# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Cong Guo' _publ_contact_author_email GCGUO@FJIRSM.AC.CN _publ_section_title ; Spontaneous Chiral Resolution, Nonlinear Optical and Luminescence of Eight-Coordinate Lanthanide(III) Complexes ; loop_ _publ_author_name 'Guo-Cong Guo' 'Hui-Fen Chen' 'Sheng-Ping Guo' 'Jin-Shun Huang' ; Ming-Sheng Wang ; 'Mei-Feng Wu' 'Gang Xu' 'Wen-Qiang Zou' # Attachment '1-left-rev.CIF' data_4-left _database_code_depnum_ccdc_archive 'CCDC 738976' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'C32 H12 Cl3 Dy N12' ; _chemical_name_common "'C32 H12 Cl3 Dy N12'" _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H12 Cl3 Dy N12' _chemical_formula_sum 'C32 H12 Cl3 Dy N12' _chemical_formula_weight 833.39 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.920(2) _cell_length_b 8.1845(16) _cell_length_c 18.107(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.74(3) _cell_angle_gamma 90.00 _cell_volume 1549.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 2.716 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.9532 _exptl_absorpt_correction_T_max 0.9998 _exptl_absorpt_process_details 'Psi (Rigaku WinAFC)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3254 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3095 _reflns_number_gt 2882 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^+0.1832P] 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 -0.004(13) _chemical_absolute_configuration ad _refine_ls_number_reflns 3095 _refine_ls_number_parameters 433 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0594 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Dy1 Dy 0.150641(14) 0.30303(3) 0.481540(9) 0.02401(4) Uani 1 1 d . . . Cl1 Cl 0.01138(15) 0.5631(2) 0.50358(10) 0.0374(3) Uani 1 1 d . . . Cl2 Cl 0.34870(11) 0.12399(16) 0.55185(7) 0.0379(3) Uani 1 1 d . . . Cl3 Cl 0.21640(11) 0.46924(16) 0.37425(6) 0.0383(3) Uani 1 1 d . . . N1 N -0.0521(3) 0.2976(9) 0.36105(16) 0.0280(7) Uani 1 1 d . . . N2 N 0.1508(3) 0.0960(5) 0.3703(2) 0.0326(10) Uani 1 1 d . . . N3 N 0.0342(4) 0.0658(6) 0.0925(2) 0.0381(11) Uani 1 1 d . . . N4 N -0.1907(3) 0.2424(5) 0.0850(2) 0.0360(10) Uani 1 1 d . . . N5 N -0.3200(4) 0.2747(8) -0.1088(2) 0.0540(15) Uani 1 1 d . . . N6 N -0.0020(5) 0.0403(9) -0.1026(3) 0.0716(19) Uani 1 1 d . . . N7 N 0.3152(3) 0.5083(5) 0.5679(2) 0.0307(10) Uani 1 1 d . . . N8 N 0.1572(3) 0.3220(5) 0.62866(17) 0.0278(9) Uani 1 1 d . . . N9 N 0.4053(3) 0.4723(6) 0.8861(2) 0.0360(10) Uani 1 1 d . . . N10 N 0.5677(3) 0.6600(5) 0.8221(2) 0.0385(11) Uani 1 1 d . . . N11 N 0.7739(4) 0.8072(12) 0.9893(2) 0.0702(15) Uani 1 1 d . . . N12 N 0.5431(5) 0.5373(8) 1.0774(3) 0.0672(18) Uani 1 1 d . . . C101 C -0.1622(4) 0.3714(6) 0.3576(3) 0.0351(12) Uani 1 1 d . . . H10A H -0.1749 0.4070 0.4036 0.042 Uiso 1 1 calc R . . C102 C -0.2590(4) 0.3988(6) 0.2902(3) 0.0354(12) Uani 1 1 d . . . H10B H -0.3352 0.4480 0.2915 0.042 Uiso 1 1 calc R . . C103 C -0.2403(4) 0.3517(6) 0.2212(3) 0.0351(13) Uani 1 1 d . . . H10C H -0.3001 0.3775 0.1746 0.042 Uiso 1 1 calc R . . C104 C -0.1300(4) 0.2647(5) 0.2226(2) 0.0280(13) Uani 1 1 d . . . C105 C -0.1056(4) 0.2054(5) 0.1530(2) 0.0287(11) Uani 1 1 d . . . C106 C -0.1611(4) 0.1956(6) 0.0222(2) 0.0340(12) Uani 1 1 d . . . C107 C -0.2516(4) 0.2401(7) -0.0514(3) 0.0410(13) Uani 1 1 d . . . C108 C -0.0209(5) 0.0662(8) -0.0460(3) 0.0531(17) Uani 1 1 d . . . C109 C -0.0499(4) 0.1107(7) 0.0255(2) 0.0379(13) Uani 1 1 d . . . C110 C 0.0056(4) 0.1124(6) 0.1565(2) 0.0309(11) Uani 1 1 d . . . C111 C 0.0910(4) 0.0647(6) 0.2311(2) 0.0311(11) Uani 1 1 d . . . C112 C 0.1865(4) -0.0509(7) 0.2378(3) 0.0376(12) Uani 1 1 d . . . H11A H 0.2012 -0.0967 0.1941 0.045 Uiso 1 1 calc R . . C113 C 0.2599(4) -0.0970(6) 0.3112(3) 0.0389(13) Uani 1 1 d . . . H11B H 0.3216 -0.1784 0.3181 0.047 Uiso 1 1 calc R . . C114 C 0.2373(4) -0.0168(6) 0.3737(3) 0.0369(12) Uani 1 1 d . . . H11C H 0.2883 -0.0460 0.4225 0.044 Uiso 1 1 calc R . . C115 C 0.0728(4) 0.1319(6) 0.2988(2) 0.0273(10) Uani 1 1 d . . . C116 C -0.0375(4) 0.2368(5) 0.2941(2) 0.0266(10) Uani 1 1 d . . . C201 C 0.3848(4) 0.6091(6) 0.5400(3) 0.0350(12) Uani 1 1 d . . . H20A H 0.3674 0.6146 0.4867 0.042 Uiso 1 1 calc R . . C202 C 0.4821(4) 0.7078(6) 0.5841(3) 0.0382(13) Uani 1 1 d . . . H20B H 0.5251 0.7799 0.5605 0.046 Uiso 1 1 calc R . . C203 C 0.5130(4) 0.6970(6) 0.6615(3) 0.0361(12) Uani 1 1 d . . . H20C H 0.5791 0.7599 0.6923 0.043 Uiso 1 1 calc R . . C204 C 0.4439(4) 0.5892(6) 0.6950(2) 0.0294(11) Uani 1 1 d . . . C205 C 0.4689(4) 0.5755(6) 0.7775(3) 0.0334(12) Uani 1 1 d . . . C206 C 0.5835(4) 0.6505(7) 0.8981(3) 0.0375(13) Uani 1 1 d . . . C207 C 0.6915(5) 0.7392(7) 0.9491(3) 0.0466(15) Uani 1 1 d . . . C208 C 0.5249(5) 0.5489(9) 1.0120(3) 0.0495(16) Uani 1 1 d . . . C209 C 0.5047(5) 0.5567(7) 0.9289(3) 0.0397(14) Uani 1 1 d . . . C210 C 0.3879(4) 0.4796(6) 0.8087(2) 0.0294(11) Uani 1 1 d . . . C211 C 0.2786(4) 0.3938(6) 0.7589(2) 0.0300(11) Uani 1 1 d . . . C212 C 0.1933(3) 0.3092(9) 0.7889(2) 0.0343(10) Uani 1 1 d . . . H21A H 0.2073 0.3004 0.8419 0.041 Uiso 1 1 calc R . . C213 C 0.0880(4) 0.2390(6) 0.7384(2) 0.0336(11) Uani 1 1 d . . . H21B H 0.0265 0.1864 0.7562 0.040 Uiso 1 1 calc R . . C214 C 0.0754(4) 0.2483(5) 0.6594(2) 0.0316(12) Uani 1 1 d . . . H21C H 0.0041 0.1991 0.6259 0.038 Uiso 1 1 calc R . . C215 C 0.2595(4) 0.4004(5) 0.6787(2) 0.0250(10) Uani 1 1 d . . . C216 C 0.3424(4) 0.4997(6) 0.6461(2) 0.0261(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02722(7) 0.02332(7) 0.02174(7) 0.00096(14) 0.00745(5) 0.00088(14) Cl1 0.0442(5) 0.0355(6) 0.0296(4) -0.0044(4) 0.0060(4) 0.0145(5) Cl2 0.0387(5) 0.0395(6) 0.0342(5) 0.0047(5) 0.0086(4) 0.0109(5) Cl3 0.0466(6) 0.0405(6) 0.0299(5) 0.0036(5) 0.0142(4) -0.0086(5) N1 0.0304(13) 0.0293(15) 0.0256(13) 0.000(3) 0.0098(11) -0.003(3) N2 0.0334(17) 0.031(2) 0.0352(19) 0.0022(17) 0.0129(15) -0.0032(17) N3 0.043(2) 0.045(3) 0.0283(18) -0.0008(18) 0.0146(16) 0.000(2) N4 0.0382(18) 0.041(2) 0.0278(17) 0.0015(16) 0.0077(15) -0.0047(17) N5 0.054(2) 0.071(4) 0.0326(18) 0.005(3) 0.0065(16) -0.002(3) N6 0.085(3) 0.100(5) 0.037(2) -0.003(3) 0.028(2) 0.018(3) N7 0.0336(18) 0.032(2) 0.0258(18) 0.0026(17) 0.0077(15) 0.0013(18) N8 0.0277(14) 0.029(2) 0.0265(14) 0.0005(17) 0.0076(12) 0.0000(17) N9 0.0363(18) 0.041(2) 0.0270(18) -0.0038(18) 0.0033(15) -0.0009(19) N10 0.0335(18) 0.042(2) 0.034(2) -0.0037(19) 0.0011(16) 0.0035(19) N11 0.064(2) 0.080(3) 0.056(2) -0.014(5) -0.001(2) -0.010(5) N12 0.068(3) 0.086(4) 0.042(3) -0.005(3) 0.007(2) 0.018(3) C101 0.039(2) 0.037(2) 0.031(2) -0.003(2) 0.0133(18) -0.005(2) C102 0.030(2) 0.034(3) 0.044(2) -0.005(2) 0.0122(18) 0.005(2) C103 0.034(2) 0.042(3) 0.030(2) 0.0004(18) 0.0103(17) -0.0018(18) C104 0.0339(18) 0.027(3) 0.0234(17) 0.0010(16) 0.0083(14) -0.0014(17) C105 0.035(2) 0.023(2) 0.029(2) -0.0007(18) 0.0100(16) -0.0038(19) C106 0.040(2) 0.037(3) 0.026(2) -0.002(2) 0.0095(17) -0.008(2) C107 0.045(2) 0.044(3) 0.036(2) 0.000(2) 0.0149(19) 0.000(2) C108 0.061(3) 0.067(4) 0.036(3) 0.008(3) 0.021(2) 0.017(3) C109 0.045(2) 