# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lang, Jian-Ping' _publ_contact_author_email jplang@suda.edu.cn _publ_section_title ; Single-crystal to single-crystal transformation of 1D coordination polymers through by photochemical [2+2] cycloaddition reactions ; loop_ _publ_author_name 'Dong Liu' 'Ni-Ya Li' 'Jian-Ping Lang' # Attachment '- JPLangCIF.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 772183' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cd Cl2 N2 O4' _chemical_formula_sum 'C26 H18 Cd Cl2 N2 O4' _chemical_formula_weight 605.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' 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' _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 9.911(2) _cell_length_b 11.151(2) _cell_length_c 11.534(2) _cell_angle_alpha 88.23(3) _cell_angle_beta 71.51(3) _cell_angle_gamma 82.74(3) _cell_volume 1199.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6256 _cell_measurement_theta_min 3.0249 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5423 _exptl_absorpt_correction_T_max 0.8533 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9385 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4206 _reflns_number_gt 3768 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0304P)^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 4206 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.078039(16) 0.110642(15) 0.580445(15) 0.02229(7) Uani 1 1 d . . . Cl1 Cl 0.19615(10) 0.50771(9) 1.17315(8) 0.0640(2) Uani 1 1 d . . . Cl2 Cl 0.45104(8) 0.11309(8) -0.21967(6) 0.0539(2) Uani 1 1 d . . . N1 N -0.09604(19) 0.26053(17) 0.55605(18) 0.0259(5) Uani 1 1 d . . . N2 N -0.77094(19) 0.94524(17) 0.61158(17) 0.0245(5) Uani 1 1 d . . . O1 O 0.02186(18) 0.16301(16) 0.79110(16) 0.0350(4) Uani 1 1 d . . . O2 O 0.17860(18) 0.26283(16) 0.65673(15) 0.0333(4) Uani 1 1 d . . . O3 O 0.10366(17) 0.01744(16) 0.37167(15) 0.0304(4) Uani 1 1 d . . . O4 O 0.23591(17) 0.15472(16) 0.39040(15) 0.0321(4) Uani 1 1 d . . . C1 C -0.2289(2) 0.2748(2) 0.6359(2) 0.0290(6) Uani 1 1 d . . . H1 H -0.2574 0.2131 0.6925 0.035 Uiso 1 1 calc R . . C2 C -0.3256(2) 0.3756(2) 0.6388(2) 0.0279(6) Uani 1 1 d . . . H2 H -0.4177 0.3817 0.6966 0.034 Uiso 1 1 calc R . . C3 C -0.2872(2) 0.4684(2) 0.5564(2) 0.0260(5) Uani 1 1 d . . . C4 C -0.1505(3) 0.4516(2) 0.4712(2) 0.0323(6) Uani 1 1 d . . . H4 H -0.1204 0.5105 0.4116 0.039 Uiso 1 1 calc R . . C5 C -0.0598(3) 0.3483(2) 0.4747(2) 0.0314(6) Uani 1 1 d . . . H5 H 0.0324 0.3390 0.4168 0.038 Uiso 1 1 calc R . . C6 C -0.3779(3) 0.5830(2) 0.5563(2) 0.0310(6) Uani 1 1 d . . . H6 H -0.3428 0.6353 0.4911 0.037 Uiso 1 1 calc R . . C7 C -0.5030(2) 0.6214(2) 0.6370(2) 0.0314(6) Uani 1 1 d . . . H7 H -0.5386 0.5716 0.7042 0.038 Uiso 1 1 calc R . . C8 C -0.5903(2) 0.7355(2) 0.6296(2) 0.0265(5) Uani 1 1 d . . . C9 C -0.7251(3) 0.7653(2) 0.7162(3) 0.0390(7) Uani 1 1 d . . . H9 H -0.7577 0.7142 0.7829 0.047 Uiso 1 1 calc R . . C10 C -0.8101(3) 0.8693(2) 0.7039(2) 0.0358(7) Uani 1 1 d . . . H10 H -0.9000 0.8875 0.7636 0.043 Uiso 1 1 calc R . . C11 C -0.6413(2) 0.9190(2) 0.5297(2) 0.0273(6) Uani 1 1 d . . . H11 H -0.6114 0.9726 0.4647 0.033 Uiso 1 1 calc R . . C12 C -0.5488(2) 0.8172(2) 0.5357(2) 0.0284(6) Uani 1 1 d . . . H12 H -0.4580 0.8034 0.4764 0.034 Uiso 1 1 calc R . . C13 C 0.1076(2) 0.2413(2) 0.7649(2) 0.0263(6) Uani 1 1 d . . . C14 C 0.1259(2) 0.3112(2) 0.8667(2) 0.0264(6) Uani 1 1 d . . . C15 C 0.0501(3) 0.2899(2) 0.9878(2) 0.0327(6) Uani 1 1 d . . . H15 H -0.0159 0.2330 1.0057 0.039 Uiso 1 1 calc R . . C16 C 0.0698(3) 0.3507(3) 1.0818(2) 0.0399(7) Uani 1 1 d . . . H16 H 0.0175 0.3362 1.1634 0.048 Uiso 1 1 calc R . . C17 C 0.1679(3) 0.4336(3) 1.0545(2) 0.0384(7) Uani 1 1 d . . . C18 C 0.2446(3) 0.4568(3) 0.9355(3) 0.0418(7) Uani 1 1 d . . . H18 