# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Gao, Shan' _publ_contact_author_email shangao67@yahoo.com _publ_section_title ; Structural diversity of Zn(II)/Cd(II) complexes based on bis(pyridyl) ligands with long flexible spacer: from zero-dimensional metallomacrocycle, one-dimensional chain, two-dimensional layer, to three-dimensional frameworks ; loop_ _publ_author_name 'Zhao-Peng Deng' 'Li-Hua Huo' 'Hui-Ling Qi' 'Li-Na Zhu' 'Hui Zhao' ; Shan Gao ; data_1 _database_code_depnum_ccdc_archive 'CCDC 786013' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Cd2 N8 O14 S2' _chemical_formula_sum 'C36 H48 Cd2 N8 O14 S2' _chemical_formula_weight 1105.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.334(2) _cell_length_b 9.0242(18) _cell_length_c 21.631(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.38(3) _cell_angle_gamma 90.00 _cell_volume 2202.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 16638 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.47 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7151 _exptl_absorpt_correction_T_max 0.7527 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20699 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5035 _reflns_number_gt 4169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+2.2968P] 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 5035 _refine_ls_number_parameters 298 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _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 0.167351(19) 0.84883(2) 0.665728(10) 0.03306(8) Uani 1 1 d . . . S1 S 0.13029(7) 0.48293(8) 0.70747(4) 0.03710(17) Uani 1 1 d . . . O1 O 0.20331(19) 0.5956(2) 0.67832(10) 0.0398(5) Uani 1 1 d . . . O1W O 0.1680(2) 0.8338(3) 0.77454(11) 0.0455(5) Uani 1 1 d D . . H1W1 H 0.115(3) 0.885(3) 0.7899(18) 0.068 Uiso 1 1 d D . . H1W2 H 0.153(3) 0.7420(13) 0.7785(19) 0.068 Uiso 1 1 d D . . O2 O 0.0099(2) 0.4846(3) 0.67554(11) 0.0479(5) Uani 1 1 d . . . O2W O 0.0829(2) 1.0770(3) 0.67476(13) 0.0526(6) Uani 1 1 d D . . H2W1 H 0.109(3) 1.165(2) 0.680(2) 0.079 Uiso 1 1 d D . . H2W2 H 0.019(2) 1.068(4) 0.6927(18) 0.079 Uiso 1 1 d D . . O3 O 0.1848(3) 0.3388(2) 0.70369(16) 0.0672(8) Uani 1 1 d . . . O3W O -0.0352(2) 0.7830(3) 0.65637(12) 0.0478(5) Uani 1 1 d D . . H3W1 H -0.072(4) 0.833(3) 0.6816(16) 0.072 Uiso 1 1 d D . . H3W2 H -0.039(4) 0.6917(13) 0.6640(18) 0.072 Uiso 1 1 d D . . O4 O 0.1248(2) 0.5240(3) 0.77328(10) 0.0488(6) Uani 1 1 d . . . N1 N 0.1685(3) 0.8486(3) 0.55880(12) 0.0437(6) Uani 1 1 d . . . N2 N 0.1456(3) 0.6006(3) 0.54277(14) 0.0527(7) Uani 1 1 d . . . H5 H 0.1378 0.5950 0.5819 0.063 Uiso 1 1 calc R . . N3 N 0.5600(2) 0.2909(3) 0.35001(14) 0.0474(7) Uani 1 1 d . . . H14 H 0.6304 0.3267 0.3503 0.057 Uiso 1 1 calc R . . N4 N 0.6387(2) 0.0702(3) 0.32031(11) 0.0371(5) Uani 1 1 d . . . C1 C 0.1778(4) 0.9858(5) 0.53488(19) 0.0715(12) Uani 1 1 d . . . H1 H 0.1838 1.0651 0.5625 0.086 Uiso 1 1 calc R . . C2 C 0.1792(5) 1.0165(6) 0.4734(2) 0.0886(16) Uani 1 1 d . . . H2 H 0.1888 1.1128 0.4594 0.106 Uiso 1 1 calc R . . C3 C 0.1662(4) 0.9018(5) 0.43378(19) 0.0717(12) Uani 1 1 d . . . H3 H 0.1646 0.9199 0.3914 0.086 Uiso 1 1 calc R . . C4 C 0.1553(4) 0.7604(5) 0.45380(17) 0.0589(10) Uani 1 1 d . . . H4 H 0.1467 0.6822 0.4258 0.071 Uiso 1 1 calc R . . C5 C 0.1573(3) 0.7348(4) 0.51904(15) 0.0417(7) Uani 1 1 d . . . C6 C 0.1446(3) 0.4607(4) 0.50791(19) 0.0562(9) Uani 1 1 d . . . H7 H 0.0991 0.4744 0.4681 0.067 Uiso 1 1 calc R . . H6 H 0.1051 0.3855 0.5305 0.067 Uiso 1 1 calc R . . C7 C 0.2678(3) 0.4052(4) 0.49691(17) 0.0487(8) Uani 1 1 d . . . C8 C 0.3090(3) 0.4150(4) 0.43852(16) 0.0488(8) Uani 1 1 d . . . H8 H 0.2611 0.4567 0.4059 0.059 Uiso 1 1 calc R . . C9 C 0.4219(3) 0.3626(4) 0.42830(16) 0.0462(8) Uani 1 1 d . . . C10 C 0.4930(3) 0.2996(4) 0.47621(18) 0.0556(9) Uani 1 1 d . . . H10 H 0.5686 0.2665 0.4698 0.067 Uiso 1 1 calc R . . C11 C 0.4513(4) 0.2857(5) 0.53437(18) 0.0656(11) Uani 1 1 d . . . H11 H 0.4982 0.2402 0.5665 0.079 Uiso 1 1 calc R . . C12 C 0.3394(4) 0.3398(4) 0.54469(18) 0.0600(10) Uani 1 1 d . . . H12 H 0.3128 0.3318 0.5839 0.072 Uiso 1 1 calc R . . C13 C 0.4654(3) 0.3889(4) 0.36543(17) 0.0517(9) Uani 1 1 d . . . H9 H 0.3991 0.3779 0.3340 0.062 Uiso 1 1 calc R . . H13 H 0.4931 0.4904 0.3637 0.062 Uiso 1 1 calc R . . C14 C 0.5430(3) 0.1463(4) 0.33523(14) 0.0392(7) Uani 1 1 d . . . C15 C 0.4321(3) 0.0782(5) 0.33461(17) 0.0527(9) Uani 1 1 d . . . H15 H 0.3667 0.1312 0.3455 0.063 Uiso 1 1 calc R . . C16 C 0.4212(3) -0.0681(5) 0.31774(18) 0.0590(10) Uani 1 1 d . . . H16 H 0.3480 -0.1148 0.3170 0.071 Uiso 1 1 calc R . . C17 C 0.5182(4) -0.1461(4) 0.30193(17) 0.0543(9) Uani 1 1 d . . . H17 H 0.5119 -0.2454 0.2906 0.065 Uiso 1 1 calc R . . C18 C 0.6235(3) -0.0733(4) 0.30344(15) 0.0457(8) Uani 1 1 d . . . H18 H 0.6890 -0.1254 0.2922 0.055 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 0.03426(12) 0.03037(12) 0.03624(12) -0.00348(9) 0.01221(8) -0.00199(8) S1 0.0383(4) 0.0272(3) 0.0481(4) 0.0011(3) 0.0164(3) -0.0032(3) O1 0.0420(12) 0.0314(10) 0.0494(12) -0.0016(10) 0.0224(10) -0.0048(9) O1W 0.0469(13) 0.0486(13) 0.0427(12) -0.0045(11) 0.0124(10) 0.0063(11) O2 0.0456(13) 0.0449(13) 0.0537(13) 0.0040(11) 0.0079(10) -0.0131(10) O2W 0.0457(14) 0.0346(12) 0.0803(17) -0.0038(12) 0.0216(12) 0.0004(10) O3 0.0624(17) 0.0298(12) 0.112(2) -0.0031(14) 0.0221(16) 0.0026(11) O3W 0.0461(14) 0.0416(13) 0.0566(14) -0.0054(12) 0.0102(11) -0.0017(11) O4 0.0454(13) 0.0609(15) 0.0421(12) 0.0057(11) 0.0150(10) -0.0065(11) N1 0.0572(17) 0.0418(15) 0.0333(13) -0.0037(12) 0.0106(12) -0.0053(12) N2 0.062(2) 0.0508(17) 0.0480(16) -0.0128(14) 0.0180(14) -0.0014(14) N3 0.0366(15) 0.0470(15) 0.0617(18) -0.0038(14) 0.0202(13) 0.0027(12) N4 0.0330(13) 0.0406(14) 0.0389(13) -0.0028(12) 0.0096(10) -0.0010(10) C1 0.114(4) 0.056(2) 0.047(2) 0.0073(19) 0.018(2) -0.016(2) C2 0.144(5) 0.069(3) 0.054(2) 0.013(2) 0.013(3) -0.019(3) C3 0.091(3) 0.081(3) 0.043(2) 0.011(2) 0.006(2) -0.005(3) C4 0.061(2) 0.071(3) 0.0451(19) -0.0173(19) 0.0052(17) 0.0016(19) C5 0.0332(16) 0.0489(19) 0.0439(17) -0.0071(15) 0.0089(13) -0.0002(13) C6 0.050(2) 0.052(2) 0.069(2) -0.0163(19) 0.0199(18) -0.0064(16) C7 0.0461(19) 0.0458(18) 0.056(2) -0.0127(17) 0.0125(16) -0.0036(15) C8 0.0456(19) 0.053(2) 0.0485(18) -0.0085(17) 0.0102(15) 0.0032(15) C9 0.0424(18) 0.052(2) 0.0463(18) -0.0041(16) 0.0128(14) 0.0018(15) C10 0.051(2) 0.060(2) 0.057(2) 0.0030(19) 0.0121(17) 0.0096(17) C11 0.074(3) 0.073(3) 0.048(2) 0.005(2) -0.0007(19) 0.009(2) C12 0.067(3) 0.065(3) 0.050(2) -0.0005(19) 0.0186(19) -0.003(2) C13 0.049(2) 0.054(2) 0.055(2) 0.0026(17) 0.0192(16) 0.0151(16) C14 0.0350(16) 0.0486(18) 0.0350(15) 0.0017(14) 0.0090(12) -0.0001(13) C15 0.0306(17) 0.069(2) 0.059(2) -0.0034(19) 0.0092(15) -0.0008(16) C16 0.0394(19) 0.078(3) 0.059(2) -0.004(2) 0.0011(16) -0.0208(18) C17 0.059(2) 0.053(2) 0.050(2) -0.0084(17) 0.0007(17) -0.0163(17) C18 0.0443(19) 0.0463(19) 0.0466(18) -0.0094(16) 0.0058(14) -0.0018(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2W 2.287(2) . ? Cd1 N4 2.309(3) 3_666 ? Cd1 N1 2.314(3) . ? Cd1 O1 2.333(2) . ? Cd1 O1W 2.357(2) . ? Cd1 O3W 2.362(2) . ? S1 O3 1.446(2) . ? S1 O2 1.471(2) . ? S1 O4 1.478(2) . ? S1 O1 1.488(2) . ? O1W H1W1 0.85(3) . ? O1W H1W2 0.851(10) . ? O2W H2W1 0.854(10) . ? O2W H2W2 0.86(3) . ? O3W H3W1 0.85(4) . ? O3W H3W2 0.842(10) . ? N1 C5 1.338(4) . ? N1 C1 1.350(5) . ? N2 C5 1.327(5) . ? N2 C6 1.470(5) . ? N2 H5 0.8600 . ? N3 C14 1.353(4) . ? N3 C13 1.452(4) . ? N3 H14 0.8600 . ? N4 C14 1.348(4) . ? N4 C18 1.353(4) . ? N4 Cd1 2.309(3) 3_666 ? C1 C2 1.360(6) . ? C1 H1 0.9300 . ? C2 C3 1.344(7) . ? C2 H2 0.9300 . ? C3 C4 1.357(6) . ? C3 H3 0.9300 . ? C4 C5 1.428(5) . ? C4 H4 0.9300 . ? C6 C7 1.523(5) . ? C6 H7 0.9700 . ? C6 H6 0.9700 . ? C7 C12 1.385(6) . ? C7 C8 1.390(5) . ? C8 C9 1.401(5) . ? C8 H8 0.9300 . ? C9 C10 1.375(5) . ? C9 C13 1.508(5) . ? C10 C11 1.390(5) . ? C10 H10 0.9300 . ? C11 C12 1.397(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H9 0.9700 . ? C13 H13 0.9700 . ? C14 C15 1.398(5) . ? C15 C16 1.373(6) . ? C15 H15 0.9300 . ? C16 C17 1.374(6) . ? C16 H16 0.9300 . ? C17 C18 1.360(5) . ? 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 O2W Cd1 N4 96.03(9) . 3_666 ? O2W Cd1 N1 97.34(10) . . ? N4 Cd1 N1 92.10(10) 3_666 . ? O2W Cd1 O1 160.40(8) . . ? N4 Cd1 O1 98.09(9) 3_666 . ? N1 Cd1 O1 95.65(9) . . ? O2W Cd1 O1W 85.90(9) . . ? N4 Cd1 O1W 88.50(9) 3_666 . ? N1 Cd1 O1W 176.62(9) . . ? O1 Cd1 O1W 80.97(8) . . ? O2W Cd1 O3W 79.78(9) . . ? N4 Cd1 O3W 175.28(8) 3_666 . ? N1 Cd1 O3W 90.60(10) . . ? O1 Cd1 O3W 85.48(8) . . ? O1W Cd1 O3W 89.03(9) . . ? O3 S1 O2 111.45(16) . . ? O3 S1 O4 109.69(18) . . ? O2 S1 O4 109.22(14) . . ? O3 S1 O1 109.43(15) . . ? O2 S1 O1 108.80(14) . . ? O4 S1 O1 108.18(13) . . ? S1 O1 Cd1 128.36(12) . . ? Cd1 O1W H1W1 115(3) . . ? Cd1 O1W H1W2 100(3) . . ? H1W1 O1W H1W2 110.1(17) . . ? Cd1 O2W H2W1 135(3) . . ? Cd1 O2W H2W2 109(3) . . ? H2W1 O2W H2W2 108.5(16) . . ? Cd1 O3W H3W1 110(3) . . ? Cd1 O3W H3W2 107(3) . . ? H3W1 O3W H3W2 111.0(17) . . ? C5 N1 C1 117.6(3) . . ? C5 N1 Cd1 129.4(2) . . ? C1 N1 Cd1 113.0(2) . . ? C5 N2 C6 125.6(3) . . ? C5 N2 H5 117.2 . . ? C6 N2 H5 117.2 . . ? C14 N3 C13 123.4(3) . . ? C14 N3 H14 118.3 . . ? C13 N3 H14 118.3 . . ? C14 N4 C18 117.9(3) . . ? C14 N4 Cd1 125.8(2) . 3_666 ? C18 N4 Cd1 115.7(2) . 3_666 ? N1 C1 C2 124.8(4) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C3 C2 C1 117.2(4) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C2 C3 C4 121.9(4) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 118.3(4) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N2 C5 N1 117.3(3) . . ? N2 C5 C4 122.5(3) . . ? N1 C5 C4 120.2(3) . . ? N2 C6 C7 113.6(3) . . ? N2 C6 H7 108.9 . . ? C7 C6 H7 108.9 . . ? N2 C6 H6 108.9 . . ? C7 C6 H6 108.9 . . ? H7 C6 H6 107.7 . . ? C12 C7 C8 118.8(3) . . ? C12 C7 C6 120.3(3) . . ? C8 C7 C6 120.8(3) . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.0(3) . . ? C10 C9 C13 121.8(3) . . ? C8 C9 C13 118.0(3) . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 120.3(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.5(4) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? N3 C13 C9 115.0(3) . . ? N3 C13 H9 108.5 . . ? C9 C13 H9 108.5 . . ? N3 C13 H13 108.5 . . ? C9 C13 H13 108.5 . . ? H9 C13 H13 107.5 . . ? N4 C14 N3 116.6(3) . . ? N4 C14 C15 121.1(3) . . ? N3 C14 C15 122.3(3) . . ? C16 C15 C14 118.9(3) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 120.3(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 117.9(3) . . ? C18 C17 H17 121.1 . . ? C16 C17 H17 121.1 . . ? N4 C18 C17 123.9(3) . . ? N4 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? 