Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cameron Jones' _publ_contact_author_address ; School of Chemistry Monash University PO Box 23 Victoria 3800 AUSTRALIA ; _publ_contact_author_email CAMERON.JONES@SCI.MONASH.EDU.AU _publ_section_title ; Synthesis and Characterisation of Zinc Gallyl Complexes: First Structural Elucidations of Zn-Ga Bonds ; loop_ _publ_author_name 'Cameron Jones' 'Richard P. Rose' 'Andreas Stasch' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 645310' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H84 Ga N5 Zn' _chemical_formula_weight 974.38 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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 11.608(2) _cell_length_b 13.803(3) _cell_length_c 17.997(4) _cell_angle_alpha 88.49(3) _cell_angle_beta 81.17(3) _cell_angle_gamma 86.69(3) _cell_volume 2844.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _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 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _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 Kappa 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 19413 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10462 _reflns_number_gt 8170 _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. During the course of refinement the methyl groups of one isopropyl substituent were found to be disordered over two sites. This disorder was successfully modelled. ; _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^)+(0.0429P)^2^+1.1064P] 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 10462 _refine_ls_number_parameters 618 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Ga1 Ga 0.75580(2) 0.379340(18) 0.306764(14) 0.03358(9) Uani 1 1 d . . . Zn1 Zn 0.74212(2) 0.225728(19) 0.260191(15) 0.03298(9) Uani 1 1 d . . . N1 N 0.77999(17) 0.08435(14) 0.27080(10) 0.0318(4) Uani 1 1 d . . . N2 N 0.67610(17) 0.14733(14) 0.18620(10) 0.0310(4) Uani 1 1 d . . . N3 N 0.70011(18) -0.02726(14) 0.19428(11) 0.0349(5) Uani 1 1 d . . . N4 N 0.78688(18) 0.42938(14) 0.39633(10) 0.0340(5) Uani 1 1 d . . . N5 N 0.74393(18) 0.50658(14) 0.26982(11) 0.0360(5) Uani 1 1 d . . . C1 C 0.7184(2) 0.06365(17) 0.21564(12) 0.0285(5) Uani 1 1 d . . . C2 C 0.8799(2) 0.03138(17) 0.29035(14) 0.0358(6) Uani 1 1 d . . . C3 C 0.8770(2) -0.00082(19) 0.36523(15) 0.0434(7) Uani 1 1 d . . . C4 C 0.9792(3) -0.0447(2) 0.38612(18) 0.0590(9) Uani 1 1 d . . . H4 H 0.9788 -0.0673 0.4365 0.071 Uiso 1 1 calc R . . C5 C 1.0796(3) -0.0557(2) 0.3357(2) 0.0664(10) Uani 1 1 d . . . H5 H 1.1481 -0.0854 0.3512 0.080 Uiso 1 1 calc R . . C6 C 1.0814(3) -0.0238(2) 0.26223(19) 0.0559(8) Uani 1 1 d . . . H6 H 1.1516 -0.0322 0.2276 0.067 Uiso 1 1 calc R . . C7 C 0.9826(2) 0.02053(18) 0.23767(15) 0.0412(6) Uani 1 1 d . . . C8 C 0.7675(3) 0.0117(2) 0.42211(14) 0.0492(7) Uani 1 1 d . . . H8 H 0.7015 0.0280 0.3934 0.059 Uiso 1 1 calc R . . C9 C 0.7735(3) 0.0967(3) 0.4740(2) 0.0753(10) Uani 1 1 d . . . H9A H 0.8398 0.0848 0.5014 0.113 Uiso 1 1 calc R . . H9B H 0.7011 0.1030 0.5100 0.113 Uiso 1 1 calc R . . H9C H 0.7833 0.1567 0.4440 0.113 Uiso 1 1 calc R . . C10 C 0.7381(4) -0.0808(3) 0.4680(2) 0.0831(12) Uani 1 1 d . . . H10A H 0.7362 -0.1347 0.4339 0.125 Uiso 1 1 calc R . . H10B H 0.6616 -0.0711 0.4993 0.125 Uiso 1 1 calc R . . H10C H 0.7977 -0.0961 0.5003 0.125 Uiso 1 1 calc R . . C11 C 0.9869(2) 0.0573(2) 0.15700(15) 0.0449(7) Uani 1 1 d . . . H11 H 0.9074 0.0515 0.1431 0.054 Uiso 1 1 calc R . . C12 C 1.0132(3) 0.1645(2) 0.15035(16) 0.0525(7) Uani 1 1 d . . . H12A H 0.9568 0.2015 0.1865 0.079 Uiso 1 1 calc R . . H12B H 1.0072 0.1884 0.0993 0.079 Uiso 1 1 calc R . . H12C H 1.0923 0.1724 0.1610 0.079 Uiso 1 1 calc R . . C13 C 1.0736(3) -0.0013(3) 0.10009(19) 0.0700(9) Uani 1 1 d . . . H13A H 1.0637 0.0199 0.0489 0.105 Uiso 1 1 calc R . . H13B H 1.0590 -0.0705 0.1067 0.105 Uiso 1 1 calc R . . H13C H 1.1534 0.0091 0.1083 0.105 Uiso 1 1 calc R . . C14 C 0.5694(2) 0.16256(17) 0.15669(13) 0.0332(5) Uani 1 1 d . . . C15 C 0.4616(2) 0.15153(19) 0.20309(13) 0.0386(6) Uani 1 1 d . . . C16 C 0.3596(2) 0.1766(2) 0.17356(15) 0.0478(7) Uani 1 1 d . . . H16 H 0.2861 0.1692 0.2040 0.057 Uiso 1 1 calc R . . C17 C 0.3636(3) 0.2120(2) 0.10089(16) 0.0518(7) Uani 1 1 d . . . H17 H 0.2931 0.2285 0.0816 0.062 Uiso 1 1 calc R . . C18 C 0.4694(3) 0.2234(2) 0.05633(14) 0.0452(7) Uani 1 1 d . . . H18 H 0.4710 0.2482 0.0065 0.054 Uiso 1 1 calc R . . C19 C 0.5743(2) 0.19947(18) 0.08271(13) 0.0364(6) Uani 1 1 d . . . C20 C 0.4549(2) 0.1181(2) 0.28466(14) 0.0453(7) Uani 1 1 d . . . H20 H 0.5304 0.0821 0.2902 0.054 Uiso 1 1 calc R . . C21 C 0.4413(3) 0.2057(3) 0.33645(16) 0.0626(9) Uani 1 1 d . . . H21A H 0.5039 0.2497 0.3198 0.094 Uiso 1 1 calc R . . H21B H 0.4458 0.1835 0.3881 0.094 Uiso 1 1 calc R . . H21C H 0.3655 0.2401 0.3346 0.094 Uiso 1 1 calc R . . C22 C 0.3562(3) 0.0496(2) 0.31003(16) 0.0568(8) Uani 1 1 d . . . H22A H 0.2806 0.0855 0.3113 0.085 Uiso 1 1 calc R . . H22B H 0.3632 0.0234 0.3604 0.085 Uiso 1 1 calc R . . H22C H 0.3618 -0.0038 0.2746 0.085 Uiso 1 1 calc R . . C23 C 0.6919(2) 0.21717(19) 0.03515(13) 0.0412(6) Uani 1 1 d . . . H23 H 0.7514 0.1719 0.0544 0.049 Uiso 1 1 calc R . . C24 C 0.6953(3) 0.1953(2) -0.04818(15) 0.0572(8) Uani 1 1 d . . . H24A H 0.6413 0.2411 -0.0698 0.086 Uiso 1 1 calc R . . H24B H 0.6720 0.1289 -0.0531 0.086 Uiso 1 1 calc R . . H24C H 0.7747 0.2019 -0.0749 0.086 Uiso 1 1 calc R . . C25 C 0.7274(3) 0.3194(2) 0.04426(19) 0.0761(11) Uani 1 1 d . . . H25A H 0.6727 0.3657 0.0239 