Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Richard Jones' _publ_contact_author_address ; Department of Chemistry Univ of Texas at Austin 1 University Station Austin Texas 78712-0165 USA ; _publ_contact_author_email RAJONES@MAIL.UTEXAS.EDU _publ_section_title ; Synthesis and Near Infrared Luminescence of a Tetrametallic Zn2Yb2 Architecture from a Trinuclear Zn3L2 Schiff Base Complex ; loop_ _publ_author_name 'Richard Jones' 'Archie L. Holmes' 'Vince Lynch' 'Michael M. Oye' 'Xiaoping Yang' data_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 232601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H40 Br4 N6 O15 Zn3' _chemical_formula_weight 1348.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3783(17) _cell_length_b 23.843(5) _cell_length_c 23.448(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.14(3) _cell_angle_gamma 90.00 _cell_volume 4665.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 5.029 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.3815 _exptl_absorpt_correction_T_max 0.7962 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19253 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10649 _reflns_number_gt 7153 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0381P)^2^+14.6621P] 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 ? _refine_ls_number_reflns 10649 _refine_ls_number_parameters 619 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.08755(7) -0.26098(2) 1.09248(2) 0.02444(14) Uani 1 1 d . . . Zn2 Zn -0.11963(7) -0.35800(2) 0.99970(2) 0.02234(14) Uani 1 1 d . . . Zn3 Zn -0.09045(6) -0.21493(2) 1.22056(2) 0.02271(14) Uani 1 1 d . . . Br1 Br -0.60835(8) -0.11523(3) 0.87417(3) 0.04617(17) Uani 1 1 d . . . Br2' Br -0.47480(7) -0.49718(2) 1.21387(3) 0.03902(15) Uani 1 1 d . . . Br2 Br 0.12612(9) -0.50416(4) 1.27549(3) 0.0705(3) Uani 1 1 d . . . O2' O 0.0215(4) -0.20551(14) 1.14656(13) 0.0240(8) Uani 1 1 d . . . O2 O -0.1821(4) -0.27775(14) 1.01204(13) 0.0234(7) Uani 1 1 d . . . O1' O 0.1076(4) -0.21079(16) 1.04354(15) 0.0339(9) Uani 1 1 d . . . O3 O -0.0175(4) -0.34153(14) 1.08116(13) 0.0228(7) Uani 1 1 d . . . O3' O -0.2018(4) -0.27092(14) 1.16550(13) 0.0246(8) Uani 1 1 d . . . N1' N 0.0787(5) -0.15881(18) 1.25588(17) 0.0250(9) Uani 1 1 d . . . O4 O 0.1948(4) -0.31405(16) 1.16480(15) 0.0332(9) Uani 1 1 d . . . O1 O -0.2349(4) -0.18071(15) 1.05558(15) 0.0351(9) Uani 1 1 d . . . N1 N -0.2746(5) -0.35781(18) 0.92398(17) 0.0261(9) Uani 1 1 d . . . C6 C -0.3584(5) -0.2597(2) 0.9271(2) 0.0235(11) Uani 1 1 d . . . O4' O -0.4215(4) -0.31260(16) 1.09237(15) 0.0332(9) Uani 1 1 d . . . N2 N -0.2143(5) -0.42930(17) 1.02850(18) 0.0242(9) Uani 1 1 d . . . C13 C -0.0555(6) -0.4328(2) 1.1211(2) 0.0254(11) Uani 1 1 d . . . O5' O -0.2632(5) -0.15627(18) 1.22831(19) 0.0467(11) Uani 1 1 d . . . C15' C -0.3999(6) -0.4233(2) 1.2018(2) 0.0289(12) Uani 1 1 d . . . C17' C -0.3841(6) -0.3440(2) 1.1402(2) 0.0245(11) Uani 1 1 d . . . C5 C -0.4539(6) -0.2196(2) 0.8959(2) 0.0277(12) Uani 1 1 d . . . H5A H -0.5033 -0.2291 0.8601 0.033 Uiso 1 1 calc R . . C4 C -0.4755(6) -0.1678(2) 0.9169(2) 0.0292(12) Uani 1 1 d . . . O5 O 0.0749(5) -0.35390(18) 0.95423(16) 0.0405(10) Uani 1 1 d . . . O7' O -0.3993(5) -0.2209(2) 1.2663(2) 0.0557(12) Uani 1 1 d . . . C12' C -0.1272(6) -0.3220(2) 1.2803(2) 0.0271(12) Uani 1 1 d . . . H12A H -0.1070 -0.3451 1.3120 0.033 Uiso 1 1 calc R . . C13' C -0.2305(6) -0.3456(2) 1.2333(2) 0.0246(11) Uani 1 1 d . . . C3 C -0.4032(6) -0.1520(2) 0.9708(2) 0.0308(12) Uani 1 1 d . . . H3A H -0.4192 -0.1163 0.9852 0.037 Uiso 1 1 calc R . . C14 C -0.0198(6) -0.4701(2) 1.1675(2) 0.0317(13) Uani 1 1 d . . . H14A