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 O3 S1 O1 Cd1 178.52(19) . . . . ? O2 S1 O1 Cd1 56.5(2) . . . . ? O4 S1 O1 Cd1 -62.0(2) . . . . ? O2W Cd1 O1 S1 9.0(4) . . . . ? N4 Cd1 O1 S1 144.73(17) 3_666 . . . ? N1 Cd1 O1 S1 -122.33(18) . . . . ? O1W Cd1 O1 S1 57.56(17) . . . . ? O3W Cd1 O1 S1 -32.17(17) . . . . ? O2W Cd1 N1 C5 -147.9(3) . . . . ? N4 Cd1 N1 C5 115.7(3) 3_666 . . . ? O1 Cd1 N1 C5 17.4(3) . . . . ? O3W Cd1 N1 C5 -68.1(3) . . . . ? O2W Cd1 N1 C1 29.5(3) . . . . ? N4 Cd1 N1 C1 -66.8(3) 3_666 . . . ? O1 Cd1 N1 C1 -165.2(3) . . . . ? O3W Cd1 N1 C1 109.3(3) . . . . ? C5 N1 C1 C2 -1.5(7) . . . . ? Cd1 N1 C1 C2 -179.2(4) . . . . ? N1 C1 C2 C3 2.4(9) . . . . ? C1 C2 C3 C4 -1.8(9) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C6 N2 C5 N1 -173.2(3) . . . . ? C6 N2 C5 C4 8.3(5) . . . . ? C1 N1 C5 N2 -178.6(4) . . . . ? Cd1 N1 C5 N2 -1.3(5) . . . . ? C1 N1 C5 C4 -0.1(5) . . . . ? Cd1 N1 C5 C4 177.2(2) . . . . ? C3 C4 C5 N2 179.1(4) . . . . ? C3 C4 C5 N1 0.7(6) . . . . ? C5 N2 C6 C7 80.8(5) . . . . ? N2 C6 C7 C12 75.8(5) . . . . ? N2 C6 C7 C8 -106.2(4) . . . . ? C12 C7 C8 C9 -1.4(6) . . . . ? C6 C7 C8 C9 -179.4(3) . . . . ? C7 C8 C9 C10 0.5(6) . . . . ? C7 C8 C9 C13 -174.6(3) . . . . ? C8 C9 C10 C11 1.2(6) . . . . ? C13 C9 C10 C11 176.2(4) . . . . ? C9 C10 C11 C12 -2.1(7) . . . . ? C8 C7 C12 C11 0.5(6) . . . . ? C6 C7 C12 C11 178.5(4) . . . . ? C10 C11 C12 C7 1.2(7) . . . . ? C14 N3 C13 C9 73.0(5) . . . . ? C10 C9 C13 N3 25.7(5) . . . . ? C8 C9 C13 N3 -159.2(3) . . . . ? C18 N4 C14 N3 -178.0(3) . . . . ? Cd1 N4 C14 N3 11.5(4) 3_666 . . . ? C18 N4 C14 C15 1.4(5) . . . . ? Cd1 N4 C14 C15 -169.2(2) 3_666 . . . ? C13 N3 C14 N4 178.2(3) . . . . ? C13 N3 C14 C15 -1.1(5) . . . . ? N4 C14 C15 C16 -0.8(5) . . . . ? N3 C14 C15 C16 178.5(3) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? C15 C16 C17 C18 -0.2(6) . . . . ? C14 N4 C18 C17 -1.5(5) . . . . ? Cd1 N4 C18 C17 170.0(3) 3_666 . . . ? C16 C17 C18 N4 0.9(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 O2 0.85(3) 1.89(3) 2.737(3) 175(3) 2_556 O1W H1W2 O4 0.851(10) 1.995(12) 2.838(4) 170(4) . O2W H2W1 O3 0.854(10) 1.835(13) 2.678(4) 169(5) 1_565 O2W H2W2 O4 0.86(3) 1.89(3) 2.744(3) 172(4) 2_556 O3W H3W1 O4 0.85(4) 2.096(15) 2.893(3) 157(3) 2_556 O3W H3W2 O2 0.842(10) 1.959(16) 2.764(3) 160(4) . N2 H5 O1 0.86 2.15 2.944(4) 153.8 . N3 H14 O1 0.86 2.16 2.989(3) 162.9 3_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.672 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.086 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 786014' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N4 O4 S Zn' _chemical_formula_sum 'C18 H18 N4 O4 S Zn' _chemical_formula_weight 451.79 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.511(3) _cell_length_b 9.2727(19) _cell_length_c 15.981(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.78(3) _cell_angle_gamma 90.00 _cell_volume 1847.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7821 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6826 _exptl_absorpt_correction_T_max 0.7468 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17715 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4218 _reflns_number_gt 2329 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4218 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Zn1 Zn 0.63022(6) 0.46997(8) 0.23950(4) 0.0364(3) Uani 1 1 d . . . S1 S 0.77443(13) 0.24443(18) 0.15891(9) 0.0379(3) Uani 1 1 d . . . O1 O 0.7538(3) 0.3912(5) 0.1931(3) 0.0519(13) Uani 1 1 d . . . O2 O 0.8479(5) 0.2592(6) 0.0957(3) 0.0833(19) Uani 1 1 d . . . O3 O 0.6759(4) 0.1752(6) 0.1333(3) 0.0767(16) Uani 1 1 d . . . O4 O 0.8276(4) 0.1646(5) 0.2315(3) 0.0581(13) Uani 1 1 d . . . N1 N 0.5789(4) 0.3583(6) 0.3351(3) 0.0378(13) Uani 1 1 d . . . N2 N 0.4655(4) 0.5424(6) 0.3684(3) 0.0470(14) Uani 1 1 d . . . H2N H 0.5047 0.6004 0.3421 0.056 Uiso 1 1 calc R . . N3 N -0.0357(4) 0.2334(6) 0.3760(3) 0.0416(14) Uani 1 1 d . . . H3N H -0.0969 0.2249 0.3477 0.050 Uiso 1 1 calc R . . N4 N -0.0073(4) -0.0093(5) 0.3506(3) 0.0306(12) Uani 1 1 d . . . C1 C 0.6143(5) 0.2224(8) 0.3478(4) 0.0467(18) Uani 1 1 d . . . H1A H 0.6737 0.1937 0.3207 0.056 Uiso 1 1 calc R . . C2 C 0.5695(5) 0.1237(8) 0.3977(4) 0.0474(18) Uani 1 1 d . . . H2A H 0.5965 0.0306 0.4042 0.057 Uiso 1 1 calc R . . C3 C 0.4812(5) 0.1695(8) 0.4385(4) 0.0513(19) Uani 1 1 d . . . H3A H 0.4477 0.1056 0.4728 0.062 Uiso 1 1 calc R . . C4 C 0.4440(5) 0.3047(8) 0.4289(4) 0.0422(17) Uani 1 1 d . . . H4A H 0.3845 0.3339 0.4557 0.051 Uiso 1 1 calc R . . C5 C 0.4956(5) 0.4027(7) 0.3776(4) 0.0379(16) Uani 1 1 d . . . C6 C 0.3678(5) 0.5975(8) 0.4019(4) 0.0504(19) Uani 1 1 d . . . H6A H 0.3670 0.7019 0.3978 0.061 Uiso 1 1 calc R . . H6B H 0.3688 0.5722 0.4609 0.061 Uiso 1 1 calc R . . C7 C 0.2673(5) 0.5383(7) 0.3560(5) 0.0472(17) Uani 1 1 d . . . C8 C 0.2550(6) 0.5415(9) 0.2692(5) 0.066(2) Uani 1 1 d . . . H8A H 0.3094 0.5790 0.2394 0.079 Uiso 1 1 calc R . . C9 C 0.1626(6) 0.4894(10) 0.2266(5) 0.072(3) Uani 1 1 d . . . H9A H 0.1557 0.4892 0.1683 0.086 Uiso 1 1 calc R . . C10 C 0.0807(6) 0.4380(9) 0.2703(4) 0.063(2) Uani 1 1 d . . . H10A H 0.0179 0.4057 0.2411 0.076 Uiso 1 1 calc R . . C11 C 0.0901(5) 0.4336(7) 0.3573(4) 0.0435(17) Uani 1 1 d . . . C12 C 0.1843(5) 0.4838(7) 0.3992(4) 0.0402(16) Uani 1 1 d . . . H12A H 0.1921 0.4809 0.4575 0.048 Uiso 1 1 calc R . . C13 C -0.0016(5) 0.3754(7) 0.4039(4) 0.0437(17) Uani 1 1 d . . . H13A H 0.0207 0.3719 0.4635 0.052 Uiso 1 1 calc R . . H13B H -0.0620 0.4411 0.3961 0.052 Uiso 1 1 calc R . . C14 C 0.0233(5) 0.1134(7) 0.3919(4) 0.0367(15) Uani 1 1 d . . . C15 C 0.1123(5) 0.1114(8) 0.4525(4) 0.0421(17) Uani 1 1 d . . . H15A H 0.1349 0.1956 0.4803 0.051 Uiso 1 1 calc R . . C16 C 0.1639(6) -0.0132(9) 0.4695(4) 0.053(2) Uani 1 1 d . . . H16A H 0.2217 -0.0148 0.5100 0.064 Uiso 1 1 calc R . . C17 C 0.1332(5) -0.1389(8) 0.4284(4) 0.0500(18) Uani 1 1 d . . . H17A H 0.1697 -0.2249 0.4402 0.060 Uiso 1 1 calc R . . C18 C 0.0472(5) -0.1329(7) 0.3697(4) 0.0441(17) Uani 1 1 d . . . H18A H 0.0252 -0.2172 0.3418 0.053 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 Zn1 0.0358(4) 0.0368(5) 0.0366(4) 0.0025(4) 0.0030(3) 0.0013(4) S1 0.0292(3) 0.0398(4) 0.0441(4) 0.0001(3) -0.0022(3) 0.0008(3) O1 0.051(3) 0.037(3) 0.071(3) -0.002(2) 0.026(3) 0.006(2) O2 0.111(5) 0.077(4) 0.072(3) 0.008(3) 0.068(4) 0.009(3) O3 0.055(3) 0.066(4) 0.101(4) 0.005(3) -0.038(3) -0.010(3) O4 0.071(3) 0.040(3) 0.058(3) 0.011(2) -0.026(2) 0.005(3) N1 0.029(3) 0.044(4) 0.040(3) 0.008(3) 0.001(2) 0.007(3) N2 0.040(3) 0.037(4) 0.065(4) 0.004(3) 0.012(3) 0.001(3) N3 0.039(3) 0.032(4) 0.052(3) -0.009(3) -0.006(3) -0.001(3) N4 0.030(3) 0.028(3) 0.034(3) -0.003(2) 0.007(2) 0.000(2) C1 0.037(4) 0.061(5) 0.043(4) 0.011(4) 0.013(3) 0.015(4) C2 0.053(4) 0.040(4) 0.050(4) 0.005(4) 0.007(4) 0.010(4) C3 0.047(4) 0.055(5) 0.053(4) 0.012(4) 0.013(4) 0.006(4) C4 0.037(4) 0.052(5) 0.039(4) 0.005(3) 0.012(3) -0.003(3) C5 0.029(3) 0.040(4) 0.044(4) 0.000(3) -0.002(3) 0.001(3) C6 0.043(4) 0.038(5) 0.072(5) -0.010(4) 0.018(4) 0.005(3) C7 0.040(4) 0.033(4) 0.067(5) -0.009(4) -0.003(4) 0.007(3) C8 0.053(5) 0.073(6) 0.071(5) 0.010(5) 0.003(4) 0.000(5) C9 0.062(5) 0.110(8) 0.044(4) 0.019(5) 0.011(4) -0.007(5) C10 0.055(5) 0.081(7) 0.051(5) 0.004(4) -0.013(4) -0.007(4) C11 0.042(4) 0.026(4) 0.063(4) -0.005(3) 0.009(4) -0.001(3) C12 0.041(4) 0.033(4) 0.046(4) -0.006(3) 0.006(3) 0.003(3) C13 0.041(4) 0.031(4) 0.058(4) -0.003(3) -0.001(3) 0.001(3) C14 0.040(4) 0.027(4) 0.044(4) 0.001(3) 0.008(3) 0.001(3) C15 0.043(4) 0.050(5) 0.032(3) -0.010(3) -0.005(3) -0.006(4) C16 0.043(4) 0.062(6) 0.052(4) 0.004(4) -0.010(3) 0.013(4) C17 0.046(4) 0.045(5) 0.057(4) -0.004(4) -0.005(4) 0.010(4) C18 0.049(4) 0.028(4) 0.055(4) -0.011(3) 0.002(4) 0.000(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 Zn1 O1 1.914(4) . ? Zn1 O4 1.926(5) 2_655 ? Zn1 N1 1.995(5) . ? Zn1 N4 2.027(5) 2 ? S1 O3 1.419(5) . ? S1 O2 1.428(4) . ? S1 O4 1.485(4) . ? S1 O1 1.497(5) . ? O4 Zn1 1.926(5) 2_645 ? N1 C1 1.346(8) . ? N1 C5 1.355(7) . ? N2 C5 1.354(8) . ? N2 C6 1.466(7) . ? N2 H2N 0.8600 . ? N3 C14 1.348(8) . ? N3 C13 1.444(8) . ? N3 H3N 0.8600 . ? N4 C14 1.354(7) . ? N4 C18 1.355(8) . ? N4 Zn1 2.027(5) 2_545 ? C1 C2 1.364(8) . ? C1 H1A 0.9300 . ? C2 C3 1.396(8) . ? C2 H2A 0.9300 . ? C3 C4 1.342(9) . ? C3 H3A 0.9300 . ? C4 C5 1.415(8) . ? C4 H4A 0.9300 . ? C6 C7 1.506(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.384(9) . ? C7 C12 1.388(8) . ? C8 C9 1.379(10) . ? C8 H8A 0.9300 . ? C9 C10 1.372(10) . ? C9 H9A 0.9300 . ? C10 C11 1.386(9) . ? C10 H10A 0.9300 . ? C11 C12 1.386(9) . ? C11 C13 1.519(8) . ? C12 H12A 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.415(8) . ? C15 C16 1.340(9) . ? C15 H15A 0.9300 . ? C16 C17 1.376(10) . ? C16 H16A 0.9300 . ? C17 C18 1.369(8) . ? C17 H17A 0.9300 . ? C18 H18A 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 O1 Zn1 O4 103.7(2) . 2_655 ? O1 Zn1 N1 114.9(2) . . ? O4 Zn1 N1 113.6(2) 2_655 . ? O1 Zn1 N4 110.52(19) . 2 ? O4 Zn1 N4 104.99(19) 2_655 2 ? N1 Zn1 N4 108.65(19) . 2 ? O3 S1 O2 115.7(4) . . ? O3 S1 O4 108.7(3) . . ? O2 S1 O4 109.1(3) . . ? O3 S1 O1 110.2(3) . . ? O2 S1 O1 108.2(3) . . ? O4 S1 O1 104.3(3) . . ? S1 O1 Zn1 131.1(3) . . ? S1 O4 Zn1 138.6(3) . 2_645 ? C1 N1 C5 117.8(5) . . ? C1 N1 Zn1 118.6(4) . . ? C5 N1 Zn1 122.5(4) . . ? C5 N2 C6 121.7(5) . . ? C5 N2 H2N 119.1 . . ? C6 N2 H2N 119.1 . . ? C14 N3 C13 123.5(5) . . ? C14 N3 H3N 118.2 . . ? C13 N3 H3N 118.2 . . ? C14 N4 C18 119.0(5) . . ? C14 N4 Zn1 126.3(4) . 2_545 ? C18 N4 Zn1 114.7(4) . 2_545 ? N1 C1 C2 124.8(6) . . ? N1 C1 H1A 117.6 . . ? C2 C1 H1A 117.6 . . ? C1 C2 C3 116.7(7) . . ? C1 C2 H2A 121.7 . . ? C3 C2 H2A 121.7 . . ? C4 C3 C2 120.7(6) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N2 C5 N1 117.0(6) . . ? N2 C5 C4 122.8(6) . . ? N1 C5 C4 120.2(6) . . ? N2 C6 C7 112.5(5) . . ? N2 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C12 118.7(7) . . ? C8 C7 C6 119.9(7) . . ? C12 C7 C6 121.3(6) . . ? C9 C8 C7 120.4(7) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C10 C9 C8 120.1(7) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 121.1(7) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? C10 C11 C12 118.2(6) . . ? C10 C11 C13 119.9(6) . . ? C12 C11 C13 121.9(6) . . ? C11 C12 C7 121.5(6) . . ? C11 C12 H12A 119.2 . . ? C7 C12 H12A 119.2 . . ? N3 C13 C11 112.8(5) . . ? N3 C13 H13A 109.0 . . ? C11 C13 H13A 109.0 . . ? N3 C13 H13B 109.0 . . ? C11 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N3 C14 N4 118.3(6) . . ? N3 C14 C15 121.8(6) . . ? N4 C14 C15 119.8(6) . . ? C16 C15 C14 119.2(6) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C17 121.6(7) . . ? C15 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C18 C17 C16 117.7(7) . . ? C18 C17 H17A 121.2 . . ? C16 C17 H17A 121.2 . . ? N4 C18 C17 122.7(6) . . ? N4 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? 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 O3 S1 O1 Zn1 22.7(5) . . . . ? O2 S1 O1 Zn1 150.1(4) . . . . ? O4 S1 O1 Zn1 -93.8(4) . . . . ? O4 Zn1 O1 S1 179.6(4) 2_655 . . . ? N1 Zn1 O1 S1 55.0(4) . . . . ? N4 Zn1 O1 S1 -68.4(4) 2 . . . ? O3 S1 O4 Zn1 52.4(6) . . . 2_645 ? O2 S1 O4 Zn1 -74.7(5) . . . 2_645 ? O1 S1 O4 Zn1 169.9(4) . . . 2_645 ? O1 Zn1 N1 C1 -15.8(6) . . . . ? O4 Zn1 N1 C1 -135.0(5) 2_655 . . . ? N4 Zn1 N1 C1 108.5(5) 2 . . . ? O1 Zn1 N1 C5 176.8(4) . . . . ? O4 Zn1 N1 C5 57.6(5) 2_655 . . . ? N4 Zn1 N1 C5 -58.9(5) 2 . . . ? C5 N1 C1 C2 3.1(10) . . . . ? Zn1 N1 C1 C2 -164.9(5) . . . . ? N1 C1 C2 C3 -0.6(10) . . . . ? C1 C2 C3 C4 -0.5(10) . . . . ? C2 C3 C4 C5 -0.9(10) . . . . ? C6 N2 C5 N1 171.5(6) . . . . ? C6 N2 C5 C4 -8.4(10) . . . . ? C1 N1 C5 N2 175.8(6) . . . . ? Zn1 N1 C5 N2 -16.7(8) . . . . ? C1 N1 C5 C4 -4.3(9) . . . . ? Zn1 N1 C5 C4 163.2(5) . . . . ? C3 C4 C5 N2 -176.8(6) . . . . ? C3 C4 C5 N1 3.4(9) . . . . ? C5 N2 C6 C7 -68.8(8) . . . . ? N2 C6 C7 C8 -49.2(9) . . . . ? N2 C6 C7 C12 132.8(6) . . . . ? C12 C7 C8 C9 -0.9(12) . . . . ? C6 C7 C8 C9 -179.1(7) . . . . ? C7 C8 C9 C10 2.0(13) . . . . ? C8 C9 C10 C11 -1.8(13) . . . . ? C9 C10 C11 C12 0.6(11) . . . . ? C9 C10 C11 C13 -179.7(7) . . . . ? C10 C11 C12 C7 0.5(10) . . . . ? C13 C11 C12 C7 -179.2(6) . . . . ? C8 C7 C12 C11 -0.3(10) . . . . ? C6 C7 C12 C11 177.8(6) . . . . ? C14 N3 C13 C11 70.8(8) . . . . ? C10 C11 C13 N3 53.6(8) . . . . ? C12 C11 C13 N3 -126.7(6) . . . . ? C13 N3 C14 N4 -168.6(5) . . . . ? C13 N3 C14 C15 14.2(9) . . . . ? C18 N4 C14 N3 -175.9(5) . . . . ? Zn1 N4 C14 N3 3.8(7) 2_545 . . . ? C18 N4 C14 C15 1.4(8) . . . . ? Zn1 N4 C14 C15 -178.9(4) 2_545 . . . ? N3 C14 C15 C16 175.8(6) . . . . ? N4 C14 C15 C16 -1.4(9) . . . . ? C14 C15 C16 C17 1.0(10) . . . . ? C15 C16 C17 C18 -0.5(10) . . . . ? C14 N4 C18 C17 -0.9(9) . . . . ? Zn1 N4 C18 C17 179.3(5) 2_545 . . . ? C16 C17 C18 N4 0.5(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O2 0.86 2.50 3.098(8) 127.3 2_655 N2 H2N O4 0.86 2.56 3.349(7) 153.1 2_655 N3 H3N O4 0.86 2.09 2.830(7) 144.0 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.536 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.120 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 786015' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Cd N8 O6' _chemical_formula_sum 'C27 H27 Cd N8 O6' _chemical_formula_weight 671.