0.114 Uiso 1 1 calc R . . H25B H 0.8064 0.3268 0.0171 0.114 Uiso 1 1 calc R . . H25C H 0.7262 0.3318 0.0977 0.114 Uiso 1 1 calc R . . C26 C 0.7110(2) -0.10936(18) 0.24863(15) 0.0425(6) Uani 1 1 d . . . H26 H 0.7155 -0.0788 0.2978 0.051 Uiso 1 1 calc R . . C27 C 0.6027(3) -0.1695(2) 0.26243(18) 0.0572(8) Uani 1 1 d . . . H27A H 0.5323 -0.1259 0.2696 0.086 Uiso 1 1 calc R . . H27B H 0.6050 -0.2105 0.3075 0.086 Uiso 1 1 calc R . . H27C H 0.6014 -0.2105 0.2190 0.086 Uiso 1 1 calc R . . C28 C 0.8212(3) -0.1763(2) 0.23196(18) 0.0544(8) Uani 1 1 d . . . H28A H 0.8085 -0.2263 0.1969 0.082 Uiso 1 1 calc R . . H28B H 0.8388 -0.2072 0.2789 0.082 Uiso 1 1 calc R . . H28C H 0.8868 -0.1382 0.2095 0.082 Uiso 1 1 calc R . . C29 C 0.6748(2) -0.04157(19) 0.11636(13) 0.0417(6) Uani 1 1 d . . . H29 H 0.6888 0.0215 0.0888 0.050 Uiso 1 1 calc R . . C30 C 0.5493(3) -0.0642(2) 0.11084(16) 0.0539(8) Uani 1 1 d . . . H30A H 0.5364 -0.1316 0.1268 0.081 Uiso 1 1 calc R . . H30B H 0.5354 -0.0548 0.0587 0.081 Uiso 1 1 calc R . . H30C H 0.4954 -0.0206 0.1435 0.081 Uiso 1 1 calc R . . C31 C 0.7595(3) -0.1173(2) 0.07382(16) 0.0579(8) Uani 1 1 d . . . H31A H 0.8398 -0.1036 0.0791 0.087 Uiso 1 1 calc R . . H31B H 0.7510 -0.1146 0.0205 0.087 Uiso 1 1 calc R . . H31C H 0.7422 -0.1821 0.0946 0.087 Uiso 1 1 calc R . . C32 C 0.7872(2) 0.52948(18) 0.39000(14) 0.0387(6) Uani 1 1 d . . . H32 H 0.8021 0.5680 0.4301 0.046 Uiso 1 1 calc R . . C33 C 0.7655(2) 0.56950(18) 0.32469(14) 0.0405(6) Uani 1 1 d . . . H33 H 0.7648 0.6377 0.3162 0.049 Uiso 1 1 calc R . . C34 C 0.8269(2) 0.38202(17) 0.46037(13) 0.0354(6) Uani 1 1 d . . . C35 C 0.9443(2) 0.34879(19) 0.45481(14) 0.0406(6) Uani 1 1 d . . . C36 C 0.9820(3) 0.3063(2) 0.51875(15) 0.0489(7) Uani 1 1 d . . . H36 H 1.0614 0.2839 0.5162 0.059 Uiso 1 1 calc R . . C37 C 0.9078(3) 0.2960(2) 0.58482(15) 0.0528(8) Uani 1 1 d . . . H37 H 0.9361 0.2685 0.6279 0.063 Uiso 1 1 calc R . . C38 C 0.7916(3) 0.3258(2) 0.58858(15) 0.0525(7) Uani 1 1 d . . . H38 H 0.7397 0.3162 0.6341 0.063 Uiso 1 1 calc R . . C39 C 0.7487(2) 0.3696(2) 0.52698(14) 0.0432(6) Uani 1 1 d . B . C40 C 1.0299(2) 0.3578(2) 0.38267(15) 0.0492(7) Uani 1 1 d . . . H40 H 0.9890 0.3960 0.3456 0.059 Uiso 1 1 calc R . . C41 C 1.0667(3) 0.2584(3) 0.34942(19) 0.0742(10) Uani 1 1 d . . . H41A H 1.1064 0.2189 0.3849 0.111 Uiso 1 1 calc R . . H41B H 1.1199 0.2662 0.3021 0.111 Uiso 1 1 calc R . . H41C H 0.9975 0.2262 0.3399 0.111 Uiso 1 1 calc R . . C42 C 1.1373(3) 0.4113(3) 0.3930(2) 0.0819(12) Uani 1 1 d . . . H42A H 1.1128 0.4738 0.4167 0.123 Uiso 1 1 calc R . . H42B H 1.1846 0.4224 0.3439 0.123 Uiso 1 1 calc R . . H42C H 1.1836 0.3721 0.4251 0.123 Uiso 1 1 calc R . . C43 C 0.6208(3) 0.4024(2) 0.53257(16) 0.0553(8) Uani 1 1 d . . . H43 H 0.6038 0.4221 0.4813 0.066 Uiso 1 1 calc R A 1 C46 C 0.7497(3) 0.54050(18) 0.19349(13) 0.0404(6) Uani 1 1 d . . . C47 C 0.8595(3) 0.55665(19) 0.15102(14) 0.0488(7) Uani 1 1 d . . . C48 C 0.8627(3) 0.5876(2) 0.07638(17) 0.0636(9) Uani 1 1 d . . . H48 H 0.9356 0.5999 0.0468 0.076 Uiso 1 1 calc R . . C49 C 0.7620(4) 0.6005(2) 0.04474(17) 0.0709(11) Uani 1 1 d . . . H49 H 0.7662 0.6208 -0.0064 0.085 Uiso 1 1 calc R . . C50 C 0.6560(3) 0.5843(2) 0.08670(17) 0.0625(9) Uani 1 1 d . . . H50 H 0.5873 0.5935 0.0641 0.075 Uiso 1 1 calc R . . C51 C 0.6468(3) 0.55472(19) 0.16171(15) 0.0479(7) Uani 1 1 d . . . C52 C 0.9718(3) 0.5369(2) 0.18331(17) 0.0554(8) Uani 1 1 d . . . H52 H 0.9501 0.5279 0.2389 0.066 Uiso 1 1 calc R . . C53 C 1.0339(4) 0.4424(3) 0.1529(2) 0.0945(13) Uani 1 1 d . . . H53A H 0.9802 0.3897 0.1624 0.142 Uiso 1 1 calc R . . H53B H 1.1020 0.4271 0.1781 0.142 Uiso 1 1 calc R . . H53C H 1.0594 0.4496 0.0987 0.142 Uiso 1 1 calc R . . C54 C 1.0536(4) 0.6197(3) 0.1705(3) 0.1066(16) Uani 1 1 d . . . H54A H 1.0753 0.6315 0.1163 0.160 Uiso 1 1 calc R . . H54B H 1.1240 0.6025 0.1928 0.160 Uiso 1 1 calc R . . H54C H 1.0143 0.6784 0.1939 0.160 Uiso 1 1 calc R . . C55 C 0.5284(3) 0.5354(2) 0.20679(16) 0.0524(7) Uani 1 1 d . . . H55 H 0.5366 0.5386 0.2612 0.063 Uiso 1 1 calc R . . C56 C 0.4308(3) 0.6099(2) 0.1931(2) 0.0697(10) Uani 1 1 d . . . H56A H 0.4553 0.6754 0.2001 0.105 Uiso 1 1 calc R . . H56B H 0.3602 0.5979 0.2288 0.105 Uiso 1 1 calc R . . H56C H 0.4144 0.6041 0.1416 0.105 Uiso 1 1 calc R . . C57 C 0.4912(3) 0.4344(2) 0.1938(2) 0.0765(10) Uani 1 1 d . . . H57A H 0.4818 0.4285 0.1410 0.115 Uiso 1 1 calc R . . H57B H 0.4169 0.4234 0.2260 0.115 Uiso 1 1 calc R . . H57C H 0.5509 0.3861 0.2061 0.115 Uiso 1 1 calc R . . C45A C 0.5422(6) 0.3216(6) 0.5634(8) 0.090(3) Uani 0.611(17) 1 d P B 1 H45A H 0.5519 0.3069 0.6157 0.135 Uiso 0.611(17) 1 calc PR B 1 H45B H 0.5635 0.2634 0.5332 0.135 Uiso 0.611(17) 1 calc PR B 1 H45C H 0.4606 0.3423 0.5612 0.135 Uiso 0.611(17) 1 calc PR B 1 C45B C 0.5485(9) 0.3149(8) 0.5083(11) 0.073(4) Uani 0.389(17) 1 d P B 2 H45D H 0.5548 0.2595 0.5429 0.110 Uiso 0.389(17) 1 calc PR B 2 H45E H 0.5806 0.2955 0.4570 0.110 Uiso 0.389(17) 1 calc PR B 2 H45F H 0.4662 0.3368 0.5104 0.110 Uiso 0.389(17) 1 calc PR B 2 C44B C 0.5656(12) 0.4405(13) 0.6043(7) 0.068(4) Uani 0.389(17) 1 d P B 2 H44A H 0.5602 0.3881 0.6423 0.102 Uiso 0.389(17) 1 calc PR B 2 H44B H 0.4871 0.4677 0.5997 0.102 Uiso 0.389(17) 1 calc PR B 2 H44C H 0.6122 0.4914 0.6194 0.102 Uiso 0.389(17) 1 calc PR B 2 C44A C 0.5941(7) 0.4931(9) 0.5859(5) 0.071(2) Uani 0.611(17) 1 d P B 1 H44D H 0.5099 0.5092 0.5947 0.106 Uiso 0.611(17) 1 calc PR B 1 H44E H 0.6349 0.5487 0.5620 0.106 Uiso 0.611(17) 1 calc PR B 1 H44F H 0.6212 0.4774 0.6340 