0.045(3) 0.022(2) -0.005(2) 0.0081(18) -0.004(2) C110 0.041(2) 0.028(2) 0.026(2) -0.0028(19) 0.0118(17) -0.006(2) C111 0.035(2) 0.034(2) 0.028(2) -0.0005(19) 0.0135(16) -0.005(2) C112 0.043(2) 0.042(3) 0.032(2) -0.005(2) 0.0180(18) 0.001(2) C113 0.040(2) 0.033(3) 0.046(3) 0.000(2) 0.016(2) 0.011(2) C114 0.039(2) 0.030(2) 0.040(2) 0.001(2) 0.009(2) 0.011(2) C115 0.0293(18) 0.023(2) 0.030(2) -0.0020(18) 0.0096(16) -0.0027(18) C116 0.0290(18) 0.0248(19) 0.0285(19) -0.0017(17) 0.0120(15) -0.0083(17) C201 0.043(2) 0.033(3) 0.028(2) -0.001(2) 0.0094(18) -0.003(2) C202 0.034(2) 0.036(3) 0.045(3) 0.005(2) 0.0129(19) -0.006(2) C203 0.0285(19) 0.037(3) 0.042(2) -0.007(2) 0.0100(18) -0.006(2) C204 0.0287(19) 0.030(2) 0.028(2) -0.0040(19) 0.0061(16) 0.0018(19) C205 0.033(2) 0.031(2) 0.035(2) -0.001(2) 0.0070(18) 0.006(2) C206 0.032(2) 0.040(3) 0.033(2) -0.010(2) -0.0017(18) -0.003(2) C207 0.043(2) 0.051(3) 0.039(2) -0.012(2) 0.001(2) -0.006(2) C208 0.048(3) 0.062(3) 0.032(3) -0.012(3) 0.003(2) -0.001(3) C209 0.040(2) 0.041(3) 0.035(3) -0.004(2) 0.006(2) 0.013(2) C210 0.033(2) 0.029(2) 0.024(2) -0.0005(19) 0.0048(17) 0.005(2) C211 0.035(2) 0.033(3) 0.0221(19) -0.0054(19) 0.0074(17) 0.001(2) C212 0.0431(18) 0.033(2) 0.0292(17) 0.007(3) 0.0149(14) -0.002(4) C213 0.043(2) 0.031(2) 0.033(2) -0.0066(18) 0.0201(17) -0.0042(19) C214 0.0321(19) 0.029(2) 0.034(2) -0.0051(17) 0.0098(17) -0.0027(17) C215 0.0292(19) 0.022(2) 0.0245(19) -0.0013(17) 0.0084(16) 0.0051(18) C216 0.0268(18) 0.026(2) 0.0239(19) 0.0028(18) 0.0049(16) 0.0081(18) _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 Dy1 Cl2 2.6190(13) . ? Dy1 N7 2.622(4) . ? Dy1 N1 2.623(3) . ? Dy1 N2 2.633(4) . ? Dy1 Cl3 2.6352(13) . ? Dy1 N8 2.649(3) . ? Dy1 Cl1 2.7081(18) 2_546 ? Dy1 Cl1 2.7114(18) . ? Cl1 Dy1 2.7081(18) 2_556 ? N1 C101 1.330(6) . ? N1 C116 1.361(6) . ? N2 C114 1.309(6) . ? N2 C115 1.362(5) . ? N3 C110 1.339(6) . ? N3 C109 1.346(6) . ? N4 C106 1.325(6) . ? N4 C105 1.346(5) . ? N5 C107 1.128(6) . ? N6 C108 1.124(8) . ? N7 C201 1.317(6) . ? N7 C216 1.361(5) . ? N8 C214 1.326(6) . ? N8 C215 1.377(5) . ? N9 C209 1.331(6) . ? N9 C210 1.360(6) . ? N10 C205 1.339(6) . ? N10 C206 1.339(6) . ? N11 C207 1.128(8) . ? N12 C208 1.147(7) . ? C101 C102 1.383(6) . ? C101 H10A 0.9300 . ? C102 C103 1.378(7) . ? C102 H10B 0.9300 . ? C103 C104 1.393(6) . ? C103 H10C 0.9300 . ? C104 C116 1.413(5) . ? C104 C105 1.446(6) . ? C105 C110 1.418(6) . ? C106 C109 1.385(7) . ? C106 C107 1.458(6) . ? C108 C109 1.464(7) . ? C110 C111 1.456(6) . ? C111 C112 1.388(7) . ? C111 C115 1.409(6) . ? C112 C113 1.392(6) . ? C112 H11A 0.9300 . ? C113 C114 1.392(7) . ? C113 H11B 0.9300 . ? C114 H11C 0.9300 . ? C115 C116 1.462(6) . ? C201 C202 1.390(6) . ? C201 H20A 0.9300 . ? C202 C203 1.347(7) . ? C202 H20B 0.9300 . ? C203 C204 1.408(7) . ? C203 H20C 0.9300 . ? C204 C216 1.409(6) . ? C204 C205 1.443(6) . ? C205 C210 1.417(7) . ? C206 C209 1.385(8) . ? C206 C207 1.464(7) . ? C208 C209 1.458(8) . ? C210 C211 1.453(6) . ? C211 C212 1.391(7) . ? C211 C215 1.407(6) . ? C212 C213 1.372(6) . ? C212 H21A 0.9300 . ? C213 C214 1.398(6) . ? C213 H21B 0.9300 . ? C214 H21C 0.9300 . ? C215 C216 1.462(6) . ? 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 Cl2 Dy1 N7 74.96(9) . . ? Cl2 Dy1 N1 140.87(15) . . ? N7 Dy1 N1 140.89(18) . . ? Cl2 Dy1 N2 80.17(9) . . ? N7 Dy1 N2 135.83(12) . . ? N1 Dy1 N2 62.55(14) . . ? Cl2 Dy1 Cl3 106.55(4) . . ? N7 Dy1 Cl3 79.84(9) . . ? N1 Dy1 Cl3 74.90(10) . . ? N2 Dy1 Cl3 73.01(9) . . ? Cl2 Dy1 N8 76.39(8) . . ? N7 Dy1 N8 63.09(12) . . ? N1 Dy1 N8 127.54(9) . . ? N2 Dy1 N8 143.27(13) . . ? Cl3 Dy1 N8 141.00(9) . . ? Cl2 Dy1 Cl1 91.01(5) . 