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.354(6) _cell_length_b 9.855(2) _cell_length_c 18.599(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.41(3) _cell_angle_gamma 90.00 _cell_volume 5850(2) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 22548 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8434 _exptl_absorpt_correction_T_max 0.8961 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35319 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5141 _reflns_number_gt 4152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0521P)^2^+12.5611P] 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 5141 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.638185(9) 0.01171(2) 0.451180(16) 0.04654(13) Uani 1 1 d . . . O1 O 0.67690(12) -0.1717(3) 0.5181(2) 0.0836(10) Uani 1 1 d . . . O2 O 0.70591(10) 0.0214(3) 0.53512(19) 0.0633(8) Uani 1 1 d . . . O3 O 0.73643(12) -0.1544(4) 0.5892(2) 0.0891(11) Uani 1 1 d . . . O4 O 0.60148(11) -0.1875(3) 0.4043(2) 0.0801(10) Uani 1 1 d . . . O5 O 0.56987(11) -0.0085(3) 0.3611(2) 0.0651(8) Uani 1 1 d . . . O6 O 0.54823(11) -0.2054(4) 0.3185(2) 0.0855(11) Uani 1 1 d . . . N1 N 0.67545(11) 0.0051(3) 0.35247(19) 0.0495(8) Uani 1 1 d . . . N2 N 0.62797(11) 0.1365(3) 0.27597(18) 0.0531(8) Uani 1 1 d . . . H2N H 0.6117 0.1294 0.3080 0.064 Uiso 1 1 calc R . . N3 N 0.64929(11) 0.8377(3) 0.12052(19) 0.0570(9) Uani 1 1 d . . . H3N H 0.6645 0.8477 0.0871 0.068 Uiso 1 1 calc R . . N4 N 0.59994(11) 0.9703(3) 0.04937(18) 0.0487(8) Uani 1 1 d . . . N5 N 0.64045(10) 0.2472(3) 0.44317(17) 0.0485(8) Uani 1 1 d . . . N6 N 0.56997(11) 0.2795(4) 0.4065(2) 0.0685(10) Uani 1 1 d . . . H6N H 0.5675 0.1927 0.4071 0.082 Uiso 1 1 calc R . . N7 N 0.70722(13) -0.1044(4) 0.5493(2) 0.0613(9) Uani 1 1 d . . . N8 N 0.57245(12) -0.1362(4) 0.3595(2) 0.0577(9) Uani 1 1 d . . . C1 C 0.66691(13) 0.0827(4) 0.2911(2) 0.0493(9) Uani 1 1 d . . . C2 C 0.69685(15) 0.1031(4) 0.2457(2) 0.0616(11) Uani 1 1 d . . . H2 H 0.6910 0.1588 0.2049 0.074 Uiso 1 1 calc R . . C3 C 0.73463(16) 0.0405(6) 0.2620(3) 0.0734(14) Uani 1 1 d . . . H3 H 0.7547 0.0536 0.2321 0.088 Uiso 1 1 calc R . . C4 C 0.74356(16) -0.0418(5) 0.3219(3) 0.0728(13) Uani 1 1 d . . . H4 H 0.7691 -0.0868 0.3326 0.087 Uiso 1 1 calc R . . C5 C 0.71322(14) -0.0555(5) 0.3658(3) 0.0622(11) Uani 1 1 d . . . H5 H 0.7193 -0.1099 0.4070 0.075 Uiso 1 1 calc R . . C6 C 0.61232(15) 0.2060(4) 0.2074(2) 0.0604(11) Uani 1 1 d . . . H6A H 0.5819 0.2060 0.2002 0.072 Uiso 1 1 calc R . . H6B H 0.6208 0.1548 0.1678 0.072 Uiso 1 1 calc R . . C7 C 0.62721(13) 0.3504(4) 0.2031(2) 0.0512(9) Uani 1 1 d . . . C8 C 0.62239(18) 0.4137(4) 0.1367(2) 0.0745(15) Uani 1 1 d . . . H8 H 0.6109 0.3661 0.0951 0.089 Uiso 1 1 calc R . . C9 C 0.63436(19) 0.5478(5) 0.1306(3) 0.0774(16) Uani 1 1 d . . . H9 H 0.6310 0.5885 0.0849 0.093 Uiso 1 1 calc R . . C10 C 0.65106(14) 0.6211(4) 0.1910(2) 0.0519(10) Uani 1 1 d . . . C11 C 0.65604(16) 0.5578(4) 0.2574(2) 0.0620(12) Uani 1 1 d . . . H11 H 0.6671 0.6059 0.2991 0.074 Uiso 1 1 calc R . . C12 C 0.64483(15) 0.4237(4) 0.2632(2) 0.0622(12) Uani 1 1 d . . . H12 H 0.6493 0.3821 0.3087 0.075 Uiso 1 1 calc R . . C13 C 0.66709(15) 0.7643(4) 0.1860(2) 0.0625(11) Uani 1 1 d . . . H13A H 0.6613 0.8149 0.2280 0.075 Uiso 1 1 calc R . . H13B H 0.6973 0.7609 0.1887 0.075 Uiso 1 1 calc R . . C14 C 0.61032(13) 0.8913(4) 0.1087(2) 0.0506(9) Uani 1 1 d . . . C15 C 0.58177(15) 0.8668(4) 0.1563(2) 0.0618(11) Uani 1 1 d . . . H15 H 0.5887 0.8079 0.1955 0.074 Uiso 1 1 calc R . . C16 C 0.54405(16) 0.9291(5) 0.1450(3) 0.0712(13) Uani 1 1 d . . . H16 H 0.5251 0.9146 0.1768 0.085 Uiso 1 1 calc R . . C17 C 0.53394(15) 1.0143(5) 0.0859(3) 0.0721(14) Uani 1 1 d . . . H17 H 0.5084 1.0595 0.0775 0.087 Uiso 1 1 calc R . . C18 C 0.56241(14) 1.0303(5) 0.0406(3) 0.0614(11) Uani 1 1 d . . . H18 H 0.5553 1.0870 0.0005 0.074 Uiso 1 1 calc R . . C19 C 0.60834(13) 0.3343(4) 0.4279(2) 0.0521(10) Uani 1 1 d . . . C20 C 0.61487(18) 0.4750(4) 0.4320(3) 0.0644(12) Uani 1 1 d . . . H20 H 0.5924 0.5349 0.4226 0.077 Uiso 1 1 calc R . . C21 C 0.65459(19) 0.5217(4) 0.4499(3) 0.0717(14) Uani 1 1 d . . . H21 H 0.6594 0.6147 0.4530 0.086 Uiso 1 1 calc R . . C22 C 0.68740(17) 0.4346(5) 0.4635(3) 0.0763(14) Uani 1 1 d . . . H22 H 0.7147 0.4667 0.4754 0.092 Uiso 1 1 calc R . . C23 C 0.67937(15) 0.2998(4) 0.4592(3) 0.0644(12) Uani 1 1 d . . . H23 H 0.7019 0.2401 0.4678 0.077 Uiso 1 1 calc R . . C24 C 0.53239(16) 0.3614(5) 0.3823(3) 0.0773(14) Uani 1 1 d . . . H24A H 0.5105 0.3029 0.3575 0.093 Uiso 1 1 calc R . . H24B H 0.5387 0.4285 0.3476 0.093 Uiso 1 1 calc R . . C25 C 0.51631(15) 0.4331(5) 0.4440(3) 0.0688(13) Uani 1 1 d . . . C26 C 0.51973(18) 0.3773(5) 0.5128(3) 0.0850(16) Uani 1 1 d . . . H26 H 0.5329 0.2938 0.5221 0.102 Uiso 1 1 calc R . . C27 C 0.49604(18) 0.5572(6) 0.4321(3) 0.0875(17) Uani 1 1 d . . . H27 H 0.4931 0.5968 0.3861 0.105 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 0.0539(2) 0.02845(16) 0.0583(2) 0.00016(11) 0.01226(14) 0.00147(12) O1 0.085(2) 0.052(2) 0.112(3) 0.0023(19) 0.008(2) -0.0033(18) O2 0.0619(19) 0.0431(17) 0.086(2) 0.0049(14) 0.0173(16) 0.0094(13) O3 0.086(2) 0.089(3) 0.089(3) 0.026(2) 0.004(2) 0.038(2) O4 0.082(2) 0.0498(19) 0.102(3) 0.0002(17) -0.003(2) 0.0013(17) O5 0.068(2) 0.0439(18) 0.087(2) 0.0014(14) 0.0228(17) -0.0003(14) O6 0.084(2) 0.084(3) 0.088(2) -0.028(2) 0.0121(19) -0.030(2) N1 0.061(2) 0.0377(18) 0.052(2) -0.0002(13) 0.0137(16) 0.0094(15) N2 0.062(2) 0.0371(18) 0.062(2) 0.0105(15) 0.0145(17) 0.0010(15) N3 0.068(2) 0.0392(18) 0.066(2) 0.0127(16) 0.0170(18) 0.0013(16) N4 0.055(2) 0.0426(17) 0.0497(19) -0.0029(14) 0.0115(15) 0.0002(15) N5 0.055(2) 0.0298(16) 0.064(2) 0.0038(14) 0.0169(16) 0.0015(14) N6 0.060(2) 0.044(2) 0.105(3) -0.0035(19) 0.027(2) 0.0082(17) N7 0.068(2) 0.051(2) 0.069(2) 0.0084(18) 0.022(2) 0.0130(19) N8 0.064(2) 0.047(2) 0.066(2) -0.0084(17) 0.0200(19) -0.0094(18) C1 0.061(3) 0.0302(19) 0.059(2) -0.0062(17) 0.0150(19) -0.0051(17) C2 0.073(3) 0.047(2) 0.069(3) 0.001(2) 0.023(2) -0.006(2) C3 0.065(3) 0.077(3) 0.085(4) -0.010(3) 0.033(3) -0.007(3) C4 0.063(3) 0.078(3) 0.078(3) -0.006(3) 0.012(2) 0.016(3) C5 0.065(3) 0.055(3) 0.068(3) -0.004(2) 0.012(2) 0.015(2) C6 0.073(3) 0.035(2) 0.070(3) 0.0088(19) 0.003(2) -0.0075(19) C7 0.060(2) 0.035(2) 0.058(2) 0.0022(17) 0.0068(19) 0.0006(18) C8 0.123(4) 0.042(2) 0.052(3) 0.0000(19) -0.006(3) -0.017(3) C9 0.135(5) 0.041(2) 0.051(3) 0.012(2) 0.003(3) -0.013(3) C10 0.068(3) 0.031(2) 0.056(2) 0.0045(17) 0.010(2) 0.0006(18) C11 0.096(3) 0.040(2) 0.050(2) 0.0011(18) 0.009(2) -0.014(2) C12 0.093(3) 0.042(2) 0.052(3) 0.0071(19) 0.013(2) -0.011(2) C13 0.079(3) 0.038(2) 0.068(3) 0.0123(19) 0.006(2) -0.008(2) C14 0.063(3) 0.034(2) 0.057(2) -0.0033(17) 0.015(2) -0.0083(18) C15 0.073(3) 0.052(3) 0.065(3) -0.002(2) 0.025(2) -0.014(2) C16 0.071(3) 0.077(3) 0.070(3) -0.015(3) 0.025(3) -0.019(3) C17 0.052(3) 0.091(4) 0.074(3) -0.019(3) 0.013(2) 0.005(2) C18 0.059(3) 0.069(3) 0.057(3) -0.008(2) 0.011(2) 0.004(2) C19 0.061(3) 0.039(2) 0.059(3) -0.0036(18) 0.019(2) 0.0050(19) C20 0.088(4) 0.035(2) 0.074(3) 0.0022(19) 0.024(3) 0.011(2) C21 0.109(4) 0.035(2) 0.075(3) -0.004(2) 0.025(3) -0.011(3) C22 0.079(3) 0.056(3) 0.093(4) -0.001(3) 0.013(3) -0.019(3) C23 0.069(3) 0.046(2) 0.079(3) 0.004(2) 0.012(2) -0.009(2) C24 0.068(3) 0.069(3) 0.096(4) 0.001(3) 0.017(3) 0.022(3) C25 0.061(3) 0.056(3) 0.092(4) 0.009(2) 0.021(2) 0.018(2) C26 0.101(4) 0.062(3) 0.099(4) 0.019(3) 0.036(3) 0.042(3) C27 0.102(4) 0.075(4) 0.091(4) 0.027(3) 0.032(3) 0.037(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 N5 2.327(3) . ? Cd1 N1 2.356(3) . ? Cd1 N4 2.374(3) 6_566 ? Cd1 O4 2.384(3) . ? Cd1 O1 2.423(3) . ? Cd1 O2 2.476(3) . ? Cd1 O5 2.554(4) . ? O1 N7 1.246(5) . ? O2 N7 1.267(4) . ? O3 N7 1.207(5) . ? O4 N8 1.255(5) . ? O5 N8 1.261(4) . ? O6 N8 1.211(4) . ? N1 C5 1.346(5) . ? N1 C1 1.364(5) . ? N2 C1 1.353(5) . ? N2 C6 1.463(5) . ? N2 H2N 0.8600 . ? N3 C14 1.351(5) . ? N3 C13 1.453(5) . ? N3 H3N 0.8600 . ? N4 C18 1.336(6) . ? N4 C14 1.348(5) . ? N4 Cd1 2.374(3) 6_565 ? N5 C19 1.342(5) . ? N5 C23 1.349(5) . ? N6 C19 1.352(5) . ? N6 C24 1.467(6) . ? N6 H6N 0.8600 . ? C1 C2 1.400(6) . ? C2 C3 1.359(7) . ? C2 H2 0.9300 . ? C3 C4 1.370(7) . ? C3 H3 0.9300 . ? C4 C5 1.382(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.509(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.370(6) . ? C7 C12 1.374(6) . ? C8 C9 1.387(6) . ? C8 H8 0.9300 . ? C9 C10 1.371(6) . ? C9 H9 0.9300 . ? C10 C11 1.369(6) . ? C10 C13 1.511(5) . ? C11 C12 1.379(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.401(6) . ? C15 C16 1.351(7) . ? C15 H15 0.9300 . ? C16 C17 1.379(7) . ? C16 H16 0.9300 . ? C17 C18 1.356(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.402(6) . ? C20 C21 1.354(8) . ? C20 H20 0.9300 . ? C21 C22 1.356(7) . ? C21 H21 0.9300 . ? C22 C23 1.354(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.510(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.382(7) . ? C25 C27 1.388(7) . ? C26 C27 1.378(7) 5_666 ? C26 H26 0.9300 . ? C27 C26 1.378(7) 5_666 ? C27 H27 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 N1 87.26(10) . . ? N5 Cd1 N4 90.04(11) . 6_566 ? N1 Cd1 N4 177.22(11) . 6_566 ? N5 Cd1 O4 144.74(12) . . ? N1 Cd1 O4 88.86(12) . . ? N4 Cd1 O4 92.96(12) 6_566 . ? N5 Cd1 O1 139.23(12) . . ? N1 Cd1 O1 95.28(12) . . ? N4 Cd1 O1 87.21(12) 6_566 . ? O4 Cd1 O1 76.03(13) . . ? N5 Cd1 O2 88.17(10) . . ? N1 Cd1 O2 88.83(12) . . ? N4 Cd1 O2 91.77(11) 6_566 . ? O4 Cd1 O2 126.79(11) . . ? O1 Cd1 O2 51.33(11) . . ? N5 Cd1 O5 93.95(10) . . ? N1 Cd1 O5 89.13(12) . . ? N4 Cd1 O5 90.37(11) 6_566 . ? O4 Cd1 O5 50.94(10) . . ? O1 Cd1 O5 126.71(11) . . ? O2 Cd1 O5 176.99(9) . . ? N7 O1 Cd1 98.3(3) . . ? N7 O2 Cd1 95.1(3) . . ? N8 O4 Cd1 100.6(2) . . ? N8 O5 Cd1 92.3(3) . . ? C5 N1 C1 117.1(4) . . ? C5 N1 Cd1 115.7(3) . . ? C1 N1 Cd1 125.2(3) . . ? C1 N2 C6 122.8(4) . . ? C1 N2 H2N 118.6 . . ? C6 N2 H2N 118.6 . . ? C14 N3 C13 124.2(4) . . ? C14 N3 H3N 117.9 . . ? C13 N3 H3N 117.9 . . ? C18 N4 C14 117.1(4) . . ? C18 N4 Cd1 116.8(3) . 6_565 ? C14 N4 Cd1 125.6(3) . 6_565 ? C19 N5 C23 117.6(4) . . ? C19 N5 Cd1 128.3(3) . . ? C23 N5 Cd1 114.0(3) . . ? C19 N6 C24 123.0(4) . . ? C19 N6 H6N 118.5 . . ? C24 N6 H6N 118.5 . . ? O3 N7 O1 123.2(4) . . ? O3 N7 O2 121.6(4) . . ? O1 N7 O2 115.3(4) . . ? O6 N8 O4 121.9(4) . . ? O6 N8 O5 122.5(4) . . ? O4 N8 O5 115.6(4) . . ? N2 C1 N1 116.6(3) . . ? N2 C1 C2 122.1(4) . . ? N1 C1 C2 121.3(4) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.9(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 117.5(5) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 124.0(4) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? N2 C6 C7 114.9(3) . . ? N2 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? N2 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C8 C7 C12 117.7(4) . . ? C8 C7 C6 119.2(4) . . ? C12 C7 C6 123.1(4) . . ? C7 C8 C9 121.1(4) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 118.1(4) . . ? C11 C10 C13 119.3(4) . . ? C9 C10 C13 122.4(4) . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C7 C12 C11 121.3(4) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? N3 C13 C10 115.0(4) . . ? N3 C13 H13A 108.5 . . ? C10 C13 H13A 108.5 . . ? N3 C13 H13B 108.5 . . ? C10 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N4 C14 N3 117.4(4) . . ? N4 C14 C15 121.0(4) . . ? N3 C14 C15 121.6(4) . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.4(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 118.0(5) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? N4 C18 C17 124.6(5) . . ? N4 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? N5 C19 N6 116.6(4) . . ? N5 C19 C20 121.1(4) . . ? N6 C19 C20 122.3(4) . . ? C21 C20 C19 118.5(5) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C22 120.9(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 118.2(5) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? N5 C23 C22 123.6(5) . . ? N5 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? N6 C24 C25 113.3(4) . . ? N6 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N6 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C27 117.6(4) . . ? C26 C25 C24 122.1(4) . . ? C27 C25 C24 120.3(5) . . ? C27 C26 C25 121.3(5) 5_666 . ? C27 C26 H26 119.4 5_666 . ? C25 C26 H26 119.4 . . ? C26 C27 C25 121.1(5) 5_666 . ? C26 C27 H27 119.4 5_666 . ? C25 C27 H27 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Cd1 O1 N7 -7.7(4) . . . . ? N1 Cd1 O1 N7 84.2(3) . . . . ? N4 Cd1 O1 N7 -94.6(3) 6_566 . . . ? O4 Cd1 O1 N7 171.7(3) . . . . ? O2 Cd1 O1 N7 -0.1(2) . . . . ? O5 Cd1 O1 N7 177.0(2) . . . . ? N5 Cd1 O2 N7 175.1(2) . . . . ? N1 Cd1 O2 N7 -97.6(2) . . . . ? N4 Cd1 O2 N7 85.1(2) 6_566 . . . ? O4 Cd1 O2 N7 -9.9(3) . . . . ? O1 Cd1 O2 N7 0.1(2) . . . . ? N5 Cd1 O4 N8 -1.7(4) . . . . ? N1 Cd1 O4 N8 -85.4(3) . . . . ? N4 Cd1 O4 N8 92.5(3) 6_566 . . . ? O1 Cd1 O4 N8 178.9(3) . . . . ? O2 Cd1 O4 N8 -173.1(2) . . . . ? O5 Cd1 O4 N8 4.4(2) . . . . ? N5 Cd1 O5 N8 172.1(2) . . . . ? N1 Cd1 O5 N8 84.9(2) . . . . ? N4 Cd1 O5 N8 -97.9(2) 6_566 . . . ? O4 Cd1 O5 N8 -4.3(2) . . . . ? O1 Cd1 O5 N8 -11.1(3) . . . . ? N5 Cd1 N1 C5 119.1(3) . . . . ? O4 Cd1 N1 C5 -96.0(3) . . . . ? O1 Cd1 N1 C5 -20.1(3) . . . . ? O2 Cd1 N1 C5 30.9(3) . . . . ? O5 Cd1 N1 C5 -146.9(3) . . . . ? N5 Cd1 N1 C1 -44.6(3) . . . . ? O4 Cd1 N1 C1 100.3(3) . . . . ? O1 Cd1 N1 C1 176.2(3) . . . . ? O2 Cd1 N1 C1 -132.8(3) . . . . ? O5 Cd1 N1 C1 49.4(3) . . . . ? N1 Cd1 N5 C19 117.3(3) . . . . ? N4 Cd1 N5 C19 -62.0(3) 6_566 . . . ? O4 Cd1 N5 C19 33.1(4) . . . . ? O1 Cd1 N5 C19 -147.8(3) . . . . ? O2 Cd1 N5 C19 -153.8(3) . . . . ? O5 Cd1 N5 C19 28.3(3) . . . . ? N1 Cd1 N5 C23 -65.7(3) . . . . ? N4 Cd1 N5 C23 115.0(3) 6_566 . . . ? O4 Cd1 N5 C23 -149.8(3) . . . . ? O1 Cd1 N5 C23 29.2(4) . . . . ? O2 Cd1 N5 C23 23.2(3) . . . . ? O5 Cd1 N5 C23 -154.6(3) . . . . ? Cd1 O1 N7 O3 -178.5(4) . . . . ? Cd1 O1 N7 O2 0.1(4) . . . . ? Cd1 O2 N7 O3 178.6(4) . . . . ? Cd1 O2 N7 O1 -0.1(4) . . . . ? Cd1 O4 N8 O6 173.3(3) . . . . ? Cd1 O4 N8 O5 -7.8(4) . . . . ? Cd1 O5 N8 O6 -174.0(4) . . . . ? Cd1 O5 N8 O4 7.1(4) . . . . ? C6 N2 C1 N1 -171.4(3) . . . . ? C6 N2 C1 C2 7.4(6) . . . . ? C5 N1 C1 N2 176.2(4) . . . . ? Cd1 N1 C1 N2 -20.4(5) . . . . ? C5 N1 C1 C2 -2.7(6) . . . . ? Cd1 N1 C1 C2 160.8(3) . . . . ? N2 C1 C2 C3 -176.6(4) . . . . ? N1 C1 C2 C3 2.2(6) . . . . ? C1 C2 C3 C4 0.1(8) . . . . ? C2 C3 C4 C5 -1.7(8) . . . . ? C1 N1 C5 C4 1.0(6) . . . . ? Cd1 N1 C5 C4 -164.1(4) . . . . ? C3 C4 C5 N1 1.2(8) . . . . ? C1 N2 C6 C7 -79.2(5) . . . . ? N2 C6 C7 C8 165.3(4) . . . . ? N2 C6 C7 C12 -16.0(6) . . . . ? C12 C7 C8 C9 -0.9(8) . . . . ? C6 C7 C8 C9 177.9(5) . . . . ? C7 C8 C9 C10 -0.6(9) . . . . ? C8 C9 C10 C11 0.8(8) . . . . ? C8 C9 C10 C13 175.9(5) . . . . ? C9 C10 C11 C12 0.4(7) . . . . ? C13 C10 C11 C12 -174.8(4) . . . . ? C8 C7 C12 C11 2.1(7) . . . . ? C6 C7 C12 C11 -176.6(4) . . . . ? C10 C11 C12 C7 -1.9(7) . . . . ? C14 N3 C13 C10 75.8(5) . . . . ? C11 C10 C13 N3 -161.3(4) . . . . ? C9 C10 C13 N3 23.7(7) . . . . ? C18 N4 C14 N3 -175.7(4) . . . . ? Cd1 N4 C14 N3 13.3(5) 6_565 . . . ? C18 N4 C14 C15 4.0(6) . . . . ? Cd1 N4 C14 C15 -167.1(3) 6_565 . . . ? C13 N3 C14 N4 172.3(3) . . . . ? C13 N3 C14 C15 -7.3(6) . . . . ? N4 C14 C15 C16 -3.7(6) . . . . ? N3 C14 C15 C16 175.9(4) . . . . ? C14 C15 C16 C17 1.1(7) . . . . ? C15 C16 C17 C18 1.0(7) . . . . ? C14 N4 C18 C17 -1.8(7) . . . . ? Cd1 N4 C18 C17 170.1(4) 6_565 . . . ? C16 C17 C18 N4 -0.7(7) . . . . ? C23 N5 C19 N6 175.1(4) . . . . ? Cd1 N5 C19 N6 -8.0(5) . . . . ? C23 N5 C19 C20 -3.1(6) . . . . ? Cd1 N5 C19 C20 173.8(3) . . . . ? C24 N6 C19 N5 -175.0(4) . . . . ? C24 N6 C19 C20 3.2(7) . . . . ? N5 C19 C20 C21 1.8(7) . . . . ? N6 C19 C20 C21 -176.3(4) . . . . ? C19 C20 C21 C22 0.1(8) . . . . ? C20 C21 C22 C23 -0.5(8) . . . . ? C19 N5 C23 C22 2.8(7) . . . . ? Cd1 N5 C23 C22 -174.6(4) . . . . ? C21 C22 C23 N5 -1.0(8) . . . . ? C19 N6 C24 C25 -74.0(6) . . . . ? N6 C24 C25 C26 -33.2(7) . . . . ? N6 C24 C25 C27 149.0(5) . . . . ? C27 C25 C26 C27 -0.6(10) . . . 5_666 ? C24 C25 C26 C27 -178.4(6) . . . 5_666 ? C26 C25 C27 C26 0.6(10) . . . 5_666 ? C24 C25 C27 C26 178.4(6) . . . 5_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O5 0.86 2.26 3.009(5) 146.2 . N3 H3N O2 0.86 2.19 2.959(5) 148.1 6_565 N6 H6N O5 0.86 2.17 2.962(5) 153.7 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.973 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.072 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 786016' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H17 N6 O6 Zn' _chemical_formula_sum 'C18 H17 N6 O6 Zn' _chemical_formula_weight 478.75 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.771(3) _cell_length_b 14.650(3) _cell_length_c 20.312(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.59(3) _cell_angle_gamma 90.00 _cell_volume 4014.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7050 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7758 _exptl_absorpt_correction_T_max 0.8319 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15441 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3529 _reflns_number_gt 2325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-97 _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^)+(0.0755P)^2^+42.2208P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3529 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1473 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Zn1 Zn 0.20923(6) 0.64415(6) 0.28975(4) 0.0459(3) Uani 1 1 d . . . O1 O 0.1201(5) 0.7150(4) 0.2204(3) 0.0814(19) Uani 1 1 d . . . O2 O 0.1881(5) 0.8172(5) 0.2875(3) 0.0708(16)) Uani 1 1 d . . . O3 O 0.0800(6) 0.8549(5) 0.2004(5) 0.118(3) Uani 1 1 d . . . O4 O 0.1517(5) 0.5197(4) 0.2563(3) 0.0702(16) Uani 1 1 d . . . O5 O 0.2220(5) 0.5494(5) 0.1740(3) 0.096(2) Uani 1 1 d . . . O6 O 0.1172(5) 0.4408(4) 0.1640(3) 0.0770(18) Uani 1 1 d . . . N1 N 0.1665(4) 0.6308(4) 0.3781(3) 0.0480(14) Uani 1 1 d . . . N2 N 0.2801(5) 0.6124(5) 0.5560(3) 0.069(2) Uani 1 1 d . . . H2N H 0.2621 0.5987 0.5929 0.083 Uiso 1 1 calc R . . N3 N 0.3564(4) 0.6479(4) 0.3097(3) 0.0440(13) Uani 1 1 d . . . N4 N 0.6687(6) 0.8148(6) 0.3637(4) 0.0564(16) Uani 1 1 d . . . H4N H 0.7052 0.8360 0.3375 0.104 Uiso 1 1 calc R . . N5 N 0.1275(5) 0.7978(5) 0.2357(3) 0.0624(18) Uani 1 1 d . . . N6 N 0.1634(5) 0.5029(4) 0.1974(3) 0.0561(16) Uani 1 1 d . . . C1 C 0.2343(5) 0.6322(5) 0.4359(3) 0.0464(16) Uani 1 1 d . . . H1 H 0.2998 0.6460 0.4345 0.056 Uiso 1 1 calc R . . C2 C 0.2094(6) 0.6134(5) 0.4980(4) 0.0528(18) Uani 1 1 d . . . C3 C 0.1097(6) 0.5959(6) 0.4987(4) 0.063(2) Uani 1 1 d . . . H3 H 0.0898 0.5844 0.5390 0.075 Uiso 1 1 calc R . . C4 C 0.0419(6) 0.5960(6) 0.4393(4) 0.067(2) Uani 1 1 d . . . H4 H -0.0244 0.5842 0.4394 0.080 Uiso 1 1 calc R . . C5 C 0.0706(6) 0.6132(6) 0.3795(4) 0.060(2) Uani 1 1 d . . . H5 H 0.0236 0.6127 0.3396 0.072 Uiso 1 1 calc R . . C6 C 0.3827(6) 0.6329(6) 0.5583(4) 0.063(2) Uani 1 1 d . . . H6A H 0.4151 0.6404 0.6050 0.076 Uiso 1 1 calc R . . H6B H 0.3865 0.6910 0.5361 0.076 Uiso 1 1 calc R . . C7 C 0.4405(6) 0.5631(5) 0.5268(3) 0.0529(18) Uani 1 1 d . . . C8 C 0.4048(6) 0.4777(5) 0.5058(4) 0.059(2) Uani 1 1 d . . . H8 H 0.3408 0.4615 0.5093 0.071 Uiso 1 1 calc R . . C9 C 0.5366(6) 0.5845(5) 0.5204(4) 0.060(2) Uani 1 1 d . . . H9 H 0.5624 0.6418 0.5339 0.072 Uiso 1 1 calc R . . C10 C 0.4093(5) 0.7254(5) 0.3195(3) 0.0435(16) Uani 1 1 d . . . H10 H 0.3754 0.7807 0.3154 0.052 Uiso 1 1 calc R . . C11 C 0.5128(5) 0.7271(5) 0.3356(3) 0.0424(15) Uani 1 1 d . . . C12 C 0.5613(5) 0.6434(5) 0.3410(3) 0.0476(17) Uani 1 1 d . . . H12 H 0.6302 0.6411 0.3517 0.057 Uiso 1 1 calc R . . C13 C 0.5072(6) 0.5641(5) 0.3305(3) 0.0507(17) Uani 1 1 d . . . H13 H 0.5395 0.5080 0.3337 0.061 Uiso 1 1 calc R . . C14 C 0.4044(6) 0.5676(5) 0.3150(3) 0.0489(17) Uani 1 1 d . . . H14 H 0.3682 0.5136 0.3081 0.059 Uiso 1 1 calc R . . C15 C 0.5619(4) 0.8085(4) 0.3444(3) 0.0410(15) Uani 1 1 d . . . H15 H 0.5251 0.8622 0.3379 0.049 Uiso 1 1 calc R . . C16 C 0.7108(5) 0.7806(5) 0.4344(3) 0.0468(17) Uani 1 1 d . . . C17 C 0.6726(6) 0.8100(6) 0.4884(4) 0.0576(19) Uani 1 1 d . . . H17 H 0.6197 0.8507 0.4813 0.069 Uiso 1 1 calc R . . C18 C 0.7112(6) 0.7800(6) 0.5534(4) 0.0563(19) Uani 1 1 d . . . H18 H 0.6842 0.8011 0.5890 0.068 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 Zn1 0.0418(5) 0.0537(6) 0.0405(5) 0.0021(4) 0.0042(3) -0.0045(4) O1 0.105(5) 0.051(4) 0.077(4) -0.004(3) -0.010(4) -0.004(3) O2 0.083(5) 0.071(4) 0.058(7) 0.010(5) 0.018(3) -0.000(3) O3 0.111(6) 0.072(4) 0.146(7) 0.034(5) -0.031(5) 0.008(4) O4 0.090(4) 0.074(4) 0.051(3) 0.000(3) 0.023(3) -0.005(3) O5 0.095(5) 0.108(5) 0.087(5) 0.007(4) 0.027(4) -0.045(4) O6 0.088(5) 0.055(3) 0.078(4) -0.015(3) -0.007(3) -0.010(3) N1 0.037(3) 0.056(4) 0.049(3) 0.002(3) 0.006(3) -0.001(3) N2 0.067(5) 0.099(5) 0.039(3) 0.009(3) 0.005(3) 0.003(4) N3 0.044(3) 0.044(3) 0.044(3) -0.003(3) 0.010(2) -0.003(3) N4 0.058(4) 0.042(4) 0.060(4) 0.013(3) 0.008(3) -0.000(3) N5 0.054(4) 0.058(4) 0.066(4) 0.011(4) -0.010(3) 0.004(3) N6 0.053(4) 0.049(4) 0.063(4) 0.006(3) 0.003(3) -0.004(3) C1 0.042(4) 0.056(4) 0.039(3) 0.003(3) 0.002(3) -0.002(3) C2 0.055(5) 0.058(4) 0.046(4) 0.006(3) 0.011(3) 0.007(4) C3 0.065(5) 0.078(6) 0.051(4) 0.004(4) 0.025(4) -0.002(4) C4 0.044(5) 0.092(6) 0.070(5) 0.005(5) 0.024(4) -0.004(4) C5 0.048(5) 0.077(5) 0.052(4) -0.003(4) 0.002(3) -0.006(4) C6 0.069(6) 0.063(5) 0.047(4) 0.003(4) -0.012(4) -0.002(4) C7 0.056(5) 0.054(4) 0.043(4) 0.004(3) -0.004(3) -0.001(4) C8 0.054(5) 0.053(4) 0.065(5) -0.002(4) -0.001(4) -0.010(4) C9 0.067(6) 0.048(4) 0.058(5) -0.007(4) -0.006(4) -0.012(4) C10 0.042(4) 0.044(4) 0.044(4) -0.006(3) 0.008(3) 0.005(3) C11 0.041(4) 0.053(4) 0.033(3) -0.001(3) 0.008(3) 0.003(3) C12 0.039(4) 0.059(4) 0.041(3) -0.002(3) -0.003(3) 0.006(3) C13 0.055(5) 0.051(4) 0.044(4) 0.003(3) 0.004(3) 0.007(4) C14 0.056(5) 0.040(4) 0.050(4) 0.001(3) 0.010(3) -0.002(3) C15 0.023(3) 0.039(3) 0.057(4) -0.001(3) -0.001(3) -0.003(3) C16 0.033(4) 0.058(4) 0.048(4) 0.001(3) 0.003(3) -0.004(3) C17 0.047(4) 0.065(5) 0.062(5) -0.004(4) 0.014(4) 0.012(4) C18 0.051(5) 0.073(5) 0.044(4) -0.013(4) 0.009(3) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.968(6) . ? Zn1 N3 1.986(6) . ? Zn1 N1 2.007(6) . ? Zn1 O4 2.049(6) . ? O1 N5 1.251(8) . ? O2 N5 1.238(8) . ? O3 N5 1.206(9) . ? O4 N6 1.262(8) . ? O5 N6 1.223(8) . ? O6 N6 1.233(8) . ? N1 C1 1.346(8) . ? N1 C5 1.351(9) . ? N2 C2 1.369(9) . ? N2 C6 1.436(11) . ? N2 H2N 0.8600 . ? N3 C10 1.342(8) . ? N3 C14 1.343(9) . ? N4 C15 1.448(9) . ? N4 C16 1.523(10) . ? N4 H4N 0.8600 . ? C1 C2 1.399(10) . ? C1 H1 0.9300 . ? C2 C3 1.399(11) . ? C3 C4 1.370(11) . ? C3 H3 0.9300 . ? C4 C5 1.375(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.515(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.380(10) . ? C7 C9 1.392(11) . ? C8 C9 1.392(11) 5_666 ? C8 H8 0.9300 . ? C9 C8 1.392(11) 5_666 ? C9 H9 0.9300 . ? C10 C11 1.397(9) . ? C10 H10 0.9300 . ? C11 C15 1.365(9) . ? C11 C12 1.390(9) . ? C12 C13 1.373(10) . ? C12 H12 0.9300 . ? C13 C14 1.389(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.376(10) . ? C16 C18 1.377(10) 7_666 ? C17 C18 1.392(10) . ? C17 H17 0.9300 . ? C18 C16 1.377(10) 7_666 ? 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 O1 Zn1 N3 126.5(3) . . ? O1 Zn1 N1 116.0(3) . . ? N3 Zn1 N1 106.9(2) . . ? O1 Zn1 O4 95.0(2) . . ? N3 Zn1 O4 113.8(2) . . ? N1 Zn1 O4 92.7(2) . . ? N5 O1 Zn1 109.0(5) . . ? N6 O4 Zn1 111.9(5) . . ? C1 N1 C5 119.6(6) . . ? C1 N1 Zn1 120.1(5) . . ? C5 N1 Zn1 120.1(5) . . ? C2 N2 C6 123.5(7) . . ? C2 N2 H2N 118.3 . . ? C6 N2 H2N 118.3 . . ? C10 N3 C14 119.0(6) . . ? C10 N3 Zn1 123.7(5) . . ? C14 N3 Zn1 117.2(5) . . ? C15 N4 C16 114.0(6) . . ? C15 N4 H4N 123.0 . . ? C16 N4 H4N 123.0 . . ? O3 N5 O2 122.5(8) . . ? O3 N5 O1 121.3(7) . . ? O2 N5 O1 116.2(7) . . ? O5 N6 O6 120.4(7) . . ? O5 N6 O4 118.6(7) . . ? O6 N6 O4 121.0(7) . . ? N1 C1 C2 122.1(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? N2 C2 C3 121.2(7) . . ? N2 C2 C1 121.1(7) . . ? C3 C2 C1 117.7(7) . . ? C4 C3 C2 119.2(7) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 120.6(7) . . ? N1 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? N2 C6 C7 116.2(7) . . ? N2 C6 H6A 108.2 . . ? C7 C6 H6A 108.2 . . ? N2 C6 H6B 108.2 . . ? C7 C6 H6B 108.2 . . ? H6A C6 H6B 107.4 . . ? C8 C7 C9 117.5(7) . . ? C8 C7 C6 123.9(8) . . ? C9 C7 C6 118.6(7) . . ? C7 C8 C9 121.0(8) . 