0.106 Uiso 0.611(17) 1 calc PR B 1 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 Ga1 0.03759(18) 0.03000(16) 0.03490(15) 0.00156(11) -0.01150(12) -0.00149(12) Zn1 0.03416(18) 0.03078(17) 0.03713(16) 0.00132(11) -0.01520(12) -0.00306(12) N1 0.0318(12) 0.0302(11) 0.0372(11) 0.0037(8) -0.0174(9) -0.0034(9) N2 0.0300(11) 0.0336(11) 0.0325(10) 0.0026(8) -0.0149(9) -0.0025(9) N3 0.0387(13) 0.0321(11) 0.0378(11) 0.0022(9) -0.0175(9) -0.0062(9) N4 0.0368(12) 0.0331(11) 0.0333(10) -0.0002(8) -0.0099(9) 0.0001(9) N5 0.0389(13) 0.0320(11) 0.0367(11) 0.0048(9) -0.0061(9) 0.0007(9) C1 0.0254(13) 0.0320(13) 0.0293(11) 0.0051(9) -0.0083(10) -0.0035(10) C2 0.0346(15) 0.0280(13) 0.0501(15) 0.0068(11) -0.0231(12) -0.0049(11) C3 0.0481(17) 0.0362(15) 0.0528(16) 0.0131(12) -0.0296(14) -0.0098(12) C4 0.059(2) 0.0563(19) 0.071(2) 0.0275(15) -0.0389(18) -0.0160(16) C5 0.047(2) 0.059(2) 0.101(3) 0.0302(18) -0.041(2) -0.0039(16) C6 0.0378(17) 0.0487(18) 0.085(2) 0.0121(15) -0.0233(15) -0.0001(13) C7 0.0313(15) 0.0373(15) 0.0589(16) 0.0031(12) -0.0197(13) -0.0033(12) C8 0.060(2) 0.0523(17) 0.0407(15) 0.0137(12) -0.0241(14) -0.0089(14) C9 0.083(3) 0.072(2) 0.077(2) -0.0081(18) -0.029(2) -0.002(2) C10 0.111(3) 0.068(2) 0.065(2) 0.0234(18) 0.001(2) -0.009(2) C11 0.0260(14) 0.0578(18) 0.0523(16) 0.0019(13) -0.0105(12) -0.0032(13) C12 0.0463(18) 0.0587(19) 0.0540(17) 0.0108(14) -0.0125(14) -0.0060(15) C13 0.052(2) 0.081(2) 0.074(2) -0.0125(18) 0.0002(17) 0.0015(18) C14 0.0323(14) 0.0360(14) 0.0350(12) -0.0019(10) -0.0171(11) -0.0007(11) C15 0.0310(15) 0.0467(16) 0.0402(14) -0.0030(11) -0.0124(11) -0.0016(12) C16 0.0299(15) 0.0672(19) 0.0488(16) -0.0071(14) -0.0137(12) -0.0002(13) C17 0.0371(17) 0.068(2) 0.0553(17) -0.0089(14) -0.0260(14) 0.0089(14) C18 0.0538(19) 0.0469(16) 0.0394(14) 0.0015(12) -0.0253(13) 0.0064(14) C19 0.0411(16) 0.0353(14) 0.0365(13) 0.0010(10) -0.0185(12) 0.0001(11) C20 0.0309(15) 0.0668(19) 0.0395(14) 0.0032(13) -0.0084(12) -0.0080(13) C21 0.062(2) 0.085(2) 0.0424(16) -0.0058(15) -0.0046(15) -0.0238(18) C22 0.0459(19) 0.072(2) 0.0535(17) 0.0023(15) -0.0048(14) -0.0153(16) C23 0.0469(17) 0.0444(16) 0.0343(13) 0.0048(11) -0.0128(12) -0.0039(13) C24 0.058(2) 0.072(2) 0.0419(15) -0.0050(14) -0.0122(14) 0.0081(16) C25 0.095(3) 0.064(2) 0.065(2) -0.0108(17) 0.0142(19) -0.032(2) C26 0.0510(18) 0.0348(14) 0.0462(15) 0.0073(11) -0.0192(13) -0.0112(13) C27 0.058(2) 0.0494(18) 0.0679(19) 0.0148(14) -0.0168(16) -0.0182(15) C28 0.057(2) 0.0342(15) 0.077(2) 0.0056(14) -0.0250(16) -0.0042(14) C29 0.0495(17) 0.0425(15) 0.0374(13) -0.0028(11) -0.0188(12) -0.0067(13) C30 0.056(2) 0.0548(18) 0.0591(17) -0.0061(14) -0.0296(15) -0.0103(15) C31 0.067(2) 0.0587(19) 0.0511(17) -0.0157(14) -0.0164(15) -0.0039(16) C32 0.0453(17) 0.0328(14) 0.0387(14) -0.0024(11) -0.0075(12) -0.0038(12) C33 0.0483(17) 0.0276(13) 0.0448(15) -0.0040(11) -0.0037(12) -0.0014(12) C34 0.0406(16) 0.0341(14) 0.0333(13) -0.0015(10) -0.0118(11) -0.0019(11) C35 0.0418(16) 0.0388(15) 0.0426(14) -0.0037(11) -0.0119(12) 0.0023(12) C36 0.0500(18) 0.0458(17) 0.0532(17) -0.0045(13) -0.0202(14) 0.0108(14) C37 0.067(2) 0.0502(18) 0.0434(16) 0.0025(13) -0.0220(15) 0.0085(15) C38 0.064(2) 0.0549(18) 0.0387(15) 0.0075(13) -0.0075(14) -0.0059(15) C39 0.0452(17) 0.0471(16) 0.0385(14) 0.0008(12) -0.0110(12) -0.0006(13) C40 0.0385(17) 0.0600(19) 0.0487(16) -0.0050(13) -0.0091(13) 0.0080(14) C41 0.074(3) 0.079(2) 0.067(2) -0.0262(18) 0.0011(18) 0.007(2) C42 0.070(3) 0.097(3) 0.077(2) -0.022(2) 0.006(2) -0.029(2) C43 0.0426(18) 0.077(2) 0.0450(16) 0.0062(15) -0.0048(13) -0.0018(16) C46 0.0558(18) 0.0284(13) 0.0366(13) 0.0033(10) -0.0069(13) -0.0004(12) C47 0.065(2) 0.0364(15) 0.0419(15) 0.0051(12) 0.0001(14) -0.0015(14) C48 0.087(3) 0.0494(19) 0.0478(17) 0.0087(14) 0.0072(17) -0.0029(17) C49 0.120(3) 0.051(2) 0.0388(17) 0.0134(14) -0.009(2) 0.007(2) C50 0.092(3) 0.0482(18) 0.0492(17) 0.0087(14) -0.0255(18) 0.0117(17) C51 0.066(2) 0.0347(15) 0.0445(15) 0.0028(12) -0.0163(14) 0.0071(14) C52 0.0509(19) 0.0566(19) 0.0531(17) 0.0020(14) 0.0103(15) -0.0055(15) C53 0.105(3) 0.084(3) 0.093(3) -0.015(2) -0.022(2) 0.033(2) C54 0.061(3) 0.084(3) 0.175(5) 0.024(3) -0.015(3) -0.020(2) C55 0.0498(19) 0.0548(19) 0.0552(17) 0.0048(14) -0.0222(15) 0.0115(15) C56 0.062(2) 0.057(2) 0.097(3) 0.0006(18) -0.0386(19) 0.0099(17) C57 0.067(2) 0.058(2) 0.102(3) 0.0098(19) -0.009(2) 0.0027(18) C45A 0.044(4) 0.104(6) 0.118(9) 0.000(6) 0.004(4) -0.016(4) C45B 0.045(6) 0.094(8) 0.083(10) -0.015(6) -0.008(6) -0.013(5) C44B 0.063(7) 0.084(10) 0.056(7) -0.018(6) -0.005(5) 0.007(7) C44A 0.044(4) 0.092(7) 0.073(4) 0.007(4) -0.012(3) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N4 1.8633(19) . ? Ga1 N5 1.867(2) . ? Ga1 Zn1 2.3230(7) . ? Zn1 N1 1.986(2) . ? Zn1 N2 2.0041(19) . ? N1 C1 1.354(3) . ? N1 C2 1.420(3) . ? N2 C1 1.356(3) . ? N2 C14 1.423(3) . ? N3 C1 1.360(3) . ? N3 C26 1.490(3) . ? N3 C29 1.497(3) . ? N4 C32 1.383(3) . ? N4 C34 1.435(3) . ? N5 C33 1.392(3) . ? N5 C46 1.433(3) . ? C2 C3 1.404(3) . ? C2 C7 1.408(4) . ? C3 C4 1.399(4) . ? C3 C8 1.509(4) . ? C4 C5 1.366(5) . ? C5 C6 1.381(4) . ? C6 C7 1.395(4) . ? C7 C11 1.520(4) . ? C8 C10 1.530(4) . ? C8 C9 1.530(4) . ? C11 C12 1.526(4) . ? C11 C13 1.533(4) . ? C14 C19 1.407(3) . ? C14 C15 1.407(4) . ? C15 C16 1.393(4) . ? C15 C20 1.519(3) . ? C16 C17 1.379(4) . ? C17 C18 1.375(4) . ? C18 C19 1.393(3) . ? C19 C23 1.525(4) . ? C20 C21 1.532(4) . ? C20 C22 1.535(4) . ? C23 C25 1.512(4) . ? C23 C24 1.532(3) . ? C26 C28 