H 0.3105 0.5137 0.9181 0.050 Uiso 1 1 calc R . . C19 C 0.2230(3) 0.3951(2) 0.8420(2) 0.0342(6) Uani 1 1 d . . . H19 H 0.2750 0.4103 0.7605 0.041 Uiso 1 1 calc R . . C20 C 0.1966(2) 0.0878(2) 0.3254(2) 0.0229(5) Uani 1 1 d . . . C21 C 0.2603(2) 0.0922(2) 0.1889(2) 0.0247(6) Uani 1 1 d . . . C22 C 0.3623(2) 0.1704(2) 0.1371(2) 0.0320(6) Uani 1 1 d . . . H22 H 0.3908 0.2194 0.1878 0.038 Uiso 1 1 calc R . . C23 C 0.4216(3) 0.1760(3) 0.0117(3) 0.0376(7) Uani 1 1 d . . . H23 H 0.4911 0.2280 -0.0233 0.045 Uiso 1 1 calc R . . C24 C 0.3783(3) 0.1050(3) -0.0612(2) 0.0354(7) Uani 1 1 d . . . C25 C 0.2782(3) 0.0269(3) -0.0127(2) 0.0367(6) Uani 1 1 d . . . H25 H 0.2500 -0.0213 -0.0642 0.044 Uiso 1 1 calc R . . C26 C 0.2195(3) 0.0204(2) 0.1135(2) 0.0301(6) Uani 1 1 d . . . H26 H 0.1516 -0.0331 0.1478 0.036 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 0.02366(10) 0.02007(10) 0.02105(11) -0.00058(7) -0.00618(7) 0.00286(7) Cl1 0.0861(6) 0.0653(6) 0.0522(5) -0.0239(4) -0.0391(5) -0.0009(5) Cl2 0.0469(4) 0.0766(6) 0.0218(3) 0.0101(4) 0.0023(3) 0.0160(4) N1 0.0280(11) 0.0204(11) 0.0285(11) 0.0001(9) -0.0101(9) 0.0028(8) N2 0.0247(10) 0.0236(11) 0.0249(11) -0.0005(9) -0.0094(9) 0.0018(8) O1 0.0406(10) 0.0355(10) 0.0287(10) -0.0032(8) -0.0069(8) -0.0142(8) O2 0.0415(10) 0.0368(11) 0.0207(9) -0.0003(8) -0.0064(8) -0.0099(8) O3 0.0294(9) 0.0349(10) 0.0233(9) 0.0033(8) -0.0020(7) -0.0078(7) O4 0.0353(10) 0.0344(10) 0.0253(9) -0.0019(8) -0.0067(8) -0.0065(8) C1 0.0314(13) 0.0219(13) 0.0330(14) 0.0028(11) -0.0102(12) -0.0012(10) C2 0.0234(12) 0.0256(13) 0.0341(14) -0.0014(11) -0.0088(11) -0.0004(10) C3 0.0267(12) 0.0228(13) 0.0310(14) -0.0005(11) -0.0139(11) 0.0010(9) C4 0.0351(14) 0.0280(14) 0.0286(14) 0.0066(11) -0.0057(12) 0.0032(11) C5 0.0307(13) 0.0285(14) 0.0287(14) 0.0006(12) -0.0041(11) 0.0054(10) C6 0.0320(13) 0.0246(13) 0.0347(15) 0.0046(12) -0.0105(12) 0.0018(10) C7 0.0306(13) 0.0240(13) 0.0361(15) 0.0082(12) -0.0079(12) 0.0004(10) C8 0.0255(12) 0.0230(13) 0.0309(14) 0.0020(11) -0.0105(11) 0.0013(9) C9 0.0323(14) 0.0371(16) 0.0363(15) 0.0173(13) 0.0002(12) 0.0047(11) C10 0.0245(13) 0.0397(16) 0.0316(15) 0.0081(13) 0.0026(11) 0.0071(11) C11 0.0268(13) 0.0267(13) 0.0256(13) 0.0048(11) -0.0063(11) 0.0010(10) C12 0.0232(12) 0.0288(14) 0.0281(13) 0.0016(11) -0.0034(10) 0.0030(10) C13 0.0279(12) 0.0237(13) 0.0255(14) -0.0017(11) -0.0083(11) 0.0038(10) C14 0.0287(13) 0.0246(13) 0.0262(14) -0.0022(11) -0.0106(11) 0.0013(10) C15 0.0303(13) 0.0381(15) 0.0280(14) -0.0028(12) -0.0066(11) -0.0038(11) C16 0.0414(16) 0.0525(19) 0.0225(14) -0.0070(13) -0.0076(12) 0.0021(13) C17 0.0508(17) 0.0356(16) 0.0328(16) -0.0122(13) -0.0221(13) 0.0067(13) C18 0.0586(18) 0.0317(16) 0.0439(18) 0.0003(14) -0.0253(15) -0.0139(13) C19 0.0450(15) 0.0307(15) 0.0270(14) 0.0013(12) -0.0106(12) -0.0079(12) C20 0.0197(11) 0.0215(12) 0.0236(13) 0.0024(11) -0.0044(10) 0.0048(9) C21 0.0220(12) 0.0262(13) 0.0230(13) 0.0036(11) -0.0049(10) 0.0012(10) C22 0.0306(13) 0.0342(15) 0.0307(15) 0.0038(12) -0.0090(12) -0.0050(11) C23 0.0292(13) 0.0423(17) 0.0330(15) 0.0130(13) 0.0002(12) -0.0035(12) C24 0.0294(13) 0.0477(17) 0.0199(13) 0.0068(12) -0.0011(11) 0.0098(12) C25 0.0378(14) 0.0422(17) 0.0277(14) -0.0048(12) -0.0091(12) 0.0019(12) C26 0.0294(13) 0.0320(14) 0.0256(13) 0.0010(11) -0.0047(11) -0.0021(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N2 2.3181(19) 1_645 ? Cd1 N1 2.3237(19) . ? Cd1 O4 2.3338(18) . ? Cd1 O3 2.3576(18) 2_556 ? Cd1 O1 2.3878(19) . ? Cd1 O2 2.3924(19) . ? Cd1 O3 2.5774(19) . ? Cd1 C13 2.725(3) . ? Cd1 C20 2.806(2) . ? Cd1 Cd1 3.8722(10) 2_556 ? Cl1 C17 1.734(3) . ? Cl2 C24 1.744(3) . ? N1 C5 1.336(3) . ? N1 C1 1.340(3) . ? N2 C10 1.329(3) . ? N2 C11 1.334(3) . ? N2 Cd1 2.3181(19) 1_465 ? O1 C13 1.258(3) . ? O2 C13 1.255(3) . ? O3 