . N17 N 0.7636(3) 0.86607(19) 0.93296(19) 0.0437(6) Uani 1 1 d . . . N18 N -0.0977(3) 0.5760(2) 0.6552(2) 0.0435(6) Uani 1 1 d . . . N19 N -0.3645(3) 0.6519(2) 0.6468(3) 0.0621(8) Uani 1 1 d . . . N20 N -0.6672(3) 0.5657(2) 0.6110(2) 0.0471(6) Uani 1 1 d . . . C1 C -0.0667(3) 0.3709(2) 0.8251(2) 0.0316(6) Uani 1 1 d . . . H1 H -0.0049 0.3199 0.7849 0.038 Uiso 1 1 calc R . . C2 C -0.1427(4) 0.5365(2) 0.8740(2) 0.0356(6) Uani 1 1 d . . . H2 H -0.1331 0.6019 0.8679 0.043 Uiso 1 1 calc R . . C3 C -0.2519(4) 0.5180(2) 0.9405(2) 0.0429(7) Uani 1 1 d . . . H3 H -0.3146 0.5697 0.9785 0.051 Uiso 1 1 calc R . . C4 C -0.2676(4) 0.4212(2) 0.9504(2) 0.0405(7) Uani 1 1 d . . . H4 H -0.3393 0.4064 0.9957 0.049 Uiso 1 1 calc R . . C5 C -0.1734(3) 0.3469(2) 0.8908(2) 0.0305(6) Uani 1 1 d . . . C6 C -0.0620(4) 0.2002(2) 0.9277(2) 0.0375(6) Uani 1 1 d . . . H6 H 0.0558 0.2289 0.9422 0.045 Uiso 1 1 calc R . . C7 C -0.3364(4) 0.1770(2) 0.8864(3) 0.0470(8) Uani 1 1 d . . . H7 H -0.4473 0.1870 0.8665 0.056 Uiso 1 1 calc R . . C8 C -0.0472(3) 0.13244(19) 0.24145(19) 0.0307(6) Uani 1 1 d . . . H8 H 0.0745 0.1430 0.2468 0.037 Uiso 1 1 calc R . . C9 C -0.3111(3) 0.0625(2) 0.1448(2) 0.0335(6) Uani 1 1 d . . . H9 H -0.3743 0.0229 0.0819 0.040 Uiso 1 1 calc R . . C10 C -0.4017(4) 0.1049(2) 0.2268(2) 0.0370(6) Uani 1 1 d . . . H10 H -0.5235 0.0945 0.2193 0.044 Uiso 1 1 calc R . . C11 C -0.3108(3) 0.1629(2) 0.3204(2) 0.0327(6) Uani 1 1 d . . . H11 H -0.3689 0.1926 0.3775 0.039 Uiso 1 1 calc R . . C12 C -0.1301(3) 0.17583(19) 0.32702(18) 0.0284(5) Uani 1 1 d . . . C13 C 0.1166(4) 0.2094(2) 0.4635(2) 0.0467(8) Uani 1 1 d . . . H13 H 0.1713 0.1517 0.4299 0.056 Uiso 1 1 calc R . . C14 C -0.0621(3) 0.3221(2) 0.49706(19) 0.0314(6) Uani 1 1 d . . . H14 H -0.1546 0.3580 0.4922 0.038 Uiso 1 1 calc R . . C15 C -0.1523(5) -0.0639(3) 0.3617(3) 0.0527(8) Uani 1 1 d . . . C16 C 0.1365(5) -0.0613(3) 0.3434(2) 0.0509(8) Uani 1 1 d . . . C17 C 0.5531(4) 0.2571(3) 0.6045(3) 0.0549(8) Uani 1 1 d . . . C18 C 0.4479(5) 0.3923(3) 0.7225(3) 0.0595(10) Uani 1 1 d . . . C19 C 0.3809(4) 0.6984(2) 0.8734(2) 0.0344(6) Uani 1 1 d . . . C20 C 0.6530(4) 0.7986(2) 0.9207(2) 0.0347(6) Uani 1 1 d . . . C21 C -0.2279(4) 0.6056(2) 0.6496(2) 0.0367(6) Uani 1 1 d . . . C22 C -0.5221(4) 0.6010(2) 0.6271(2) 0.0382(6) Uani 1 1 d . . . O1 O 0.3027(7) 0.2622(4) 0.8468(4) 0.0725(14) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02593(14) 0.02199(13) 0.02532(14) 