1.530(4) . ? C26 C27 1.532(4) . ? C29 C30 1.526(4) . ? C29 C31 1.529(4) . ? C32 C33 1.338(4) . ? C34 C39 1.401(4) . ? C34 C35 1.402(4) . ? C35 C36 1.396(4) . ? C35 C40 1.516(4) . ? C36 C37 1.366(4) . ? C37 C38 1.380(4) . ? C38 C39 1.394(4) . ? C39 C43 1.517(4) . ? C40 C42 1.522(4) . ? C40 C41 1.523(4) . ? C43 C44B 1.447(12) . ? C43 C45A 1.522(8) . ? C43 C44A 1.584(10) . ? C43 C45B 1.616(11) . ? C46 C51 1.403(4) . ? C46 C47 1.407(4) . ? C47 C48 1.395(4) . ? C47 C52 1.515(4) . ? C48 C49 1.377(5) . ? C49 C50 1.368(5) . ? C50 C51 1.390(4) . ? C51 C55 1.519(4) . ? C52 C54 1.517(5) . ? C52 C53 1.527(5) . ? C55 C57 1.517(5) . ? C55 C56 1.530(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 N4 Ga1 N5 88.12(9) . . ? N4 Ga1 Zn1 136.01(6) . . ? N5 Ga1 Zn1 135.85(6) . . ? N1 Zn1 N2 67.40(8) . . ? N1 Zn1 Ga1 146.40(5) . . ? N2 Zn1 Ga1 146.12(6) . . ? C1 N1 C2 127.0(2) . . ? C1 N1 Zn1 91.89(14) . . ? C2 N1 Zn1 132.08(15) . . ? C1 N2 C14 127.2(2) . . ? C1 N2 Zn1 91.07(13) . . ? C14 N2 Zn1 129.65(15) . . ? C1 N3 C26 118.40(19) . . ? C1 N3 C29 118.93(19) . . ? C26 N3 C29 122.6(2) . . ? C32 N4 C34 118.9(2) . . ? C32 N4 Ga1 109.29(15) . . ? C34 N4 Ga1 130.88(16) . . ? C33 N5 C46 119.6(2) . . ? C33 N5 Ga1 108.78(16) . . ? C46 N5 Ga1 128.92(16) . . ? N1 C1 N2 109.5(2) . . ? N1 C1 N3 125.1(2) . . ? N2 C1 N3 125.4(2) . . ? C3 C2 C7 121.2(2) . . ? C3 C2 N1 118.1(2) . . ? C7 C2 N1 120.4(2) . . ? C4 C3 C2 118.0(3) . . ? C4 C3 C8 120.6(2) . . ? C2 C3 C8 121.4(2) . . ? C5 C4 C3 121.5(3) . . ? C4 C5 C6 120.0(3) . . ? C5 C6 C7 121.5(3) . . ? C6 C7 C2 117.8(2) . . ? C6 C7 C11 120.8(3) . . ? C2 C7 C11 121.4(2) . . ? C3 C8 C10 113.0(3) . . ? C3 C8 C9 111.6(3) . . ? C10 C8 C9 110.6(3) . . ? C7 C11 C12 110.9(2) . . ? C7 C11 C13 113.8(2) . . ? C12 C11 C13 110.0(2) . . ? C19 C14 C15 120.9(2) . . ? C19 C14 N2 118.1(2) . . ? C15 C14 N2 120.6(2) . . ? C16 C15 C14 118.3(2) . . ? C16 C15 C20 120.0(2) . . ? C14 C15 C20 121.6(2) . . ? C17 C16 C15 121.1(3) . . ? C18 C17 C16 120.0(3) . . ? C17 C18 C19 121.5(2) . . ? C18 C19 C14 118.1(2) . . ? C18 C19 C23 121.7(2) . . ? C14 C19 C23 120.1(2) . . ? C15 C20 C21 110.4(2) . . ? C15 C20 C22 113.4(2) . . ? C21 C20 C22 109.7(2) . . ? C25 C23 C19 111.2(2) . . ? C25 C23 C24 110.5(2) . . ? C19 C23 C24 113.1(2) . . ? N3 C26 C28 115.9(2) . . ? N3 C26 C27 112.9(2) . . ? C28 C26 C27 110.1(2) . . ? N3 C29 C30 115.5(2) . . ? N3 C29 C31 112.1(2) . . ? C30 C29 C31 110.0(2) . . ? C33 C32 N4 116.8(2) . . ? C32 C33 N5 117.0(2) . . ? C39 C34 C35 121.1(2) . . ? C39 C34 N4 119.9(2) . . ? C35 C34 N4 119.0(2) . . ? C36 C35 C34 117.8(2) . . ? C36 C35 C40 119.7(3) . . ? C34 C35 C40 122.4(2) . . ? C37 C36 C35 121.8(3) . . ? C36 C37 C38 119.6(3) . . ? C37 C38 C39 121.3(3) . . ? C38 C39 C34 118.2(3) . . ? C38 C39 C43 120.4(3) . . ? C34 C39 C43 121.4(2) . . ? C35 C40 C42 112.8(2) . . ? C35 C40 C41 110.9(3) . . ? C42 C40 C41 110.0(3) . . ? C44B C43 C39 116.2(5) . . ? C44B C43 C45A 77.9(6) . . ? C39 C43 C45A 111.3(4) . . ? C44B C43 C44A 32.3(5) . . ? C39 C43 C44A 109.4(4) . . ? C45A C43 C44A 109.3(5) . . ? C44B C43 C45B 110.3(7) . . ? C39 C43 C45B 109.4(5) . . ? C45A C43 C45B 36.6(4) . . ? C44A C43 C45B 136.5(5) . . ? C51 C46 C47 121.1(2) . . ? C51 C46 N5 119.7(2) . . ? C47 C46 N5 119.1(2) . . ? C48 C47 C46 117.9(3) . . ? C48 C47 C52 120.3(3) . . ? C46 C47 C52 121.8(2) . . ? C49 C48 C47 121.2(3) . . ? C50 C49 C48 120.2(3) . . ? C49 C50 C51 121.4(3) . . ? C50 C51 C46 118.2(3) . . ? C50 C51 C55 120.4(3) . . ? C46 C51 C55 121.3(2) . . ? C47 C52 C54 113.6(3) . . ? C47 C52 C53 110.4(3) . . ? C54 C52 C53 110.7(3) . . ? C57 C55 C51 111.9(3) . . ? C57 C55 C56 109.2(3) . . ? C51 C55 C56 114.2(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.745 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.051 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 645311' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H93 Ga2 N6 O0.50 Zn' _chemical_formula_weight 1111.21 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.953(3) _cell_length_b 21.070(4) _cell_length_c 46.243(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13595(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4728 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _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 Kappa 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 22106 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.1203 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11852 _reflns_number_gt 7515 _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. During the couse of refinement a molecule of diethyl ether was located in the crystal lattice. its atoms were successfully isotropically refined at 50% occupancy. The carbon atoms of the tmeda ligand were all found to be disordered over 2 sites. This disorder was successfully modelled. The poor r-factors for the structure are due to this disorder and the poor quality of the crystal used in the experiment. Despite this, the molecular connectivity of the structure is unambiguous. 