C20 1.263(3) . ? O3 Cd1 2.3576(18) 2_556 ? O4 C20 1.250(3) . ? C1 C2 1.376(3) . ? C1 H1 0.9400 . ? C2 C3 1.388(3) . ? C2 H2 0.9400 . ? C3 C4 1.393(3) . ? C3 C6 1.467(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.321(4) . ? C6 H6 0.9400 . ? C7 C8 1.461(3) . ? C7 H7 0.9400 . ? C8 C12 1.387(3) . ? C8 C9 1.398(3) . ? C9 C10 1.376(3) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.381(3) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.499(4) . ? C14 C19 1.386(3) . ? C14 C15 1.389(3) . ? C15 C16 1.374(4) . ? C15 H15 0.9400 . ? C16 C17 1.382(4) . ? C16 H16 0.9400 . ? C17 C18 1.377(4) . ? C18 C19 1.382(4) . ? C18 H18 0.9400 . ? C19 H19 0.9400 . ? C20 C21 1.501(3) . ? C21 C26 1.381(4) . ? C21 C22 1.396(3) . ? C22 C23 1.381(4) . ? C22 H22 0.9400 . ? C23 C24 1.368(4) . ? C23 H23 0.9400 . ? C24 C25 1.375(4) . ? C25 C26 1.389(4) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N1 172.75(6) 1_645 . ? N2 Cd1 O4 93.77(7) 1_645 . ? N1 Cd1 O4 91.01(7) . . ? N2 Cd1 O3 86.89(7) 1_645 2_556 ? N1 Cd1 O3 85.87(7) . 2_556 ? O4 Cd1 O3 129.41(7) . 2_556 ? N2 Cd1 O1 88.34(7) 1_645 . ? N1 Cd1 O1 91.56(7) . . ? O4 Cd1 O1 139.52(6) . . ? O3 Cd1 O1 91.06(7) 2_556 . ? N2 Cd1 O2 97.60(7) 1_645 . ? N1 Cd1 O2 88.25(7) . . ? O4 Cd1 O2 84.81(7) . . ? O3 Cd1 O2 145.29(6) 2_556 . ? O1 Cd1 O2 54.91(6) . . ? N2 Cd1 O3 88.20(7) 1_645 . ? N1 Cd1 O3 90.36(7) . . ? O4 Cd1 O3 52.79(6) . . ? O3 Cd1 O3 76.72(6) 2_556 . ? O1 Cd1 O3 167.46(5) . . ? O2 Cd1 O3 137.56(5) . . ? N2 Cd1 C13 93.08(7) 1_645 . ? N1 Cd1 C13 90.16(7) . . ? O4 Cd1 C13 112.14(7) . . ? O3 Cd1 C13 118.34(7) 2_556 . ? O1 Cd1 C13 27.49(7) . . ? O2 Cd1 C13 27.43(6) . . ? O3 Cd1 C13 164.93(6) . . ? N2 Cd1 C20 92.18(7) 1_645 . ? N1 Cd1 C20 89.71(7) . . ? O4 Cd1 C20 26.13(6) . . ? O3 Cd1 C20 103.29(7) 2_556 . ? O1 Cd1 C20 165.64(7) . . ? O2 Cd1 C20 110.86(7) . . ? O3 Cd1 C20 26.70(6) . . ? C13 Cd1 C20 138.24(7) . . ? N2 Cd1 Cd1 86.91(5) 1_645 2_556 ? N1 Cd1 Cd1 87.73(5) . 2_556 ? O4 Cd1 Cd1 89.09(5) . 2_556 ? O3 Cd1 Cd1 40.38(4) 2_556 2_556 ? O1 Cd1 Cd1 131.38(5) . 2_556 ? O2 Cd1 Cd1 172.63(4) . 2_556 ? O3 Cd1 Cd1 36.34(4) . 2_556 ? C13 Cd1 Cd1 158.71(5) . 2_556 ? C20 Cd1 Cd1 62.96(6) . 2_556 ? C5 N1 C1 117.2(2) . . ? C5 N1 Cd1 120.29(15) . . ? C1 N1 Cd1 121.48(16) . . ? C10 N2 C11 117.3(2) . . ? C10 N2 Cd1 123.14(15) . 1_465 ? C11 N2 Cd1 119.37(15) . 1_465 ? C13 O1 Cd1 91.35(15) . . ? C13 O2 Cd1 91.20(15) . . ? C20 O3 Cd1 168.44(17) . 2_556 ? C20 O3 Cd1 86.81(15) . . ? Cd1 O3 Cd1 103.28(6) 2_556 . ? C20 O4 Cd1 98.54(13) . . ? N1 C1 C2 123.0(2) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 120.0(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 116.8(2) . . ? C2 C3 C6 124.7(2) . . ? C4 C3 C6 118.5(2) . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.3(2) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C7 C6 C3 127.6(2) . . ? C7 C6 H6 116.2 . . ? C3 C6 H6 116.2 . . ? C6 C7 C8 124.9(2) . . ? C6 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C12 C8 C9 116.3(2) . . ? C12 C8 C7 123.0(2) . . ? C9 C8 C7 120.7(2) . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 123.0(2) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N2 C11 C12 123.3(2) . . ? N2 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C8 119.8(2) . . ? C11 C12 H12 120.1 . . ? C8 C12 H12 120.1 . . ? O2 C13 O1 122.5(2) . . ? O2 C13 C14 118.8(2) . . ? O1 C13 C14 118.7(2) . . ? O2 C13 Cd1 61.37(13) . . ? O1 C13 Cd1 61.16(14) . . ? C14 C13 Cd1 178.87(16) . . ? C19 C14 C15 118.7(2) . . ? C19 C14 C13 120.5(2) . . ? C15 C14 C13 120.8(2) . . ? C16 C15 C14 121.1(2) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.0(2) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 121.4(3) . . ? C18 C17 Cl1 119.6(2) . . ? C16 C17 Cl1 119.1(2) . . ? C17 C18 C19 118.9(3) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C18 C19 C14 121.0(2) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? O4 C20 O3 121.7(2) . . ? O4 C20 C21 119.2(2) . . ? O3 C20 C21 119.1(2) . . ? O4 C20 Cd1 55.33(12) . . ? O3 C20 Cd1 66.49(13) . . ? C21 C20 Cd1 172.94(17) . . ? C26 C21 C22 119.4(2) . . ? C26 C21 C20 121.2(2) . . ? C22 C21 C20 119.4(2) . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.4(2) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 121.7(2) . . ? C23 C24 Cl2 119.6(2) . . ? C25 C24 Cl2 118.7(2) . . ? C24 C25 C26 119.0(3) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 120.3(2) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.373 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.098 #===END #========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 772184' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 Cd Cl2 N2 O4' _chemical_formula_sum 'C26 H18 Cd Cl2 N2 O4' _chemical_formula_weight 605.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' 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' _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 10.196(2) _cell_length_b 10.634(2) _cell_length_c 11.847(2) _cell_angle_alpha 88.76(3) _cell_angle_beta 70.26(3) _cell_angle_gamma 83.15(3) _cell_volume 1200.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5308 _cell_measurement_theta_min 3.0459 _cell_measurement_theta_max 27.4855 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6213 _exptl_absorpt_correction_T_max 0.9439 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9426 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4214 _reflns_number_gt 3636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0320P)^2^+0.3356P] 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 4214 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.09434(2) 0.60834(2) 0.08304(2) 0.02284(9) Uani 1 1 d . . . Cl1 Cl 0.45692(11) 0.61722(11) -0.70640(9) 0.0649(3) Uani 1 1 d . . . Cl2 Cl 0.18833(13) 1.01083(10) 0.67941(9) 0.0611(3) Uani 1 1 d . . . N1 N -0.0719(3) 0.7694(2) 0.0649(2) 0.0244(6) Uani 1 1 d . . . N2 N -0.7506(3) 1.4374(2) 0.1046(2) 0.0236(6) Uani 1 1 d . . . O1 O 0.2406(2) 0.6423(2) -0.1073(2) 0.0335(5) Uani 1 1 d . . . O2 O 0.0867(2) 0.5239(2) -0.1282(2) 0.0364(6) Uani 1 1 d . . . O3 O 0.0368(2) 0.6557(2) 0.2903(2) 0.0347(5) Uani 1 1 d . . . O4 O 0.1925(2) 0.76406(19) 0.16419(19) 0.0294(5) Uani 1 1 d . . . C1 C -0.2049(3) 0.7779(3) 0.1385(3) 0.0252(7) Uani 1 1 d . . . H1 H -0.2276 0.7235 0.2041 0.030 Uiso 1 1 calc R . . C2 C -0.3103(3) 0.8624(3) 0.1231(3) 0.0257(7) Uani 1 1 d . . . H2 H -0.4022 0.8656 0.1780 0.031 Uiso 1 1 calc R . . C3 C -0.2806(3) 0.9433(3) 0.0260(3) 0.0217(6) Uani 1 1 d . . . C4 C -0.1403(3) 0.9382(3) -0.0472(3) 0.0264(7) Uani 1 1 d . . . H4 H -0.1137 0.9940 -0.1114 0.032 Uiso 1 1 calc R . . C5 C -0.0410(3) 0.8510(3) -0.0250(3) 0.0267(7) Uani 1 1 d . . . H5 H 0.0529 0.8489 -0.0755 0.032 Uiso 1 1 calc R . . C6 C -0.3909(3) 1.0205(3) -0.0133(3) 0.0217(6) Uani 1 1 d . . . H6 H -0.3526 1.0931 -0.0618 0.026 Uiso 1 1 calc R . . C7 C -0.5365(3) 1.0623(3) 0.0825(3) 0.0216(6) Uani 1 1 d . . . H7 H -0.5420 1.0253 0.1612 0.026 Uiso 1 1 calc R . . C8 C -0.5936(3) 1.2003(3) 0.0971(3) 0.0213(6) Uani 1 1 d . . . C9 C -0.7173(3) 1.2373(3) 0.1914(3) 0.0282(7) Uani 1 1 d . . . H9 H -0.7500 1.1818 0.2549 0.034 Uiso 1 1 calc R . . C10 C -0.7922(3) 1.3543(3) 0.1923(3) 0.0308(7) Uani 1 1 d . . . H10 H -0.8754 1.3766 0.2570 0.037 Uiso 1 1 calc R . . C11 C -0.6263(3) 1.4068(3) 0.0196(3) 0.0241(7) Uani 1 1 d . . . H11 H -0.5926 1.4665 -0.0397 0.029 Uiso 1 1 calc R . . C12 C -0.5439(3) 1.2920(3) 0.0137(3) 0.0250(7) Uani 1 1 d . . . H12 H -0.4553 1.2765 -0.0462 0.030 Uiso 1 1 calc R . . C13 C 0.1901(3) 0.5853(3) -0.1717(3) 0.0261(7) Uani 1 1 d . . . C14 C 0.2557(3) 