5_666 ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 5_666 . ? C7 C9 C8 121.5(7) . 5_666 ? C7 C9 H9 119.2 . . ? C8 C9 H9 119.2 5_666 . ? N3 C10 C11 123.2(6) . . ? N3 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C15 C11 C12 122.9(6) . . ? C15 C11 C10 120.0(6) . . ? C12 C11 C10 117.0(6) . . ? C13 C12 C11 119.8(7) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.0(7) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? N3 C14 C13 120.9(7) . . ? N3 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C11 C15 N4 122.7(7) . . ? C11 C15 H15 118.6 . . ? N4 C15 H15 118.6 . . ? C17 C16 C18 117.9(7) . 7_666 ? C17 C16 N4 121.0(7) . . ? C18 C16 N4 121.1(7) 7_666 . ? C16 C17 C18 121.5(7) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C16 C18 C17 120.6(7) 7_666 . ? C16 C18 H18 119.7 7_666 . ? C17 C18 H18 119.7 . . ? 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 N3 Zn1 O1 N5 -66.7(7) . . . . ? N1 Zn1 O1 N5 73.1(6) . . . . ? O4 Zn1 O1 N5 168.6(6) . . . . ? O1 Zn1 O4 N6 62.4(5) . . . . ? N3 Zn1 O4 N6 -71.4(5) . . . . ? N1 Zn1 O4 N6 178.8(5) . . . . ? O1 Zn1 N1 C1 -143.0(5) . . . . ? N3 Zn1 N1 C1 4.2(6) . . . . ? O4 Zn1 N1 C1 120.1(6) . . . . ? O1 Zn1 N1 C5 42.3(7) . . . . ? N3 Zn1 N1 C5 -170.4(6) . . . . ? O4 Zn1 N1 C5 -54.6(6) . . . . ? O1 Zn1 N3 C10 50.1(6) . . . . ? N1 Zn1 N3 C10 -92.6(5) . . . . ? O4 Zn1 N3 C10 166.6(5) . . . . ? O1 Zn1 N3 C14 -131.4(5) . . . . ? N1 Zn1 N3 C14 85.9(5) . . . . ? O4 Zn1 N3 C14 -14.9(6) . . . . ? Zn1 O1 N5 O3 179.7(8) . . . . ? Zn1 O1 N5 O2 1.8(10) . . . . ? Zn1 O4 N6 O5 14.8(9) . . . . ? Zn1 O4 N6 O6 -165.4(5) . . . . ? C5 N1 C1 C2 1.7(11) . . . . ? Zn1 N1 C1 C2 -173.0(5) . . . . ? C6 N2 C2 C3 -177.8(8) . . . . ? C6 N2 C2 C1 2.1(12) . . . . ? N1 C1 C2 N2 178.0(7) . . . . ? N1 C1 C2 C3 -2.1(11) . . . . ? N2 C2 C3 C4 -178.8(8) . . . . ? C1 C2 C3 C4 1.3(12) . . . . ? C2 C3 C4 C5 -0.2(14) . . . . ? C1 N1 C5 C4 -0.5(12) . . . . ? Zn1 N1 C5 C4 174.2(7) . . . . ? C3 C4 C5 N1 -0.3(14) . . . . ? C2 N2 C6 C7 -69.9(10) . . . . ? N2 C6 C7 C8 -10.0(11) . . . . ? N2 C6 C7 C9 172.3(6) . . . . ? C9 C7 C8 C9 0.3(12) . . . 5_666 ? C6 C7 C8 C9 -177.4(7) . . . 5_666 ? C8 C7 C9 C8 -0.3(12) . . . 5_666 ? C6 C7 C9 C8 177.5(7) . . . 5_666 ? C14 N3 C10 C11 -0.5(10) . . . . ? Zn1 N3 C10 C11 178.0(5) . . . . ? N3 C10 C11 C15 179.6(6) . . . . ? N3 C10 C11 C12 0.4(10) . . . . ? C15 C11 C12 C13 -179.1(7) . . . . ? C10 C11 C12 C13 0.1(10) . . . . ? C11 C12 C13 C14 -0.4(10) . . . . ? C10 N3 C14 C13 0.2(10) . . . . ? Zn1 N3 C14 C13 -178.4(5) . . . . ? C12 C13 C14 N3 0.3(10) . . . . ? C12 C11 C15 N4 -3.3(11) . . . . ? C10 C11 C15 N4 177.6(6) . . . . ? C16 N4 C15 C11 -67.1(10) . . . . ? C15 N4 C16 C17 -49.8(11) . . . . ? C15 N4 C16 C18 130.8(8) . . . 7_666 ? C18 C16 C17 C18 0.3(13) 7_666 . . . ? N4 C16 C17 C18 -179.2(7) . . . . ? C16 C17 C18 C16 -0.3(13) . . . 7_666 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.831 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.131 # Attachment '5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 786017' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Cd N10 O6' _chemical_formula_sum 'C36 H36 Cd N10 O6' _chemical_formula_weight 817.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 23.105(5) _cell_length_b 12.069(2) _cell_length_c 12.498(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3485.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27618 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8304 _exptl_absorpt_correction_T_max 0.8802 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32698 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7935 _reflns_number_gt 7142 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0368P)^2^+0.1590P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.338(13) _refine_ls_number_reflns 7935 _refine_ls_number_parameters 479 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.119406(5) 0.220312(11) 0.215969(17) 0.03801(5) Uani 1 1 d . . . O1 O 0.10209(9) 0.42405(15) 0.24619(13) 0.0587(5) Uani 1 1 d . . . O2 O 0.10174(9) 0.4927(2) 0.08793(15) 0.0715(6) Uani 1 1 d . . . O3 O 0.11750(9) 0.59815(15) 0.2221(4) 0.0738(6) Uani 1 1 d . . . O4 O 0.09878(14) 0.0149(2) 0.2422(2) 0.0730(6) Uani 1 1 d . . . O5 O 0.17703(14) 0.0119(3) 0.1672(2) 0.1361(14) Uani 1 1 d . . . O6 O 0.13629(13) -0.13992(15) 0.2185(4) 0.1023(8) Uani 1 1 d . . . N1 N 0.18361(9) 0.22680(17) 0.36138(16) 0.0413(4) Uani 1 1 d . . . N2 N 0.31766(8) 0.08516(17) 0.43569(15) 0.0486(5) Uani 1 1 d . . . H2N H 0.3464 0.0994 0.4772 0.058 Uiso 1 1 calc R . . N3 N 0.45707(10) 0.1244(2) -0.07868(17) 0.0669(7) Uani 1 1 d . . . H3N H 0.4335 0.1311 -0.1315 0.080 Uiso 1 1 calc R . . N4 N 0.56230(9) 0.29468(17) 0.06382(16) 0.0414(5) Uani 1 1 d . . . N5 N 0.04353(9) 0.21775(16) 0.34465(17) 0.0394(5) Uani 1 1 d . . . N6 N 0.01113(9) 0.09504(19) 0.60700(15) 0.0532(5) Uani 1 1 d . . . H6N H -0.0098 0.1143 0.6608 0.064 Uiso 1 1 calc R . . N7 N 0.28231(9) 0.1714(2) 0.88193(16) 0.0527(5) Uani 1 1 d . . . H7N H 0.3075 0.1958 0.8370 0.063 Uiso 1 1 calc R . . N8 N 0.19894(8) 0.27369(17) 1.10898(15) 0.0409(4) Uani 1 1 d . . . N9 N 0.10698(8) 0.50515(18) 0.18585(14) 0.0439(5) Uani 1 1 d . . . N10 N 0.13838(9) -0.03974(15) 0.2098(3) 0.0735(6) Uani 1 1 d . . . C1 C 0.22909(9) 0.1576(2) 0.35978(16) 0.0396(4) Uani 1 1 d . . . H1 H 0.2323 0.1081 0.3031 0.047 Uiso 1 1 calc R . . C2 C 0.27161(9) 0.1562(2) 0.43851(16) 0.0396(5) Uani 1 1 d . . . C3 C 0.26611(12) 0.2333(2) 0.5220(2) 0.0463(6) Uani 1 1 d . . . H3 H 0.2937 0.2365 0.5761 0.056 Uiso 1 1 calc R . . C4 C 0.21933(12) 0.3040(2) 0.52258(18) 0.0508(6) Uani 1 1 d . . . H4 H 0.2151 0.3556 0.5774 0.061 Uiso 1 1 calc R . . C5 C 0.17849(11) 0.2984(2) 0.44153(18) 0.0464(5) Uani 1 1 d . . . H5 H 0.1468 0.3458 0.4433 0.056 Uiso 1 1 calc R . . C6 C 0.32184(10) -0.0118(2) 0.3685(2) 0.0529(6) Uani 1 1 d . . . H6A H 0.2831 -0.0331 0.3467 0.063 Uiso 1 1 calc R . . H6B H 0.3376 -0.0721 0.4107 0.063 Uiso 1 1 calc R . . C7 C 0.35862(10) 0.0016(2) 0.26923(19) 0.0464(5) Uani 1 1 d . . . C8 C 0.35016(10) 0.0866(2) 0.1973(2) 0.0637(8) Uani 1 1 d . . . H8 H 0.3220 0.1397 0.2111 0.076 Uiso 1 1 calc R . . C9 C 0.38288(11) 0.0941(3) 0.1047(2) 0.0625(7) Uani 1 1 d . . . H9 H 0.3760 0.1519 0.0572 0.075 Uiso 1 1 calc R . . C10 C 0.42537(10) 0.0176(2) 0.08172(19) 0.0491(5) Uani 1 1 d . . . C11 C 0.43514(13) -0.0645(3) 0.1558(2) 0.0680(8) Uani 1 1 d . . . H11 H 0.4644 -0.1159 0.1434 0.082 Uiso 1 1 calc R . . C12 C 0.40253(13) -0.0724(2) 0.2483(2) 0.0613(7) Uani 1 1 d . . . H12 H 0.4104 -0.1286 0.2971 0.074 Uiso 1 1 calc R . . C13 C 0.45873(12) 0.0208(3) -0.0224(2) 0.0632(7) Uani 1 1 d . . . H13A H 0.4988 0.0027 -0.0075 0.076 Uiso 1 1 calc R . . H13B H 0.4436 -0.0364 -0.0692 0.076 Uiso 1 1 calc R . . C14 C 0.52651(10) 0.2115(2) 0.03816(18) 0.0432(5) Uani 1 1 d . . . H14 H 0.5252 0.1499 0.0829 0.052 Uiso 1 1 calc R . . C15 C 0.49110(11) 0.2125(2) -0.05247(18) 0.0499(6) Uani 1 1 d . . . C16 C 0.49226(12) 0.3087(3) -0.11459(19) 0.0596(8) Uani 1 1 d . . . H16 H 0.4679 0.3153 -0.1735 0.072 Uiso 1 1 calc R . . C17 C 0.52899(12) 0.3929(3) -0.0888(2) 0.0612(7) Uani 1 1 d . . . H17 H 0.5304 0.4563 -0.1312 0.073 Uiso 1 1 calc R . . C18 C 0.56431(11) 0.3842(2) 0.00052(19) 0.0490(6) Uani 1 1 d . . . H18 H 0.5898 0.4414 0.0168 0.059 Uiso 1 1 calc R . . C19 C 0.04867(10) 0.15784(19) 0.43419(17) 0.0395(5) Uani 1 1 d . . . H19 H 0.0819 0.1156 0.4439 0.047 Uiso 1 1 calc R . . C20 C 0.00609(10) 0.1559(2) 0.51412(17) 0.0402(5) Uani 1 1 d . . . C21 C -0.04258(10) 0.2227(2) 0.4979(2) 0.0488(6) Uani 1 1 d . . . H21 H -0.0714 0.2270 0.5498 0.059 Uiso 1 1 calc R . . C22 C -0.04741(11) 0.2820(2) 0.4045(2) 0.0523(6) Uani 1 1 d . . . H22 H -0.0803 0.3245 0.3919 0.063 Uiso 1 1 calc R . . C23 C -0.00389(10) 0.2789(2) 0.3297(2) 0.0464(5) Uani 1 1 d . . . H23 H -0.0076 0.3203 0.2673 0.056 Uiso 1 1 calc R . . C24 C 0.04926(11) 0.0007(2) 0.6200(2) 0.0542(6) Uani 1 1 d . . . H24A H 0.0621 -0.0231 0.5498 0.065 Uiso 1 1 calc R . . H24B H 0.0273 -0.0597 0.6511 0.065 Uiso 1 1 calc R . . C25 C 0.10199(9) 0.0215(2) 0.68890(16) 0.0417(5) Uani 1 1 d . . . C26 C 0.13044(10) 0.1219(2) 0.69109(17) 0.0464(6) Uani 1 1 d . . . H26 H 0.1158 0.1810 0.6518 0.056 Uiso 1 1 calc R . . C27 C 0.18034(10) 0.1360(2) 0.75067(18) 0.0467(5) Uani 1 1 d . . . H27 H 0.1989 0.2044 0.7502 0.056 Uiso 1 1 calc R . . C28 C 0.20310(10) 0.0509(2) 0.81070(17) 0.0440(5) Uani 1 1 d . . . C29 C 0.17359(11) -0.0489(2) 0.81188(19) 0.0517(6) Uani 1 1 d . . . H29 H 0.1872 -0.1068 0.8540 0.062 Uiso 1 1 calc R . . C30 C 0.12398(10) -0.0636(2) 0.7511(2) 0.0516(6) Uani 1 1 d . . . H30 H 0.1052 -0.1317 0.7521 0.062 Uiso 1 1 calc R . . C31 C 0.26067(10) 0.0610(2) 0.87008(19) 0.0533(6) Uani 1 1 d . . . H31A H 0.2561 0.0289 0.9407 0.064 Uiso 1 1 calc R . . H31B H 0.2894 0.0175 0.8323 0.064 Uiso 1 1 calc R . . C32 C 0.21712(10) 0.21093(18) 1.02687(17) 0.0378(5) Uani 1 1 d . . . H32 H 0.1974 0.1455 1.0122 0.045 Uiso 1 1 calc R . . C33 C 0.26400(10) 0.2390(2) 0.96276(18) 0.0383(5) Uani 1 1 d . . . C34 C 0.29160(10) 0.3395(2) 0.98298(18) 0.0459(5) Uani 1 1 d . . . H34 H 0.3227 0.3622 0.9410 0.055 Uiso 1 1 calc R . . C35 C 0.27231(10) 0.4044(2) 1.06571(19) 0.0491(5) Uani 1 1 d . . . H35 H 0.2900 0.4721 1.0799 0.059 Uiso 1 1 calc R . . C36 C 0.22679(9) 0.3689(2) 1.12738(18) 0.0467(5) Uani 1 1 d . . . H36 H 0.2148 0.4129 1.1843 0.056 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 0.03157(6) 0.05127(8) 0.03120(7) -0.00137(9) 0.00024(9) 0.00357(5) O1 0.0778(11) 0.0487(10) 0.0496(10) 0.0058(7) 0.0200(8) 0.0095(9) O2 0.0793(12) 0.0914(15) 0.0439(10) 0.0043(10) 0.0036(10) -0.0271(12) O3 0.0989(14) 0.0515(9) 0.0710(13) -0.0151(16) 0.0086(14) -0.0124(9) O4 0.0992(13) 0.0508(10) 0.0703(13) -0.0146(16) 0.0094(13) -0.0118(9) O5 0.142(2) 0.186(3) 0.0806(16) 0.0075(18) 0.0027(16) -0.111(3) O6 0.155(2) 0.0465(10) 0.1056(17) -0.006(2) 0.011(3) 0.0104(12) N1 0.0364(10) 0.0525(12) 0.0348(9) 0.0023(8) 0.0005(8) 0.0029(8) N2 0.0379(9) 0.0621(13) 0.0458(10) 0.0071(9) -0.0075(8) 0.0016(9) N3 0.0540(12) 0.109(2) 0.0376(10) -0.0104(12) -0.0103(9) -0.0169(13) N4 0.0370(11) 0.0519(12) 0.0353(10) 0.0014(8) -0.0003(9) 0.0036(8) N5 0.0356(11) 0.0416(11) 0.0411(10) 0.0000(8) 0.0020(9) 0.0002(8) N6 0.0455(10) 0.0767(15) 0.0374(9) 0.0075(9) 0.0029(8) 0.0015(10) N7 0.0446(10) 0.0711(15) 0.0425(10) -0.0174(10) 0.0090(9) 0.0006(10) N8 0.0358(10) 0.0552(12) 0.0318(9) -0.0102(8) -0.0007(8) 0.0023(8) N9 0.0385(9) 0.0520(12) 0.0413(11) 0.0003(8) 0.0080(7) -0.0020(8) N10 0.0991(14) 0.0518(9) 0.0717(13) -0.0158(16) 0.0081(14) -0.0119(9) C1 0.0351(10) 0.0493(13) 0.0343(10) -0.0003(9) -0.0004(8) 0.0007(9) C2 0.0324(10) 0.0477(13) 0.0385(10) 0.0095(9) 0.0006(8) -0.0087(9) C3 0.0483(14) 0.0561(15) 0.0344(12) 0.0027(11) -0.0090(11) -0.0137(11) C4 0.0619(15) 0.0525(14) 0.0380(11) -0.0057(10) 0.0006(11) -0.0054(11) C5 0.0499(13) 0.0465(13) 0.0428(11) -0.0019(9) 0.0044(10) 0.0042(10) C6 0.0437(12) 0.0532(15) 0.0617(15) 0.0146(12) 0.0015(11) 0.0021(10) C7 0.0389(10) 0.0466(13) 0.0537(13) 0.0017(10) -0.0061(10) -0.0010(10) C8 0.0466(12) 0.0771(17) 0.067(2) 0.0266(15) 0.0145(13) 0.0235(11) C9 0.0503(14) 0.082(2) 0.0553(15) 0.0202(14) 0.0038(11) 0.0117(12) C10 0.0421(11) 0.0569(14) 0.0483(12) -0.0156(11) -0.0042(10) -0.0071(10) C11 0.0647(17) 0.0569(17) 0.082(2) -0.0081(14) 0.0096(15) 0.0198(14) C12 0.0617(15) 0.0483(15) 0.0740(19) 0.0089(12) 0.0027(13) 