96 restraints were used during the course of refinement. These involved the DFIX command of SHELXL to restrain the C-O distances in the dietheyl ether of crystallisation towards a target of 1.42 ang., the C-N distances of both disordered sets of the tmeda ligand to 1.43 ang., and the C-C distances of the diethyl ether and the tmeda ligand to 1.52 ang. ; _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^)+(0.0991P)^2^+120.0323P] 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 11852 _refine_ls_number_parameters 701 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1774 _refine_ls_R_factor_gt 0.1271 _refine_ls_wR_factor_ref 0.3198 _refine_ls_wR_factor_gt 0.3003 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.42916(8) 0.28547(6) 0.16869(3) 0.0412(3) Uani 1 1 d . . . Ga2 Ga 0.66305(8) 0.35475(6) 0.11518(3) 0.0407(3) Uani 1 1 d . . . Zn1 Zn 0.58931(8) 0.27762(6) 0.14732(3) 0.0397(3) Uani 1 1 d . A . O1 O 0.7765(16) 0.0911(10) 0.0511(4) 0.088(6) Uiso 0.50 1 d PD . . N1 N 0.3048(6) 0.3093(4) 0.1557(2) 0.042(2) Uani 1 1 d . . . N2 N 0.3711(6) 0.2714(4) 0.2054(2) 0.047(2) Uani 1 1 d . . . N3 N 0.7223(6) 0.4347(4) 0.12094(19) 0.040(2) Uani 1 1 d . . . N4 N 0.6766(7) 0.3700(4) 0.0752(2) 0.051(2) Uani 1 1 d . . . N5 N 0.6155(7) 0.1827(4) 0.1305(2) 0.051(2) Uiso 1 1 d D . . N6 N 0.6950(6) 0.2525(4) 0.17974(19) 0.044(2) Uani 1 1 d D . . C1 C 0.2382(8) 0.3042(5) 0.1783(3) 0.044(3) Uani 1 1 d . . . H1 H 0.1722 0.3136 0.1756 0.053 Uiso 1 1 calc R . . C2 C 0.2726(8) 0.2854(6) 0.2040(3) 0.058(3) Uani 1 1 d . . . H2 H 0.2323 0.2816 0.2205 0.070 Uiso 1 1 calc R . . C3 C 0.2680(7) 0.3216(5) 0.1277(2) 0.040(3) Uani 1 1 d . . . C4 C 0.2779(8) 0.3809(6) 0.1153(3) 0.051(3) Uani 1 1 d . . . C5 C 0.2343(8) 0.3903(6) 0.0878(3) 0.055(3) Uani 1 1 d . . . H5 H 0.2406 0.4304 0.0787 0.066 Uiso 1 1 calc R . . C6 C 0.1849(10) 0.3445(7) 0.0745(3) 0.064(4) Uani 1 1 d . . . H6 H 0.1553 0.3533 0.0565 0.077 Uiso 1 1 calc R . . C7 C 0.1760(9) 0.2858(7) 0.0863(3) 0.059(3) Uani 1 1 d . . . H7 H 0.1412 0.2540 0.0763 0.071 Uiso 1 1 calc R . . C8 C 0.2179(8) 0.2718(5) 0.1133(3) 0.052(3) Uani 1 1 d . . . C9 C 0.3330(8) 0.4346(5) 0.1301(3) 0.051(3) Uani 1 1 d . . . H9 H 0.3815 0.4134 0.1428 0.061 Uiso 1 1 calc R . . C10 C 0.3907(12) 0.4771(6) 0.1093(3) 0.069(4) Uani 1 1 d . . . H10A H 0.3699 0.4690 0.0893 0.104 Uiso 1 1 calc R . . H10B H 0.4591 0.4674 0.1111 0.104 Uiso 1 1 calc R . . H10C H 0.3797 0.5218 0.1141 0.104 Uiso 1 1 calc R . . C11 C 0.2677(11) 0.4677(7) 0.1498(3) 0.082(5) Uani 1 1 d . . . H11A H 0.2192 0.4905 0.1385 0.124 Uiso 1 1 calc R . . H11B H 0.3041 0.4981 0.1615 0.124 Uiso 1 1 calc R . . H11C H 0.2363 0.4368 0.1625 0.124 Uiso 1 1 calc R . . C12 C 0.2093(10) 0.2069(6) 0.1258(3) 0.066(4) Uani 1 1 d . . . H12 H 0.2473 0.2065 0.1442 0.079 Uiso 1 1 calc R . . C13 C 0.2548(12) 0.1571(7) 0.1052(4) 0.100(6) Uani 1 1 d . . . H13A H 0.2168 0.1543 0.0875 0.150 Uiso 1 1 calc R . . H13B H 0.2561 0.1156 0.1148 0.150 Uiso 1 1 calc R . . H13C H 0.3204 0.1700 0.1004 0.150 Uiso 1 1 calc R . . C14 C 0.1072(13) 0.1879(9) 0.1334(4) 0.104(6) Uani 1 1 d U . . H14A H 0.0856 0.2123 0.1503 0.155 Uiso 1 1 calc R . . H14B H 0.1052 0.1425 0.1380 0.155 Uiso 1 1 calc R . . H14C H 0.0650 0.1966 0.1170 0.155 Uiso 1 1 calc R . . C15 C 0.4076(7) 0.2445(6) 0.2309(2) 0.044(3) Uani 1 1 d . . . C16 C 0.4601(8) 0.2832(6) 0.2504(3) 0.052(3) Uani 1 1 d . . . C17 C 0.4996(9) 0.2569(7) 0.2754(3) 0.060(3) Uani 1 1 d . . . H17 H 0.5358 0.2822 0.2884 0.072 Uiso 1 1 calc R . . C18 C 0.4842(9) 0.1913(7) 0.2809(3) 0.064(4) Uani 1 1 d . . . H18 H 0.5087 0.1726 0.2981 0.077 Uiso 1 1 calc R . . C19 C 0.4346(9) 0.1549(6) 0.2617(3) 0.059(3) Uani 1 1 d . . . H19 H 0.4277 0.1108 0.2655 0.071 Uiso 1 1 calc R . . C20 C 0.3947(8) 0.1792(6) 0.2374(2) 0.044(3) Uani 1 1 d . . . C21 C 0.4715(9) 0.3541(6) 0.2449(3) 0.053(3) Uani 1 1 d . . . H21 H 0.4851 0.3596 0.2238 0.063 Uiso 1 1 calc R . . C22 C 0.5557(12) 0.3816(7) 0.2613(3) 0.087(5) Uani 1 1 d . . . H22A H 0.5424 0.3803 0.2821 0.131 Uiso 1 1 calc R . . H22B H 0.5659 0.4257 0.2552 0.131 Uiso 1 1 calc R . . H22C H 0.6133 0.3567 0.2571 0.131 Uiso 1 1 calc R . . C23 C 0.3765(12) 0.3900(7) 0.2515(4) 0.085(5) Uani 1 1 d . . . H23A H 0.3247 0.3723 0.2397 0.127 Uiso 1 1 calc R . . H23B H 0.3845 0.4351 0.2470 0.127 Uiso 1 1 calc R . . H23C H 0.3606 0.3852 0.2720 0.127 Uiso 1 1 calc R . . C24 C 0.3395(9) 0.1388(6) 0.2166(3) 0.055(3) Uani 1 1 d . . . H24 H 0.3256 0.1655 0.1992 0.067 Uiso 1 1 calc R . . C25 C 0.3991(9) 0.0811(6) 0.2062(3) 0.074(4) Uani 1 1 d . . . H25A H 0.4494 0.0956 0.1929 0.111 Uiso 1 1 calc R . . H25B H 0.3572 0.0510 0.1961 0.111 Uiso 1 1 calc R . . H25C H 0.4285 0.0601 0.2229 0.111 Uiso 1 1 calc R . . C26 C 0.2416(10) 0.1181(7) 0.2294(3) 0.080(4) Uani 1 1 d . . . H26A H 0.2083 0.0905 0.2157 0.120 Uiso 1 1 calc R . . H26B H 0.2024 0.1558 0.2332 0.120 Uiso 1 1 calc R . . H26C H 0.2522 0.0950 0.2476 0.120 Uiso 1 1 calc R . . C27 C 0.7416(9) 0.4636(6) 0.0944(3) 0.060(4) Uani 1 1 d . . . H27 H 0.7700 0.5045 0.0932 0.072 Uiso 1 1 calc R . . C28 C 0.7176(9) 0.4301(6) 0.0703(3) 0.054(3) Uani 1 1 d . . . H28 H 0.7278 0.4463 0.0514 0.065 Uiso 1 1 calc R . . C29 C 0.7641(8) 0.4620(5) 0.1467(3) 0.046(3) Uani 1 1 d . . . C30 C 0.8657(7) 0.4579(5) 0.1502(3) 0.046(3) Uani 1 1 d . . . C31 C 0.9034(7) 0.4843(5) 0.1754(3) 0.045(3) Uani 1 1 d . . . H31 H 0.9706 0.4817 0.1786 0.054 Uiso 1 1 calc R . . C32 C 0.8477(8) 0.5139(5) 0.1957(3) 0.052(3) Uani 1 1 d . . . H32 H 0.8764 0.5331 0.2121 0.062 Uiso 1 1 calc R . . C33 C 0.7485(8) 0.5158(5) 0.1921(3) 0.046(3) Uani 1 1 d . . . H33 H 0.7091 0.5337 0.2067 0.055 Uiso 1 1 calc R . . C34 C 0.7071(7) 0.4911(4) 0.1669(2) 0.036(2) Uani 1 1 d . . . C35 C 0.9302(8) 0.4219(6) 0.1292(3) 0.052(3) Uani 1 1 d . . . H35 H 0.8888 0.3977 0.1154 0.062 Uiso 1 1 calc R . . C36 C 0.9985(8) 0.3750(6) 0.1443(3) 0.058(3) Uani 1 1 d . . . H36A H 1.0432 0.3985 0.1567 0.088 Uiso 1 1 calc R . . H36B H 1.0345 0.3512 0.1297 0.088 Uiso 1 1 calc R . . H36C H 0.9612 0.3454 0.1562 0.088 Uiso 1 1 