# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Simon Pope' _publ_contact_author_email POPESJ@CARDIFF.AC.UK _publ_section_title ; A Wavelength and Lifetime Responsive Cryptate-Containing Fluorescent Probe for Zinc Ions in Water ; loop_ _publ_author_name 'Simon Pope' 'Cara Felton' 'Lindsay P. Harding' 'Jennifer E. Jones' 'Benson M Kariuki' 'Craig Rice' # Attachment 'sjp0807_final.cif' data_sjp0807 _database_code_depnum_ccdc_archive 'CCDC 697886' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 Ba N6 O4, 2(Cl1 O4)' _chemical_formula_sum 'C28 H42 Ba Cl2 N6 O12' _chemical_formula_weight 862.92 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' 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' Ba Ba -0.3244 2.2819 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9010(4) _cell_length_b 12.8430(5) _cell_length_c 14.1790(5) _cell_angle_alpha 112.394(2) _cell_angle_beta 94.887(2) _cell_angle_gamma 113.231(2) _cell_volume 1769.16(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5561 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.42 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5775 _exptl_absorpt_correction_T_max 0.9609 _exptl_absorpt_process_details DENZO/SCALEPACK _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11548 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.1286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.42 _reflns_number_total 7946 _reflns_number_gt 5561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+3.6971P] 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 7946 _refine_ls_number_parameters 534 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1977 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.005 _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 C1 C 0.1006(6) -0.1215(7) 0.4205(6) 0.0299(14) Uani 1 1 d U A 1 H1A H 0.1299 -0.0402 0.4851 0.036 Uiso 1 1 calc R A 1 H1B H 0.0710 -0.1908 0.4416 0.036 Uiso 1 1 calc R A 1 C2 C -0.0096(6) -0.1407(7) 0.3421(6) 0.0341(15) Uani 1 1 d U A 1 H2A H -0.0370 -0.2193 0.2754 0.041 Uiso 1 1 calc R A 1 H2B H -0.0828 -0.1482 0.3723 0.041 Uiso 1 1 calc R A 1 C3 C -0.0677(7) -0.0268(8) 0.2646(6) 0.0357(16) Uani 1 1 d U A 1 H3A H -0.1296 -0.0216 0.3063 0.043 Uiso 1 1 calc R A 1 H3B H -0.1127 -0.1046 0.1960 0.043 Uiso 1 1 calc R A 1 C4 C -0.0137(7) 0.0873(8) 0.2454(6) 0.0359(16) Uani 1 1 d U A 1 H4A H -0.0833 0.0969 0.2122 0.043 Uiso 1 1 calc R A 1 H4B H 0.0369 0.1647 0.3134 0.043 Uiso 1 1 calc R A 1 C5 C 0.1047(7) 0.1660(7) 0.1395(6) 0.0325(15) Uani 1 1 d U A 