H -0.0682 -0.5052 1.1675 0.038 Uiso 1 1 calc R . . N2' N -0.0599(5) -0.27354(18) 1.28406(16) 0.0246(9) Uani 1 1 d . . . C17 C 0.1285(6) -0.3661(2) 1.1686(2) 0.0261(11) Uani 1 1 d . . . C2 C -0.3087(6) -0.1901(2) 1.0017(2) 0.0254(11) Uani 1 1 d . . . C8 C -0.3560(6) -0.3160(2) 0.9033(2) 0.0252(11) Uani 1 1 d . . . H8A H -0.4206 -0.3223 0.8695 0.030 Uiso 1 1 calc R . . O6 O 0.1519(6) -0.4251(2) 1.0032(2) 0.0630(14) Uani 1 1 d . . . C6' C 0.1773(6) -0.1229(2) 1.1684(2) 0.0251(11) Uani 1 1 d . . . C11' C 0.0210(6) -0.2599(2) 1.3410(2) 0.0327(13) Uani 1 1 d . . . H11A H 0.0682 -0.2939 1.3578 0.039 Uiso 1 1 calc R . . H11B H -0.0590 -0.2471 1.3655 0.039 Uiso 1 1 calc R . . O6' O -0.4871(5) -0.1363(2) 1.2615(2) 0.0596(13) Uani 1 1 d . . . O7 O 0.2949(5) -0.39461(19) 0.93816(17) 0.0479(11) Uani 1 1 d . . . N3' N -0.3823(5) -0.1705(2) 1.25078(19) 0.0321(11) Uani 1 1 d . . . N3 N 0.1703(4) -0.39067(17) 0.96453(15) 0.0150(8) Uani 1 1 d . . . C8' C 0.1622(6) -0.1244(2) 1.2299(2) 0.0259(11) Uani 1 1 d . . . H8'A H 0.2191 -0.0976 1.2521 0.031 Uiso 1 1 calc R . . C16' C -0.4475(6) -0.3958(2) 1.1509(2) 0.0279(12) Uani 1 1 d . . . H16A H -0.5216 -0.4124 1.1241 0.033 Uiso 1 1 calc R . . C9' C 0.0967(6) -0.1582(2) 1.3185(2) 0.0297(12) Uani 1 1 d . . . H9'A H -0.0048 -0.1488 1.3329 0.036 Uiso 1 1 calc R . . H9'B H 0.1748 -0.1300 1.3319 0.036 Uiso 1 1 calc R . . C11 C -0.3266(6) -0.4594(2) 0.9870(2) 0.0308(12) Uani 1 1 d . . . H11C H -0.4292 -0.4403 0.9833 0.037 Uiso 1 1 calc R . . H11D H -0.3434 -0.4972 1.0006 0.037 Uiso 1 1 calc R . . C2' C 0.1610(6) -0.1652(2) 1.0743(2) 0.0291(12) Uani 1 1 d . . . C18 C 0.0175(5) -0.3796(2) 1.1218(2) 0.0219(11) Uani 1 1 d . . . C18' C -0.2694(6) -0.3184(2) 1.1800(2) 0.0240(11) Uani 1 1 d . . . C14' C -0.2976(6) -0.3985(2) 1.2430(2) 0.0293(12) Uani 1 1 d . . . H14B H -0.2720 -0.4168 1.2776 0.035 Uiso 1 1 calc R . . C10 C -0.2580(6) -0.4618(2) 0.9286(2) 0.0318(12) Uani 1 1 d . . . H10A H -0.1424 -0.4651 0.9346 0.038 Uiso 1 1 calc R . . H10B H -0.2985 -0.4951 0.9084 0.038 Uiso 1 1 calc R . . C12 C -0.1700(6) -0.4535(2) 1.0760(2) 0.0273(12) Uani 1 1 d . . . H12B H -0.2164 -0.4881 1.0824 0.033 Uiso 1 1 calc R . . C9 C -0.2990(7) -0.4113(2) 0.8916(2) 0.0345(13) Uani 1 1 d . . . H9A H -0.2327 -0.4112 0.8598 0.041 Uiso 1 1 calc R . . H9B H -0.4100 -0.4138 0.8761 0.041 Uiso 1 1 calc R . . C16 C 0.1633(6) -0.4032(3) 1.2133(2) 0.0335(13) Uani 1 1 d . . . H16B H 0.2378 -0.3939 1.2436 0.040 Uiso 1 1 calc R . . C10' C 0.1515(6) -0.2154(2) 1.3407(2) 0.0304(12) Uani 1 1 d . . . H10C H 0.2006 -0.2110 1.3795 0.036 Uiso 1 1 calc R . . H10D H 0.2336 -0.2290 1.3175 0.036 Uiso 1 1 calc R . . C19 C 0.2979(6) -0.2940(3) 1.2122(2) 0.0383(14) Uani 1 1 d . . . H19A H 0.3339 -0.2569 1.2041 0.057 Uiso 1 1 calc R . . H19B H 0.3887 -0.3185 1.2185 0.057 Uiso 1 1 calc R . . H19C H 0.2405 -0.2932 1.2458 0.057 Uiso 1 1 calc R . . C15 C 0.0857(6) -0.4544(3) 1.2123(2) 0.0351(14) Uani 1 1 d . . . C1' C 0.1486(9) -0.2148(3) 0.9854(2) 0.0518(18) Uani 1 1 d . . . H1'A H 0.2343 -0.1892 0.9797 0.078 Uiso 1 1 calc R . . H1'B H 0.0567 -0.2054 0.9597 0.078 Uiso 1 1 calc R . . H1'C H 0.1820 -0.2524 0.9779 0.078 Uiso 1 1 calc R . . C19' C -0.5488(6) -0.3314(3) 1.0530(2) 0.0388(14) Uani 1 1 d . . . H19D H -0.5623 -0.3058 1.0213 0.058 Uiso 1 1 calc R . . H19E H -0.6460 -0.3329 1.0718 0.058 Uiso 1 1 calc R . . H19F H -0.5243 -0.3681 1.0394 0.058 Uiso 1 1 calc R . . Br1' Br 0.42514(8) -0.01989(3) 1.06377(3) 0.05343(19) Uani 1 1 d . . . C7' C 0.1165(6) -0.1656(2) 1.1313(2) 0.0232(11) Uani 1 1 d . . . C5' C 0.2723(6) -0.0800(2) 1.1480(2) 0.0318(12) Uani 1 1 d . . . H5'A H 0.3148 -0.0524 1.1729 