calc R . . C37 C 0.9924(10) 0.4699(6) 0.1116(3) 0.069(4) Uani 1 1 d . . . H37A H 0.9522 0.4914 0.0973 0.103 Uiso 1 1 calc R . . H37B H 1.0441 0.4470 0.1018 0.103 Uiso 1 1 calc R . . H37C H 1.0201 0.5013 0.1248 0.103 Uiso 1 1 calc R . . C38 C 0.5984(8) 0.4966(6) 0.1625(3) 0.049(3) Uani 1 1 d . . . H38 H 0.5809 0.4740 0.1442 0.059 Uiso 1 1 calc R . . C39 C 0.5700(9) 0.5640(6) 0.1598(4) 0.085(5) Uani 1 1 d . . . H39A H 0.6016 0.5889 0.1749 0.127 Uiso 1 1 calc R . . H39B H 0.5003 0.5676 0.1619 0.127 Uiso 1 1 calc R . . H39C H 0.5891 0.5799 0.1407 0.127 Uiso 1 1 calc R . . C40 C 0.5438(10) 0.4661(8) 0.1876(3) 0.086(5) Uani 1 1 d . . . H40A H 0.5773 0.4749 0.2058 0.129 Uiso 1 1 calc R . . H40B H 0.5402 0.4201 0.1846 0.129 Uiso 1 1 calc R . . H40C H 0.4788 0.4837 0.1885 0.129 Uiso 1 1 calc R . . C41 C 0.6735(8) 0.3286(6) 0.0514(3) 0.052(3) Uani 1 1 d . . . C42 C 0.7612(10) 0.3035(8) 0.0399(3) 0.075(4) Uani 1 1 d . . . C43 C 0.7596(13) 0.2680(9) 0.0155(4) 0.103(6) Uani 1 1 d . . . H43 H 0.8180 0.2552 0.0067 0.124 Uiso 1 1 calc R . . C44 C 0.6688(16) 0.2496(11) 0.0027(4) 0.120(7) Uani 1 1 d . . . H44 H 0.6669 0.2245 -0.0144 0.144 Uiso 1 1 calc R . . C45 C 0.5859(11) 0.2692(8) 0.0158(3) 0.082(5) Uani 1 1 d . . . H45 H 0.5261 0.2554 0.0083 0.099 Uiso 1 1 calc R . . C46 C 0.5868(8) 0.3083(7) 0.0395(3) 0.056(3) Uani 1 1 d . . . C47 C 0.8582(9) 0.3235(9) 0.0534(3) 0.082(5) Uani 1 1 d . . . H47 H 0.8430 0.3490 0.0710 0.098 Uiso 1 1 calc R . . C48 C 0.9201(14) 0.3661(10) 0.0336(4) 0.119(7) Uani 1 1 d U . . H48A H 0.9722 0.3849 0.0449 0.178 Uiso 1 1 calc R . . H48B H 0.8802 0.3999 0.0254 0.178 Uiso 1 1 calc R . . H48C H 0.9472 0.3404 0.0179 0.178 Uiso 1 1 calc R . . C49 C 0.9080(14) 0.2630(9) 0.0637(4) 0.107(6) Uani 1 1 d U . . H49A H 0.8672 0.2412 0.0778 0.161 Uiso 1 1 calc R . . H49B H 0.9693 0.2740 0.0728 0.161 Uiso 1 1 calc R . . H49C H 0.9195 0.2349 0.0471 0.161 Uiso 1 1 calc R . . C50 C 0.4936(9) 0.3312(7) 0.0515(3) 0.065(4) Uani 1 1 d . . . H50 H 0.5100 0.3611 0.0675 0.078 Uiso 1 1 calc R . . C51 C 0.4331(13) 0.3683(9) 0.0305(4) 0.109(6) Uani 1 1 d . . . H51A H 0.4006 0.3390 0.0173 0.163 Uiso 1 1 calc R . . H51B H 0.4741 0.3971 0.0194 0.163 Uiso 1 1 calc R . . H51C H 0.3853 0.3930 0.0412 0.163 Uiso 1 1 calc R . . C52 C 0.4377(17) 0.2784(11) 0.0649(5) 0.147(9) Uani 1 1 d U . . H52A H 0.3778 0.2951 0.0729 0.220 Uiso 1 1 calc R . . H52B H 0.4756 0.2590 0.0805 0.220 Uiso 1 1 calc R . . H52C H 0.4231 0.2463 0.0502 0.220 Uiso 1 1 calc R . . C53 C 0.531(2) 0.1440(19) 0.1384(10) 0.065(11) Uani 0.38(3) 1 d PDU A 1 H53A H 0.5363 0.1019 0.1296 0.098 Uiso 0.38(3) 1 calc PR A 1 H53B H 0.4726 0.1649 0.1314 0.098 Uiso 0.38(3) 1 calc PR A 1 H53C H 0.5276 0.1397 0.1595 0.098 Uiso 0.38(3) 1 calc PR A 1 C54A C 0.646(4) 0.180(2) 0.1006(5) 0.15(3) Uani 0.62(3) 1 d PD A 2 H54A H 0.5976 0.1581 0.0891 0.230 Uiso 0.62(3) 1 calc PR A 2 H54B H 0.7072 0.1575 0.0993 0.230 Uiso 0.62(3) 1 calc PR A 2 H54C H 0.6542 0.2236 0.0933 0.230 Uiso 0.62(3) 1 calc PR A 2 C55 C 0.699(3) 0.161(2) 0.1466(8) 0.058(13) Uani 0.38(3) 1 d PDU A 1 H55A H 0.7571 0.1758 0.1363 0.069 Uiso 0.38(3) 1 calc PR A 1 H55B H 0.6993 0.1145 0.1467 0.069 Uiso 0.38(3) 1 calc PR A 1 C56 C 0.704(7) 0.1847(12) 0.1776(10) 0.17(4) Uani 0.38(3) 1 d PDU A 1 H56A H 0.6517 0.1646 0.1889 0.201 Uiso 0.38(3) 1 calc PR A 1 H56B H 0.7656 0.1714 0.1861 0.201 Uiso 0.38(3) 1 calc PR A 1 C57 C 0.7890(16) 0.2790(16) 0.1739(8) 0.037(8) Uani 0.38(3) 1 d PDU A 1 H57A H 0.7901 0.3237 0.1798 0.056 Uiso 0.38(3) 1 calc PR A 1 H57B H 0.8028 0.2758 0.1532 0.056 Uiso 0.38(3) 1 calc PR A 1 H57C H 0.8375 0.2554 0.1849 0.056 Uiso 0.38(3) 1 calc PR A 1 C58 C 0.671(2) 0.2704(18) 0.2092(4) 0.042(9) Uani 0.38(3) 1 d PDU A 1 H58A H 0.6254 0.2396 0.2173 0.064 Uiso 0.38(3) 1 calc PR A 1 H58B H 0.6417 0.3127 0.2093 0.064 Uiso 0.38(3) 1 calc PR A 1 H58C H 0.7292 0.2709 0.2210 0.064 Uiso 0.38(3) 1 calc PR A 1 C59 C 0.8793(19) 0.088(2) 0.0481(9) 0.131(15) Uiso 0.50 1 d PD . . H59A H 0.9014 0.1244 0.0360 0.158 Uiso 0.50 1 calc PR . . H59B H 0.8979 0.0485 0.0384 0.158 Uiso 0.50 1 calc PR . . C60 C 0.927(4) 0.092(3) 0.0776(9) 0.17(2) Uiso 0.50 1 d PD . . H60A H 0.8924 0.0643 0.0912 0.248 Uiso 0.50 1 calc PR . . H60B H 0.9244 0.1358 0.0847 0.248 Uiso 0.50 1 calc PR . . H60C H 0.9935 0.0782 0.0761 0.248 Uiso 0.50 1 calc PR . . C61 C 0.7319(18) 0.0842(16) 0.0243(5) 0.087(9) Uiso 0.50 1 d PD . . H61A H 0.7598 0.0479 0.0136 0.104 Uiso 0.50 1 calc PR . . H61B H 0.7402 0.1231 0.0126 0.104 Uiso 0.50 1 calc PR . . C62 C 0.6278(18) 0.0726(14) 0.0304(6) 0.077(8) Uiso 0.50 1 d PD . . H62A H 0.6010 0.1091 0.0407 0.116 Uiso 0.50 1 calc PR . . H62B H 0.6209 0.0344 0.0422 0.116 Uiso 0.50 1 calc PR . . H62C H 0.5934 0.0668 0.0121 0.116 Uiso 0.50 1 calc PR . . C53A C 0.5275(15) 0.1489(13) 0.1236(7) 0.073(8) Uani 0.62(3) 1 d PDU A 2 H53D H 0.5425 0.1117 0.1117 0.109 Uiso 0.62(3) 1 calc PR A 2 H53E H 0.4842 0.1771 0.1130 0.109 Uiso 0.62(3) 1 calc PR A 2 H53F H 0.4964 0.1350 0.1416 0.109 Uiso 0.62(3) 1 calc PR A 2 C54 C 0.670(5) 0.185(4) 0.1041(10) 0.073(18) Uani 0.38(3) 1 d PDU A 1 H54D H 0.6723 0.1420 0.0955 0.110 Uiso 0.38(3) 1 calc PR A 1 H54E H 0.7359 0.1986 0.1083 0.110 Uiso 0.38(3) 1 calc PR A 1 H54F H 0.6405 0.2142 0.0905 0.110 Uiso 0.38(3) 1 calc PR A 1 C55A C 0.673(2) 0.1536(11) 0.1523(6) 0.070(9) Uani 0.62(3) 1 d PDU A 2 H55C H 0.7105 0.1190 0.1431 0.083 Uiso 0.62(3) 1 calc PR A 2 H55D H 0.6303 0.1339 0.1667 0.083 Uiso 0.62(3) 1 calc PR A 2 C56A C 0.7426(18) 0.1961(10) 0.1682(7) 0.077(9) Uani 0.62(3) 1 d PD A 2 