0.00744(10) -0.00051(10) 0.00032(10) Cd2 0.02375(11) 0.02780(11) 0.02959(11) 0.00866(8) -0.00073(7) 0.00214(7) Cd3 0.04262(19) 0.04259(18) 0.0554(2) 0.02010(15) 0.01645(15) 0.01482(14) N1 0.0357(13) 0.0319(12) 0.0357(12) 0.0165(10) 0.0016(10) 0.0043(10) N2 0.0384(14) 0.0401(14) 0.0622(17) 0.0261(13) -0.0090(12) -0.0030(11) N3 0.0336(12) 0.0304(11) 0.0364(12) 0.0177(10) 0.0025(10) 0.0047(9) N4 0.0322(12) 0.0279(11) 0.0327(12) 0.0121(9) 0.0026(9) 0.0034(9) N5 0.0320(12) 0.0331(12) 0.0298(12) 0.0076(9) -0.0014(9) 0.0059(9) N6 0.0494(15) 0.0429(14) 0.0403(14) 0.0011(11) -0.0117(12) 0.0184(12) N7 0.0300(12) 0.0277(11) 0.0254(11) 0.0064(9) -0.0021(9) 0.0019(9) N8 0.0327(12) 0.0305(11) 0.0264(11) 0.0078(9) -0.0001(9) 0.0029(9) N9 0.064(2) 0.0627(19) 0.085(2) 0.0371(17) 0.0379(18) 0.0232(16) N10 0.056(2) 0.071(2) 0.068(2) -0.0045(16) 0.0250(16) 0.0096(16) N11 0.062(2) 0.074(2) 0.066(2) 0.0187(17) 0.0061(16) 0.0234(17) N12 0.0634(19) 0.0479(16) 0.0600(18) 0.0192(15) 0.0257(15) 0.0163(14) N13 0.045(2) 0.095(3) 0.128(3) -0.038(3) -0.015(2) 0.0210(19) N14 0.0499(16) 0.0496(16) 0.0495(16) 0.0062(13) -0.0126(13) 0.0206(13) N15 0.0410(15) 0.0349(13) 0.0475(15) 0.0090(11) -0.0016(12) -0.0072(11) N16 0.0421(16) 0.0432(15) 0.092(2) 0.0383(15) -0.0148(15) -0.0110(12) N17 0.0343(14) 0.0367(13) 0.0516(15) 0.0117(11) -0.0075(11) -0.0068(11) N18 0.0258(13) 0.0538(15) 0.0609(17) 0.0329(13) 0.0023(11) 0.0069(11) N19 0.0277(14) 0.0526(16) 0.114(3) 0.0398(17) 0.0023(15) 0.0082(12) N20 0.0283(14) 0.0613(17) 0.0594(17) 0.0310(14) 0.0066(11) 0.0080(12) C1 0.0338(14) 0.0280(13) 0.0320(14) 0.0095(11) 0.0015(11) 0.0064(11) C2 0.0418(16) 0.0286(13) 0.0402(16) 0.0158(12) 0.0055(12) 0.0088(12) C3 0.0500(18) 0.0392(16) 0.0464(17) 0.0184(14) 0.0158(14) 0.0201(14) C4 0.0451(17) 0.0440(16) 0.0414(16) 0.0230(13) 0.0145(13) 0.0129(13) C5 0.0311(14) 0.0304(13) 0.0343(14) 0.0171(11) 0.0004(11) 0.0059(11) C6 0.0334(15) 0.0355(15) 0.0478(17) 0.0209(13) 0.0014(12) 0.0048(12) C7 0.0338(16) 0.0465(17) 0.066(2) 0.0311(16) -0.0083(14) 0.0010(13) C8 0.0250(13) 0.0311(13) 0.0321(14) 0.0086(11) -0.0006(11) 0.0009(10) C9 0.0338(15) 0.0334(14) 0.0284(14) 0.0087(11) -0.0041(11) -0.0015(11) C10 0.0281(14) 0.0437(16) 0.0373(16) 0.0141(13) -0.0001(12) 0.0021(12) C11 0.0324(14) 0.0358(14) 0.0280(14) 0.0103(11) 0.0040(11) 0.0029(11) C12 0.0327(14) 0.0255(12) 0.0261(13) 0.0100(10) -0.0013(11) 0.0013(10) C13 0.0466(18) 0.0409(16) 0.0437(17) 0.0031(13) -0.0097(14) 0.0189(14) C14 