1 H5A H 0.1527 0.2516 0.2007 0.039 Uiso 1 1 calc R A 1 H5B H 0.0292 0.1619 0.0999 0.039 Uiso 1 1 calc R A 1 C6 C 0.1882(7) 0.1416(8) 0.0677(6) 0.0349(16) Uani 1 1 d U A 1 H6A H 0.1376 0.0560 0.0071 0.042 Uiso 1 1 calc R A 1 H6B H 0.2107 0.2039 0.0388 0.042 Uiso 1 1 calc R A 1 C7 C 0.3603(7) 0.0929(7) 0.0318(6) 0.0357(16) Uani 1 1 d U A 1 H7A H 0.4529 0.1282 0.0617 0.043 Uiso 1 1 calc R A 1 H7B H 0.3485 0.1189 -0.0242 0.043 Uiso 1 1 calc R A 1 C8 C 0.2999(8) -0.0510(8) -0.0184(5) 0.0390(17) Uani 1 1 d U A 1 H8A H 0.2062 -0.0881 -0.0431 0.047 Uiso 1 1 calc R A 1 H8B H 0.3312 -0.0834 -0.0803 0.047 Uiso 1 1 calc R A 1 C9 C 0.3030(8) -0.2158(7) 0.0173(6) 0.0402(18) Uani 1 1 d U A 1 H9A H 0.3480 -0.2363 -0.0372 0.048 Uiso 1 1 calc R A 1 H9B H 0.2103 -0.2693 -0.0166 0.048 Uiso 1 1 calc R A 1 C10 C 0.3429(8) -0.2421(7) 0.1065(6) 0.0378(16) Uani 1 1 d U A 1 H10A H 0.3272 -0.3315 0.0780 0.045 Uiso 1 1 calc R A 1 H10B H 0.4348 -0.1859 0.1428 0.045 Uiso 1 1 calc R A 1 C11 C 0.2821(7) -0.2630(7) 0.2556(6) 0.0331(15) Uani 1 1 d U A 1 H11A H 0.3706 -0.2136 0.3017 0.040 Uiso 1 1 calc R A 1 H11B H 0.2625 -0.3535 0.2191 0.040 Uiso 1 1 calc R A 1 C12 C 0.1924(7) -0.2485(7) 0.3217(6) 0.0306(15) Uani 1 1 d U A 1 H12A H 0.1041 -0.3053 0.2754 0.037 Uiso 1 1 calc R A 1 H12B H 0.2040 -0.2772 0.3757 0.037 Uiso 1 1 calc R A 1 C13 C 0.3316(6) -0.0342(6) 0.4587(5) 0.0252(13) Uani 1 1 d U A 1 H13A H 0.4018 -0.0289 0.4249 0.030 Uiso 1 1 calc R A 1 H13B H 0.3380 -0.0706 0.5080 0.030 Uiso 1 1 calc R A 1 C14 C 0.3465(6) 0.0984(6) 0.5211(5) 0.0220(12) Uani 1 1 d U A 1 C15 C 0.3710(6) 0.1503(7) 0.6292(5) 0.0289(14) Uani 1 1 d U A 1 H15 H 0.3921 0.1103 0.6670 0.035 Uiso 1 1 calc R A 1 C16 C 0.3645(6) 0.2606(7) 0.6818(5) 0.0286(14) Uani 1 1 d U A 1 H16 H 0.3790 0.2969 0.7567 0.034 Uiso 1 1 calc R A 1 C17 C 0.3363(6) 0.3213(7) 0.6251(5) 0.0275(14) Uani 1 1 d U A 1 C18 C 0.3277(6) 0.2707(6) 0.5150(5) 0.0234(13) Uani 1 1 d U A 1 C19 C 0.3288(6) 0.3368(6) 0.4467(5) 0.0247(13) Uani 1 1 d U A 1 C20 C 0.3172(7) 0.4500(7) 0.4766(6) 0.0300(14) Uani 1 1 d U A 1 C21 C 0.3448(6) 0.5106(7) 0.4110(6) 0.0315(15) Uani 1 1 d U A 1 H21 H 0.3425 0.5891 0.4310 0.038 Uiso 1 1 calc R A 1 C22 C 0.3746(6) 0.4598(6) 0.3202(6) 0.0279(14) Uani 1 1 d U A 1 H22 H 0.3960 0.5029 0.2778 0.033 Uiso 1 1 calc R A 1 C23 C 0.3732(6) 0.3423(6) 0.2905(5) 0.0245(13) Uani 1 1 d U A 1 C24 C 0.4029(7) 0.2814(7) 0.1884(5) 0.0298(14) Uani 1 1 d U A 1 H24A H 0.4111 0.3329 0.1498 0.036 Uiso 1 1 calc R A 1 H24B H 0.4862 0.2833 0.2059 0.036 Uiso 1 1 calc R A 