0.038 Uiso 1 1 calc R . . C4' C 0.3023(7) -0.0789(2) 1.0913(2) 0.0351(13) Uani 1 1 d . . . C7 C -0.2800(5) -0.2443(2) 0.98072(19) 0.0223(11) Uani 1 1 d . . . C3' C 0.2505(7) -0.1219(2) 1.0541(2) 0.0343(13) Uani 1 1 d . . . H3'A H 0.2755 -0.1216 1.0162 0.041 Uiso 1 1 calc R . . C1 C -0.2791(10) -0.1313(3) 1.0850(3) 0.078(3) Uani 1 1 d . . . H1A H -0.3399 -0.1070 1.0586 0.117 Uiso 1 1 calc R . . H1B H -0.1842 -0.1122 1.1006 0.117 Uiso 1 1 calc R . . H1C H -0.3429 -0.1416 1.1154 0.117 Uiso 1 1 calc R . . O1W' O 0.0000 -0.5000 1.5000 0.313(15) Uani 1 2 d SD . . O1W O 0.028(3) -0.4662(10) 1.4207(7) 0.23(2) Uani 0.50 1 d PD . . C1W' C 0.042(3) -0.4849(14) 1.4443(7) 0.113(10) Uani 0.50 1 d PD . . C1W C -0.060(3) -0.4181(11) 1.4098(11) 0.095(8) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0321(3) 0.0238(3) 0.0169(3) -0.0034(2) -0.0006(2) -0.0027(3) Zn2 0.0251(3) 0.0220(3) 0.0199(3) -0.0016(2) 0.0016(2) -0.0027(2) Zn3 0.0222(3) 0.0276(3) 0.0180(3) -0.0030(2) 0.0005(2) -0.0008(2) Br1 0.0530(4) 0.0361(3) 0.0448(4) 0.0007(3) -0.0206(3) 0.0102(3) Br2' 0.0363(3) 0.0275(3) 0.0517(4) 0.0054(3) -0.0051(3) -0.0056(2) Br2 0.0528(4) 0.0915(6) 0.0650(5) 0.0543(5) -0.0073(3) -0.0070(4) O2' 0.0275(18) 0.026(2) 0.0183(17) -0.0035(15) 0.0040(14) -0.0082(15) O2 0.0292(18) 0.0216(19) 0.0188(17) -0.0024(15) -0.0024(14) 0.0003(15) O1' 0.048(2) 0.033(2) 0.0226(19) -0.0062(17) 0.0132(16) -0.0119(18) O3 0.0295(18) 0.0214(19) 0.0170(17) 0.0000(15) -0.0001(14) -0.0007(15) O3' 0.0258(18) 0.029(2) 0.0191(17) -0.0019(15) 0.0016(14) -0.0075(15) N1' 0.023(2) 0.029(2) 0.022(2) -0.007(2) -0.0013(17) 0.0015(19) O4 0.036(2) 0.036(2) 0.0258(19) -0.0034(17) -0.0057(16) -0.0006(17) O1 0.048(2) 0.031(2) 0.0239(19) -0.0094(17) -0.0101(17) 0.0109(18) N1 0.028(2) 0.027(2) 0.023(2) -0.005(2) 0.0005(18) -0.0042(19) C6 0.019(2) 0.027(3) 0.025(3) -0.002(2) 0.003(2) -0.005(2) O4' 0.031(2) 0.041(2) 0.0257(19) 0.0050(17) -0.0066(15) -0.0117(17) N2 0.021(2) 0.023(2) 0.029(2) -0.0022(19) 0.0042(17) -0.0012(17) C13 0.024(3) 0.028(3) 0.025(3) 0.001(2) 0.006(2) 0.006(2) O5' 0.036(2) 0.040(3) 0.066(3) -0.007(2) 0.013(2) -0.0006(19) C15' 0.022(3) 0.024(3) 0.040(3) -0.003(3) 0.004(2) 0.000(2) C17' 0.023(3) 0.030(3) 0.021(3) 0.000(2) 0.006(2) 0.004(2) C5 0.026(3) 0.035(3) 0.021(3) -0.002(2) -0.005(2) -0.004(2) C4 0.027(3) 0.030(3) 0.030(3) 0.005(2) -0.006(2) 0.001(2) O5 0.040(2) 0.052(3) 0.031(2) 0.008(2) 0.0130(17) 0.009(2) O7' 0.050(3) 0.063(3) 0.056(3) 0.000(3) 0.018(2) 0.004(2) C12' 0.022(3) 0.034(3) 0.025(3) 0.003(2) -0.003(2) 0.005(2) C13' 0.023(2) 0.031(3) 0.021(3) -0.005(2) 0.004(2) 0.003(2) C3 0.038(3) 0.021(3) 0.032(3) -0.005(2) -0.002(2) 0.003(2) C14 0.026(3) 0.031(3) 0.039(3) 0.005(3) 0.010(2) 0.002(2) N2' 0.022(2) 0.033(3) 0.018(2) -0.0001(19) -0.0026(17) 0.0004(19) C17 0.022(3) 0.028(3) 0.029(3) -0.003(2) 0.007(2) 0.003(2) C2 0.030(3) 0.024(3) 0.022(3) -0.004(2) -0.001(2) -0.004(2) C8 0.023(3) 0.033(3) 0.020(2) -0.002(2) -0.001(2) -0.008(2) O6 0.062(3) 0.050(3) 0.081(4) 0.017(3) 0.030(3) 0.018(2) C6' 0.027(3) 0.024(3) 0.025(3) -0.001(2) 0.003(2) 0.000(2) C11' 0.036(3) 0.040(3) 0.021(3) -0.003(3) -0.002(2) 0.000(3) O6' 0.041(3) 0.073(3) 0.064(3) -0.015(3) 0.002(2) 0.022(2) O7 0.033(2) 0.072(3) 0.039(2) 0.007(2) 0.0044(18) 0.014(2) N3' 0.026(2) 0.035(3) 0.034(3) -0.010(2) -0.006(2) 0.011(2) N3 0.0144(19) 0.021(2) 0.0100(18) -0.0040(17) 0.0044(15) -0.0013(17) C8' 0.023(3) 0.023(3) 0.031(3) -0.006(2) -0.003(2) 0.000(2) C16' 0.020(3) 0.033(3) 0.031(3) -0.008(2) 0.003(2) 0.001(2) C9' 0.033(3) 0.033(3) 0.022(3) -0.011(2) -0.003(2) 0.002(2) C11 0.025(3) 0.025(3) 0.042(3) 0.002(3) -0.001(2) -0.005(2) C2' 