0.0307(14) 0.0319(13) 0.0300(14) 0.0097(11) 0.0001(11) 0.0057(11) C15 0.061(2) 0.0482(19) 0.056(2) 0.0241(16) 0.0230(18) 0.0145(17) C16 0.065(3) 0.0497(19) 0.0411(18) 0.0129(15) 0.0189(17) 0.0270(18) C17 0.0392(18) 0.053(2) 0.065(2) 0.0097(19) 0.0080(16) 0.0165(15) C18 0.045(2) 0.052(2) 0.059(2) -0.0034(17) -0.0248(17) 0.0142(17) C19 0.0423(18) 0.0252(13) 0.0337(15) 0.0109(11) 0.0044(13) -0.0030(12) C20 0.0324(15) 0.0315(14) 0.0370(15) 0.0096(12) -0.0030(12) 0.0052(13) C21 0.0308(16) 0.0405(15) 0.0436(16) 0.0230(13) 0.0033(12) 0.0004(12) C22 0.0333(18) 0.0461(16) 0.0450(17) 0.0248(14) 0.0090(13) 0.0151(13) O1 0.060(3) 0.075(3) 0.083(4) 0.030(3) -0.007(3) 0.016(3) _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 N17 2.321(2) 2_666 ? Cd1 N17 2.321(2) 1_444 ? Cd1 N1 2.342(2) 2_556 ? Cd1 N1 2.342(2) 1_554 ? Cd1 N8 2.372(2) 2 ? Cd1 N8 2.372(2) . ? Cd2 N18 2.278(2) . ? Cd2 N5 2.298(2) . ? Cd2 N20 2.336(3) 1_655 ? Cd2 N15 2.356(2) . ? Cd2 N14 2.360(3) . ? Cd2 N4 2.365(2) . ? Cd3 N12 2.300(3) . ? Cd3 N12 2.300(3) 2_656 ? Cd3 N9 2.324(3) 1_655 ? Cd3 N9 2.324(3) 2_556 ? Cd3 N11 2.375(3) . ? Cd3 N11 2.375(3) 2_656 ? N1 C6 1.300(3) . ? N1 N2 1.377(3) . ? N1 Cd1 2.342(2) 1_556 ? N2 C7 1.296(4) . ? N3 C6 1.343(3) . ? N3 C7 1.355(4) . ? N3 C5 1.431(3) . ? N4 C2 1.332(3) . ? N4 C1 1.339(3) . ? N5 C14 1.302(3) . ? N5 N6 1.383(3) . ? N6 C13 1.296(4) . ? N7 C14 1.350(3) . ? N7 C13 1.364(3) . ? N7 C12 1.431(3) . ? N8 C9 1.335(3) . ? N8 C8 1.340(3) . ? N9 C15 1.130(4) . ? N9 Cd3 2.324(3) 1_455 ? N10 C15 1.295(4) . ? N10 C16 1.302(5) . ? N11 C16 1.157(5) . ? N12 C17 1.125(4) . ? N13 C17 1.289(5) . ? N13 C18 1.304(5) . ? N14 C18 1.136(4) . ? N15 C19 1.146(4) . ? N16 C20 1.290(4) . ? N16 C19 1.298(4) . ? N17 C20 1.142(3) . ? N17 Cd1 2.321(2) 1_666 ? N18 C21 1.140(3) . ? N19 C22 1.294(4) . ? N19 C21 1.303(4) . ? N20 C22 1.145(4) . ? N20 Cd2 2.336(3) 1_455 ? C1 C5 1.376(4) . ? C1 H1 0.9300 . ? C2 C3 1.368(4) . ? C2 H2 0.9300 . ? C3 C4 1.382(4) . ? C3 H3 0.9300 . ? C4 C5 1.381(4) . ? C4 H4 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.373(4) . ? C8 H8 0.9300 . ? C9 C10 1.369(4) . ? C9 H9 0.9300 . ? C10 C11 1.373(4) . ? C10 H10 0.9300 . ? C11 C12 1.381(4) . ? C11 H11 0.9300 . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? 