0.5925(3) -0.3058(3) 0.0265(7) Uani 1 1 d . . . C15 C 0.3613(3) 0.6699(3) -0.3544(3) 0.0340(8) Uani 1 1 d . . . H15 H 0.3915 0.7168 -0.3033 0.041 Uiso 1 1 calc R . . C16 C 0.4218(4) 0.6780(4) -0.4772(3) 0.0430(9) Uani 1 1 d . . . H16 H 0.4920 0.7313 -0.5101 0.052 Uiso 1 1 calc R . . C17 C 0.3789(4) 0.6080(4) -0.5506(3) 0.0405(9) Uani 1 1 d . . . C18 C 0.2758(4) 0.5299(3) -0.5051(3) 0.0411(9) Uani 1 1 d . . . H18 H 0.2476 0.4819 -0.5567 0.049 Uiso 1 1 calc R . . C19 C 0.2143(3) 0.5230(3) -0.3821(3) 0.0344(8) Uani 1 1 d . . . H19 H 0.1433 0.4704 -0.3501 0.041 Uiso 1 1 calc R . . C20 C 0.1189(3) 0.7388(3) 0.2695(3) 0.0248(7) Uani 1 1 d . . . C21 C 0.1313(3) 0.8099(3) 0.3717(3) 0.0248(7) Uani 1 1 d . . . C22 C 0.0516(3) 0.7878(3) 0.4894(3) 0.0333(8) Uani 1 1 d . . . H22 H -0.0148 0.7297 0.5050 0.040 Uiso 1 1 calc R . . C23 C 0.0686(4) 0.8496(3) 0.5835(3) 0.0394(9) Uani 1 1 d . . . H23 H 0.0147 0.8337 0.6630 0.047 Uiso 1 1 calc R . . C24 C 0.1655(4) 0.9351(3) 0.5595(3) 0.0378(8) Uani 1 1 d . . . C25 C 0.2446(4) 0.9609(3) 0.4448(3) 0.0423(9) Uani 1 1 d . . . H25 H 0.3094 1.0204 0.4298 0.051 Uiso 1 1 calc R . . C26 C 0.2269(4) 0.8969(3) 0.3510(3) 0.0346(8) Uani 1 1 d . . . H26 H 0.2812 0.9131 0.2716 0.042 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 0.02088(13) 0.02089(13) 0.02693(14) 0.00080(9) -0.00984(10) 0.00210(9) Cl1 0.0564(6) 0.0858(8) 0.0276(5) 0.0177(5) 0.0053(5) 0.0267(6) Cl2 0.0837(8) 0.0632(7) 0.0455(6) -0.0181(5) -0.0328(6) -0.0074(6) N1 0.0251(13) 0.0191(13) 0.0334(15) -0.0005(12) -0.0168(12) 0.0017(11) N2 0.0250(13) 0.0201(13) 0.0249(14) -0.0047(11) -0.0089(11) 0.0027(11) O1 0.0324(12) 0.0413(13) 0.0273(12) 0.0001(11) -0.0113(10) -0.0023(11) O2 0.0346(13) 0.0360(13) 0.0319(13) 0.0024(11) -0.0008(11) -0.0102(11) O3 0.0353(13) 0.0341(13) 0.0338(13) 0.0004(11) -0.0078(11) -0.0124(11) O4 0.0321(12) 0.0304(12) 0.0266(12) 0.0010(10) -0.0102(10) -0.0058(10) C1 0.0244(16) 0.0268(16) 0.0235(16) 0.0022(14) -0.0085(13) 0.0018(14) C2 0.0226(15) 0.0270(16) 0.0267(17) 0.0014(14) -0.0083(13) -0.0005(13) C3 0.0212(15) 0.0167(14) 0.0294(17) -0.0009(13) -0.0116(13) -0.0014(12) C4 0.0206(15) 0.0240(16) 0.0323(18) 0.0074(14) -0.0063(14) -0.0032(13) C5 0.0181(15) 0.0252(16) 0.0364(19) 0.0012(15) -0.0096(14) 0.0001(13) C6 0.0196(14) 0.0186(15) 0.0261(17) 0.0038(13) -0.0078(13) 0.0005(12) C7 0.0196(15) 0.0218(15) 0.0238(16) 0.0006(13) -0.0089(13) 0.0013(13) C8 0.0202(15) 0.0216(15) 0.0252(16) 0.0012(13) -0.0125(13) 0.0002(13) C9 0.0294(17) 0.0232(16) 0.0257(17) 0.0076(14) -0.0037(14) 0.0034(14) C10 0.0267(17) 0.0278(17) 0.0305(19) 0.0000(15) -0.0027(14) 0.0047(14) C11 0.0245(16) 0.0189(15) 0.0299(17) 0.0044(14) -0.0107(14) -0.0022(13) C12 0.0202(15) 0.0225(16) 0.0294(17) -0.0010(14) -0.0056(13) 0.0004(13) C13 0.0241(16) 0.0213(16) 0.0294(18) 0.0042(14) -0.0079(14) 0.0067(14) C14 0.0237(16) 0.0283(17) 0.0243(17) 0.0067(14) -0.0058(14) 0.0021(14) C15 0.0299(18) 0.0334(18) 0.038(2) 0.0057(16) -0.0112(16) -0.0034(15) C16 0.0306(19) 0.048(2) 0.038(2) 0.0205(19) 0.0027(16) -0.0027(17) C17 0.036(2) 0.053(2) 0.0207(18) 0.0116(17) -0.0009(16) 0.0162(18) C18 0.043(2) 0.048(2) 0.029(2) -0.0013(17) -0.0112(17) 0.0060(18) C19 0.0305(18) 0.039(2) 0.0302(19) 0.0027(16) -0.0075(15) -0.0016(16) C20 0.0225(15) 0.0231(16) 0.0278(18) -0.0012(14) -0.0096(14) 0.0048(13) C21 0.0267(16) 0.0219(15) 0.0263(17) 0.0029(14) -0.0109(14) 0.0013(13) C22 0.0317(18) 0.0379(19) 0.0294(19) -0.0003(16) -0.0084(15) -0.0064(16) C23 0.0355(19) 0.052(2) 0.0265(19) -0.0012(17) -0.0058(16) -0.0017(18) C24 0.051(2) 0.0323(19) 0.034(2) -0.0099(16) -0.0216(18) 0.0061(17) C25 0.064(3) 0.0341(19) 0.040(2) 0.0051(17) -0.027(2) -0.0182(19) C26 0.045(2) 0.0326(18) 0.0278(18) 0.0077(15) -0.0125(16) -0.0103(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.294(2) . ? Cd1 