1 C25 C 0.2212(7) 0.4403(7) 0.6219(6) 0.0313(14) Uani 1 1 d U A 1 H25 H 0.1516 0.3534 0.5724 0.038 Uiso 1 1 calc R A 1 C26 C 0.1640(7) 0.5093(7) 0.6975(6) 0.0350(16) Uani 1 1 d U A 1 H26A H 0.2322 0.5947 0.7488 0.042 Uiso 1 1 calc R A 1 H26B H 0.1281 0.4623 0.7380 0.042 Uiso 1 1 calc R A 1 C27 C 0.0586(8) 0.5241(8) 0.6414(7) 0.0446(19) Uani 1 1 d U A 1 H27A H 0.0936 0.5702 0.6001 0.054 Uiso 1 1 calc R A 1 H27B H -0.0109 0.4389 0.5913 0.054 Uiso 1 1 calc R A 1 C28 C 0.0060(9) 0.5952(10) 0.7198(9) 0.066(3) Uani 1 1 d U A 1 H28A H -0.0250 0.5519 0.7631 0.099 Uiso 1 1 calc R A 1 H28B H -0.0644 0.5982 0.6815 0.099 Uiso 1 1 calc R A 1 H28C H 0.0731 0.6820 0.7658 0.099 Uiso 1 1 calc R A 1 O1 O 0.0337(4) -0.0325(5) 0.3216(4) 0.0333(11) Uani 1 1 d U A 1 O2 O 0.0659(4) 0.0704(5) 0.1760(4) 0.0301(10) Uani 1 1 d U A 1 O3 O 0.3337(5) -0.0858(5) 0.0601(4) 0.0349(11) Uani 1 1 d U A 1 O4 O 0.2699(5) -0.2188(5) 0.1793(4) 0.0325(11) Uani 1 1 d U A 1 Ba1 Ba 0.25525(4) 0.00994(4) 0.24256(3) 0.02635(16) Uani 1 1 d U A 1 N1 N 0.2080(5) -0.1197(5) 0.3755(4) 0.0234(11) Uani 1 1 d U A 1 N2 N 0.3297(5) 0.1586(5) 0.4659(4) 0.0240(11) Uani 1 1 d U A 1 N3 N 0.3523(5) 0.2842(5) 0.3526(4) 0.0223(11) Uani 1 1 d U A 1 N4 N 0.3070(5) 0.1487(6) 0.1171(4) 0.0288(12) Uani 1 1 d U A 1 N5 N 0.3175(6) 0.4255(6) 0.6800(5) 0.0361(14) Uani 1 1 d U A 1 H5 H 0.3611 0.4801 0.7464 0.043 Uiso 1 1 calc R A 1 N6 N 0.2733(7) 0.5018(6) 0.5595(5) 0.0412(15) Uani 1 1 d U A 1 H6 H 0.2775 0.5767 0.5749 0.049 Uiso 1 1 calc R A 1 O5 O 0.5108(4) 0.0513(5) 0.3134(4) 0.0424(13) Uani 1 1 d DU A 1 O6 O 0.6188(5) 0.1964(5) 0.2474(4) 0.0425(13) Uani 1 1 d DU A 1 O7 O 0.7007(5) 0.0647(6) 0.2683(5) 0.0513(15) Uani 1 1 d DU A 1 O8 O 0.7070(6) 0.2350(5) 0.4156(4) 0.0572(17) Uani 1 1 d DU A 1 Cl1 Cl 0.63456(15) 0.13683(15) 0.31015(12) 0.0271(4) Uani 1 1 d DU A 1 O9 O 0.0279(6) -0.2180(5) 0.0703(6) 0.033(2) Uani 0.544(5) 1 d PDU A 1 O10 O -0.0652(10) -0.4041(8) 0.0943(7) 0.085(5) Uani 0.544(5) 1 d PDU A 1 O11 O -0.1829(7) -0.3758(10) -0.0273(10) 0.123(6) Uani 0.544(5) 1 d PDU A 1 O12 O -0.0128(11) -0.4197(9) -0.0611(8) 0.139(8) Uani 0.544(5) 1 d PDU A 1 Cl2 Cl -0.0593(4) -0.3548(4) 0.0196(4) 0.0784(18) Uani 0.544(5) 1 d PDU A 1 O9A O -0.3154(19) -0.4599(18) -0.0728(10) 0.064(6) Uani 0.228(2) 1 d PDU A 2 O10A O -0.4860(11) -0.5276(14) 0.0013(17) 0.073(6) Uani 0.228(2) 1 d PDU . 2 O11A O -0.3459(18) -0.3098(11) 0.0678(14) 0.038(5) Uani 0.228(2) 1 d PDU A 2 O12A O -0.2810(15) -0.4471(17) 0.0989(12) 0.035(4) Uani 0.228(2) 1 d PDU A 2 Cl2A Cl -0.3584(9) -0.4361(8) 0.0238(8) 0.041(3) Uani 0.228(2) 1 d PDU . 