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 N17 Cd1 N17 180.0(2) 2_666 1_444 ? N17 Cd1 N1 92.86(8) 2_666 2_556 ? N17 Cd1 N1 87.14(8) 1_444 2_556 ? N17 Cd1 N1 87.14(8) 2_666 1_554 ? N17 Cd1 N1 92.86(8) 1_444 1_554 ? N1 Cd1 N1 180.00(8) 2_556 1_554 ? N17 Cd1 N8 90.78(8) 2_666 2 ? N17 Cd1 N8 89.22(8) 1_444 2 ? N1 Cd1 N8 88.27(8) 2_556 2 ? N1 Cd1 N8 91.73(8) 1_554 2 ? N17 Cd1 N8 89.22(8) 2_666 . ? N17 Cd1 N8 90.78(8) 1_444 . ? N1 Cd1 N8 91.73(8) 2_556 . ? N1 Cd1 N8 88.27(8) 1_554 . ? N8 Cd1 N8 180.00(11) 2 . ? N18 Cd2 N5 91.69(9) . . ? N18 Cd2 N20 96.06(9) . 1_655 ? N5 Cd2 N20 90.95(9) . 1_655 ? N18 Cd2 N15 93.23(9) . . ? N5 Cd2 N15 174.91(8) . . ? N20 Cd2 N15 87.25(9) 1_655 . ? N18 Cd2 N14 174.00(10) . . ? N5 Cd2 N14 88.71(8) . . ? N20 Cd2 N14 89.92(10) 1_655 . ? N15 Cd2 N14 86.53(9) . . ? N18 Cd2 N4 87.32(8) . . ? N5 Cd2 N4 93.69(8) . . ? N20 Cd2 N4 174.18(8) 1_655 . ? N15 Cd2 N4 87.83(8) . . ? N14 Cd2 N4 86.68(9) . . ? N12 Cd3 N12 180.0 . 2_656 ? N12 Cd3 N9 94.23(10) . 1_655 ? N12 Cd3 N9 85.77(10) 2_656 1_655 ? N12 Cd3 N9 85.77(10) . 2_556 ? N12 Cd3 N9 94.23(10) 2_656 2_556 ? N9 Cd3 N9 180.000(1) 1_655 2_556 ? N12 Cd3 N11 93.69(11) . . ? N12 Cd3 N11 86.31(11) 2_656 . ? N9 Cd3 N11 94.66(12) 1_655 . ? N9 Cd3 N11 85.34(12) 2_556 . ? N12 Cd3 N11 86.31(11) . 2_656 ? N12 Cd3 N11 93.69(11) 2_656 2_656 ? N9 Cd3 N11 85.34(12) 1_655 2_656 ? N9 Cd3 N11 94.66(12) 2_556 2_656 ? N11 Cd3 N11 180.000(1) . 2_656 ? C6 N1 N2 107.4(2) . . ? C6 N1 Cd1 131.12(18) . 1_556 ? N2 N1 Cd1 120.82(16) . 1_556 ? C7 N2 N1 106.1(2) . . ? C6 N3 C7 103.9(2) . . ? C6 N3 C5 128.1(2) . . ? C7 N3 C5 127.7(2) . . ? C2 N4 C1 118.1(2) . . ? C2 N4 Cd2 118.78(17) . . ? C1 N4 Cd2 123.15(17) . . ? C14 N5 N6 107.8(2) . . ? C14 N5 Cd2 130.03(17) . . ? N6 N5 Cd2 119.68(15) . . ? C13 N6 N5 106.2(2) . . ? C14 N7 C13 104.3(2) . . ? C14 N7 C12 127.5(2) . . ? C13 N7 C12 128.3(2) . . ? C9 N8 C8 117.8(2) . . ? C9 N8 Cd1 118.93(16) . . ? C8 N8 Cd1 123.27(17) . . ? C15 N9 Cd3 163.5(3) . 1_455 ? C15 N10 C16 121.0(3) . . ? C16 N11 Cd3 135.9(3) . . ? C17 N12 Cd3 143.1(3) . . ? C17 N13 C18 122.7(4) . . ? C18 N14 Cd2 123.8(3) . . ? C19 N15 Cd2 123.4(2) . . ? C20 N16 C19 125.0(3) . . ? C20 N17 Cd1 164.8(2) . 1_666 ? C21 N18 Cd2 163.6(2) . . ? C22 N19 C21 122.0(3) . . ? C22 N20 Cd2 133.6(2) . 1_455 ? N4 C1 C5 121.7(2) . . ? N4 C1 H1 119.1 . . ? C5 C1 H1 119.1 . . ? N4 C2 C3 123.4(2) . . ? N4 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 117.9(3) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C1 C5 C4 120.0(2) . . ? C1 C5 N3 120.5(2) . . ? C4 C5 N3 119.5(2) . . ? N1 C6 N3 111.0(2) . . ? N1 C6 H6 124.5 . . ? N3 C6 H6 124.5 . . ? N2 C7 N3 111.6(3) . . ? N2 C7 H7 124.2 . . ? N3 C7 H7 124.2 . . ? N8 C8 C12 121.9(2) . . ? N8 C8 H8 119.1 . . ? C12 C8 H8 119.1 . . ? N8 C9 C10 123.2(2) . . ? N8 C9 H9 118.4 . . ? C10 C9 H9 118.4 . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C12 117.8(3) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C8 C12 C11 120.0(2) . . ? C8 C12 N7 120.4(2) . . ? C11 C12 N7 119.5(2) . . ? N6 C13 N7 111.3(3) . . ? N6 C13 H13 124.3 . . ? N7 C13 H13 124.3 . . ? N5 C14 N7 110.4(2) . . ? N5 C14 H14 124.8 . . ? N7 C14 H14 124.8 . . ? N9 C15 N10 173.5(4) . . ? N11 C16 N10 174.6(4) . . ? N12 C17 N13 171.0(4) . . ? N14 C18 N13 171.5(4) . . ? N15 C19 N16 171.5(3) . . ? N17 C20 N16 172.3(3) . . ? N18 C21 N19 172.4(3) . . ? N20 C22 N19 173.0(3) . . ? 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 C6 N1 N2 C7 -0.1(3) . . . . ? Cd1 N1 N2 C7 171.5(2) 1_556 . . . ? N18 Cd2 N4 C2 -46.3(2) . . . . ? N5 Cd2 N4 C2 -137.80(19) . . . . ? N20 Cd2 N4 C2 79.4(8) 1_655 . . . ? N15 Cd2 N4 C2 47.1(2) . . . . ? N14 Cd2 N4 C2 133.7(2) . . . . ? N18 Cd2 N4 C1 132.2(2) . . . . ? N5 Cd2 N4 C1 40.6(2) . . . . ? N20 Cd2 N4 C1 -102.1(8) 1_655 . . . ? N15 Cd2 N4 C1 -134.5(2) . . . . ? N14 Cd2 N4 C1 -47.8(2) . . . . ? N18 Cd2 N5 C14 8.9(2) . . . . ? N20 Cd2 N5 C14 -87.2(2) 1_655 . . . ? N15 Cd2 N5 C14 -156.5(8) . . . . ? N14 Cd2 N5 C14 -177.1(2) . . . . ? N4 Cd2 N5 C14 96.3(2) . . . . ? N18 Cd2 N5 N6 168.6(2) . . . . ? N20 Cd2 N5 N6 72.5(2) 1_655 . . . ? N15 Cd2 N5 N6 3.3(10) . . . . ? N14 Cd2 N5 N6 -17.4(2) . . . . ? N4 Cd2 N5 N6 -104.0(2) . . . . ? C14 N5 N6 C13 0.5(3) . . . . ? Cd2 N5 N6 C13 -163.3(2) . . . . ? N17 Cd1 N8 C9 150.64(19) 2_666 . . . ? N17 Cd1 N8 C9 -29.36(19) 1_444 . . . ? N1 Cd1 N8 C9 -116.52(19) 2_556 . . . ? N1 Cd1 N8 C9 63.48(19) 1_554 . . . ? N8 Cd1 N8 C9 -10(100) 2 . . . ? N17 Cd1 N8 C8 -27.8(2) 2_666 . . . ? N17 Cd1 N8 C8 152.2(2) 1_444 . . . ? N1 Cd1 N8 C8 65.0(2) 2_556 . . . ? N1 Cd1 N8 C8 -115.0(2) 1_554 . . . ? N8 Cd1 N8 C8 172(100) 2 . . . ? N12 Cd3 N11 C16 -120.3(4) . . . . ? N12 Cd3 N11 C16 59.7(4) 2_656 . . . ? N9 Cd3 N11 C16 145.2(4) 1_655 . . . ? N9 Cd3 N11 C16 -34.8(4) 2_556 . . . ? N11 Cd3 N11 C16 18(100) 2_656 . . . ? N12 Cd3 N12 C17 52(100) 2_656 . . . ? N9 Cd3 N12 C17 -144.7(5) 1_655 . . . ? N9 Cd3 N12 C17 35.3(5) 2_556 . . . ? N11 Cd3 N12 C17 120.4(5) . . . . ? N11 Cd3 N12 C17 -59.6(5) 2_656 . . . ? N18 Cd2 N14 C18 141.9(8) . . . . ? N5 Cd2 N14 C18 48.1(3) . . . . ? N20 Cd2 N14 C18 -42.9(3) 1_655 . . . ? N15 Cd2 N14 C18 -130.1(3) . . . . ? N4 Cd2 N14 C18 141.9(3) . . . . ? N18 Cd2 N15 C19 -150.5(3) . . . . ? N5 Cd2 N15 C19 14.8(11) . . . . ? N20 Cd2 N15 C19 -54.5(3) 1_655 . . . ? N14 Cd2 N15 C19 35.5(3) . . . . ? N4 Cd2 N15 C19 122.3(3) . . . . ? N5 Cd2 N18 C21 106.4(9) . . . . ? N20 Cd2 N18 C21 -162.5(9) 1_655 . . . ? N15 Cd2 N18 C21 -74.9(9) . . . . ? N14 Cd2 N18 C21 12.7(15) . . . . ? N4 Cd2 N18 C21 12.8(9) . . . . ? C2 N4 C1 C5 -1.7(4) . . . . ? Cd2 N4 C1 C5 179.84(18) . . . . ? C1 N4 C2 C3 1.4(4) . . . . ? Cd2 N4 C2 C3 179.9(2) . . . . ? N4 C2 C3 C4 0.0(5) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? N4 C1 C5 C4 0.7(4) . . . . ? N4 C1 C5 N3 -179.5(2) . . . . ? C3 C4 C5 C1 0.7(4) . . . . ? C3 C4 C5 N3 -179.1(3) . . . . ? C6 N3 C5 C1 62.3(4) . . . . ? C7 N3 C5 C1 -125.4(3) . . . . ? C6 N3 C5 C4 -117.8(3) . . . . ? C7 N3 C5 C4 54.4(4) . . . . ? N2 N1 C6 N3 -0.2(3) . . . . ? Cd1 N1 C6 N3 -170.57(17) 1_556 . . . ? C7 N3 C6 N1 0.4(3) . . . . ? C5 N3 C6 N1 174.1(2) . . . . ? N1 N2 C7 N3 0.4(4) . . . . ? C6 N3 C7 N2 -0.5(4) . . . . ? C5 N3 C7 N2 -174.2(3) . . . . ? C9 N8 C8 C12 0.9(4) . . . . ? Cd1 N8 C8 C12 179.37(18) . . . . ? C8 N8 C9 C10 0.0(4) . . . . ? Cd1 N8 C9 C10 -178.5(2) . . . . ? N8 C9 C10 C11 -0.5(4) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? N8 C8 C12 C11 -1.4(4) . . . . ? N8 C8 C12 N7 177.3(2) . . . . ? C10 C11 C12 C8 0.8(4) . . . . ? C10 C11 C12 N7 -177.8(2) . . . . ? C14 N7 C12 C8 140.2(3) . . . . ? C13 N7 C12 C8 -40.0(4) . . . . ? C14 N7 C12 C11 -41.1(4) . . . . ? C13 N7 C12 C11 138.6(3) . . . . ? N5 N6 C13 N7 -0.8(4) . . . . ? C14 N7 C13 N6 0.7(4) . . . . ? C12 N7 C13 N6 -179.1(3) . . . . ? N6 N5 C14 N7 -0.1(3) . . . . ? Cd2 N5 C14 N7 161.50(17) . . . . ? C13 N7 C14 N5 -0.4(3) . . . . ? C12 N7 C14 N5 179.4(2) . . . . ? Cd3 N9 C15 N10 114(3) 1_455 . . . ? C16 N10 C15 N9 164(3) . . . . ? Cd3 N11 C16 N10 -140(4) . . . . ? C15 N10 C16 N11 -156(4) . . . . ? Cd3 N12 C17 N13 133(3) . . . . ? C18 N13 C17 N12 167(3) . . . . ? Cd2 N14 C18 N13 106(3) . . . . ? C17 N13 C18 N14 -177(3) . . . . ? Cd2 N15 C19 N16 -67(2) . . . . ? C20 N16 C19 N15 -174(2) . . . . ? Cd1 N17 C20 N16 -42(3) 1_666 . . . ? C19 N16 C20 N17 178(2) . . . . ? Cd2 N18 C21 N19 109(2) . . . . ? C22 N19 C21 N18 -177(2) . . . . ? Cd2 N20 C22 N19 -104(3) 1_455 . . . ? C21 N19 C22 N20 179(100) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.841 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.062