0.0128(12) C13 0.0553(14) 0.081(2) 0.0528(14) -0.0292(14) 0.0033(12) -0.0187(14) C14 0.0405(12) 0.0556(15) 0.0333(10) 0.0014(9) -0.0029(10) 0.0047(10) C15 0.0356(12) 0.0834(19) 0.0307(10) -0.0066(11) 0.0029(9) 0.0051(11) C16 0.0507(16) 0.099(2) 0.0286(11) 0.0079(13) 0.0004(11) 0.0146(15) C17 0.0671(17) 0.076(2) 0.0406(12) 0.0175(13) 0.0125(13) 0.0191(15) C18 0.0478(13) 0.0554(15) 0.0438(11) 0.0074(11) 0.0103(10) 0.0039(11) C19 0.0323(10) 0.0448(13) 0.0415(11) -0.0010(10) -0.0001(9) 0.0041(9) C20 0.0355(12) 0.0485(14) 0.0366(11) -0.0035(10) 0.0002(9) -0.0053(9) C21 0.0370(12) 0.0648(16) 0.0446(12) -0.0095(11) 0.0087(10) 0.0056(10) C22 0.0391(12) 0.0611(16) 0.0568(14) 0.0018(12) 0.0001(11) 0.0154(10) C23 0.0430(12) 0.0515(14) 0.0449(12) 0.0022(9) -0.0016(10) 0.0047(10) C24 0.0572(14) 0.0547(14) 0.0508(13) 0.0095(12) -0.0056(11) -0.0086(12) C25 0.0418(10) 0.0478(12) 0.0355(12) 0.0027(8) 0.0056(8) -0.0017(9) C26 0.0555(13) 0.0443(11) 0.0395(14) 0.0045(8) -0.0042(9) 0.0029(10) C27 0.0535(12) 0.0431(12) 0.0436(11) -0.0038(9) -0.0001(9) -0.0033(10) C28 0.0479(11) 0.0493(13) 0.0348(10) -0.0110(9) 0.0031(9) 0.0114(10) C29 0.0567(14) 0.0516(14) 0.0467(12) 0.0073(11) -0.0010(11) 0.0116(11) C30 0.0540(13) 0.0494(13) 0.0514(13) 0.0105(10) 0.0030(10) -0.0047(11) C31 0.0505(13) 0.0639(16) 0.0456(12) -0.0191(11) -0.0044(11) 0.0183(12) C32 0.0375(11) 0.0410(12) 0.0348(10) -0.0074(8) 0.0006(9) 0.0014(8) C33 0.0326(10) 0.0519(13) 0.0303(10) -0.0014(9) -0.0024(9) 0.0021(9) C34 0.0353(11) 0.0596(15) 0.0428(11) 0.0037(10) -0.0052(9) -0.0067(10) C35 0.0473(12) 0.0453(13) 0.0545(13) -0.0060(10) -0.0113(11) -0.0095(10) C36 0.0417(11) 0.0545(14) 0.0438(11) -0.0195(10) -0.0054(10) 0.0017(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 N4 2.321(2) 4_455 ? Cd1 N1 2.347(2) . ? Cd1 N8 2.362(2) 1_554 ? Cd1 N5 2.379(2) . ? Cd1 O1 2.5197(19) . ? Cd1 O4 2.546(3) . ? O1 N9 1.241(3) . ? O2 N9 1.239(3) . ? O3 N9 1.234(3) . ? O4 N10 1.198(3) . ? O5 N10 1.213(3) . ? O6 N10 1.215(3) . ? N1 C5 1.328(3) . ? N1 C1 1.342(3) . ? N2 C2 1.367(3) . ? N2 C6 1.444(3) . ? N2 H2N 0.8600 . ? N3 C15 1.363(4) . ? N3 C13 1.434(4) . ? N3 H3N 0.8600 . ? N4 C18 1.340(3) . ? N4 C14 1.340(3) . ? N4 Cd1 2.321(2) 4 ? N5 C23 1.334(3) . ? N5 C19 1.338(3) . ? N6 C20 1.379(3) . ? N6 C24 1.449(3) . ? N6 H6N 0.8600 . ? N7 C33 1.366(3) . ? N7 C31 1.431(4) . ? N7 H7N 0.8600 . ? N8 C36 1.337(3) . ? N8 C32 1.343(3) . ? N8 Cd1 2.362(2) 1_556 ? C1 C2 1.391(3) . ? C1 H1 0.9300 . ? C2 C3 1.404(3) . ? C3 C4 1.378(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.513(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.377(4) . ? C7 C8 1.378(3) . ? C8 C9 1.385(4) . ? C8 H8 0.9300 . ? C9 C10 1.378(4) . ? C9 H9 0.9300 . ? C10 C11 1.375(4) . ? C10 C13 1.513(4) . ? C11 C12 1.383(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.397(3) . ? C14 H14 0.9300 . ? C15 C16 1.397(4) . ? C16 C17 1.362(4) . ? C16 H16 0.9300 . ? C17 C18 1.387(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.402(3) . ? C19 H19 0.9300 . ? C20 C21 1.398(3) . ? C21 C22 1.374(4) . ? C21 H21 0.9300 . ? C22 C23 1.374(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.513(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.378(3) . ? C25 C30 1.385(3) . ? C26 C27 1.383(3) . ? C26 H26 0.9300 . ? C27 C28 1.377(3) . ? C27 H27 0.9300 . ? C28 C29 1.384(4) . ? C28 C31 1.528(3) . ? C29 C30 1.387(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.389(3) . ? C32 H32 0.9300 . ? C33 C34 1.393(4) . ? C34 C35 1.372(3) . ? C34 H34 0.9300 . ? C35 C36 1.373(3) . ? C35 H35 0.9300 . ? C36 H36 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 N4 Cd1 N1 174.86(7) 4_455 . ? N4 Cd1 N8 89.98(7) 4_455 1_554 ? N1 Cd1 N8 86.42(7) . 1_554 ? N4 Cd1 N5 97.70(8) 4_455 . ? N1 Cd1 N5 86.72(8) . . ? N8 Cd1 N5 163.61(7) 1_554 . ? N4 Cd1 O1 96.24(7) 4_455 . ? N1 Cd1 O1 87.23(7) . . ? N8 Cd1 O1 86.69(6) 1_554 . ? N5 Cd1 O1 78.13(6) . . ? N4 Cd1 O4 85.59(8) 4_455 . ? N1 Cd1 O4 92.94(8) . . ? N8 Cd1 O4 118.95(8) 1_554 . ? N5 Cd1 O4 76.26(8) . . ? O1 Cd1 O4 154.34(8) . . ? N9 O1 Cd1 131.63(14) . . ? N10 O4 Cd1 110.5(2) . . ? C5 N1 C1 119.1(2) . . ? C5 N1 Cd1 123.32(16) . . ? C1 N1 Cd1 117.55(15) . . ? C2 N2 C6 125.13(19) . . ? C2 N2 H2N 117.4 . . ? C6 N2 H2N 117.4 . . ? C15 N3 C13 123.2(2) . . ? C15 N3 H3N 118.4 . . ? C13 N3 H3N 118.4 . . ? C18 N4 C14 119.0(2) . . ? C18 N4 Cd1 121.79(17) . 4 ? C14 N4 Cd1 119.23(15) . 4 ? C23 N5 C19 119.3(2) . . ? C23 N5 Cd1 120.21(16) . . ? C19 N5 Cd1 120.47(15) . . ? C20 N6 C24 124.4(2) . . ? C20 N6 H6N 117.8 . . ? C24 N6 H6N 117.8 . . ? C33 N7 C31 121.6(2) . . ? C33 N7 H7N 119.2 . . ? C31 N7 H7N 119.2 . . ? C36 N8 C32 117.8(2) . . ? C36 N8 Cd1 120.76(14) . 1_556 ? C32 N8 Cd1 121.48(16) . 1_556 ? O3 N9 O2 119.4(3) . . ? O3 N9 O1 120.8(3) . . ? O2 N9 O1 119.7(2) . . ? O4 N10 O5 115.3(3) . . ? O4 N10 O6 119.2(3) . . ? O5 N10 O6 125.5(3) . . ? N1 C1 C2 123.4(2) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? N2 C2 C1 122.7(2) . . ? N2 C2 C3 120.3(2) . . ? C1 C2 C3 117.0(2) . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? N2 C6 C7 115.3(2) . . ? N2 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? N2 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C12 C7 C8 117.6(2) . . ? C12 C7 C6 120.0(2) . . ? C8 C7 C6 122.4(2) . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 121.3(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 117.3(2) . . ? C11 C10 C13 120.9(2) . . ? C9 C10 C13 121.7(3) . . ? C10 C11 C12 121.5(2) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C7 C12 C11 121.0(2) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? N3 C13 C10 115.5(2) . . ? N3 C13 H13A 108.4 . . ? C10 C13 H13A 108.4 . . ? N3 C13 H13B 108.4 . . ? C10 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? N4 C14 C15 123.3(2) . . ? N4 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? N3 C15 C16 121.8(2) . . ? N3 C15 C14 121.7(3) . . ? C16 C15 C14 116.6(2) . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N4 C18 C17 121.1(3) . . ? N4 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? N5 C19 C20 122.9(2) . . ? N5 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? N6 C20 C21 119.8(2) . . ? N6 C20 C19 123.3(2) . . ? C21 C20 C19 116.9(2) . . ? C22 C21 C20 119.2(2) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.3(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? N5 C23 C22 121.4(2) . . ? N5 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? N6 C24 C25 115.0(2) . . ? N6 C24 H24A 108.5 . . ? C25 C24 H24A 108.5 . . ? N6 C24 H24B 108.5 . . ? C25 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C26 C25 C30 117.8(2) . . ? C26 C25 C24 122.8(2) . . ? C30 C25 C24 119.5(2) . . ? C25 C26 C27 121.1(2) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 121.3(2) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 117.9(2) . . ? C27 C28 C31 122.5(2) . . ? C29 C28 C31 119.6(2) . . ? C28 C29 C30 120.9(2) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 121.0(2) . . ? C25 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? N7 C31 C28 115.4(2) . . ? N7 C31 H31A 108.4 . . ? C28 C31 H31A 108.4 . . ? N7 C31 H31B 108.4 . . ? C28 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? N8 C32 C33 123.2(2) . . ? N8 C32 H32 118.4 . . ? C33 C32 H32 118.4 . . ? N7 C33 C32 121.5(2) . . ? N7 C33 C34 120.8(2) . . ? C32 C33 C34 117.7(2) . . ? C35 C34 C33 119.0(2) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C34 C35 C36 119.6(2) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? N8 C36 C35 122.7(2) . . ? N8 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? 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 N4 Cd1 O1 N9 -52.1(2) 4_455 . . . ? N1 Cd1 O1 N9 124.1(2) . . . . ? N8 Cd1 O1 N9 37.5(2) 1_554 . . . ? N5 Cd1 O1 N9 -148.7(2) . . . . ? O4 Cd1 O1 N9 -144.9(2) . . . . ? N4 Cd1 O4 N10 98.7(2) 4_455 . . . ? N1 Cd1 O4 N10 -76.3(2) . . . . ? N8 Cd1 O4 N10 11.2(3) 1_554 . . . ? N5 Cd1 O4 N10 -162.2(3) . . . . ? O1 Cd1 O4 N10 -166.1(2) . . . . ? N8 Cd1 N1 C5 115.06(19) 1_554 . . . ? N5 Cd1 N1 C5 -50.1(2) . . . . ? O1 Cd1 N1 C5 28.20(19) . . . . ? O4 Cd1 N1 C5 -126.1(2) . . . . ? N8 Cd1 N1 C1 -61.74(18) 1_554 . . . ? N5 Cd1 N1 C1 133.15(17) . . . . ? O1 Cd1 N1 C1 -148.59(17) . . . . ? O4 Cd1 N1 C1 57.10(18) . . . . ? N4 Cd1 N5 C23 -44.99(17) 4_455 . . . ? N1 Cd1 N5 C23 137.67(18) . . . . ? N8 Cd1 N5 C23 72.3(3) 1_554 . . . ? O1 Cd1 N5 C23 49.81(17) . . . . ? O4 Cd1 N5 C23 -128.50(19) . . . . ? N4 Cd1 N5 C19 137.10(18) 4_455 . . . ? N1 Cd1 N5 C19 -40.25(18) . . . . ? N8 Cd1 N5 C19 -105.6(3) 1_554 . . . ? O1 Cd1 N5 C19 -128.11(18) . . . . ? O4 Cd1 N5 C19 53.58(18) . . . . ? Cd1 O1 N9 O3 -152.75(18) . . . . ? Cd1 O1 N9 O2 26.6(3) . . . . ? Cd1 O4 N10 O5 -4.0(4) . . . . ? Cd1 O4 N10 O6 178.2(3) . . . . ? C5 N1 C1 C2 0.3(3) . . . . ? Cd1 N1 C1 C2 177.27(16) . . . . ? C6 N2 C2 C1 -15.1(3) . . . . ? C6 N2 C2 C3 166.1(2) . . . . ? N1 C1 C2 N2 180.0(2) . . . . ? N1 C1 C2 C3 -1.2(3) . . . . ? N2 C2 C3 C4 179.8(2) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C1 N1 C5 C4 0.8(4) . . . . ? Cd1 N1 C5 C4 -175.99(18) . . . . ? C3 C4 C5 N1 -0.9(4) . . . . ? C2 N2 C6 C7 101.3(3) . . . . ? N2 C6 C7 C12 127.1(3) . . . . ? N2 C6 C7 C8 -52.8(3) . . . . ? C12 C7 C8 C9 2.9(4) . . . . ? C6 C7 C8 C9 -177.2(3) . . . . ? C7 C8 C9 C10 -0.6(5) . . . . ? C8 C9 C10 C11 -1.9(4) . . . . ? C8 C9 C10 C13 176.0(3) . . . . ? C9 C10 C11 C12 2.0(4) . . . . ? C13 C10 C11 C12 -176.0(3) . . . . ? C8 C7 C12 C11 -2.9(4) . . . . ? C6 C7 C12 C11 177.3(2) . . . . ? C10 C11 C12 C7 0.4(5) . . . . ? C15 N3 C13 C10 80.2(3) . . . . ? C11 C10 C13 N3 -163.2(2) . . . . ? C9 C10 C13 N3 19.0(3) . . . . ? C18 N4 C14 C15 0.5(3) . . . . ? Cd1 N4 C14 C15 -179.17(18) 4 . . . ? C13 N3 C15 C16 174.2(2) . . . . ? C13 N3 C15 C14 -6.0(4) . . . . ? N4 C14 C15 N3 177.1(2) . . . . ? N4 C14 C15 C16 -3.1(4) . . . . ? N3 C15 C16 C17 -176.7(3) . . . . ? C14 C15 C16 C17 3.5(4) . . . . ? C15 C16 C17 C18 -1.5(4) . . . . ? C14 N4 C18 C17 1.7(3) . . . . ? Cd1 N4 C18 C17 -178.58(18) 4 . . . ? C16 C17 C18 N4 -1.3(4) . . . . ? C23 N5 C19 C20 0.1(3) . . . . ? Cd1 N5 C19 C20 178.04(17) . . . . ? C24 N6 C20 C21 161.1(2) . . . . ? C24 N6 C20 C19 -21.0(4) . . . . ? N5 C19 C20 N6 -179.6(2) . . . . ? N5 C19 C20 C21 -1.6(3) . . . . ? N6 C20 C21 C22 -179.3(2) . . . . ? C19 C20 C21 C22 2.7(4) . . . . ? C20 C21 C22 C23 -2.4(4) . . . . ? C19 N5 C23 C22 0.3(3) . . . . ? Cd1 N5 C23 C22 -177.64(19) . . . . ? C21 C22 C23 N5 0.9(4) . . . . ? C20 N6 C24 C25 107.1(3) . . . . ? N6 C24 C25 C26 -34.6(3) . . . . ? N6 C24 C25 C30 146.9(2) . . . . ? C30 C25 C26 C27 2.1(3) . . . . ? C24 C25 C26 C27 -176.5(2) . . . . ? C25 C26 C27 C28 -0.6(3) . . . . ? C26 C27 C28 C29 -1.7(3) . . . . ? C26 C27 C28 C31 175.0(2) . . . . ? C27 C28 C29 C30 2.5(3) . . . . ? C31 C28 C29 C30 -174.2(2) . . . . ? C26 C25 C30 C29 -1.2(4) . . . . ? C24 C25 C30 C29 177.4(2) . . . . ? C28 C29 C30 C25 -1.1(4) . . . . ? C33 N7 C31 C28 83.5(3) . . . . ? C27 C28 C31 N7 15.0(3) . . . . ? C29 C28 C31 N7 -168.4(2) . . . . ? C36 N8 C32 C33 1.7(3) . . . . ? Cd1 N8 C32 C33 -179.42(16) 1_556 . . . ? C31 N7 C33 C32 -10.4(3) . . . . ? C31 N7 C33 C34 170.2(2) . . . . ? N8 C32 C33 N7 178.0(2) . . . . ? N8 C32 C33 C34 -2.6(3) . . . . ? N7 C33 C34 C35 -179.3(2) . . . . ? C32 C33 C34 C35 1.3(3) . . . . ? C33 C34 C35 C36 0.7(4) . . . . ? C32 N8 C36 C35 0.5(3) . . . . ? Cd1 N8 C36 C35 -178.40(18) 1_556 . . . ? C34 C35 C36 N8 -1.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O2 0.86 2.24 2.887(3) 132.2 3_545 N3 H3N O3 0.86 2.21 3.045(4) 162.8 3_544 N7 H7N O3 0.86 2.54 3.183(4) 132.2 3_545 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.746 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.051 # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 786018' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 N8 Zn, 2(Cl O4)' _chemical_formula_sum 'C36 H36 Cl2 N8 O8 Zn' _chemical_formula_weight 845.00 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4c2' _symmetry_space_group_name_Hall 'P -4 -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x, -y, z+1/2' '-x, y, z+1/2' 'y, x, -z+1/2' '-y, -x, -z+1/2' _cell_length_a 10.7613(15) _cell_length_b 10.7613(15) _cell_length_c 16.348(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1893.