2 O9B O -0.3524(16) -0.5051(14) 0.0913(12) 0.020(3) Uani 0.228(2) 1 d PDU A 3 O10B O -0.4091(19) -0.3638(19) 0.0544(18) 0.073(7) Uani 0.228(2) 1 d PDU A 3 O11B O -0.2005(13) -0.3380(18) 0.0680(18) 0.082(7) Uani 0.228(2) 1 d PDU A 3 O12B O -0.372(2) -0.5082(17) -0.0773(9) 0.070(7) Uani 0.228(2) 1 d PDU A 3 Cl2B Cl -0.3331(10) -0.4274(9) 0.0347(9) 0.046(3) Uani 0.228(2) 1 d PDU A 3 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 C1 0.021(3) 0.037(3) 0.036(3) 0.022(3) 0.012(3) 0.011(3) C2 0.018(3) 0.040(4) 0.049(4) 0.026(3) 0.012(3) 0.011(3) C3 0.020(3) 0.050(4) 0.051(4) 0.035(3) 0.012(3) 0.017(3) C4 0.027(3) 0.049(4) 0.046(4) 0.028(3) 0.013(3) 0.024(3) C5 0.026(3) 0.036(3) 0.044(4) 0.027(3) 0.005(3) 0.015(3) C6 0.029(3) 0.042(4) 0.036(3) 0.025(3) 0.006(3) 0.012(3) C7 0.037(4) 0.043(4) 0.033(3) 0.021(3) 0.019(3) 0.018(3) C8 0.042(4) 0.046(4) 0.024(3) 0.013(3) 0.009(3) 0.019(3) C9 0.040(4) 0.031(4) 0.032(3) 0.004(3) 0.014(3) 0.009(3) C10 0.039(4) 0.033(3) 0.044(4) 0.015(3) 0.022(3) 0.020(3) C11 0.033(3) 0.034(3) 0.039(3) 0.017(3) 0.009(3) 0.022(3) C12 0.029(3) 0.030(3) 0.039(3) 0.021(3) 0.011(3) 0.015(3) C13 0.020(3) 0.029(3) 0.033(3) 0.019(3) 0.007(2) 0.014(3) C14 0.017(3) 0.029(3) 0.027(3) 0.020(2) 0.007(2) 0.009(2) C15 0.026(3) 0.031(3) 0.033(3) 0.021(3) 0.006(3) 0.011(3) C16 0.023(3) 0.035(3) 0.030(3) 0.018(3) 0.010(2) 0.012(3) C17 0.021(3) 0.032(3) 0.032(3) 0.016(3) 0.008(2) 0.013(3) C18 0.015(3) 0.025(3) 0.033(3) 0.016(2) 0.007(2) 0.010(2) C19 0.017(3) 0.026(3) 0.032(3) 0.016(2) 0.011(2) 0.008(2) C20 0.029(3) 0.027(3) 0.039(3) 0.019(3) 0.011(3) 0.014(3) C21 0.025(3) 0.028(3) 0.047(4) 0.021(3) 0.013(3) 0.013(3) C22 0.023(3) 0.022(3) 0.042(3) 0.022(3) 0.008(3) 0.006(3) C23 0.016(3) 0.031(3) 0.031(3) 0.019(2) 0.005(2) 0.009(2) C24 0.026(3) 0.037(3) 0.034(3) 0.024(3) 0.010(3) 0.014(3) C25 0.037(3) 0.031(3) 0.040(3) 0.022(3) 0.016(3) 0.022(3) C26 0.033(4) 0.036(4) 0.041(4) 0.021(3) 0.012(3) 0.015(3) C27 0.035(4) 0.041(4) 0.058(4) 0.025(4) 0.007(3) 0.017(3) C28 0.045(5) 0.050(6) 0.089(7) 0.016(5) 0.016(5) 0.024(5) O1 0.020(2) 0.044(3) 0.049(3) 0.032(2) 0.012(2) 0.015(2) O2 0.021(2) 0.041(3) 0.040(3) 0.028(2) 0.0119(19) 0.016(2) O3 0.038(3) 0.034(3) 0.027(2) 0.009(2) 0.008(2) 0.015(2) O4 0.028(2) 0.034(3) 0.040(3) 0.019(2) 0.013(2) 0.016(2) Ba1 0.0232(2) 0.0307(3) 0.0290(2) 0.01627(18) 0.00751(16) 0.01333(18) N1 0.022(3) 0.029(3) 0.027(3) 0.017(2) 0.008(2) 0.016(2) N2 0.011(2) 0.028(3) 0.032(3) 0.016(2) 0.004(2) 