N1 2.321(2) . ? Cd1 N2 2.331(2) 1_645 ? Cd1 O2 2.364(2) 2_565 ? Cd1 O3 2.375(2) . ? Cd1 O4 2.405(2) . ? Cd1 O2 2.706(2) . ? Cd1 C20 2.731(3) . ? Cd1 C13 2.847(3) . ? Cl1 C17 1.752(3) . ? Cl2 C24 1.743(3) . ? N1 C1 1.335(4) . ? N1 C5 1.337(4) . ? N2 C11 1.335(4) . ? N2 C10 1.339(4) . ? N2 Cd1 2.331(2) 1_465 ? O1 C13 1.255(4) . ? O2 C13 1.259(4) . ? O2 Cd1 2.364(2) 2_565 ? O3 C20 1.253(4) . ? O4 C20 1.262(4) . ? C1 C2 1.375(4) . ? C1 H1 0.9400 . ? C2 C3 1.392(4) . ? C2 H2 0.9400 . ? C3 C4 1.395(4) . ? C3 C6 1.507(4) . ? C4 C5 1.378(4) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.554(4) . ? C6 C7 1.611(4) 2_475 ? C6 H6 0.9900 . ? C7 C8 1.504(4) . ? C7 C6 1.611(4) 2_475 ? C7 H7 0.9900 . ? C8 C12 1.386(4) . ? C8 C9 1.394(4) . ? C9 C10 1.379(4) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.386(4) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.506(4) . ? C14 C19 1.379(5) . ? C14 C15 1.392(4) . ? C15 C16 1.381(5) . ? C15 H15 0.9400 . ? C16 C17 1.365(5) . ? C16 H16 0.9400 . ? C17 C18 1.375(5) . ? C18 C19 1.382(5) . ? C18 H18 0.9400 . ? C19 H19 0.9400 . ? C20 C21 1.490(4) . ? C21 C26 1.382(4) . ? C21 C22 1.388(4) . ? C22 C23 1.376(5) . ? C22 H22 0.9400 . ? C23 C24 1.378(5) . ? C23 H23 0.9400 . ? C24 C25 1.367(5) . ? C25 C26 1.389(5) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N1 91.04(9) . . ? O1 Cd1 N2 91.23(9) . 1_645 ? N1 Cd1 N2 176.08(8) . 1_645 ? O1 Cd1 O2 124.19(8) . 2_565 ? N1 Cd1 O2 86.15(8) . 2_565 ? N2 Cd1 O2 89.93(8) 1_645 2_565 ? O1 Cd1 O3 145.51(8) . . ? N1 Cd1 O3 91.72(9) . . ? N2 Cd1 O3 88.22(9) 1_645 . ? O2 Cd1 O3 90.29(8) 2_565 . ? O1 Cd1 O4 90.96(8) . . ? N1 Cd1 O4 87.88(8) . . ? N2 Cd1 O4 95.27(8) 1_645 . ? O2 Cd1 O4 144.39(8) 2_565 . ? O3 Cd1 O4 54.82(7) . . ? O1 Cd1 O2 51.50(7) . . ? N1 Cd1 O2 84.09(8) . . ? N2 Cd1 O2 94.83(8) 1_645 . ? O2 Cd1 O2 72.81(8) 2_565 . ? O3 Cd1 O2 162.79(7) . . ? O4 Cd1 O2 141.24(7) . . ? O1 Cd1 C20 118.40(9) . . ? N1 Cd1 C20 89.64(9) . . ? N2 Cd1 C20 92.09(9) 1_645 . ? O2 Cd1 C20 117.30(9) 2_565 . ? O3 Cd1 C20 27.30(8) . . ? O4 Cd1 C20 27.53(8) . . ? O2 Cd1 C20 167.80(7) . . ? O1 Cd1 C13 25.45(8) . . ? N1 Cd1 C13 86.81(9) . . ? N2 Cd1 C13 93.88(9) 1_645 . ? O2 Cd1 C13 98.84(9) 2_565 . ? O3 Cd1 C13 170.62(8) . . ? O4 Cd1 C13 115.84(8) . . ? O2 Cd1 C13 26.06(7) . . ? C20 Cd1 C13 143.35(9) . . ? C1 N1 C5 117.3(2) . . ? C1 N1 Cd1 121.15(19) . . ? C5 N1 Cd1 121.3(2) . . ? C11 N2 C10 117.0(3) . . ? C11 N2 Cd1 121.22(19) . 1_465 ? C10 N2 Cd1 120.8(2) . 1_465 ? C13 O1 Cd1 102.76(18) . . ? C13 O2 Cd1 169.3(2) . 2_565 ? C13 O2 Cd1 83.23(19) . . ? Cd1 O2 Cd1 107.19(8) 2_565 . ? C20 O3 Cd1 92.38(18) . . ? C20 O4 Cd1 90.76(17) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 116.6(3) . . ? C2 C3 C6 124.1(3) . . ? C4 C3 C6 118.8(3) . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.1(3) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C3 C6 C7 118.6(2) . . ? C3 C6 C7 113.3(2) . 2_475 ? C7 C6 C7 90.2(2) . 2_475 ? C3 C6 H6 111.1 . . ? C7 C6 H6 111.1 . . ? C7 C6 H6 111.1 2_475 . ? C8 C7 C6 119.5(2) . . ? C8 C7 C6 113.9(2) . 2_475 ? C6 C7 C6 89.8(2) . 2_475 ? C8 C7 H7 110.7 . . ? C6 C7 H7 110.7 . . ? C6 C7 H7 110.7 2_475 . ? C12 C8 C9 116.3(3) . . ? C12 C8 C7 124.6(3) . . ? C9 C8 C7 118.5(3) . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? N2 C10 C9 122.4(3) . . ? N2 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? N2 C11 C12 123.7(3) . . ? N2 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C8 119.3(3) . . ? C11 C12 H12 120.4 . . ? C8 C12 H12 120.4 . . ? O1 C13 O2 122.5(3) . . ? O1 C13 C14 118.1(3) . . ? O2 C13 C14 119.4(3) . . ? O1 C13 Cd1 51.79(15) . . ? O2 C13 Cd1 70.71(17) . . ? C14 C13 Cd1 169.6(2) . . ? C19 C14 C15 119.1(3) . . ? C19 C14 C13 121.3(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.6(3) . . ? C16 C17 Cl1 119.4(3) . . ? C18 C17 Cl1 119.1(3) . . ? C17 C18 C19 118.9(3) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C14 C19 C18 120.8(3) . . ? C14 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? O3 C20 O4 122.0(3) . . ? O3 C20 C21 119.4(3) . . ? O4 C20 C21 118.6(3) . . ? O3 C20 Cd1 60.32(16) . . ? O4 C20 Cd1 61.71(16) . . ? C21 C20 Cd1 179.6(2) . . ? C26 C21 C22 118.5(3) . . ? C26 C21 C20 120.2(3) . . ? C22 C21 C20 121.3(3) . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 119.1(3) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 121.8(3) . . ? C25 C24 Cl2 119.4(3) . . ? C23 C24 Cl2 118.7(3) . . ? C24 C25 C26 118.3(3) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C21 C26 C25 121.4(3) . . ? C21 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.887 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.078 #===END #========================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 772188' #TrackingRef '- JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Cd Cl2 N4, 2(H2 O)' _chemical_formula_sum 'C24 H24 Cd Cl2 N4 O2' _chemical_formula_weight 583.78 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' 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 orthorhombic _symmetry_space_group_name_H-M 'P c c a' _symmetry_space_group_name_Hall '-P 2a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.419(4) _cell_length_b 9.1351(18) _cell_length_c 15.583(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2479.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8713 _cell_measurement_theta_min 3.2318 _cell_measurement_theta_max 27.5126 _exptl_crystal_description Platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5519 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10959 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2822 _reflns_number_gt 2327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0142(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2822 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 0.7500 0.0000 -0.03918(2) 0.0327(2) Uani 1 2 d S . . Cl1 Cl 0.64002(5) -0.19519(11) -0.04894(7) 0.0535(3) Uani 1 1 d . . . N1 N 0.67893(14) 0.1135(3) 0.07339(17) 0.0329(6) Uani 1 1 d . . . C1 C 0.60288(19) 0.1024(4) 0.0754(3) 0.0457(9) Uani 1 1 d . . . H1 H 0.5790 0.0393 0.0360 0.055 Uiso 1 1 calc R . . C2 C 0.55696(18) 0.1787(4) 0.1325(2) 0.0412(8) Uani 1 1 d . . . H2 H 0.5033 0.1681 0.1309 0.049 Uiso 1 1 calc R . . N2 N 0.68374(17) 0.8412(3) 0.36723(18) 0.0387(7) Uani 1 1 d . . . C3 C 0.59078(15) 0.2707(3) 0.19187(19) 0.0249(6) Uani 1 1 d . . . C4 C 0.67022(18) 0.2773(4) 0.1915(2) 0.0380(7) Uani 1 1 d . . . H4 H 0.6959 0.3358 0.2320 0.046 Uiso 1 1 calc R . . C5 C 0.71171(17) 0.1984(4) 0.1321(2) 0.0367(7) Uani 1 1 d . . . H5 H 0.7656 0.2049 0.1332 0.044 Uiso 1 1 calc R . . C6 C 0.54451(15) 0.3638(3) 0.25219(17) 0.0238(6) Uani 1 1 d . . . H6 H 0.5615 0.3467 0.3120 0.029 Uiso 1 1 calc R . . C7 C 0.54281(16) 0.5309(3) 0.2332(2) 0.0255(6) Uani 1 1 d . . . H7 H 0.5438 0.5481 0.1705 0.031 Uiso 1 1 calc R . . C8 C 0.59640(16) 0.6352(3) 0.27752(19) 0.0271(6) Uani 1 1 d . . . C9 C 0.63973(18) 0.5954(3) 0.3480(2) 0.0355(7) Uani 1 1 d . . . H9 H 0.6400 0.4978 0.3670 0.043 Uiso 1 1 calc R . . C10 C 0.6826(2) 0.6998(4) 0.3904(2) 0.0408(8) Uani 1 1 d . . . H10 H 0.7124 0.6704 0.4376 0.049 Uiso 1 1 calc R . . C11 C 0.6435(2) 0.8800(3) 0.2978(2) 0.0390(8) Uani 1 1 d . . . H11 H 0.6447 0.9783 0.2800 0.047 Uiso 1 1 calc R . . C12 C 0.60058(19) 0.7816(3) 0.2512(2) 0.0352(7) Uani 1 1 d . . . H12 H 0.5741 0.8125 0.2019 0.042 Uiso 1 1 calc R . . O1 O 0.6687(6) 0.4712(9) 0.5563(6) 0.146(3) Uani 1 1 d DU . . H1W H 0.628(3) 0.437(9) 0.537(5) 0.146(4) Uiso 1 1 d DU . . H2W H 0.676(5) 0.554(4) 0.537(5) 0.146(4) Uiso 1 1 d DU . . 