0.036(3) 0.023(3) 0.028(3) -0.006(2) 0.004(2) -0.007(2) C18 0.024(3) 0.026(3) 0.017(2) -0.004(2) 0.0063(19) 0.003(2) C18' 0.021(2) 0.028(3) 0.024(3) -0.006(2) 0.006(2) 0.000(2) C14' 0.030(3) 0.026(3) 0.032(3) -0.001(2) 0.003(2) 0.002(2) C10 0.030(3) 0.029(3) 0.035(3) -0.012(3) -0.005(2) 0.000(2) C12 0.025(3) 0.025(3) 0.034(3) 0.004(2) 0.013(2) 0.001(2) C9 0.038(3) 0.032(3) 0.032(3) -0.010(3) -0.005(2) -0.004(3) C16 0.023(3) 0.051(4) 0.026(3) 0.007(3) 0.002(2) 0.008(3) C10' 0.033(3) 0.042(3) 0.015(2) -0.008(2) -0.001(2) 0.007(3) C19 0.030(3) 0.051(4) 0.032(3) -0.016(3) -0.006(2) 0.007(3) C15 0.029(3) 0.044(4) 0.033(3) 0.018(3) 0.011(2) 0.009(3) C1' 0.082(5) 0.051(4) 0.025(3) -0.011(3) 0.022(3) -0.020(4) C19' 0.034(3) 0.052(4) 0.029(3) 0.003(3) -0.007(2) -0.005(3) Br1' 0.0642(4) 0.0299(4) 0.0701(5) 0.0017(3) 0.0278(4) -0.0156(3) C7' 0.023(2) 0.019(3) 0.027(3) -0.001(2) 0.003(2) -0.003(2) C5' 0.030(3) 0.027(3) 0.038(3) -0.006(3) 0.001(2) -0.007(2) C4' 0.039(3) 0.023(3) 0.045(3) 0.003(3) 0.011(3) -0.010(2) C7 0.021(2) 0.028(3) 0.018(2) 0.000(2) -0.0005(19) -0.001(2) C3' 0.043(3) 0.031(3) 0.032(3) 0.000(3) 0.013(3) -0.005(3) C1 0.096(6) 0.072(5) 0.057(5) -0.042(4) -0.042(4) 0.048(5) O1W' 0.181(14) 0.57(4) 0.204(16) -0.25(2) 0.119(12) -0.27(2) O1W 0.22(3) 0.45(5) 0.026(9) -0.008(19) 0.019(14) -0.28(3) C1W' 0.103(18) 0.17(2) 0.069(19) 0.057(18) 0.002(14) -0.008(17) C1W 0.079(14) 0.13(2) 0.076(17) -0.001(14) 0.028(12) -0.038(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2' 1.996(3) . ? Zn1 O2 2.019(3) . ? Zn1 O3 2.033(3) . ? Zn1 O3' 2.049(3) . ? Zn1 O1 2.397(4) . ? Zn1 O1' 2.400(4) . ? Zn2 O2 2.012(3) . ? Zn2 N2 2.018(4) . ? Zn2 O5 2.028(4) . ? Zn2 O3 2.060(3) . ? Zn2 N1 2.104(4) . ? Zn3 O3' 2.026(3) . ? Zn3 O5' 2.032(4) . ? Zn3 N2' 2.041(4) . ? Zn3 O2' 2.057(3) . ? Zn3 N1' 2.068(4) . ? Br1 C4 1.902(5) . ? Br2' C15' 1.900(5) . ? Br2 C15 1.905(5) . ? O2' C7' 1.311(6) . ? O2 C7 1.319(6) . ? O1' C2' 1.359(6) . ? O1' C1' 1.439(6) . ? O3 C18 1.329(6) . ? O3' C18' 1.324(6) . ? N1' C8' 1.269(7) . ? N1' C9' 1.463(6) . ? O4 C17 1.366(6) . ? O4 C19 1.427(6) . ? O1 C2 1.375(6) . ? O1 C1 1.430(7) . ? N1 C8 1.278(6) . ? N1 C9 1.489(7) . ? C6 C5 1.408(7) . ? C6 C7 1.414(7) . ? C6 C8 1.454(7) . ? O4' C17' 1.361(6) . ? O4' C19' 1.418(6) . ? N2 C12 1.280(6) . ? N2 C11 1.478(6) . ? C13 C18 1.408(7) . ? C13 C14 1.418(7) . ? C13 C12 1.448(7) . ? O5' N3' 1.218(6) . ? C15' C14' 1.366(7) . ? C15' C16' 1.389(7) . ? C17' C16' 1.377(7) . ? C17' C18' 1.416(7) . ? C5 C4 1.348(7) . ? C4 C3 1.402(7) . ? O5 N3 1.196(5) . ? O7' N3' 1.266(6) . ? C12' N2' 1.285(6) . ? C12' C13' 1.452(7) . ? C13' C14' 1.408(7) . ? C13' C18' 1.420(7) . ? C3 C2 1.370(7) . ? C14 C15 1.363(8) . ? N2' C11' 1.479(6) . ? C17 C16 1.383(7) . ? C17 C18 1.411(7) . ? C2 C7 1.410(7) . ? O6 N3 1.244(6) . ? C6' C7' 1.402(7) . ? C6' C5' 1.406(7) . ? C6' C8' 1.460(7) . ? C11' C10' 1.524(8) . ? O6' N3' 1.241(6) . ? O7 N3 1.264(5) . ? C9' C10' 1.515(7) . ? C11 C10 1.534(7) . ? C2' C3' 1.384(7) . ? C2' C7' 1.420(7) . ? C10 C9 1.504(8) . ? C16 C15 1.381(8) . ? Br1' C4' 1.891(5) . ? C5' C4' 1.374(8) . ? C4' C3' 1.391(8) . ? O1W' C1W' 1.429(9) 3_548 ? O1W' C1W' 1.429(9) . ? O1W C1W' 0.71(3) . ? O1W C1W 1.371(10) . ? C1W' C1W 1.95(4) . ? 