2_546 ? N7 Dy1 Cl1 139.48(9) . 2_546 ? N1 Dy1 Cl1 69.60(13) . 2_546 ? N2 Dy1 Cl1 75.75(10) . 2_546 ? Cl3 Dy1 Cl1 140.56(5) . 2_546 ? N8 Dy1 Cl1 76.79(9) . 2_546 ? Cl2 Dy1 Cl1 141.93(4) . . ? N7 Dy1 Cl1 74.11(9) . . ? N1 Dy1 Cl1 76.17(14) . . ? N2 Dy1 Cl1 137.89(9) . . ? Cl3 Dy1 Cl1 89.24(5) . . ? N8 Dy1 Cl1 70.11(9) . . ? Cl1 Dy1 Cl1 98.304(17) 2_546 . ? Dy1 Cl1 Dy1 173.76(7) 2_556 . ? C101 N1 C116 117.4(3) . . ? C101 N1 Dy1 124.5(3) . . ? C116 N1 Dy1 117.4(2) . . ? C114 N2 C115 116.3(4) . . ? C114 N2 Dy1 125.2(3) . . ? C115 N2 Dy1 116.8(3) . . ? C110 N3 C109 115.7(4) . . ? C106 N4 C105 116.4(4) . . ? C201 N7 C216 117.0(4) . . ? C201 N7 Dy1 123.0(3) . . ? C216 N7 Dy1 119.6(3) . . ? C214 N8 C215 116.9(3) . . ? C214 N8 Dy1 124.7(3) . . ? C215 N8 Dy1 118.0(3) . . ? C209 N9 C210 115.2(4) . . ? C205 N10 C206 115.6(4) . . ? N1 C101 C102 124.5(4) . . ? N1 C101 H10A 117.7 . . ? C102 C101 H10A 117.7 . . ? C103 C102 C101 118.6(4) . . ? C103 C102 H10B 120.7 . . ? C101 C102 H10B 120.7 . . ? C102 C103 C104 118.6(4) . . ? C102 C103 H10C 120.7 . . ? C104 C103 H10C 120.7 . . ? C103 C104 C116 119.1(4) . . ? C103 C104 C105 122.1(3) . . ? C116 C104 C105 118.8(4) . . ? N4 C105 C110 121.2(4) . . ? N4 C105 C104 118.0(4) . . ? C110 C105 C104 120.8(4) . . ? N4 C106 C109 122.4(4) . . ? N4 C106 C107 116.3(4) . . ? C109 C106 C107 121.3(4) . . ? N5 C107 C106 178.8(6) . . ? N6 C108 C109 175.9(7) . . ? N3 C109 C106 122.5(4) . . ? N3 C109 C108 117.6(5) . . ? C106 C109 C108 119.8(4) . . ? N3 C110 C105 121.6(4) . . ? N3 C110 C111 118.6(4) . . ? C105 C110 C111 119.8(4) . . ? C112 C111 C115 118.7(4) . . ? C112 C111 C110 121.9(4) . . ? C115 C111 C110 119.3(4) . . ? C111 C112 C113 118.7(4) . . ? C111 C112 H11A 120.6 . . ? C113 C112 H11A 120.6 . . ? C112 C113 C114 117.4(4) . . ? C112 C113 H11B 121.3 . . ? C114 C113 H11B 121.3 . . ? N2 C114 C113 126.1(4) . . ? N2 C114 H11C 117.0 . . ? C113 C114 H11C 117.0 . . ? N2 C115 C111 122.5(4) . . ? N2 C115 C116 117.4(4) . . ? C111 C115 C116 120.0(4) . . ? N1 C116 C104 121.4(4) . . ? N1 C116 C115 118.0(4) . . ? C104 C116 C115 120.5(4) . . ? N7 C201 C202 125.0(4) . . ? N7 C201 H20A 117.5 . . ? C202 C201 H20A 117.5 . . ? C203 C202 C201 118.7(5) . . ? C203 C202 H20B 120.6 . . ? C201 C202 H20B 120.6 . . ? C202 C203 C204 119.0(4) . . ? C202 C203 H20C 120.5 . . ? C204 C203 H20C 120.5 . . ? C203 C204 C216 118.5(4) . . ? C203 C204 C205 122.0(4) . . ? C216 C204 C205 119.4(4) . . ? N10 C205 C210 122.2(4) . . ? N10 C205 C204 117.6(4) . . ? C210 C205 C204 120.1(4) . . ? N10 C206 C209 122.4(4) . . ? N10 C206 C207 117.4(5) . . ? C209 C206 C207 120.1(5) . . ? N11 C207 C206 178.9(6) . . ? N12 C208 C209 177.4(8) . . ? N9 C209 C206 123.4(5) . . ? N9 C209 C208 115.7(5) . . ? C206 C209 C208 120.9(5) . . ? N9 C210 C205 121.2(4) . . ? N9 C210 C211 117.7(4) . . ? C205 C210 C211 121.0(4) . . ? C212 C211 C215 120.4(4) . . ? C212 C211 C210 121.3(4) . . ? C215 C211 C210 118.3(4) . . ? C213 C212 C211 118.3(4) . . ? C213 C212 H21A 120.8 . . ? C211 C212 H21A 120.8 . . ? C212 C213 C214 118.4(4) . . ? C212 C213 H21B 120.8 . . ? C214 C213 H21B 120.8 . . ? N8 C214 C213 125.0(4) . . ? N8 C214 H21C 117.5 . . ? C213 C214 H21C 117.5 . . ? N8 C215 C211 120.8(4) . . ? N8 C215 C216 118.2(4) . . ? C211 C215 C216 120.9(4) . . ? N7 C216 C204 121.6(4) . . ? N7 C216 C215 118.2(4) . . ? C204 C216 C215 120.