H56C H 0.7723 0.1721 0.1842 0.093 Uiso 0.62(3) 1 calc PR A 2 H56D H 0.7943 0.2093 0.1548 0.093 Uiso 0.62(3) 1 calc PR A 2 C57A C 0.7630(19) 0.3041(12) 0.1835(6) 0.072(8) Uani 0.62(3) 1 d PD A 2 H57D H 0.7854 0.3186 0.1646 0.108 Uiso 0.62(3) 1 calc PR A 2 H57E H 0.8177 0.2892 0.1949 0.108 Uiso 0.62(3) 1 calc PR A 2 H57F H 0.7317 0.3394 0.1936 0.108 Uiso 0.62(3) 1 calc PR A 2 C58A C 0.6563(17) 0.2352(14) 0.2072(4) 0.068(7) Uani 0.62(3) 1 d PDU A 2 H58D H 0.7079 0.2197 0.2198 0.102 Uiso 0.62(3) 1 calc PR A 2 H58E H 0.6084 0.2016 0.2046 0.102 Uiso 0.62(3) 1 calc PR A 2 H58F H 0.6260 0.2723 0.2162 0.102 Uiso 0.62(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0289(6) 0.0418(7) 0.0529(7) 0.0031(6) 0.0021(5) 0.0005(5) Ga2 0.0315(6) 0.0392(6) 0.0516(7) 0.0002(6) 0.0001(6) -0.0038(5) Zn1 0.0288(6) 0.0371(7) 0.0532(8) 0.0009(6) 0.0017(6) 0.0008(5) N1 0.029(5) 0.048(5) 0.050(6) 0.003(4) 0.005(4) 0.001(4) N2 0.027(5) 0.051(6) 0.063(6) -0.003(5) 0.000(4) 0.009(4) N3 0.039(5) 0.035(5) 0.047(5) 0.001(4) -0.003(4) -0.010(4) N4 0.045(6) 0.050(6) 0.058(6) 0.000(5) 0.001(5) -0.005(5) N6 0.030(5) 0.051(5) 0.051(6) 0.000(5) -0.003(4) 0.011(4) C1 0.021(5) 0.048(6) 0.063(7) -0.004(6) -0.001(5) 0.007(5) C2 0.022(6) 0.075(8) 0.078(9) 0.015(7) 0.013(6) 0.011(6) C3 0.029(6) 0.032(6) 0.059(7) 0.004(5) -0.007(5) 0.010(4) C4 0.043(7) 0.048(7) 0.061(8) 0.004(6) -0.003(6) 0.006(5) C5 0.031(6) 0.060(8) 0.073(9) 0.008(7) -0.011(6) -0.004(6) C6 0.059(9) 0.073(10) 0.062(9) 0.001(7) -0.017(7) 0.015(7) C7 0.043(7) 0.069(9) 0.065(9) -0.032(7) 0.005(6) -0.004(6) C8 0.042(7) 0.048(7) 0.065(8) -0.005(6) 0.006(6) 0.000(5) C9 0.046(7) 0.034(6) 0.072(8) -0.003(6) -0.011(6) 0.007(5) C10 0.111(12) 0.041(7) 0.056(8) 0.011(6) 0.002(8) -0.018(7) C11 0.070(10) 0.075(10) 0.102(12) -0.023(9) -0.009(9) -0.010(8) C12 0.061(8) 0.044(7) 0.091(10) -0.009(7) -0.009(8) -0.012(6) C13 0.077(11) 0.058(9) 0.165(17) -0.008(10) -0.012(12) 0.013(8) C14 0.100(8) 0.100(8) 0.111(8) 0.001(6) 0.004(6) -0.008(6) C15 0.027(6) 0.058(7) 0.045(6) 0.004(6) -0.002(5) 0.017(5) C16 0.043(7) 0.068(8) 0.043(7) -0.004(7) 0.007(5) 0.012(6) C17 0.039(7) 0.073(9) 0.067(9) -0.005(7) 0.013(7) -0.010(6) C18 0.043(8) 0.088(10) 0.062(8) 0.002(8) 0.004(7) 0.015(7) C19 0.045(7) 0.055(8) 0.077(9) 0.016(7) 0.005(7) -0.002(6) C20 0.032(6) 0.058(7) 0.041(6) 0.008(6) 0.004(5) 0.008(5) C21 0.056(8) 0.057(7) 0.044(7) 0.001(6) 0.001(6) 0.005(6) C22 0.125(15) 0.072(10) 0.065(9) 0.008(8) -0.032(10) -0.020(10) C23 0.103(13) 0.064(9) 0.088(11) -0.006(8) -0.004(10) 0.016(9) C24 0.053(8) 0.051(7) 0.063(8) 0.001(6) 0.004(6) -0.001(6) C25 0.047(8) 0.066(9) 0.109(12) -0.020(8) -0.004(8) 0.009(7) C26 0.057(9) 0.076(10) 0.108(12) 0.006(9) 0.017(9) -0.010(7) C27 0.047(7) 0.044(7) 0.089(10) 0.032(7) -0.009(7) -0.015(6) C28 0.063(8) 0.057(8) 0.041(7) 0.002(6) -0.003(6) -0.020(6) C29 0.031(6) 0.044(6) 0.064(8) 0.002(6) -0.004(6) -0.001(5) C30 0.023(5) 0.041(6) 0.074(8) -0.009(6) -0.005(6) -0.001(4) C31 0.019(5) 0.038(6) 0.079(9) 0.003(6) -0.005(6) -0.004(4) C32 0.043(7) 0.047(7) 0.065(8) 0.002(6) -0.008(6) 0.003(5) C33 0.045(7) 0.035(6) 0.058(7) -0.005(5) 0.007(6) -0.004(5) C34 0.036(6) 0.026(5) 0.047(6) 0.003(5) 0.002(5) 0.008(4) C35 0.034(6) 0.050(7) 0.071(8) -0.009(6) 0.000(6) -0.001(5) C36 0.034(7) 0.061(8) 0.080(9) -0.005(7) -0.007(6) 0.010(6) C37 0.080(10) 0.046(7) 0.079(9) 0.029(7) -0.013(8) 0.016(7) C38 0.036(6) 0.056(7) 0.057(7) -0.010(6) -0.004(6) -0.005(5) C39 0.045(8) 0.052(8) 0.158(15) -0.016(9) -0.041(9) 0.005(6) C40 0.038(8) 0.126(14) 0.094(11) -0.006(10) 0.021(8) -0.030(8) C41 0.039(7) 0.064(8) 0.053(7) -0.009(6) -0.002(6) 0.000(6) C42 0.046(8) 0.128(13) 0.051(8) -0.027(9) 0.007(7) 0.018(8) C43 0.070(11) 0.126(15) 0.113(14) -0.056(12) 0.026(11) 0.009(10) C44 0.138(19) 0.155(18) 0.067(11) -0.058(12) 0.010(12) -0.015(15) C45 0.058(9) 0.111(13) 0.078(10) -0.030(10) -0.013(8) 0.003(9) C46 0.038(7) 0.088(9) 0.042(7) -0.017(7) -0.002(6) -0.002(6) C47 0.039(8) 0.128(14) 0.078(10) -0.002(10) -0.003(7) 0.023(8) C48 0.110(9) 0.126(9) 0.120(9) -0.002(6) 0.009(6) -0.002(6) C49 0.101(8) 0.104(8) 0.116(8) 0.000(6) -0.002(6) 0.002(6) C50 0.037(7) 0.096(11) 0.063(8) 0.009(8) 0.009(6) -0.016(7) C51 0.091(13) 0.103(14) 0.133(16) 0.040(12) 0.041(12) 0.022(11) C52 0.142(10) 0.145(10) 0.154(10) 0.012(7) 0.007(7) 0.006(7) C53 0.064(13) 0.064(13) 0.068(13) -0.003(7) -0.009(7) -0.006(7) C54A 0.26(6) 0.13(3) 0.07(2) -0.05(2) -0.01(3) 0.16(4) C55 0.061(14) 0.056(14) 0.057(14) 0.003(7) 0.002(7) 0.002(7) C56 0.17(4) 0.17(4) 0.17(4) 0.000(7) 0.000(7) 0.001(7) C57 0.034(10) 0.040(10) 0.037(10) -0.001(7) -0.006(6) -0.002(6) C58 0.041(10) 0.045(11) 0.041(10) 0.002(6) 0.004(6) 0.001(7) C53A 0.076(10) 0.071(9) 0.071(10) -0.004(7) -0.003(6) -0.002(6) C54 0.072(18) 0.074(19) 0.074(19) -0.003(7) 0.003(7) 0.003(7) C55A 0.070(11) 0.067(11) 0.072(11) 0.000(6) 0.002(7) -0.002(6) C56A 0.057(16) 0.053(13) 0.12(2) -0.009(14) -0.052(17) 0.027(11) C57A 0.060(16) 0.10(2) 0.061(16) -0.023(15) -0.021(13) -0.009(14) C58A 0.068(9) 0.067(9) 0.069(9) 0.002(6) 0.000(6) 0.004(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 Ga1 N2 1.905(10) . ? Ga1 N1 1.903(9) . ? Ga1 Zn1 2.4491(17) . ? Ga2 N4 1.886(10) . ? Ga2 N3 1.895(8) . ? Ga2 Zn1 2.4307(17) . ? Zn1 N6 2.168(9) . ? Zn1 N5 2.177(10) . ? O1 C61 1.394(18) . ? O1 C59 1.442(19) . ? N1 C1 1.403(13) . ? N1 C3 1.419(13) . ? N2 C2 1.408(13) . ? N2 C15 1.402(14) . ? N3 C27 1.396(14) . ? N3 C29 1.445(14) . ? N4 C41 1.402(15) . ? N4 C28 1.409(14) . ? N5 C55A 1.428(16) . ? N5 C54 