0.007(2) N3 0.018(2) 0.028(3) 0.027(3) 0.018(2) 0.006(2) 0.012(2) N4 0.026(3) 0.037(3) 0.033(3) 0.020(2) 0.010(2) 0.018(2) N5 0.033(3) 0.038(3) 0.035(3) 0.011(3) 0.011(2) 0.020(3) N6 0.055(4) 0.028(3) 0.052(3) 0.020(3) 0.030(3) 0.025(3) O5 0.027(3) 0.047(3) 0.050(3) 0.023(3) 0.012(2) 0.013(2) O6 0.059(4) 0.044(3) 0.044(3) 0.032(3) 0.015(3) 0.031(3) O7 0.054(4) 0.060(4) 0.080(4) 0.046(3) 0.040(3) 0.044(3) O8 0.064(4) 0.051(4) 0.037(3) 0.022(3) -0.002(3) 0.010(3) Cl1 0.0267(8) 0.0279(9) 0.0331(9) 0.0180(7) 0.0103(7) 0.0141(7) O9 0.015(4) 0.046(5) 0.041(5) 0.026(4) 0.002(3) 0.011(4) O10 0.079(9) 0.063(8) 0.065(7) 0.045(6) -0.013(6) -0.020(7) O11 0.107(9) 0.089(8) 0.111(9) 0.042(7) -0.038(8) 0.006(8) O12 0.139(13) 0.070(10) 0.092(10) -0.021(8) 0.030(10) -0.002(10) Cl2 0.052(3) 0.076(3) 0.080(3) 0.048(3) -0.014(2) -0.001(2) O9A 0.086(10) 0.041(9) 0.053(8) 0.025(7) 0.004(8) 0.017(8) O10A 0.074(7) 0.044(7) 0.070(7) 0.004(7) 0.006(7) 0.025(7) O11A 0.066(10) 0.028(8) 0.032(8) 0.020(7) 0.025(8) 0.024(8) O12A 0.036(4) 0.036(4) 0.034(4) 0.016(2) 0.006(2) 0.018(2) Cl2A 0.062(5) 0.032(4) 0.033(4) 0.012(3) 0.000(3) 0.029(3) O9B 0.021(4) 0.020(4) 0.019(4) 0.008(2) 0.007(2) 0.010(2) O10B 0.077(11) 0.056(10) 0.054(10) 0.009(9) 0.006(10) 0.020(9) O11B 0.066(9) 0.063(9) 0.065(9) 0.003(9) -0.007(9) 0.011(8) O12B 0.091(11) 0.047(10) 0.043(9) 0.009(8) 0.005(9) 0.020(9) Cl2B 0.058(5) 0.036(4) 0.041(4) 0.008(3) 0.005(4) 0.029(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 C1 N1 1.472(8) . ? C1 C2 1.518(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O1 1.431(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.437(8) . ? C3 C4 1.491(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.438(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O2 1.438(8) . ? C5 C6 1.515(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.475(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N4 1.486(9) . ? C7 C8 1.518(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O3 1.430(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O3 1.413(9) . ? C9 C10 1.513(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O4 1.425(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O4 1.421(8) . ? C11 C12 1.499(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N1 1.458(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N1 1.484(8) . ? C13 C14 1.517(9) . ? C13 Ba1 3.434(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N2 1.344(8) . ? C14 C15 1.369(9) . ? C15 C16 1.364(10) . ? C15 H15 0.9500 . ? C16 C17 