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.585 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.086 # Attachment '1-right-rev.CIF' data_4-right _database_code_depnum_ccdc_archive 'CCDC 738977' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'C32 H12 Cl3 Dy N12' ; _chemical_name_common "'C32 H12 Cl3 Dy N12'" _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H12 Cl3 Dy N12' _chemical_formula_sum 'C32 H12 Cl3 Dy N12' _chemical_formula_weight 833.39 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.900(3) _cell_length_b 8.168(2) _cell_length_c 18.093(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.6970(10) _cell_angle_gamma 90.00 _cell_volume 1543.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4576 _cell_measurement_theta_min 3.1680 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 2.728 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7335 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10169 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5017 _reflns_number_gt 4898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics ? _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0391P)^2^+0.5429P] 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 0.000(8) _chemical_absolute_configuration ad _refine_ls_number_reflns 5017 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 Dy1 Dy 0.349369(7) 0.88902(2) 0.018505(4) 0.02368(2) Uani 1 1 d . . . Cl1 Cl 0.48927(8) 0.62971(11) -0.00327(5) 0.03702(15) Uani 1 1 d . . . Cl2 Cl 0.28343(6) 0.72317(9) 0.12589(3) 0.03774(17) Uani 1 1 d . . . Cl3 Cl 0.15100(6) 1.06780(9) -0.05169(4) 0.03867(18) Uani 1 1 d . . . N1 N 0.34171(14) 0.8711(3) -0.12884(9) 0.0254(5) Uani 1 1 d . . . N2 N 0.18362(18) 0.6867(3) -0.06727(11) 0.0278(6) Uani 1 1 d . . . N3 N -0.06763(19) 0.5323(3) -0.32297(12) 0.0370(6) Uani 1 1 d . . . N4 N 0.09485(19) 0.7192(3) -0.38551(11) 0.0354(6) Uani 1 1 d . . . N5 N -0.0427(3) 0.6533(4) -0.57750(14) 0.0673(10) Uani 1 1 d . . . N6 N -0.2737(2) 0.3843(6) -0.48963(13) 0.0660(8) Uani 1 1 d . . . N7 N 0.34923(19) 1.0959(3) 0.13010(11) 0.0296(5) Uani 1 1 d . . . N8 N 0.55210(14) 0.8935(4) 0.13900(9) 0.0272(4) Uani 1 1 d . . . N9 N 0.69145(19) 0.9494(3) 0.41492(11) 0.0342(6) Uani 1 1 d . . . N10 N 0.4661(2) 1.1270(3) 0.40769(12) 0.0356(6) Uani 1 1 d . . . N11 N 0.8198(2) 0.9147(4) 0.60898(12) 0.0557(8) Uani 1 1 d . . . N12 N 0.5026(3) 1.1531(4) 0.60271(15) 0.0712(10) Uani 1 1 d . . . C101 C 0.1167(2) 0.5807(4) -0.03890(15) 0.0356(7) Uani 1 1 d . . . H10A H 0.1364 0.5703 0.0144 0.043 Uiso 1 1 calc R . . C102 C 0.0187(2) 0.4844(4) -0.08438(16) 0.0376(7) Uani 1 1 d . . . H10C H -0.0247 0.4112 -0.0615 0.045 Uiso 1 1 calc R . . C103 C -0.0131(2) 0.4976(3) -0.16197(15) 0.0347(7) Uani 1 1 d . . . H10B H -0.0806 0.4371 -0.1931 0.042 Uiso 1 1 calc R . . C104 C 0.0569(2) 0.6032(3) -0.19434(14) 0.0287(6) Uani 1 1 d . . . C105 C 0.0313(2) 0.6177(3) -0.27761(14) 0.0306(7) Uani 1 1 d . . . C106 C -0.0834(2) 0.5434(4) -0.39847(15) 0.0370(7) Uani 1 1 d . . . C107 C -0.1921(3) 0.4519(4) -0.44842(17) 0.0482(9) Uani 1 1 d . . . C108 C -0.0247(3) 0.6456(4) -0.51257(17) 0.0465(9) Uani 1 1 d . . . C109 C -0.0034(3) 0.6347(4) -0.42924(15) 0.0382(8) Uani 1 1 d . . . C110 C 0.1119(2) 0.7119(3) -0.30914(13) 0.0286(6) Uani 1 1 d . . . C111 C 0.2205(2) 0.7984(3) -0.25882(13) 0.0268(6) Uani 1 1 d . . . C112 C 0.30700(19) 0.8829(5) -0.28838(11) 0.0326(5) Uani 1 1 d . . . H11A H 0.2936 0.8915 -0.3414 0.039 Uiso 1 1 calc R . . C113 C 0.4119(2) 0.9530(3) -0.23804(14) 0.0354(7) Uani 1 1 d . . . H11C H 0.4731 1.0065 -0.2560 0.042 Uiso 1 1 calc R . . C114 C 0.4251(2) 