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 O2' Zn1 O2 147.52(14) . . ? O2' Zn1 O3 126.02(13) . . ? O2 Zn1 O3 77.56(13) . . ? O2' Zn1 O3' 76.53(13) . . ? O2 Zn1 O3' 125.75(13) . . ? O3 Zn1 O3' 99.31(13) . . ? O2' Zn1 O1 83.79(13) . . ? O2 Zn1 O1 71.01(12) . . ? O3 Zn1 O1 148.52(12) . . ? O3' Zn1 O1 97.47(13) . . ? O2' Zn1 O1' 71.38(12) . . ? O2 Zn1 O1' 83.06(13) . . ? O3 Zn1 O1' 101.06(13) . . ? O3' Zn1 O1' 147.84(13) . . ? O1 Zn1 O1' 77.30(14) . . ? O2 Zn2 N2 129.65(15) . . ? O2 Zn2 O5 105.15(16) . . ? N2 Zn2 O5 125.11(17) . . ? O2 Zn2 O3 77.11(13) . . ? N2 Zn2 O3 89.62(15) . . ? O5 Zn2 O3 101.05(15) . . ? O2 Zn2 N1 88.31(15) . . ? N2 Zn2 N1 93.03(17) . . ? O5 Zn2 N1 91.18(16) . . ? O3 Zn2 N1 162.95(15) . . ? O3' Zn3 O5' 102.69(16) . . ? O3' Zn3 N2' 91.96(15) . . ? O5' Zn3 N2' 116.73(17) . . ? O3' Zn3 O2' 75.70(13) . . ? O5' Zn3 O2' 112.48(16) . . ? N2' Zn3 O2' 130.77(15) . . ? O3' Zn3 N1' 160.34(15) . . ? O5' Zn3 N1' 89.25(17) . . ? N2' Zn3 N1' 96.56(17) . . ? O2' Zn3 N1' 85.36(15) . . ? C7' O2' Zn1 124.3(3) . . ? C7' O2' Zn3 130.0(3) . . ? Zn1 O2' Zn3 104.26(14) . . ? C7 O2 Zn2 130.7(3) . . ? C7 O2 Zn1 124.9(3) . . ? Zn2 O2 Zn1 103.73(14) . . ? C2' O1' C1' 117.5(4) . . ? C2' O1' Zn1 110.5(3) . . ? C1' O1' Zn1 130.6(3) . . ? C18 O3 Zn1 126.8(3) . . ? C18 O3 Zn2 125.5(3) . . ? Zn1 O3 Zn2 101.56(14) . . ? C18' O3' Zn3 125.7(3) . . ? C18' O3' Zn1 123.8(3) . . ? Zn3 O3' Zn1 103.51(14) . . ? C8' N1' C9' 117.7(4) . . ? C8' N1' Zn3 127.8(3) . . ? C9' N1' Zn3 114.4(3) . . ? C17 O4 C19 118.4(4) . . ? C2 O1 C1 117.6(4) . . ? C2 O1 Zn1 112.1(3) . . ? C1 O1 Zn1 129.1(4) . . ? C8 N1 C9 115.5(4) . . ? C8 N1 Zn2 126.2(4) . . ? C9 N1 Zn2 118.3(3) . . ? C5 C6 C7 118.8(5) . . ? C5 C6 C8 117.0(4) . . ? C7 C6 C8 124.0(5) . . ? C17' O4' C19' 117.8(4) . . ? C12 N2 C11 118.2(4) . . ? C12 N2 Zn2 125.4(4) . . ? C11 N2 Zn2 115.8(3) . . ? C18 C13 C14 119.7(5) . . ? C18 C13 C12 125.0(5) . . ? C14 C13 C12 115.2(5) . . ? N3' O5' Zn3 117.7(4) . . ? C14' C15' C16' 121.2(5) . . ? C14' C15' Br2' 119.3(4) . . ? C16' C15' Br2' 119.4(4) . . ? O4' C17' C16' 125.4(5) . . ? O4' C17' C18' 113.5(4) . . ? C16' C17' C18' 121.1(5) . . ? C4 C5 C6 121.4(5) . . ? C5 C4 C3 121.0(5) . . ? C5 C4 Br1 120.2(4) . . ? C3 C4 Br1 118.8(4) . . ? N3 O5 Zn2 114.3(3) . . ? N2' C12' C13' 129.0(5) . . ? C14' C13' C18' 119.2(5) . . ? C14' C13' C12' 116.4(5) . . ? C18' C13' C12' 124.4(5) . . ? C2 C3 C4 118.7(5) . . ? C15 C14 C13 119.7(5) . . ? C12' N2' C11' 115.0(4) . . ? C12' N2' Zn3 122.6(3) . . ? C11' N2' Zn3 121.7(3) . . ? O4 C17 C16 124.9(5) . . ? O4 C17 C18 113.6(4) . . ? C16 C17 C18 121.6(5) . . ? C3 C2 O1 124.7(5) . . ? C3 C2 C7 122.2(5) . . ? O1 C2 C7 113.2(4) . . ? N1 C8 C6 126.8(5) . . ? C7' C6' C5' 120.2(5) . . ? C7' C6' C8' 122.4(5) . . ? C5' C6' C8' 117.1(5) . . ? N2' C11' C10' 114.8(4) . . ? O5' N3' O6' 121.7(5) . . ? O5' N3' O7' 120.4(4) . . ? O6' N3' O7' 117.8(5) . . ? O5 N3 O6 120.5(4) . . ? O5 N3 O7 121.5(4) . . ? O6 N3 O7 118.0(4) . . ? N1' C8' C6' 126.2(5) . . ? C17' C16' C15' 119.6(5) . . ? N1' C9' C10' 109.8(4) . . ? N2 C11 C10 109.8(4) . . ? O1' C2' C3' 125.2(5) . . ? O1' C2' C7' 113.2(4) . . ? C3' C2' C7' 121.6(5) . . ? O3 C18 C13 122.6(4) . . ? O3 C18 C17 119.3(4) . . ? C13 C18 C17 118.0(4) . . ? O3' C18' C17' 118.7(4) . . ? O3' C18' C13' 123.1(4) . . ? C17' C18' C13' 118.2(5) . . ? C15' C14' C13' 120.5(5) . . ? C9 C10 C11 113.6(5) . . ? N2 C12 C13 127.1(5) . . ? N1 C9 C10 112.2(4) . . ? C15 C16 C17 119.1(5) . . ? C9' C10' C11' 115.6(4) . . ? C14 C15 C16 121.9(5) . . ? C14 C15 Br2 119.0(4) . . ? C16 C15 Br2 119.1(4) . . ? O2' C7' C6' 123.6(4) . . ? O2' C7' C2' 118.6(4) . . ? C6' C7' C2' 117.8(4) . . ? C4' C5' C6' 120.1(5) . . ? C5' C4' C3' 121.3(5) . . ? C5' C4' Br1' 119.8(4) . . ? C3' C4' Br1' 118.8(4) . . ? O2 C7 C2 118.5(4) . . ? O2 C7 C6 123.6(5) . . ? C2 C7 C6 117.9(4) . . ? C2' C3' C4' 118.8(5) . . ? C1W' O1W' C1W' 180.000(15) 3_548 . ? C1W' O1W C1W 136(4) . . ? O1W C1W' O1W' 146(4) . . ? O1W C1W' C1W 29(3) . . ? O1W' C1W' C1W 116.8(17) . . ? O1W C1W C1W' 14.8(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.230 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.126 data_Complex-2 _database_code_depnum_ccdc_archive 'CCDC 232602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Br2 Cl2 N3 O5 Yb Zn' _chemical_formula_weight 864.