1.415(9) . ? C16 H16 0.9500 . ? C17 N5 1.385(9) . ? C17 C18 1.421(9) . ? C18 N2 1.350(8) . ? C18 C19 1.510(9) . ? C19 N3 1.356(8) . ? C19 C20 1.418(9) . ? C20 N6 1.370(9) . ? C20 C21 1.407(10) . ? C21 C22 1.353(10) . ? C21 H21 0.9500 . ? C22 C23 1.396(9) . ? C22 H22 0.9500 . ? C23 N3 1.337(8) . ? C23 C24 1.509(10) . ? C24 N4 1.478(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N6 1.425(9) . ? C25 N5 1.470(9) . ? C25 C26 1.508(10) . ? C25 H25 1.0000 . ? C26 C27 1.541(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.502(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O1 Ba1 2.888(5) . ? O2 Ba1 2.855(4) . ? O3 Ba1 2.823(5) . ? O4 Ba1 2.809(5) . ? Ba1 N2 2.836(5) . ? Ba1 O5 2.888(5) . ? Ba1 N4 2.908(6) . ? Ba1 N3 2.910(6) . ? Ba1 N1 2.911(5) . ? Ba1 O9 3.006(6) . ? N5 H5 0.8800 . ? N6 H6 0.8800 . ? O5 Cl1 1.467(5) . ? O6 Cl1 1.420(4) . ? O7 Cl1 1.437(5) . ? O8 Cl1 1.433(5) . ? O9 Cl2 1.468(5) . ? O10 Cl2 1.419(4) . ? O11 Cl2 1.436(5) . ? O12 Cl2 1.434(5) . ? O9A Cl2A 1.467(5) . ? O10A O10A 0.90(4) 2_445 ? O10A Cl2A 1.419(4) . ? O10A Cl2A 1.69(2) 2_445 ? O11A Cl2A 1.436(5) . ? O12A Cl2A 1.434(5) . ? Cl2A O10A 1.69(2) 2_445 ? O9B Cl2B 1.467(5) . ? O10B Cl2B 1.419(4) . ? O11B Cl2B 1.436(5) . ? O12B Cl2B 1.433(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 N1 C1 C2 112.0(6) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O1 C2 C1 107.4(6) . . ? O1 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O1 C3 C4 109.3(6) . . ? O1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? O2 C4 C3 108.1(6) . . ? O2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O2 C5 C6 108.0(6) . . ? O2 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O2 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N4 C6 C5 116.2(6) . . ? N4 C6 H6A 108.2 . . ? C5 C6 H6A 108.2 . . ? N4 C6 H6B 108.2 . . ? C5 C6 H6B 108.2 . . ? H6A C6 H6B 107.4 . . ? N4 C7 C8 113.7(6) . . ? N4 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N4 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O3 C8 C7 107.9(6) . . ? O3 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O3 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? O3 C9 C10 108.5(6) . . ? O3 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O4 C10 C9 107.8(6) . . ? O4 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O4 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? O4 C11 C12 109.6(5) . . ? O4 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O4 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N1 C12 C11 