0.9427(3) -0.15934(14) 0.0326(7) Uani 1 1 d . . . H11B H 0.4977 0.9893 -0.1257 0.039 Uiso 1 1 calc R . . C115 C 0.2417(2) 0.7936(3) -0.17829(13) 0.0248(6) Uani 1 1 d . . . C116 C 0.1573(2) 0.6938(3) -0.14588(13) 0.0263(6) Uani 1 1 d . . . C201 C 0.2629(2) 1.2096(4) 0.12572(15) 0.0375(7) Uani 1 1 d . . . H20C H 0.2126 1.2401 0.0769 0.045 Uiso 1 1 calc R . . C202 C 0.2408(2) 1.2887(4) 0.18926(16) 0.0407(8) Uani 1 1 d . . . H20B H 0.1789 1.3700 0.1825 0.049 Uiso 1 1 calc R . . C203 C 0.3126(2) 1.2436(4) 0.26160(15) 0.0369(7) Uani 1 1 d . . . H20A H 0.2975 1.2897 0.3052 0.044 Uiso 1 1 calc R . . C204 C 0.4089(2) 1.1270(3) 0.26873(13) 0.0295(7) Uani 1 1 d . . . C205 C 0.4951(2) 1.0805(3) 0.34334(13) 0.0296(6) Uani 1 1 d . . . C206 C 0.5482(2) 1.0821(4) 0.47405(14) 0.0376(7) Uani 1 1 d . . . C207 C 0.5210(3) 1.1258(4) 0.54594(17) 0.0493(9) Uani 1 1 d . . . C208 C 0.7512(2) 0.9536(3) 0.55151(15) 0.0388(8) Uani 1 1 d . . . C209 C 0.6610(2) 0.9960(4) 0.47779(13) 0.0329(7) Uani 1 1 d . . . C210 C 0.6054(2) 0.9880(3) 0.34677(14) 0.0303(7) Uani 1 1 d . . . C211 C 0.6298(2) 0.9266(3) 0.27690(12) 0.0274(7) Uani 1 1 d . . . C212 C 0.7402(2) 0.8410(3) 0.27854(14) 0.0318(8) Uani 1 1 d . . . H21A H 0.8007 0.8172 0.3251 0.038 Uiso 1 1 calc R . . C213 C 0.7583(2) 0.7920(3) 0.20972(15) 0.0342(7) Uani 1 1 d . . . H21C H 0.8337 0.7400 0.2086 0.041 Uiso 1 1 calc R . . C214 C 0.6620(2) 0.8214(3) 0.14210(14) 0.0298(6) Uani 1 1 d . . . H21B H 0.6756 0.7883 0.0959 0.036 Uiso 1 1 calc R . . C215 C 0.5379(2) 0.9557(3) 0.20591(14) 0.0272(6) Uani 1 1 d . . . C216 C 0.4294(2) 1.0593(3) 0.20203(13) 0.0267(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02665(4) 0.02380(5) 0.02105(4) 0.00087(6) 0.00761(3) 0.00073(6) Cl1 0.0450(3) 0.0355(3) 0.0286(2) -0.0032(2) 0.0075(2) 0.0149(2) Cl2 0.0463(3) 0.0397(4) 0.0293(3) 0.0035(3) 0.0142(2) -0.0087(3) Cl3 0.0383(3) 0.0426(4) 0.0344(3) 0.0048(3) 0.0092(2) 0.0119(3) N1 0.0264(7) 0.0277(11) 0.0216(7) -0.0008(10) 0.0063(6) -0.0029(11) N2 0.0309(10) 0.0241(11) 0.0243(10) 0.0028(8) 0.0012(8) -0.0052(9) N3 0.0344(10) 0.0409(13) 0.0316(11) -0.0039(10) 0.0030(9) -0.0035(10) N4 0.0371(10) 0.0405(13) 0.0256(10) -0.0009(10) 0.0040(8) 0.0043(11) N5 0.0707(16) 0.097(2) 0.0298(12) 0.0051(14) 0.0080(12) 0.0168(17) N6 0.0517(12) 0.0801(16) 0.0551(13) -0.024(2) -0.0023(11) -0.021(2) N7 0.0387(10) 0.0246(11) 0.0275(10) -0.0008(8) 0.0130(8) 0.0036(9) N8 0.0317(7) 0.0280(9) 0.0238(7) 0.0021(13) 0.0110(6) -0.0022(14) N9 0.0389(10) 0.0409(13) 0.0218(9) -0.0013(8) 0.0074(8) -0.0014(9) N10 0.0428(11) 0.0381(13) 0.0288(10) -0.0065(9) 0.0148(9) 0.0012(10) N11 0.0537(11) 0.077(2) 0.0359(10) 0.0112(14) 0.0122(9) 0.0006(16) N12 0.0848(17) 0.096(2) 0.0382(13) 0.0017(15) 0.0259(12) 0.0302(17) C101 0.0368(11) 0.0398(16) 0.0325(12) 0.0042(12) 0.0137(10) -0.0037(13) C102 0.0326(11) 0.0398(16) 0.0425(14) 0.0026(12) 0.0141(10) -0.0104(12) C103 0.0283(11) 0.0345(15) 0.0427(14) -0.0045(11) 0.0122(10) -0.0040(11) C104 0.0285(10) 0.0284(13) 0.0277(11) -0.0008(10) 0.0058(9) 0.0068(11) C105 0.0250(10) 0.0332(15) 0.0313(12) -0.0032(10) 0.0046(10) 0.0066(11) C106 0.0328(11) 0.0397(16) 0.0343(13) -0.0043(12) 0.0031(10) -0.0014(12) C107 0.0430(14) 0.058(2) 0.0402(14) -0.0095(13) 0.0067(12) -0.0004(14) C108 0.0476(16) 0.0538(18) 0.0353(15) -0.0022(13) 0.0072(12) 0.0055(15) C109 0.0369(13) 0.0393(16) 0.0311(14) -0.0012(12) -0.0017(11) 0.0085(13) C110 0.0292(10) 0.0290(13) 0.0250(11) 0.0008(10) 0.0037(9) 0.0057(11) C111 0.0257(10) 0.0267(13) 0.0257(11) 0.0027(10) 0.0040(9) 0.0032(10) C112 