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 11.263(2) _cell_length_b 12.000(2) _cell_length_c 12.366(3) _cell_angle_alpha 102.71(3) _cell_angle_beta 108.26(3) _cell_angle_gamma 112.82(3) _cell_volume 1347.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 7.542 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8620 _diffrn_reflns_av_R_equivalents 0.1236 _diffrn_reflns_av_sigmaI/netI 0.1676 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4493 _reflns_number_gt 2599 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1992P)^2^+47.9765P] 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 0.0005(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4493 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2426 _refine_ls_wR_factor_gt 0.2048 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.475 _refine_ls_shift/su_mean 0.060 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 Yb1 Yb 1.92492(4) 1.85203(4) 1.02557(4) 0.03587(15) Uani 1 1 d . . . Zn1 Zn 1.78756(11) 1.57872(11) 0.75917(11) 0.0366(4) Uani 1 1 d . . . Cl1 Cl 1.9051(4) 1.8022(4) 1.2143(4) 0.0842(14) Uani 1 1 d . . . Cl2 Cl 1.8554(2) 1.6940(3) 0.6442(2) 0.0427(9) Uani 1 1 d . . . Br1 Br 2.52037(11) 1.69234(11) 1.13649(11) 0.0502(4) Uani 1 1 d . . . Br2 Br 1.16224(10) 1.68915(11) 0.70266(11) 0.0504(4) Uani 1 1 d . . . N1 N 1.8566(8) 1.4437(8) 0.7436(9) 0.044(3) Uani 1 1 d . . . N2 N 1.5745(8) 1.4489(9) 0.6480(8) 0.042(3) Uani 1 1 d . . . O1 O 2.1717(7) 1.8908(7) 1.1255(7) 0.050(3) Uani 1 1 d . . . O2 O 1.9557(7) 1.6849(6) 0.9326(6) 0.040(2) Uani 1 1 d . . . O3 O 1.7217(6) 1.6843(6) 0.8623(6) 0.033(2) Uani 1 1 d . . . O4 O 1.7146(7) 1.8769(6) 0.9947(7) 0.043(3) Uani 1 1 d . . . O5 O 2.0362(6) 2.0635(5) 1.1088(5) 0.0293(19) Uani 1 1 d . . . C1 C 2.2790(11) 1.9932(12) 1.2461(13) 0.060(5) Uani 1 1 d . . . H1A H 2.3673 1.9907 1.2666 0.090 Uiso 1 1 calc R . . H1B H 2.2458 1.9793 1.3072 0.090 Uiso 1 1 calc R . . H1C H 2.2950 2.0772 1.2444 0.090 Uiso 1 1 calc R . . C2 C 2.1972(9) 1.7902(9) 1.0831(8) 0.030(3) Uani 1 1 d . . . C3 C 2.3295(10) 1.7968(9) 1.1273(10) 0.041(3) Uani 1 1 d . . . H3A H 2.4091 1.8713 1.1929 0.049 Uiso 1 1 calc R . . C4 C 2.3421(11) 1.6879(12) 1.0710(10) 0.055(4) Uani 1 1 d . . . C5 C 2.2271(10) 1.5788(10) 0.9785(9) 0.038(3) Uani 1 1 d . . . H5A H 2.2343 1.5043 0.9502 0.045 Uiso 1 1 calc R . . C6 C 2.0943(10) 1.5761(11) 0.9234(11) 0.046(4) Uani 1 1 d . . . C7 C 2.0774(8) 1.6786(9) 0.9762(10) 0.042(4) Uani 1 1 d . . . C8 C 1.9747(11) 1.4567(11) 0.8149(9) 0.046(4) Uani 1 1 d . . . H8A H 1.9873 1.3838 0.7972 0.055 Uiso 1 1 calc R . . C9 C 1.7764(10) 1.3235(11) 0.6319(12) 0.050(5) Uani 1 1 d . . . H9A H 1.8095 1.2623 0.6468 0.060 Uiso 1 1 calc R . . H9B H 1.7948 1.3439 0.5652 0.060 Uiso 1 1 calc R . . C10 C 1.6130(10) 1.2584(11) 0.5928(10) 0.070(4) Uani 1 1 d . . . H10B H 1.5684 1.1710 0.5301 0.084 Uiso 1 1 calc R . . H10A H 1.5987 1.2475 0.6640 0.084 Uiso 1 1 calc R . . C11 C 1.5337(10) 1.3230(9) 0.5446(12) 0.045(4) Uani 1 1 d . . . H11A H 1.4313 1.2632 0.5091 0.054 Uiso 1 1 calc R . . H11B H 1.5554 1.3450 0.4796 0.054 Uiso 1 1 calc R . . C12 C 1.4671(12) 1.4635(9) 0.6429(8) 0.045(4) Uani 1 1 d . . . H12A H 1.3768 1.3966 0.5824 0.054 Uiso 1 1 calc R . . C13 C 1.4740(10) 1.5720(10) 0.7210(9) 0.037(3) Uani 1 1 d . . . C14 C 1.3381(10) 1.5749(9) 0.6858(10) 0.039(3) Uani 1 1 d . . . H14A H 1.2537 1.5037 0.6213 