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 0.0341(3) 0.0359(3) 0.0280(3) 0.000 0.000 0.01574(12) Cl1 0.0343(5) 0.0529(5) 0.0733(7) -0.0253(4) -0.0106(4) 0.0048(4) N1 0.0274(13) 0.0387(14) 0.0325(14) -0.0050(11) -0.0005(11) 0.0076(10) C1 0.0311(17) 0.0512(19) 0.055(2) -0.0258(18) -0.0036(15) 0.0033(15) C2 0.0235(14) 0.0439(17) 0.056(2) -0.0174(16) 0.0026(14) 0.0006(13) N2 0.0430(16) 0.0346(13) 0.0385(15) 0.0019(11) -0.0059(12) -0.0147(11) C3 0.0215(13) 0.0250(12) 0.0281(13) 0.0026(11) 0.0014(11) 0.0011(10) C4 0.0262(15) 0.0482(17) 0.0398(17) -0.0132(16) -0.0034(13) -0.0011(13) C5 0.0231(14) 0.0486(17) 0.0385(17) -0.0047(14) 0.0000(12) 0.0021(13) C6 0.0220(14) 0.0222(12) 0.0273(13) 0.0002(10) 0.0001(11) 0.0005(10) C7 0.0222(15) 0.0250(12) 0.0292(14) 0.0002(12) -0.0002(13) -0.0019(11) C8 0.0252(14) 0.0251(12) 0.0311(14) -0.0019(11) 0.0014(11) -0.0032(11) C9 0.0398(17) 0.0289(13) 0.0378(16) 0.0033(12) -0.0076(14) -0.0066(12) C10 0.0429(18) 0.0388(16) 0.0409(18) 0.0061(14) -0.0144(15) -0.0092(14) C11 0.0475(19) 0.0297(14) 0.0397(18) 0.0019(13) -0.0017(14) -0.0101(14) C12 0.0357(16) 0.0327(14) 0.0373(17) 0.0044(13) -0.0061(13) -0.0064(13) O1 0.157(4) 0.139(4) 0.141(4) -0.003(3) -0.003(3) 0.004(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 N2 2.359(3) 8_745 ? Cd1 N2 2.359(3) 7_565 ? Cd1 N1 2.384(3) 2_655 ? Cd1 N1 2.384(3) . ? Cd1 Cl1 2.6215(10) . ? Cd1 Cl1 2.6215(10) 2_655 ? N1 C5 1.329(4) . ? N1 C1 1.329(4) . ? C1 C2 1.385(5) . ? C1 H1 0.9400 . ? C2 C3 1.382(4) . ? C2 H2 0.9400 . ? N2 C11 1.337(4) . ? N2 C10 1.342(4) . ? N2 Cd1 2.359(3) 7_566 ? C3 C4 1.385(4) . ? C3 C6 1.502(4) . ? C4 C5 1.378(5) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C6 1.552(5) 3_655 ? C6 C7 1.556(4) . ? C6 H6 0.9900 . ? C7 C8 1.502(4) . ? C7 C7 1.581(6) 3_655 ? C7 H7 0.9900 . ? C8 C9 1.381(4) . ? C8 C12 1.400(4) . ? C9 C10 1.379(5) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.376(5) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? O1 H1W 0.83(6) . ? O1 H2W 0.82(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 103.61(13) 8_745 7_565 ? N2 Cd1 N1 86.18(9) 8_745 2_655 ? N2 Cd1 N1 167.54(9) 7_565 2_655 ? N2 Cd1 N1 167.54(9) 8_745 . ? N2 Cd1 N1 86.18(9) 7_565 . ? N1 Cd1 N1 85.27(13) 2_655 . ? N2 Cd1 Cl1 84.46(8) 8_745 . ? N2 Cd1 Cl1 91.42(8) 7_565 . ? N1 Cd1 Cl1 97.26(7) 2_655 . ? N1 Cd1 Cl1 87.66(7) . . ? N2 Cd1 Cl1 91.42(8) 8_745 2_655 ? N2 Cd1 Cl1 84.46(8) 7_565 2_655 ? N1 Cd1 Cl1 87.66(7) 2_655 2_655 ? N1 Cd1 Cl1 97.26(7) . 2_655 ? Cl1 Cd1 Cl1 173.34(5) . 2_655 ? C5 N1 C1 117.2(3) . . ? C5 N1 Cd1 122.5(2) . . ? C1 N1 Cd1 120.1(2) . . ? N1 C1 C2 123.5(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C11 N2 C10 117.7(3) . . ? C11 N2 Cd1 126.5(2) . 7_566 ? C10 N2 Cd1 115.7(2) . 7_566 ? C2 C3 C4 116.7(3) . . ? C2 C3 C6 122.3(2) . . ? C4 C3 C6 120.9(3) . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 122.9(3) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C3 C6 C6 120.6(2) . 3_655 ? C3 C6 C7 116.5(2) . . ? C6 C6 C7 88.43(15) 3_655 . ? C3 C6 H6 109.9 . . ? C6 C6 H6 109.9 3_655 . ? C7 C6 H6 109.9 . . ? C8 C7 C6 121.6(2) . . ? C8 C7 C7 115.7(3) . 3_655 ? C6 C7 C7 87.42(15) . 3_655 ? C8 C7 H7 110.1 . . ? C6 C7 H7 110.1 . . ? C7 C7 H7 110.1 3_655 . ? C9 C8 C12 117.1(3) . . ? C9 C8 C7 122.6(3) . . ? C12 C8 C7 120.2(3) . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 123.1(3) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N2 C11 C12 122.6(3) . . ? N2 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C8 119.8(3) . . ? C11 C12 H12 120.1 . . ? C8 C12 H12 120.1 . . ? H1W O1 H2W 110(8) . . ? 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 O1 H1W Cl1 0.83(6) 2.60(8) 3.049(8) 116(8) 7_556 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.308 _refine_diff_density_min -1.411 _refine_diff_density_rms 0.194 #===END