0.0378(9) 0.0347(12) 0.0258(9) -0.0037(17) 0.0099(8) 0.0022(19) C113 0.0426(11) 0.0354(14) 0.0353(12) 0.0025(10) 0.0226(10) 0.0010(11) C114 0.0294(11) 0.0321(15) 0.0337(12) -0.0018(10) 0.0052(10) -0.0058(10) C115 0.0264(10) 0.0213(13) 0.0267(11) 0.0018(10) 0.0079(9) 0.0037(10) C116 0.0265(10) 0.0281(13) 0.0249(11) 0.0001(10) 0.0084(9) 0.0039(10) C201 0.0388(12) 0.0367(16) 0.0357(13) -0.0051(12) 0.0085(11) 0.0028(13) C202 0.0351(12) 0.0405(17) 0.0460(15) -0.0006(13) 0.0107(11) 0.0107(13) C203 0.0408(12) 0.0408(16) 0.0334(12) -0.0072(12) 0.0172(10) 0.0027(12) C204 0.0333(11) 0.0313(14) 0.0252(11) -0.0035(10) 0.0103(9) -0.0089(11) C205 0.0378(11) 0.0288(13) 0.0265(11) -0.0050(10) 0.0159(9) -0.0034(11) C206 0.0463(13) 0.0387(16) 0.0288(12) -0.0049(11) 0.0125(10) -0.0103(13) C207 0.0568(15) 0.059(2) 0.0333(14) -0.0022(14) 0.0145(12) 0.0120(15) C208 0.0427(12) 0.0480(17) 0.0281(12) 0.0015(11) 0.0141(10) -0.0018(12) C209 0.0394(13) 0.0323(16) 0.0271(13) 0.0025(10) 0.0096(10) -0.0056(11) C210 0.0363(11) 0.0270(14) 0.0293(12) 0.0017(10) 0.0124(9) -0.0052(11) C211 0.0322(10) 0.0287(18) 0.0200(10) -0.0037(9) 0.0053(8) -0.0042(10) C212 0.0322(11) 0.0350(18) 0.0270(11) -0.0008(9) 0.0068(9) 0.0013(10) C213 0.0309(11) 0.0346(15) 0.0379(13) -0.0043(11) 0.0112(10) 0.0029(12) C214 0.0305(10) 0.0347(14) 0.0272(11) -0.0054(10) 0.0128(9) -0.0038(10) C215 0.0293(10) 0.0241(12) 0.0283(11) -0.0020(9) 0.0085(9) -0.0058(10) C216 0.0345(10) 0.0234(13) 0.0244(10) 0.0019(10) 0.0121(9) -0.0031(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 Dy1 N2 2.606(2) . ? Dy1 Cl3 2.6159(8) . ? Dy1 N8 2.6208(15) . ? Dy1 Cl2 2.6324(8) . ? Dy1 N7 2.633(2) . ? Dy1 N1 2.6472(17) . ? Dy1 Cl1 2.7041(11) . ? Dy1 Cl1 2.7043(10) 2_655 ? Cl1 Dy1 2.7043(10) 2_645 ? N1 C114 1.327(3) . ? N1 C115 1.352(3) . ? N2 C101 1.327(4) . ? N2 C116 1.369(3) . ? N3 C106 1.330(4) . ? N3 C105 1.347(3) . ? N4 C109 1.327(3) . ? N4 C110 1.342(3) . ? N5 C108 1.136(4) . ? N6 C107 1.127(4) . ? N7 C201 1.309(3) . ? N7 C216 1.376(3) . ? N8 C214 1.322(3) . ? N8 C215 1.362(3) . ? N9 C209 1.329(3) . ? N9 C210 1.355(3) . ? N10 C206 1.327(3) . ? N10 C205 1.346(3) . ? N11 C208 1.138(3) . ? N12 C207 1.124(4) . ? C101 C102 1.390(4) . ? C101 H10A 0.9300 . ? C102 C103 1.350(4) . ? C102 H10C 0.9300 . ? C103 C104 1.387(4) . ? C103 H10B 0.9300 . ? C104 C116 1.402(3) . ? C104 C105 1.456(3) . ? C105 C110 1.405(4) . ? C106 C109 1.380(4) . ? C106 C107 1.472(4) . ? C108 C109 1.461(4) . ? C110 C111 1.453(3) . ? C111 C112 1.394(4) . ? C111 C115 1.409(3) . ? C112 C113 1.366(3) . ? C112 H11A 0.9300 . ? C113 C114 1.392(4) . ? C113 H11C 0.9300 . ? C114 H11B 0.9300 . ? C115 C116 1.471(3) . ? C201 C202 1.398(4) . ? C201 H20C 0.9300 . ? C202 C203 1.368(4) . ? C202 H20B 0.9300 . ? C203 C204 1.395(4) . ? C203 H20A 0.9300 . ? C204 C216 1.402(4) . ? C204 C205 1.456(3) . ? C205 C210 1.405(4) . ? C206 C209 1.401(4) . ? C206 C207 1.459(4) . ? C208 C209 1.453(3) . ? C210 C211 1.454(3) . ? C211 C212 1.385(3) . ? C211 C215 1.403(3) . ? C212 C213 1.375(4) . ? C212 H21A 0.9300 . ? C213 C214 1.385(3) . ? C213 H21C 0.9300 . ? C214 H21B 0.9300 . ? C215 C216 1.439(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 N2 Dy1 Cl3 74.33(5) . . ? N2 Dy1 N8 141.15(8) . . ? Cl3 Dy1 N8 141.06(7) . . ? N2 Dy1 Cl2 79.84(5) . . ? Cl3 Dy1 Cl2 106.43(3) . . ? N8 Dy1 Cl2 74.75(5) . . ? N2 Dy1 N7 135.27(7) . . ? Cl3 Dy1 N7 80.30(5) . . ? N8 Dy1 N7 62.56(7) . . ? Cl2 Dy1 N7 72.77(5) . . ? N2 Dy1 N1 63.21(7) . . ? Cl3 Dy1 N1 76.08(5) . . ? N8 Dy1 N1 127.85(5) . . ? Cl2 Dy1 N1 141.13(5) . . ? N7 Dy1 N1 143.22(7) . . ? N2 Dy1 Cl1 74.93(5) . . ? Cl3 Dy1 Cl1 142.05(2) . . ? N8 Dy1 Cl1 75.89(6) . . ? Cl2 Dy1 Cl1 89.39(3) . . ? N7 Dy1 Cl1 137.64(4) . . ? N1 Dy1 Cl1 70.48(5) . . ? N2 Dy1 Cl1 139.48(5) . 