0.047 Uiso 1 1 calc R . . C15 C 1.3369(11) 1.6836(10) 0.7492(11) 0.047(4) Uani 1 1 d . . . C16 C 1.4560(11) 1.7786(10) 0.8559(8) 0.042(3) Uani 1 1 d . . . H16A H 1.4467 1.8412 0.9067 0.050 Uiso 1 1 calc R . . C17 C 1.5884(10) 1.7863(11) 0.8918(9) 0.042(4) Uani 1 1 d . . . C18 C 1.5963(10) 1.6795(11) 0.8286(10) 0.041(4) Uani 1 1 d . . . C19 C 1.7122(10) 1.9843(9) 1.0700(11) 0.047(4) Uani 1 1 d . . . H19A H 1.6167 1.9722 1.0375 0.070 Uiso 1 1 calc R . . H19B H 1.7772 2.0648 1.0699 0.070 Uiso 1 1 calc R . . H19C H 1.7411 1.9882 1.1531 0.070 Uiso 1 1 calc R . . N3 N 2.6291(13) 2.0330(10) 1.3830(14) 0.091(6) Uani 1 1 d . . . C20 C 2.8880(15) 2.070(2) 1.440(2) 0.183(10) Uani 1 1 d . . . H20A H 2.9087 2.0043 1.4589 0.274 Uiso 1 1 calc R . . H20B H 2.9493 2.1524 1.5097 0.274 Uiso 1 1 calc R . . H20C H 2.9044 2.0791 1.3698 0.274 Uiso 1 1 calc R . . C21 C 2.7419(15) 2.0317(17) 1.4116(17) 0.111(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02625(16) 0.03450(18) 0.0435(2) 0.01254(16) 0.01250(15) 0.01571(13) Zn1 0.0260(4) 0.0366(5) 0.0432(6) 0.0111(5) 0.0130(4) 0.0163(4) Cl1 0.0863(16) 0.118(2) 0.077(2) 0.0398(17) 0.0401(14) 0.0721(13) Cl2 0.0264(9) 0.0490(12) 0.0427(13) 0.0096(11) 0.0118(9) 0.0169(8) Br1 0.0326(4) 0.0681(5) 0.0636(6) 0.0355(4) 0.0217(4) 0.0318(3) Br2 0.0316(4) 0.0684(5) 0.0589(6) 0.0259(5) 0.0199(4) 0.0312(3) N1 0.028(3) 0.040(4) 0.048(5) 0.005(4) 0.010(3) 0.016(3) N2 0.024(3) 0.057(5) 0.030(4) 0.002(4) 0.006(3) 0.019(3) O1 0.040(3) 0.060(3) 0.059(4) 0.022(3) 0.018(3) 0.037(2) O2 0.043(3) 0.046(3) 0.047(3) 0.024(3) 0.029(2) 0.025(2) O3 0.029(2) 0.041(3) 0.045(3) 0.016(3) 0.023(2) 0.0257(19) O4 0.057(3) 0.030(3) 0.041(4) 0.009(3) 0.018(3) 0.027(2) O5 0.031(2) 0.048(2) 0.029(3) 0.033(2) 0.014(2) 0.0283(19) C1 0.014(4) 0.060(6) 0.077(8) 0.005(6) 0.008(5) 0.014(4) C2 0.035(4) 0.053(4) 0.023(3) 0.025(3) 0.024(3) 0.026(3) C3 0.059(4) 0.039(4) 0.045(5) 0.017(4) 0.023(4) 0.041(3) C4 0.016(4) 0.093(7) 0.049(5) 0.045(5) 0.005(4) 0.018(4) C5 0.045(4) 0.044(4) 0.047(4) 0.029(4) 0.038(3) 0.022(3) C6 0.030(4) 0.061(5) 0.048(6) 0.015(5) 0.017(4) 0.026(4) C7 0.016(3) 0.045(4) 0.083(6) 0.032(4) 0.030(3) 0.021(3) C8 0.050(5) 0.065(6) 0.029(4) 0.023(4) 0.023(4) 0.029(4) C9 0.011(4) 0.033(5) 0.070(7) 0.003(5) 0.005(5) -0.005(4) C10 0.047(4) 0.149(6) 0.092(4) 0.111(4) 0.055(3) 0.065(4) C11 0.029(4) 0.026(4) 0.069(7) 0.005(5) 0.018(4) 0.014(3) C12 0.049(6) 0.024(5) 0.020(4) 0.012(3) 0.008(4) -0.014(4) C13 0.034(4) 0.056(5) 0.035(5) 0.021(4) 0.018(3) 0.031(3) C14 0.030(4) 0.050(4) 0.052(5) 0.026(4) 0.022(3) 0.027(3) C15 0.042(4) 0.054(5) 0.054(6) 0.031(4) 0.016(4) 0.032(3) C16 0.059(4) 0.073(5) 0.034(4) 0.042(3) 0.034(3) 0.047(3) C17 0.039(4) 0.055(5) 0.044(5) 0.013(4) 0.032(3) 0.026(3) C18 0.024(4) 0.053(5) 0.040(5) 0.007(4) 0.012(4) 0.020(3) C19 0.036(4) 0.049(4) 0.054(6) 0.022(4) 0.001(4) 0.035(3) N3 0.078(6) 0.031(5) 0.123(11) -0.004(6) 0.025(7) 0.025(4) C20 0.131(6) 0.244(14) 0.353(17) 0.187(13) 0.193(7) 0.149(7) C21 0.066(6) 0.105(9) 0.114(11) -0.033(8) 0.034(6) 0.045(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O5 2.155(6) . ? Yb1 O5 2.198(7) 2_997 ? Yb1 O3 2.261(5) . ? Yb1 O2 2.289(8) . ? Yb1 O4 2.425(9) . ? Yb1 O1 2.462(8) . ? Yb1 Cl1 2.587(5) . ? Yb1 C18 3.179(9) . ? Yb1 Zn1 3.481(2) . ? Yb1 Yb1 3.5878(15) 2_997 ? Zn1 N2 2.041(7) . ? Zn1 N1 2.049(11) . ? Zn1 O2 2.047(6) . ? Zn1 O3 2.096(8) . ? Zn1 Cl2 2.291(4) . ? Br1 C4 1.889(13) . ? Br2 C15 1.901(13) . ? N1 C8 1.271(15) . ? N1 C9 1.461(13) . ? N2 C12 1.272(18) . ? N2 C11 1.540(15) . ? O1 C2 1.379(15) . ? O1 C1 1.452(13) . ? O2 C7 1.345(13) . ? O3 C18 1.314(13) . ? O4 C17 1.371(10) . ? O4 C19 1.430(14) . ? O5 Yb1 2.198(7) 2_997 ? C2 C3 1.380(15) . ? C2 C7 1.437(10) . ? C3 C4 1.420(19) . ? C4 C5 1.341(12) . ? C5 C6 1.420(17) . ? C6 C7 1.371(18) . ? C6 C8 1.481(12) . ? C9 C10 1.546(15) . ? C10 C11 1.471(19) . ? C12 C13 1.398(17) . ? C13 C18 1.432(11) . ? C13 C14 1.471(16) . ? C14 C15 1.373(17) . ? C15 C16 1.372(11) . ? C16 C17 1.375(17) . ? C17 C18 1.397(18) . ? N3 C21 1.22(2) . ? C20 C21 1.42(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Yb1 O5 69.0(3) . 