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 10117 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8617 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14112 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1672 _reflns_number_gt 1307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.1119P)^2^+0.7750P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 1672 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Zn1 Zn 1.0000 1.0000 1.0000 0.0537(4) Uani 1 4 d S . . Cl1 Cl 0.65920(16) 0.34080(16) 0.7500 0.0866(7) Uani 1 2 d S . . N1 N 0.8657(5) 0.9361(4) 0.9264(3) 0.0581(11) Uani 1 1 d . . . N2 N 0.6957(5) 0.6499(4) 0.8953(4) 0.0725(14) Uani 1 1 d . . . H2N H 0.6431 0.6194 0.8611 0.087 Uiso 1 1 calc R . . C1 C 0.8224(5) 0.8203(5) 0.9371(3) 0.0559(11) Uani 1 1 d . . . H1 H 0.8512 0.7742 0.9813 0.067 Uiso 1 1 calc R . . C2 C 0.7357(5) 0.7663(5) 0.8842(3) 0.0566(13) Uani 1 1 d . . . C3 C 0.6918(6) 0.8399(6) 0.8214(3) 0.0651(16) Uani 1 1 d . . . H3 H 0.6324 0.8085 0.7856 0.078 Uiso 1 1 calc R . . C4 C 0.7348(6) 0.9588(7) 0.8112(3) 0.0694(17) Uani 1 1 d . . . H4 H 0.7041 1.0080 0.7690 0.083 Uiso 1 1 calc R . . C5 C 0.8222(7) 1.0046(5) 0.8627(4) 0.0691(17) Uani 1 1 d . . . H5 H 0.8529 1.0844 0.8544 0.083 Uiso 1 1 calc R . . C6 C 0.7389(6) 0.5709(6) 0.9646(5) 0.0766(18) Uani 1 1 d . . . H6A H 0.6897 0.4954 0.9655 0.092 Uiso 1 1 calc R . . H6B H 0.7232 0.6148 1.0154 0.092 Uiso 1 1 calc R . . C7 C 0.8742(6) 0.5357(5) 0.9616(4) 0.0600(13) Uani 1 1 d . . . C8 C 0.9364(7) 0.5179(6) 1.0320(4) 0.0693(17) Uani 1 1 d . . . H8 H 0.8955 0.5292 1.0816 0.083 Uiso 1 1 calc R . . C9 C 0.9378(7) 0.5172(6) 0.8860(4) 0.0691(16) Uani 1 1 d . . . H9 H 0.8959 0.5280 0.8368 0.083 Uiso 1 1 calc R . . O1 O 0.5549(10) 0.2957(13) 0.7657(13) 0.291(9) Uani 1 1 d . A . O2 O 0.7493(18) 0.2956(19) 0.8067(13) 0.207(10) Uani 0.58(2) 1 d P A 1 O2' O 0.616(4) 0.390(3) 0.8282(10) 0.215(18) Uani 0.42(2) 1 d P A 2 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 Zn1 0.0480(4) 0.0480(4) 0.0652(7) 0.000 0.000 0.000 Cl1 0.0667(8) 0.0667(8) 0.1265(18) 0.0010(11) 0.0010(11) -0.0201(9) N1 0.058(3) 0.047(2) 0.069(3) 0.002(2) 0.001(2) 0.0055(19) N2 0.058(3) 0.052(3) 0.107(4) -0.007(3) -0.014(3) -0.001(2) C1 0.052(3) 0.045(3) 0.071(3) 0.003(2) -0.004(3) 0.0073(19) C2 0.046(3) 0.056(3) 0.067(3) -0.013(2) -0.003(2) 0.004(2) C3 0.059(3) 0.080(4) 0.056(3) -0.013(3) -0.009(3) 0.005(3) C4 0.079(4) 0.075(4) 0.054(3) 0.005(3) -0.015(3) 0.008(3) C5 0.083(5) 0.053(3) 0.072(4) 0.011(3) 0.001(3) 0.004(3) C6 0.062(4) 0.059(3) 0.109(5) 0.010(3) 0.011(3) -0.009(3) C7 0.065(3) 0.040(3) 0.074(3) 0.000(3) 0.006(3) -0.005(3) C8 0.086(5) 0.055(3) 0.067(3) 0.002(3) 0.015(4) 0.003(3) C9 0.065(4) 0.072(4) 0.070(4) -0.006(3) 0.002(3) 0.006(3) O1 0.154(9) 0.268(13) 0.45(2) 0.019(18) 0.104(15) -0.119(9) O2 0.157(16) 0.187(19) 0.28(2) 0.041(15) -0.093(15) 0.022(13) O2' 0.36(5) 0.19(3) 0.098(11) -0.066(14) 0.007(17) -0.07(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 Zn1 N1 2.002(5) . ? Zn1 N1 2.002(5) 4_757 ? Zn1 N1 2.002(5) 3_577 ? Zn1 N1 2.002(5) 2_775 ? Cl1 O1 1.249(8) 8_666 ? Cl1 O1 1.249(8) . ? Cl1 O2 1.427(14) 8_666 ? Cl1 O2 1.427(14) . ? Cl1 O2' 1.460(19) . ? Cl1 O2' 1.460(19) 8_666 ? N1 C1 1.341(7) . ? N1 C5 1.360(8) . ? N2 C2 1.337(8) . ? N2 C6 1.491(8) . ? N2 H2N 0.8600 . ? C1 C2 1.398(7) . ? C1 H1 0.9300 . ? C2 C3 1.380(8) . ? C3 C4 1.371(9) . ? C3 H3 0.9300 . ? C4 C5 1.355(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.505(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.345(8) . ? C7 C9 1.427(9) . ? C8 C8 1.422(15) 2_765 ? C8 H8 0.9300 . ? C9 C9 1.390(14) 2_765 ? C9 H9 0.9300 . ? O1 O2' 1.59(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N1 111.15(14) . 4_757 ? N1 Zn1 N1 111.15(14) . 3_577 ? N1 Zn1 N1 106.2(3) 4_757 3_577 ? N1 Zn1 N1 106.2(3) . 2_775 ? N1 Zn1 N1 111.15(14) 4_757 2_775 ? N1 Zn1 N1 111.15(14) 3_577 2_775 ? O1 Cl1 O1 137.7(14) 8_666 . ? O1 Cl1 O2 110.1(13) 8_666 8_666 ? O1 Cl1 O2 100.2(12) . 8_666 ? O1 Cl1 O2 100.2(12) 8_666 . ? O1 Cl1 O2 110.1(13) . . ? O2 Cl1 O2 87.6(19) 8_666 . ? O1 Cl1 O2' 88.6(13) 8_666 . ? O1 Cl1 O2' 71.2(15) . . ? O2 Cl1 O2' 157.6(18) 8_666 . ? O2 Cl1 O2' 76.7(14) . . ? O1 Cl1 O2' 71.2(15) 8_666 8_666 ? O1 Cl1 O2' 88.6(14) . 8_666 ? O2 Cl1 O2' 76.7(14) 8_666 8_666 ? O2 Cl1 O2' 157.6(18) . 8_666 ? O2' Cl1 O2' 122(3) . 8_666 ? C1 N1 C5 118.9(5) . . ? C1 N1 Zn1 119.5(4) . . ? C5 N1 Zn1 121.5(4) . . ? C2 N2 C6 122.5(5) . . ? C2 N2 H2N 118.8 . . ? C6 N2 H2N 118.8 . . ? N1 C1 C2 122.6(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? N2 C2 C3 121.9(5) . . ? N2 C2 C1 121.4(5) . . ? C3 C2 C1 116.7(5) . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 N1 121.2(6) . . ? C4 C5 H5 119.4 . . ? N1 C5 H5 119.4 . . ? N2 C6 C7 114.8(5) . . ? N2 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? N2 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C8 C7 C9 118.8(6) . . ? C8 C7 C6 119.3(6) . . ? C9 C7 C6 121.8(6) . . ? C7 C8 C8 121.2(4) . 2_765 ? C7 C8 H8 119.4 . . ? C8 C8 H8 119.4 2_765 . ? C9 C9 C7 120.0(4) 2_765 . ? C9 C9 H9 120.0 2_765 . ? C7 C9 H9 120.0 . . ? Cl1 O1 O2' 60.6(13) . . ? Cl1 O2' O1 48.2(7) . . ? 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 Zn1 N1 C1 6.7(4) 4_757 . . . ? N1 Zn1 N1 C1 -111.4(5) 3_577 . . . ? N1 Zn1 N1 C1 127.7(5) 2_775 . . . ? N1 Zn1 N1 C5 -169.5(5) 4_757 . . . ? N1 Zn1 N1 C5 72.5(4) 3_577 . . . ? N1 Zn1 N1 C5 -48.5(4) 2_775 . . . ? C5 N1 C1 C2 1.2(9) . . . . ? Zn1 N1 C1 C2 -175.0(4) . . . . ? C6 N2 C2 C3 -177.7(5) . . . . ? C6 N2 C2 C1 0.9(8) . . . . ? N1 C1 C2 N2 178.7(5) . . . . ? N1 C1 C2 C3 -2.6(8) . . . . ? N2 C2 C3 C4 -179.7(6) . . . . ? C1 C2 C3 C4 1.6(8) . . . . ? C2 C3 C4 C5 0.6(9) . . . . ? C3 C4 C5 N1 -2.1(10) . . . . ? C1 N1 C5 C4 1.2(10) . . . . ? Zn1 N1 C5 C4 177.3(5) . . . . ? C2 N2 C6 C7 -66.5(8) . . . . ? N2 C6 C7 C8 149.4(6) . . . . ? N2 C6 C7 C9 -32.5(8) . . . . ? C9 C7 C8 C8 0.5(12) . . . 2_765 ? C6 C7 C8 C8 178.7(7) . . . 2_765 ? C8 C7 C9 C9 -0.8(11) . . . 2_765 ? C6 C7 C9 C9 -179.0(7) . . . 2_765 ? O1 Cl1 O1 O2' -65.6(15) 8_666 . . . ? O2 Cl1 O1 O2' 159(2) 8_666 . . . ? O2 Cl1 O1 O2' 67.4(16) . . . . ? O2' Cl1 O1 O2' -125(3) 8_666 . . . ? O1 Cl1 O2' O1 142.2(15) 8_666 . . . ? O2 Cl1 O2' O1 -70(5) 8_666 . . . ? O2 Cl1 O2' O1 -117.0(15) . . . . ? O2' Cl1 O2' O1 75.7(12) 8_666 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O2' 0.86 2.54 3.12(3) 125.6 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.366 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.073 # Attachment '7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 786019' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H54 Cd N12, 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C54 H58 Cd Cl2 N12 O10' _chemical_formula_weight 1218.42 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' Cl Cl 0.1484 0.1585 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.998(2) _cell_length_b 11.800(2) _cell_length_c 12.793(3) _cell_angle_alpha 70.09(3) _cell_angle_beta 66.74(3) _cell_angle_gamma 73.43(3) _cell_volume 1412.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8648 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8934 _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10730 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4890 _reflns_number_gt 3480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.1217P)^2^+0.9976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.014(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4890 _refine_ls_number_parameters 396 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.1768 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.082 _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 0.0000 0.5000 0.5000 0.0611(3) Uani 1 2 d S . . Cl1 Cl 0.3104(3) 0.0651(2) 0.8562(2) 0.1162(8) Uani 1 1 d D . . O1W O 0.9058(11) 0.1888(8) 0.0539(9) 0.193(4) Uani 1 1 d . . . H1W1 H 0.8452 0.1515 0.0632 0.232 Uiso 1 1 d R . . H1W2 H 0.9821 0.1464 0.0271 0.232 Uiso 1 1 d R . . O1 O 0.2076(14) 0.1094(16) 0.8050(15) 0.254(12) Uani 0.641(13) 1 d PD A 1 O2 O 0.3040(16) 0.1358(12) 0.9289(11) 0.199(9) Uani 0.641(13) 1 d PD A 1 O3 O 0.4402(11) 0.0800(11) 0.7558(9) 0.178(7) Uani 0.641(13) 1 d PD A 1 O4 O 0.3227(13) -0.0611(6) 0.9111(10) 0.150(6) Uani 0.641(13) 1 d PD A 1 O1' O 0.324(3) -0.013(2) 0.7855(19) 0.234(19) Uani 0.359(13) 1 d PD A 2 O2' O 0.295(2) 0.1895(10) 0.7919(17) 0.157(11) Uani 0.359(13) 1 d PD A 2 O3' O 0.4188(16) 0.031(2) 0.9003(19) 0.190(14) Uani 0.359(13) 1 d PD A 2 O4' O 0.1852(14) 0.047(2) 0.9568(14) 0.197(15) Uani 0.359(13) 1 d PD A 2 N1 N 0.2007(5) 0.3531(5) 0.4394(4) 0.0669(13) Uani 1 1 d . . . N2 N 0.3676(7) 0.2105(6) 0.1921(5) 0.0895(18) Uani 1 1 d . . . H2N H 0.4039 0.1376 0.1843 0.107 Uiso 1 1 calc R . . N3 N 0.1139(5) 0.6638(5) 0.3590(4) 0.0677(13) Uani 1 1 d . . . N4 N 0.4654(6) 0.7026(6) 0.2091(5) 0.0859(17) Uani 1 1 d . . . H4N H 0.5094 0.7604 0.1621 0.103 Uiso 1 1 calc R . . N5 N -0.0711(5) 0.4797(5) 0.3526(4) 0.0627(12) Uani 1 1 d . . . N6 N -0.1733(8) 0.2420(6) 0.2954(7) 0.104(2) Uani 1 1 d . . . H6N H -0.1766 0.2272 0.2353 0.125 Uiso 1 1 calc R . . C1 C 0.2373(6) 0.3313(6) 0.3336(5) 0.0701(16) Uani 1 1 d . . . H1 H 0.1948 0.3838 0.2804 0.084 Uiso 1 1 calc R . . C2 C 0.3357(6) 0.2338(6) 0.3000(5) 0.0710(17) Uani 1 1 d . . . C3 C 0.3975(7) 0.1577(7) 0.3818(7) 0.0811(19) Uani 1 1 d . . . H3 H 0.4644 0.0916 0.3634 0.097 Uiso 1 1 calc R . . C4 C 0.3594(7) 0.1804(7) 0.4897(6) 0.0825(19) Uani 1 1 d . . . H4 H 0.4004 0.1298 0.5446 0.099 Uiso 1 1 calc R . . C5 C 0.2605(6) 0.2780(6) 0.5163(5) 0.0723(17) Uani 1 1 d . . . H5 H 0.2347 0.2921 0.5900 0.087 Uiso 1 1 calc R . . C6 C 0.3418(9) 0.3043(8) 0.0935(6) 0.092(2) Uani 1 1 d . . . H6A H 0.2469 0.3394 0.1163 0.111 Uiso 1 1 calc R . . H6B H 0.3611 0.2670 0.0305 0.111 Uiso 1 1 calc R . . C7 C 0.4223(7) 0.4063(7) 0.0465(5) 0.0795(19) Uani 1 1 d . . . C8 C 0.3628(8) 0.5279(8) 0.0277(6) 0.088(2) Uani 1 1 d . . . H8 H 0.2701 0.5486 0.0450 0.105 Uiso 1 1 calc R . . C9 C 0.5612(8) 0.3804(8) 0.0165(6) 0.089(2) Uani 1 1 d . . . H9 H 0.6044 0.2992 0.0264 0.107 Uiso 1 1 calc R . . C10 C 0.2480(6) 0.6402(6) 0.3217(5) 0.0622(14) Uani 1 1 d . . . H10 H 0.2903 0.5614 0.3492 0.075 Uiso 1 1 calc R . . C11 C 0.3288(6) 0.7277(6) 0.2433(5) 0.0667(15) Uani 1 1 d . . . C12 C 0.2623(8) 0.8435(7) 0.2009(6) 0.0814(19) Uani 1 1 d . . . H12 H 0.3113 0.9043 0.1479 0.098 Uiso 1 1 calc R . . C13 C 0.1262(9) 0.8676(7) 0.2369(7) 0.091(2) Uani 1 1 d . . . H13 H 0.0815 0.9444 0.2072 0.109 Uiso 1 1 calc R . . C14 C 0.0532(7) 0.7770(7) 0.3186(7) 0.0825(19) Uani 1 1 d . . . H14 H -0.0402 0.7958 0.3456 0.099 Uiso 1 1 calc R . . C15 C 0.5387(7) 0.5851(8) 0.2476(6) 0.083(2) Uani 1 1 d . . . H15A H 0.6336 0.5862 0.2049 0.100 Uiso 1 1 calc R . . H15B H 0.5136 0.5257 0.2263 0.100 Uiso 1 1 calc R . . C16 C 0.5185(6) 0.5415(7) 0.3793(6) 0.0740(18) Uani 1 1 d . . . C17 C 0.5000(7) 0.6213(8) 0.4424(6) 0.0824(19) Uani 1 1 d . . . H17 H 0.5000 0.7040 0.4046 0.099 Uiso 1 1 calc R . . C18 C 0.5187(7) 0.4191(8) 0.4375(6) 0.084(2) Uani 1 1 d . . . H18 H 0.5316 0.3631 0.3960 0.101 Uiso 1 1 calc R . . C19 C -0.1126(6) 0.3769(6) 0.3681(6) 0.0711(16) Uani 1 1 d . . . H19 H -0.1293 0.3217 0.4420 0.085 Uiso 1 1 calc R . . C20 C -0.1321(7) 0.3485(7) 0.2797(6) 0.0790(18) Uani 1 1 d . . . C21 C -0.1086(8) 0.4339(8) 0.1697(6) 0.085(2) Uani 1 1 d . . . H21 H -0.1196 0.4190 0.1074 0.102 Uiso 1 1 calc R . . C22 C -0.0688(7) 0.5401(8) 0.1554(6) 0.086(2) Uani 1 1 d . . . H22 H -0.0546 0.5989 0.0835 0.103 Uiso 1 1 calc R . . C23 C -0.0503(7) 0.5589(7) 0.2478(5) 0.0747(17) Uani 1 1 d . . . H23 H -0.0218 0.6306 0.2362 0.090 Uiso 1 1 calc R . . C24 C -0.2107(9) 0.1550(8) 0.4077(9) 0.110(3) Uani 1 1 d . . . H24A H -0.2601 