114.9(6) . . ? N1 C12 H12A 108.5 . . ? C11 C12 H12A 108.5 . . ? N1 C12 H12B 108.5 . . ? C11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? N1 C13 C14 112.0(5) . . ? N1 C13 Ba1 57.2(3) . . ? C14 C13 Ba1 83.7(3) . . ? N1 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? Ba1 C13 H13A 73.8 . . ? N1 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? Ba1 C13 H13B 164.9 . . ? H13A C13 H13B 107.9 . . ? N2 C14 C15 122.4(6) . . ? N2 C14 C13 117.6(5) . . ? C15 C14 C13 120.0(6) . . ? C16 C15 C14 118.7(6) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 120.2(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? N5 C17 C16 118.1(6) . . ? N5 C17 C18 124.0(6) . . ? C16 C17 C18 117.9(6) . . ? N2 C18 C17 119.2(6) . . ? N2 C18 C19 114.7(6) . . ? C17 C18 C19 125.8(6) . . ? N3 C19 C20 120.1(6) . . ? N3 C19 C18 114.1(6) . . ? C20 C19 C18 125.6(6) . . ? N6 C20 C21 116.5(6) . . ? N6 C20 C19 126.2(6) . . ? C21 C20 C19 117.2(6) . . ? C22 C21 C20 121.6(7) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 118.3(6) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? N3 C23 C22 121.9(6) . . ? N3 C23 C24 118.4(6) . . ? C22 C23 C24 119.7(6) . . ? N4 C24 C23 114.5(6) . . ? N4 C24 H24A 108.6 . . ? C23 C24 H24A 108.6 . . ? N4 C24 H24B 108.6 . . ? C23 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? N6 C25 N5 111.0(6) . . ? N6 C25 C26 112.1(6) . . ? N5 C25 C26 110.4(6) . . ? N6 C25 H25 107.7 . . ? N5 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C25 C26 C27 113.3(6) . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 111.5(7) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C2 O1 C3 113.0(5) . . ? C2 O1 Ba1 113.6(4) . . ? C3 O1 Ba1 115.5(4) . . ? C4 O2 C5 111.5(5) . . ? C4 O2 Ba1 115.4(4) . . ? C5 O2 Ba1 117.3(4) . . ? C9 O3 C8 112.8(5) . . ? C9 O3 Ba1 116.1(4) . . ? C8 O3 Ba1 112.0(4) . . ? C11 O4 C10 112.5(5) . . ? C11 O4 Ba1 119.1(4) . . ? C10 O4 Ba1 116.8(4) . . ? O4 Ba1 O3 59.22(14) . . ? O4 Ba1 N2 113.56(15) . . ? O3 Ba1 N2 146.54(14) . . ? O4 Ba1 O2 132.74(14) . . ? O3 Ba1 O2 105.08(14) . . ? N2 Ba1 O2 101.74(15) . . ? O4 Ba1 O1 104.49(14) . . ? O3 Ba1 O1 142.30(15) . . ? N2 Ba1 O1 69.87(14) . . ? O2 Ba1 O1 58.89(13) . . ? O4 Ba1 O5 67.67(14) . . ? O3 Ba1 O5 72.50(14) . . ? N2 Ba1 O5 74.81(15) . . ? O2 Ba1 O5 155.80(14) . . ? O1 Ba1 O5 136.59(13) . . ? O4 Ba1 N4 121.36(15) . . ? O3 Ba1 N4 62.22(15) . . ? N2 Ba1 N4 116.35(16) . . ? O2 Ba1 N4 61.63(14) . . ? O1 Ba1 N4 119.95(14) . . ? O5 Ba1 N4 97.88(15) . . ? O4 Ba1 N3 155.43(14) . . ? O3 Ba1 N3 116.73(15) . . ? N2 