2_655 ? Cl3 Dy1 Cl1 90.90(3) . 2_655 ? N8 Dy1 Cl1 69.94(6) . 2_655 ? Cl2 Dy1 Cl1 140.61(2) . 2_655 ? N7 Dy1 Cl1 75.84(5) . 2_655 ? N1 Dy1 Cl1 76.75(5) . 2_655 ? Cl1 Dy1 Cl1 98.29(2) . 2_655 ? Dy1 Cl1 Dy1 174.16(4) . 2_645 ? C114 N1 C115 116.70(19) . . ? C114 N1 Dy1 124.55(14) . . ? C115 N1 Dy1 118.58(15) . . ? C101 N2 C116 117.1(2) . . ? C101 N2 Dy1 123.19(16) . . ? C116 N2 Dy1 119.61(16) . . ? C106 N3 C105 115.8(2) . . ? C109 N4 C110 116.1(2) . . ? C201 N7 C216 117.5(2) . . ? C201 N7 Dy1 124.61(15) . . ? C216 N7 Dy1 116.47(16) . . ? C214 N8 C215 117.47(17) . . ? C214 N8 Dy1 124.50(16) . . ? C215 N8 Dy1 117.44(14) . . ? C209 N9 C210 115.8(2) . . ? C206 N10 C205 116.1(2) . . ? N2 C101 C102 123.7(2) . . ? N2 C101 H10A 118.2 . . ? C102 C101 H10A 118.2 . . ? C103 C102 C101 119.6(3) . . ? C103 C102 H10C 120.2 . . ? C101 C102 H10C 120.2 . . ? C102 C103 C104 118.7(2) . . ? C102 C103 H10B 120.6 . . ? C104 C103 H10B 120.6 . . ? C103 C104 C116 119.3(2) . . ? C103 C104 C105 121.5(2) . . ? C116 C104 C105 119.1(2) . . ? N3 C105 C110 121.4(2) . . ? N3 C105 C104 118.0(2) . . ? C110 C105 C104 120.6(2) . . ? N3 C106 C109 122.8(2) . . ? N3 C106 C107 116.1(3) . . ? C109 C106 C107 121.2(3) . . ? N6 C107 C106 176.7(4) . . ? N5 C108 C109 179.2(4) . . ? N4 C109 C106 122.4(3) . . ? N4 C109 C108 116.5(3) . . ? C106 C109 C108 121.2(2) . . ? N4 C110 C105 121.6(2) . . ? N4 C110 C111 118.1(2) . . ? C105 C110 C111 120.2(2) . . ? C112 C111 C115 118.9(2) . . ? C112 C111 C110 121.3(2) . . ? C115 C111 C110 119.8(2) . . ? C113 C112 C111 118.7(2) . . ? C113 C112 H11A 120.6 . . ? C111 C112 H11A 120.6 . . ? C112 C113 C114 118.5(2) . . ? C112 C113 H11C 120.7 . . ? C114 C113 H11C 120.7 . . ? N1 C114 C113 124.7(2) . . ? N1 C114 H11B 117.6 . . ? C113 C114 H11B 117.6 . . ? N1 C115 C111 122.2(2) . . ? N1 C115 C116 118.2(2) . . ? C111 C115 C116 119.5(2) . . ? N2 C116 C104 121.3(2) . . ? N2 C116 C115 118.01(19) . . ? C104 C116 C115 120.6(2) . . ? N7 C201 C202 124.6(2) . . ? N7 C201 H20C 117.7 . . ? C202 C201 H20C 117.7 . . ? C203 C202 C201 118.4(3) . . ? C203 C202 H20B 120.8 . . ? C201 C202 H20B 120.8 . . ? C202 C203 C204 118.7(3) . . ? C202 C203 H20A 120.6 . . ? C204 C203 H20A 120.6 . . ? C203 C204 C216 119.4(2) . . ? C203 C204 C205 122.1(2) . . ? C216 C204 C205 118.4(2) . . ? N10 C205 C210 121.6(2) . . ? N10 C205 C204 118.6(2) . . ? C210 C205 C204 119.8(2) . . ? N10 C206 C209 122.5(2) . . ? N10 C206 C207 118.8(3) . . ? C209 C206 C207 118.7(2) . . ? N12 C207 C206 176.9(4) . . ? N11 C208 C209 177.5(3) . . ? N9 C209 C206 122.3(2) . . ? N9 C209 C208 116.6(2) . . ? C206 C209 C208 121.1(2) . . ? N9 C210 C205 121.7(2) . . ? N9 C210 C211 117.3(2) . . ? C205 C210 C211 121.0(2) . . ? C212 C211 C215 119.5(2) . . ? C212 C211 C210 122.05(19) . . ? C215 C211 C210 118.5(2) . . ? C213 C212 C211 118.5(2) . . ? C213 C212 H21A 120.7 . . ? C211 C212 H21A 120.7 . . ? C212 C213 C214 118.7(2) . . ? C212 C213 H21C 120.7 . . ? C214 C213 H21C 120.7 . . ? N8 C214 C213 124.2(2) . . ? N8 C214 H21B 117.9 . . ? C213 C214 H21B 117.9 . . ? N8 C215 C211 121.1(2) . . ? N8 C215 C216 118.5(2) . . ? C211 C215 C216 120.3(2) . . ? N7 C216 C204 120.9(2) . . ? N7 C216 C215 117.6(2) . . ? C204 C216 C215 121.4(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.963 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.064