2_997 ? O5 Yb1 O3 139.6(3) . . ? O5 Yb1 O3 85.9(2) 2_997 . ? O5 Yb1 O2 139.8(3) . . ? O5 Yb1 O2 88.9(3) 2_997 . ? O3 Yb1 O2 66.7(2) . . ? O5 Yb1 O4 83.0(2) . . ? O5 Yb1 O4 92.2(3) 2_997 . ? O3 Yb1 O4 66.3(2) . . ? O2 Yb1 O4 132.8(2) . . ? O5 Yb1 O1 81.4(3) . . ? O5 Yb1 O1 93.9(3) 2_997 . ? O3 Yb1 O1 133.2(3) . . ? O2 Yb1 O1 66.6(2) . . ? O4 Yb1 O1 159.9(2) . . ? O5 Yb1 Cl1 99.3(2) . . ? O5 Yb1 Cl1 168.27(17) 2_997 . ? O3 Yb1 Cl1 103.9(2) . . ? O2 Yb1 Cl1 100.8(2) . . ? O4 Yb1 Cl1 86.0(2) . . ? O1 Yb1 Cl1 84.2(2) . . ? O5 Yb1 C18 123.4(3) . . ? O5 Yb1 C18 87.3(3) 2_997 . ? O3 Yb1 C18 20.2(3) . . ? O2 Yb1 C18 86.8(3) . . ? O4 Yb1 C18 46.1(3) . . ? O1 Yb1 C18 153.3(3) . . ? Cl1 Yb1 C18 99.7(3) . . ? O5 Yb1 Zn1 145.18(19) . . ? O5 Yb1 Zn1 76.25(15) 2_997 . ? O3 Yb1 Zn1 35.4(2) . . ? O2 Yb1 Zn1 34.28(16) . . ? O4 Yb1 Zn1 100.78(15) . . ? O1 Yb1 Zn1 99.30(19) . . ? Cl1 Yb1 Zn1 115.47(10) . . ? C18 Yb1 Zn1 55.1(2) . . ? O5 Yb1 Yb1 34.88(18) . 2_997 ? O5 Yb1 Yb1 34.11(15) 2_997 2_997 ? O3 Yb1 Yb1 114.4(2) . 2_997 ? O2 Yb1 Yb1 116.6(2) . 2_997 ? O4 Yb1 Yb1 87.16(19) . 2_997 ? O1 Yb1 Yb1 87.2(2) . 2_997 ? Cl1 Yb1 Yb1 134.16(9) . 2_997 ? C18 Yb1 Yb1 107.6(2) . 2_997 ? Zn1 Yb1 Yb1 110.34(4) . 2_997 ? N2 Zn1 N1 96.6(4) . . ? N2 Zn1 O2 149.5(4) . . ? N1 Zn1 O2 87.1(3) . . ? N2 Zn1 O3 86.7(3) . . ? N1 Zn1 O3 146.2(4) . . ? O2 Zn1 O3 74.2(3) . . ? N2 Zn1 Cl2 103.6(3) . . ? N1 Zn1 Cl2 106.9(3) . . ? O2 Zn1 Cl2 104.3(2) . . ? O3 Zn1 Cl2 104.9(2) . . ? N2 Zn1 Yb1 125.2(3) . . ? N1 Zn1 Yb1 125.6(2) . . ? O2 Zn1 Yb1 39.0(2) . . ? O3 Zn1 Yb1 38.62(14) . . ? Cl2 Zn1 Yb1 96.07(8) . . ? C8 N1 C9 111.9(11) . . ? C8 N1 Zn1 127.5(8) . . ? C9 N1 Zn1 120.0(8) . . ? C12 N2 C11 113.2(7) . . ? C12 N2 Zn1 128.3(7) . . ? C11 N2 Zn1 118.0(7) . . ? C2 O1 C1 116.3(9) . . ? C2 O1 Yb1 117.5(4) . . ? C1 O1 Yb1 123.6(8) . . ? C7 O2 Zn1 127.5(7) . . ? C7 O2 Yb1 124.3(5) . . ? Zn1 O2 Yb1 106.7(4) . . ? C18 O3 Zn1 128.6(6) . . ? C18 O3 Yb1 123.3(6) . . ? Zn1 O3 Yb1 106.0(3) . . ? C17 O4 C19 116.1(9) . . ? C17 O4 Yb1 118.2(7) . . ? C19 O4 Yb1 125.5(5) . . ? Yb1 O5 Yb1 111.0(3) . 2_997 ? O1 C2 C3 124.8(7) . . ? O1 C2 C7 114.8(9) . . ? C3 C2 C7 120.1(10) . . ? C2 C3 C4 118.9(8) . . ? C5 C4 C3 120.9(12) . . ? C5 C4 Br1 119.8(11) . . ? C3 C4 Br1 119.2(6) . . ? C4 C5 C6 120.5(12) . . ? C7 C6 C5 119.8(8) . . ? C7 C6 C8 122.1(11) . . ? C5 C6 C8 118.0(12) . . ? O2 C7 C6 124.5(8) . . ? O2 C7 C2 116.4(10) . . ? C6 C7 C2 119.1(9) . . ? N1 C8 C6 126.6(13) . . ? N1 C9 C10 111.6(11) . . ? C11 C10 C9 119.2(10) . . ? C10 C11 N2 110.9(9) . . ? N2 C12 C13 125.3(8) . . ? C12 C13 C18 128.0(11) . . ? C12 C13 C14 115.0(8) . . ? C18 C13 C14 117.0(10) . . ? C15 C14 C13 119.4(8) . . ? C14 C15 C16 119.6(12) . . ? C14 C15 Br2 119.7(6) . . ? C16 C15 Br2 120.1(10) . . ? C15 C16 C17 123.6(12) . . ? O4 C17 C16 128.8(11) . . ? O4 C17 C18 112.5(10) . . ? C16 C17 C18 117.9(8) . . ? O3 C18 C17 118.9(7) . . ? O3 C18 C13 119.7(11) . . ? C17 C18 C13 121.1(10) . . ? O3 C18 Yb1 36.4(4) . . ? C17 C18 Yb1 82.5(5) . . ? C13 C18 Yb1 156.1(9) . . ? N3 C21 C20 161(2) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.203 _refine_diff_density_min -1.703 _refine_diff_density_rms 0.317