Ba1 N3 54.63(15) . . ? O2 Ba1 N3 71.52(14) . . ? O1 Ba1 N3 91.67(15) . . ? O5 Ba1 N3 87.85(15) . . ? N4 Ba1 N3 62.07(15) . . ? O4 Ba1 N1 60.44(14) . . ? O3 Ba1 N1 119.49(15) . . ? N2 Ba1 N1 61.45(15) . . ? O2 Ba1 N1 118.38(14) . . ? O1 Ba1 N1 59.78(14) . . ? O5 Ba1 N1 81.58(14) . . ? N4 Ba1 N1 177.80(15) . . ? N3 Ba1 N1 115.75(15) . . ? O4 Ba1 O9 65.65(17) . . ? O3 Ba1 O9 71.25(18) . . ? N2 Ba1 O9 139.06(18) . . ? O2 Ba1 O9 67.09(17) . . ? O1 Ba1 O9 71.05(18) . . ? O5 Ba1 O9 130.86(17) . . ? N4 Ba1 O9 93.49(17) . . ? N3 Ba1 O9 138.36(17) . . ? N1 Ba1 O9 88.46(17) . . ? O4 Ba1 C13 69.19(15) . . ? O3 Ba1 C13 120.35(15) . . ? N2 Ba1 C13 44.72(16) . . ? O2 Ba1 C13 132.40(15) . . ? O1 Ba1 C13 75.79(14) . . ? O5 Ba1 C13 61.34(14) . . ? N4 Ba1 C13 152.92(16) . . ? N3 Ba1 C13 97.85(15) . . ? N1 Ba1 C13 25.38(15) . . ? O9 Ba1 C13 113.13(17) . . ? C12 N1 C1 109.8(5) . . ? C12 N1 C13 110.9(5) . . ? C1 N1 C13 111.3(5) . . ? C12 N1 Ba1 112.5(4) . . ? C1 N1 Ba1 114.4(4) . . ? C13 N1 Ba1 97.4(4) . . ? C14 N2 C18 120.8(6) . . ? C14 N2 Ba1 113.9(4) . . ? C18 N2 Ba1 124.3(4) . . ? C23 N3 C19 120.7(6) . . ? C23 N3 Ba1 115.1(4) . . ? C19 N3 Ba1 119.4(4) . . ? C6 N4 C24 111.7(6) . . ? C6 N4 C7 108.7(6) . . ? C24 N4 C7 108.5(5) . . ? C6 N4 Ba1 109.9(4) . . ? C24 N4 Ba1 107.8(4) . . ? C7 N4 Ba1 110.2(4) . . ? C17 N5 C25 116.7(6) . . ? C17 N5 H5 121.6 . . ? C25 N5 H5 121.6 . . ? C20 N6 C25 123.2(6) . . ? C20 N6 H6 118.4 . . ? C25 N6 H6 118.4 . . ? Cl1 O5 Ba1 132.5(3) . . ? O6 Cl1 O8 107.5(3) . . ? O6 Cl1 O7 110.8(3) . . ? O8 Cl1 O7 109.8(4) . . ? O6 Cl1 O5 110.8(3) . . ? O8 Cl1 O5 109.2(3) . . ? O7 Cl1 O5 108.7(3) . . ? Cl2 O9 Ba1 149.9(4) . . ? O10 Cl2 O12 107.3(4) . . ? O10 Cl2 O11 111.0(3) . . ? O12 Cl2 O11 109.7(4) . . ? O10 Cl2 O9 110.8(3) . . ? O12 Cl2 O9 109.2(3) . . ? O11 Cl2 O9 108.8(3) . . ? O10A O10A Cl2A 90.5(15) 2_445 . ? O10A O10A Cl2A 57.2(12) 2_445 2_445 ? Cl2A O10A Cl2A 147.6(13) . 2_445 ? O10A Cl2A O12A 107.3(4) . . ? O10A Cl2A O11A 110.9(3) . . ? O12A Cl2A O11A 109.8(4) . . ? O10A Cl2A O9A 110.8(3) . . ? O12A Cl2A O9A 109.2(3) . . ? O11A Cl2A O9A 108.7(3) . . ? O10A Cl2A O10A 32.4(13) . 2_445 ? O12A Cl2A O10A 130.9(14) . 2_445 ? O11A Cl2A O10A 80.7(12) . 2_445 ? O9A Cl2A O10A 112.1(15) . 2_445 ? O10B Cl2B O12B 107.4(4) . . ? O10B Cl2B O11B 110.9(3) . . ? O12B Cl2B O11B 109.8(4) . . ? O10B Cl2B O9B 110.9(3) . . ? O12B Cl2B O9B 109.3(3) . . ? O11B Cl2B O9B 108.7(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.126 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.175