0.1017 0.4029 0.132 Uiso 1 1 calc R . . H24B H -0.2720 0.1993 0.4653 0.132 Uiso 1 1 calc R . . C25 C -0.0996(9) 0.0761(7) 0.4531(8) 0.090(2) Uani 1 1 d . . . C26 C -0.1313(8) -0.0024(8) 0.5640(8) 0.095(2) Uani 1 1 d . . . H26 H -0.2213 -0.0046 0.6088 0.114 Uiso 1 1 calc R . . C27 C 0.0351(9) 0.0770(8) 0.3896(8) 0.099(2) Uani 1 1 d . . . H27 H 0.0604 0.1291 0.3144 0.119 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 0.0547(4) 0.0712(5) 0.0501(4) -0.0098(3) -0.0124(3) -0.0144(3) Cl1 0.145(2) 0.0886(15) 0.0992(16) -0.0012(13) -0.0399(15) -0.0256(14) O1W 0.284(12) 0.158(7) 0.207(9) -0.052(7) -0.118(9) -0.083(8) O1 0.26(2) 0.26(2) 0.26(2) 0.041(19) -0.19(2) -0.05(2) O2 0.25(2) 0.196(16) 0.186(15) -0.125(14) -0.011(13) -0.088(14) O3 0.251(19) 0.152(12) 0.131(11) -0.039(9) -0.023(11) -0.091(12) O4 0.206(15) 0.094(8) 0.122(10) 0.006(7) -0.043(9) -0.040(8) O1' 0.29(4) 0.26(4) 0.19(3) -0.12(3) -0.02(3) -0.10(3) O2' 0.15(2) 0.114(16) 0.133(18) 0.053(14) -0.055(15) -0.009(14) O3' 0.108(17) 0.17(3) 0.21(3) 0.04(2) -0.059(18) 0.001(16) O4' 0.13(2) 0.28(4) 0.111(17) -0.023(19) 0.035(14) -0.06(2) N1 0.059(3) 0.074(3) 0.050(3) -0.011(2) -0.006(2) -0.010(2) N2 0.102(5) 0.084(4) 0.066(3) -0.023(3) -0.007(3) -0.018(3) N3 0.059(3) 0.077(4) 0.064(3) -0.010(3) -0.020(2) -0.016(3) N4 0.073(4) 0.111(5) 0.060(3) 0.004(3) -0.013(3) -0.041(3) N5 0.067(3) 0.069(3) 0.053(3) -0.015(2) -0.024(2) -0.009(2) N6 0.128(6) 0.093(5) 0.120(6) -0.027(4) -0.065(5) -0.029(4) C1 0.059(4) 0.080(4) 0.053(3) -0.011(3) -0.009(3) -0.008(3) C2 0.062(4) 0.076(4) 0.059(3) -0.015(3) 0.001(3) -0.021(3) C3 0.065(4) 0.072(4) 0.083(5) -0.012(4) -0.015(3) 0.000(3) C4 0.071(4) 0.085(5) 0.075(4) -0.009(4) -0.025(3) -0.003(4) C5 0.066(4) 0.086(5) 0.054(3) -0.007(3) -0.017(3) -0.015(3) C6 0.101(6) 0.111(6) 0.060(4) -0.027(4) -0.010(4) -0.029(5) C7 0.080(5) 0.104(6) 0.043(3) -0.012(3) -0.011(3) -0.022(4) C8 0.074(5) 0.109(6) 0.061(4) -0.013(4) -0.013(3) -0.013(4) C9 0.086(5) 0.100(6) 0.065(4) -0.017(4) -0.013(4) -0.015(4) C10 0.061(4) 0.070(4) 0.049(3) -0.003(3) -0.019(3) -0.016(3) C11 0.070(4) 0.080(4) 0.045(3) -0.004(3) -0.016(3) -0.027(3) C12 0.089(5) 0.083(5) 0.063(4) 0.006(4) -0.023(4) -0.036(4) C13 0.109(6) 0.067(4) 0.081(5) 0.007(4) -0.034(4) -0.022(4) C14 0.070(4) 0.084(5) 0.087(5) -0.015(4) -0.029(4) -0.007(4) C15 0.060(4) 0.121(6) 0.054(3) -0.015(4) -0.010(3) -0.018(4) C16 0.051(3) 0.107(6) 0.060(3) -0.015(4) -0.015(3) -0.020(3) C17 0.082(5) 0.097(5) 0.064(4) -0.006(4) -0.021(3) -0.033(4) C18 0.081(5) 0.102(6) 0.073(4) -0.025(4) -0.023(4) -0.023(4) C19 0.074(4) 0.079(4) 0.060(3) -0.013(3) -0.025(3) -0.015(3) C20 0.077(5) 0.089(5) 0.080(5) -0.027(4) -0.032(4) -0.013(4) C21 0.102(6) 0.097(5) 0.067(4) -0.026(4) -0.036(4) -0.015(4) C22 0.087(5) 0.104(6) 0.057(4) -0.015(4) -0.019(3) -0.016(4) C23 0.077(4) 0.087(5) 0.056(4) -0.010(3) -0.021(3) -0.020(3) C24 0.105(7) 0.088(6) 0.144(8) -0.010(6) -0.057(6) -0.030(5) C25 0.093(6) 0.073(5) 0.116(6) -0.020(5) -0.040(5) -0.027(4) C26 0.079(5) 0.083(5) 0.119(7) -0.018(5) -0.026(5) -0.025(4) C27 0.093(6) 0.088(6) 0.107(6) -0.012(5) -0.026(5) -0.027(5) _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 N3 2.405(5) . ? Cd1 N3 2.405(5) 2_566 ? Cd1 N5 2.409(4) 2_566 ? Cd1 N5 2.409(4) . ? Cd1 N1 2.420(5) 2_566 ? Cd1 N1 2.420(5) . ? Cl1 O4 1.406(6) . ? Cl1 O1 1.412(7) . ? Cl1 O2' 1.417(8) . ? Cl1 O3' 1.417(8) . ? Cl1 O2 1.418(7) . ? Cl1 O1' 1.438(8) . ? Cl1 O4' 1.475(8) . ? Cl1 O3 1.504(7) . ? O1W H1W1 0.8501 . ? O1W H1W2 0.8500 . ? N1 C5 1.331(8) . ? N1 C1 1.344(7) . ? N2 C2 1.388(8) . ? N2 C6 1.432(10) . ? N2 H2N 0.8600 . ? N3 C10 1.334(7) . ? N3 C14 1.338(9) . ? N4 C11 1.360(8) . ? N4 C15 1.423(10) . ? N4 H4N 0.8600 . ? N5 C23 1.323(8) . ? N5 C19 1.342(8) . ? N6 C20 1.381(10) . ? N6 C24 1.434(11) . ? N6 H6N 0.8600 . ? C1 C2 1.392(9) . ? C1 H1 0.9300 . ? C2 C3 1.392(10) . ? C3 C4 1.373(10) . ? C3 H3 0.9300 . ? C4 C5 1.373(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.514(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.377(11) . ? C7 C9 1.388(10) . ? C8 C9 1.384(11) 2_665 ? C8 H8 0.9300 . ? C9 C8 1.384(11) 2_665 ? C9 H9 0.9300 . ? C10 C11 1.405(9) . ? C10 H10 0.9300 . ? C11 C12 1.391(10) . ? C12 C13 1.355(11) . ? C12 H12 0.9300 . ? C13 C14 1.395(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.527(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.364(10) . ? C16 C18 1.381(10) . ? C17 C18 1.392(10) 2_666 ? C17 H17 0.9300 . ? C18 C17 1.392(10) 2_666 ? C18 H18 0.9300 . ? C19 C20 1.389(9) . ? C19 H19 0.9300 . ? C20 C21 1.399(10) . ? C21 C22 1.375(11) . ? C21 H21 0.9300 . ? C22 C23 1.372(10) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.497(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.375(12) . ? C25 C27 1.381(11) . ? C26 C27 1.361(11) 2_556 ? C26 H26 0.9300 . ? C27 C26 1.361(11) 2_556 ? C27 H27 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 N3 Cd1 N3 180.000(1) . 2_566 ? N3 Cd1 N5 89.72(17) . 2_566 ? N3 Cd1 N5 90.28(17) 2_566 2_566 ? N3 Cd1 N5 90.28(17) . . ? N3 Cd1 N5 89.72(17) 2_566 . ? N5 Cd1 N5 180.0(2) 2_566 . ? N3 Cd1 N1 90.09(18) . 2_566 ? N3 Cd1 N1 89.91(18) 2_566 2_566 ? N5 Cd1 N1 88.44(17) 2_566 2_566 ? N5 Cd1 N1 91.56(17) . 2_566 ? N3 Cd1 N1 89.91(18) . . ? N3 Cd1 N1 90.09(18) 2_566 . ? N5 Cd1 N1 91.56(17) 2_566 . ? N5 Cd1 N1 88.44(17) . . ? N1 Cd1 N1 180.000(1) 2_566 . ? O4 Cl1 O1 113.2(7) . . ? O4 Cl1 O2' 174.1(10) . . ? O1 Cl1 O2' 62.1(9) . . ? O4 Cl1 O3' 72.2(9) . . ? O1 Cl1 O3' 174.3(10) . . ? O2' Cl1 O3' 112.4(8) . . ? O4 Cl1 O2 113.0(6) . . ? O1 Cl1 O2 113.3(7) . . ? O2' Cl1 O2 72.8(10) . . ? O3' Cl1 O2 64.7(11) . . ? O4 Cl1 O1' 63.9(11) . . ? O1 Cl1 O1' 70.9(12) . . ? O2' Cl1 O1' 110.4(8) . . ? O3' Cl1 O1' 111.2(8) . . ? O2 Cl1 O1' 175.8(12) . . ? O4 Cl1 O4' 73.4(9) . . ? O1 Cl1 O4' 75.5(11) . . ? O2' Cl1 O4' 107.7(7) . . ? O3' Cl1 O4' 108.5(7) . . ? O2 Cl1 O4' 74.7(10) . . ? O1' Cl1 O4' 106.4(8) . . ? O4 Cl1 O3 105.1(6) . . ? O1 Cl1 O3 106.1(6) . . ? O2' Cl1 O3 73.8(9) . . ? O3' Cl1 O3 70.0(10) . . ? O2 Cl1 O3 105.2(6) . . ? O1' Cl1 O3 73.6(10) . . ? O4' Cl1 O3 178.2(10) . . ? H1W1 O1W H1W2 108.5 . . ? C5 N1 C1 118.8(6) . . ? C5 N1 Cd1 120.8(4) . . ? C1 N1 Cd1 119.2(4) . . ? C2 N2 C6 121.9(6) . . ? C2 N2 H2N 119.1 . . ? C6 N2 H2N 119.1 . . ? C10 N3 C14 118.0(6) . . ? C10 N3 Cd1 117.0(4) . . ? C14 N3 Cd1 125.0(5) . . ? C11 N4 C15 123.0(6) . . ? C11 N4 H4N 118.5 . . ? C15 N4 H4N 118.5 . . ? C23 N5 C19 117.8(5) . . ? C23 N5 Cd1 121.3(4) . . ? C19 N5 Cd1 120.0(4) . . ? C20 N6 C24 122.8(7) . . ? C20 N6 H6N 118.6 . . ? C24 N6 H6N 118.6 . . ? N1 C1 C2 123.1(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? N2 C2 C3 121.2(6) . . ? N2 C2 C1 121.9(7) . . ? C3 C2 C1 116.8(6) . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.8(7) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.7(6) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N2 C6 C7 114.6(7) . . ? N2 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? N2 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C9 117.2(7) . . ? C8 C7 C6 122.1(7) . . ? C9 C7 C6 120.7(8) . . ? C7 C8 C9 121.0(7) . 2_665 ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 2_665 . ? C8 C9 C7 121.8(8) 2_665 . ? C8 C9 H9 119.1 2_665 . ? C7 C9 H9 119.1 . . ? N3 C10 C11 123.7(6) . . ? N3 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? N4 C11 C12 120.6(6) . . ? N4 C11 C10 122.8(6) . . ? C12 C11 C10 116.6(6) . . ? C13 C12 C11 119.9(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.8(7) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? N3 C14 C13 121.8(7) . . ? N3 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? N4 C15 C16 115.8(6) . . ? N4 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? N4 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C18 118.2(6) . . ? C17 C16 C15 121.4(7) . . ? C18 C16 C15 120.4(7) . . ? C16 C17 C18 121.0(7) . 2_666 ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 2_666 . ? C16 C18 C17 120.7(7) . 2_666 ? C16 C18 H18 119.6 . . ? C17 C18 H18 119.6 2_666 . ? N5 C19 C20 123.6(6) . . ? N5 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? N6 C20 C19 123.5(7) . . ? N6 C20 C21 119.3(7) . . ? C19 C20 C21 117.2(7) . . ? C22 C21 C20 118.8(6) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C23 C22 C21 119.6(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N5 C23 C22 123.0(7) . . ? N5 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? N6 C24 C25 117.1(8) . . ? N6 C24 H24A 108.0 . . ? C25 C24 H24A 108.0 . . ? N6 C24 H24B 108.0 . . ? C25 C24 H24B 108.0 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C27 117.2(8) . . ? C26 C25 C24 119.1(8) . . ? C27 C25 C24 123.7(9) . . ? C27 C26 C25 122.1(8) 2_556 . ? C27 C26 H26 118.9 2_556 . ? C25 C26 H26 118.9 . . ? C26 C27 C25 120.7(9) 2_556 . ? C26 C27 H27 119.6 2_556 . ? C25 C27 H27 119.6 . . ? 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 N3 Cd1 N1 C5 120.8(5) . . . . ? N3 Cd1 N1 C5 -59.2(5) 2_566 . . . ? N5 Cd1 N1 C5 31.1(5) 2_566 . . . ? N5 Cd1 N1 C5 -148.9(5) . . . . ? N3 Cd1 N1 C1 -71.7(5) . . . . ? N3 Cd1 N1 C1 108.3(5) 2_566 . . . ? N5 Cd1 N1 C1 -161.4(5) 2_566 . . . ? N5 Cd1 N1 C1 18.6(5) . . . . ? N5 Cd1 N3 C10 70.6(4) 2_566 . . . ? N5 Cd1 N3 C10 -109.4(4) . . . . ? N1 Cd1 N3 C10 159.0(4) 2_566 . . . ? N1 Cd1 N3 C10 -21.0(4) . . . . ? N5 Cd1 N3 C14 -107.1(5) 2_566 . . . ? N5 Cd1 N3 C14 72.9(5) . . . . ? N1 Cd1 N3 C14 -18.7(5) 2_566 . . . ? N1 Cd1 N3 C14 161.3(5) . . . . ? N3 Cd1 N5 C23 -7.2(5) . . . . ? N3 Cd1 N5 C23 172.8(5) 2_566 . . . ? N1 Cd1 N5 C23 82.9(5) 2_566 . . . ? N1 Cd1 N5 C23 -97.1(5) . . . . ? N3 Cd1 N5 C19 161.8(5) . . . . ? N3 Cd1 N5 C19 -18.2(5) 2_566 . . . ? N1 Cd1 N5 C19 -108.1(5) 2_566 . . . ? N1 Cd1 N5 C19 71.9(5) . . . . ? C5 N1 C1 C2 -0.3(10) . . . . ? Cd1 N1 C1 C2 -168.0(5) . . . . ? C6 N2 C2 C3 -158.9(7) . . . . ? C6 N2 C2 C1 23.5(10) . . . . ? N1 C1 C2 N2 177.3(6) . . . . ? N1 C1 C2 C3 -0.4(10) . . . . ? N2 C2 C3 C4 -177.2(7) . . . . ? C1 C2 C3 C4 0.5(10) . . . . ? C2 C3 C4 C5 0.0(11) . . . . ? C1 N1 C5 C4 0.9(10) . . . . ? Cd1 N1 C5 C4 168.4(5) . . . . ? C3 C4 C5 N1 -0.7(11) . . . . ? C2 N2 C6 C7 65.3(9) . . . . ? N2 C6 C7 C8 -129.4(7) . . . . ? N2 C6 C7 C9 53.0(9) . . . . ? C9 C7 C8 C9 -1.6(11) . . . 2_665 ? C6 C7 C8 C9 -179.3(7) . . . 2_665 ? C8 C7 C9 C8 1.6(12) . . . 2_665 ? C6 C7 C9 C8 179.3(7) . . . 2_665 ? C14 N3 C10 C11 0.5(9) . . . . ? Cd1 N3 C10 C11 -177.3(4) . . . . ? C15 N4 C11 C12 -178.6(6) . . . . ? C15 N4 C11 C10 1.4(10) . . . . ? N3 C10 C11 N4 178.0(6) . . . . ? N3 C10 C11 C12 -2.0(9) . . . . ? N4 C11 C12 C13 -179.2(7) . . . . ? C10 C11 C12 C13 0.9(10) . . . . ? C11 C12 C13 C14 1.6(11) . . . . ? C10 N3 C14 C13 2.1(10) . . . . ? Cd1 N3 C14 C13 179.8(5) . . . . ? C12 C13 C14 N3 -3.2(12) . . . . ? C11 N4 C15 C16 -64.8(9) . . . . ? N4 C15 C16 C17 -35.2(9) . . . . ? N4 C15 C16 C18 144.9(7) . . . . ? C18 C16 C17 C18 -0.3(11) . . . 2_666 ? C15 C16 C17 C18 179.8(6) . . . 2_666 ? C17 C16 C18 C17 0.3(11) . . . 2_666 ? C15 C16 C18 C17 -179.8(6) . . . 2_666 ? C23 N5 C19 C20 1.3(9) . . . . ? Cd1 N5 C19 C20 -168.0(5) . . . . ? C24 N6 C20 C19 5.4(12) . . . . ? C24 N6 C20 C21 -174.4(8) . . . . ? N5 C19 C20 N6 179.2(7) . . . . ? N5 C19 C20 C21 -1.0(10) . . . . ? N6 C20 C21 C22 179.4(7) . . . . ? C19 C20 C21 C22 -0.4(11) . . . . ? C20 C21 C22 C23 1.4(11) . . . . ? C19 N5 C23 C22 -0.2(10) . . . . ? Cd1 N5 C23 C22 169.0(5) . . . . ? C21 C22 C23 N5 -1.2(11) . . . . ? C20 N6 C24 C25 -74.5(11) . . . . ? N6 C24 C25 C26 175.3(8) . . . . ? N6 C24 C25 C27 -4.8(13) . . . . ? C27 C25 C26 C27 -0.2(14) . . . 2_556 ? C24 C25 C26 C27 179.6(8) . . . 2_556 ? C26 C25 C27 C26 0.2(13) . . . 2_556 ? C24 C25 C27 C26 -179.6(8) . . . 2_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 O4 0.85 2.25 3.098(15) 177.2 2_656 O1W H1W2 O4' 0.85 2.19 3.041(19) 176.1 1_654 N4 H4N O2 0.86 2.38 3.181(14) 155.9 2_666 N6 H6N O1W 0.86 2.29 3.096(11) 156.5 1_455 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.980 _refine_diff_density_min -1.269 _refine_diff_density_rms 0.103