1.443(19) . ? N5 C54A 1.446(18) . ? N5 C55 1.449(18) . ? N5 C53A 1.456(16) . ? N5 C53 1.481(18) . ? N6 C58A 1.429(16) . ? N6 C56 1.44(2) . ? N6 C57A 1.455(16) . ? N6 C57 1.450(17) . ? N6 C58 1.455(17) . ? N6 C56A 1.463(16) . ? C1 C2 1.339(16) . ? C3 C4 1.382(15) . ? C3 C8 1.426(15) . ? C4 C5 1.421(16) . ? C4 C9 1.531(16) . ? C5 C6 1.336(17) . ? C6 C7 1.357(18) . ? C7 C8 1.409(17) . ? C8 C12 1.489(17) . ? C9 C11 1.463(18) . ? C9 C10 1.543(17) . ? C12 C14 1.52(2) . ? C12 C13 1.55(2) . ? C15 C16 1.420(16) . ? C15 C20 1.421(16) . ? C16 C17 1.396(17) . ? C16 C21 1.522(17) . ? C17 C18 1.423(19) . ? C18 C19 1.361(18) . ? C19 C20 1.353(16) . ? C20 C24 1.501(16) . ? C21 C22 1.513(18) . ? C21 C23 1.556(19) . ? C24 C25 1.549(17) . ? C24 C26 1.553(17) . ? C27 C28 1.359(17) . ? C29 C34 1.374(15) . ? C29 C30 1.429(15) . ? C30 C31 1.394(16) . ? C30 C35 1.524(16) . ? C31 C32 1.370(16) . ? C32 C33 1.395(16) . ? C33 C34 1.397(15) . ? C34 C38 1.535(15) . ? C35 C36 1.540(16) . ? C35 C37 1.562(17) . ? C38 C39 1.479(17) . ? C38 C40 1.531(17) . ? C41 C46 1.396(16) . ? C41 C42 1.436(17) . ? C42 C43 1.35(2) . ? C42 C47 1.55(2) . ? C43 C44 1.45(2) . ? C44 C45 1.37(2) . ? C45 C46 1.370(18) . ? C46 C50 1.495(17) . ? C47 C49 1.53(2) . ? C47 C48 1.55(2) . ? C50 C52 1.50(2) . ? C50 C51 1.50(2) . ? C55 C56 1.52(2) . ? C59 C60 1.520(19) . ? C61 C62 1.500(18) . ? C55A C56A 1.507(18) . ? 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 Ga1 N1 86.2(4) . . ? N2 Ga1 Zn1 137.5(3) . . ? N1 Ga1 Zn1 136.3(3) . . ? N4 Ga2 N3 86.7(4) . . ? N4 Ga2 Zn1 139.1(3) . . ? N3 Ga2 Zn1 133.9(3) . . ? N6 Zn1 N5 84.7(3) . . ? N6 Zn1 Ga2 107.3(2) . . ? N5 Zn1 Ga2 109.0(3) . . ? N6 Zn1 Ga1 111.0(2) . . ? N5 Zn1 Ga1 111.1(3) . . ? Ga2 Zn1 Ga1 126.00(6) . . ? C61 O1 C59 111(2) . . ? C1 N1 C3 117.1(9) . . ? C1 N1 Ga1 110.4(7) . . ? C3 N1 Ga1 131.7(7) . . ? C2 N2 C15 118.6(10) . . ? C2 N2 Ga1 109.9(8) . . ? C15 N2 Ga1 131.1(7) . . ? C27 N3 C29 118.3(9) . . ? C27 N3 Ga2 110.4(7) . . ? C29 N3 Ga2 130.2(7) . . ? C41 N4 C28 116.5(10) . . ? C41 N4 Ga2 131.3(8) . . ? C28 N4 Ga2 110.5(8) . . ? C55A N5 C54 108(4) . . ? C55A N5 C54A 119(3) . . ? C54 N5 C54A 15(5) . . ? C55A N5 C55 19(2) . . ? C54 N5 C55 91(4) . . ? C54A N5 C55 104(3) . . ? C55A N5 C53A 115.0(17) . . ? C54 N5 C53A 106(3) . . ? C54A N5 C53A 91(3) . . ? C55 N5 C53A 130(2) . . ? C55A N5 C53 92(2) . . ? C54 N5 C53 130(4) . . ? C54A N5 C53 117(3) . . ? C55 N5 C53 110(3) . . ? C53A N5 C53 27.3(16) . . ? C55A N5 Zn1 103.7(12) . . ? C54 N5 Zn1 111(3) . . ? C54A N5 Zn1 115.0(19) . . ? C55 N5 Zn1 103.6(17) . . ? C53A N5 Zn1 112.7(12) . . ? C53 N5 Zn1 106.4(18) . . ? C58A N6 C56 81(3) . . ? C58A N6 C57A 109.3(16) . . ? C56 N6 C57A 134(4) . . ? C58A N6 C57 127.2(18) . . ? C56 N6 C57 107(4) . . ? C57A N6 C57 31.2(13) . . ? C58A N6 C58 31.2(13) . . ? C56 N6 C58 110(3) . . ? C57A N6 C58 81.0(17) . . ? C57 N6 C58 106(2) . . ? C58A N6 C56A 106.8(19) . . ? C56 N6 C56A 29(3) . . ? C57A N6 C56A 110.8(17) . . ? C57 N6 C56A 80.4(18) . . ? C58 N6 C56A 131.2(19) . . ? C58A N6 Zn1 114.9(11) . . ? C56 N6 Zn1 105(3) . . ? C57A N6 Zn1 110.1(12) . . ? C57 N6 Zn1 113.1(14) . . ? C58 N6 Zn1 115.3(13) . . ? C56A N6 Zn1 104.7(10) . . ? C2 C1 N1 116.4(10) . . ? C1 C2 N2 117.0(11) . . ? C4 C3 N1 120.5(10) . . ? C4 C3 C8 121.4(10) . . ? N1 C3 C8 118.1(10) . . ? C3 C4 C5 117.0(11) . . ? C3 C4 C9 122.2(11) . . ? C5 C4 C9 120.8(11) . . ? C6 C5 C4 122.1(12) . . ? C5 C6 C7 121.4(12) . . ? C6 C7 C8 120.6(12) . . ? C7 C8 C3 117.5(11) . . ? C7 C8 C12 120.3(11) . . ? C3 C8 C12 122.2(11) . . ? C11 C9 C4 108.6(11) . . ? C11 C9 C10 115.9(11) . . ? C4 C9 C10 114.2(10) . . ? C8 C12 C14 114.0(12) . . ? C8 C12 C13 110.4(12) . . ? C14 C12 C13 110.3(12) . . ? N2 C15 C16 119.2(11) . . ? N2 C15 C20 121.7(10) . . ? C16 C15 C20 119.1(10) . . ? C17 C16 C15 120.1(12) . . ? C17 C16 C21 119.1(11) . . ? C15 C16 C21 120.8(11) . . ? C16 C17 C18 118.3(13) . . ? C19 C18 C17 120.5(13) . . ? C20 C19 C18 122.5(13) . . ? C19 C20 C15 119.4(11) . . ? C19 C20 C24 122.0(11) . . ? C15 C20 C24 118.5(10) . . ? C22 C21 C16 111.9(11) . . ? C22 C21 C23 112.1(12) . . ? C16 C21 C23 110.8(11) . . ? C20 C24 C25 111.6(10) . . ? C20 C24 C26 111.3(11) . . ? C25 C24 C26 111.9(11) . . ? C28 C27 N3 116.5(10) . . ? C27 C28 N4 115.9(11) . . ? C34 C29 C30 121.7(11) . . ? C34 C29 N3 120.4(9) . . ? C30 C29 N3 118.0(10) . . ? C31 C30 C29 116.4(10) . . ? C31 C30 C35 120.4(9) . . ? C29 C30 C35 123.0(10) . . ? C32 C31 C30 122.7(10) . . ? C31 C32 C33 119.6(11) . . ? C32 C33 C34 120.0(11) . . ? C29 C34 C33 119.5(10) . . ? C29 C34 C38 121.0(10) . . ? C33 C34 C38 119.5(10) . . ? C30 C35 C36 113.5(10) . . ? C30 C35 C37 109.7(10) . . ? C36 C35 C37 107.9(9) . . ? C39 C38 C40 109.5(12) . . ? C39 C38 C34 110.4(9) . . ? C40 C38 C34 111.0(10) . . ? C46 C41 N4 121.8(11) . . ? C46 C41 C42 118.6(11) . . ? N4 C41 C42 119.5(11) . . ? C43 C42 C41 119.9(14) . . ? C43 C42 C47 120.0(13) . . ? C41 C42 C47 119.7(12) . . ? C42 C43 C44 120.2(15) . . ? C45 C44 C43 118.4(14) . . ? C44 C45 C46 121.8(14) . . ? C45 C46 C41 120.6(12) . . ? C45 C46 C50 118.8(12) . . ? C41 C46 C50 120.5(11) . . ? C49 C47 C42 107.3(15) . . ? C49 C47 C48 114.5(13) . . ? C42 C47 C48 114.1(14) . . ? C52 C50 C51 111.3(14) . . ? C52 C50 C46 111.5(15) . . ? C51 C50 C46 114.7(12) . . ? N5 C55 C56 115(4) . . ? N6 C56 C55 113(3) . . ? O1 C59 C60 110(3) . . ? O1 C61 C62 106(2) . . ? N5 C55A C56A 116.8(18) . . ? N6 C56A C55A 111.6(19) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.131 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.128