data_global _journal_coden_Cambridge 222 #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Imre Toth' _publ_contact_author_address ; Department of Inorganic and Analytical Chemistry, University of Debrecen, H 4010 Debrecen, Pf. 21., Hungary ; _publ_contact_author_email 'imretoth@delfin.unideb.hu' _publ_contact_author_fax '+ 36 52 489667' _publ_contact_author_phone '+36 52 512900 x 22371' _publ_requested_journal 'Dalton Trans.' _publ_requested_category 'FM' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Equilibrium and Structure of the Al(III)-Ethylenediamine-N,N'-bis 3-hydroxy-2-propionate (EDBHP) Complex. A Multi-method study by Potentiometry, NMR, ESI MS and X-ray Diffraction. ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Joszai, Robert' 'Department of Inorganic and Analytical Chemistry, University of Debrecen' 'H 4010 Debrecen, Pf. 21., Hungary' 'Kerekes, Imola' 'Department of Inorganic and Analytical Chemistry, University of Debrecen' 'H 4010 Debrecen, Pf. 21., Hungary' 'Igarashi, Satoshi' 'Department of Chemistry, Faculty of Science, Niigata University' '8050 Ikarashi Nino-cho, Niigata 950-2181, Japan' 'Sawada, Kiyoshi' 'Department of Chemistry, Faculty of Science, Niigata University' '8050 Ikarashi Nino-cho, Niigata 950-2181, Japan' 'Zekany, Laszlo' 'Department of Inorganic and Analytical Chemistry, University of Debrecen' 'H 4010 Debrecen, Pf. 21., Hungary' 'Toth, Imre' 'Department of Inorganic and Analytical Chemistry, University of Debrecen' 'H 4010 Debrecen, Pf. 21., Hungary' _publ_section_synopsis ; ? ; #------------------------------------------------------------------------------ data_[Al2(OH)2(EDBHP)2].2H2O #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_name_common '[Al2(OH)2(EDDHPA)2].2(H2O)' _chemical_formula_sum 'C16 H34 Al2 N4 O16 ' _chemical_formula_moiety '(C16 H30 Al2 N4 O14), 2(H2 O)' _chemical_formula_weight 592.42 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.294(1) _cell_length_b 11.964(2) _cell_length_c 14.631(2) _cell_angle_alpha 73.594(7) _cell_angle_beta 88.023(7) _cell_angle_gamma 82.037(6) _cell_volume 1878.1(4) _cell_formula_units_Z 3 _cell_measurement_reflns_used 154 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 32.6 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936.00 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.987 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 296.2 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 19046 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_max 32.58 _diffrn_measured_fraction_theta_max 0.8260 _diffrn_reflns_theta_full 32.58 _diffrn_measured_fraction_theta_full 0.8260 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11289 _reflns_number_gt 6906 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2662 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 11289 _refine_ls_number_parameters 524 _refine_ls_goodness_of_fit_ref 1.608 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.09600(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_shift/su_max 0.0432 _refine_diff_density_max 1.29 _refine_diff_density_min -1.23 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.127(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Al' 'Al' 0.064 0.051 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al(1) Al -0.01500(9) 0.12291(9) -0.00613(7) 0.0294(2) Uani 1.00 d . . . Al(2) Al 0.50923(9) 0.39719(9) 0.07833(7) 0.0306(2) Uani 1.00 d . . . Al(3) Al 0.09767(10) 0.06751(10) 0.49607(7) 0.0348(3) Uani 1.00 d . . . O(1) O -0.0291(2) 0.1128(2) 0.1229(2) 0.0352(6) Uani 1.00 d . . . O(2) O -0.0034(2) 0.1993(3) 0.2354(2) 0.0424(7) Uani 1.00 d . . . O(3) O 0.1613(3) 0.4576(3) 0.0407(3) 0.0584(9) Uani 1.00 d . . . O(4) O -0.1494(2) 0.2432(2) -0.0328(2) 0.0326(6) Uani 1.00 d . . . O(5) O -0.2680(3) 0.3704(3) -0.1456(2) 0.0601(9) Uani 1.00 d . . . O(6) O -0.1043(3) 0.1220(3) -0.2942(2) 0.0506(8) Uani 1.00 d . . . O(7) O 0.1037(2) -0.0043(2) 0.0045(2) 0.0352(6) Uani 1.00 d . . . O(8) O 0.4140(2) 0.3085(2) 0.0316(2) 0.0386(6) Uani 1.00 d . . . O(9) O 0.3646(3) 0.1296(3) 0.0510(3) 0.0562(9) Uani 1.00 d . . . O(10) O 0.6508(3) 0.0546(3) 0.0177(3) 0.059(1) Uani 1.00 d . . . O(11) O 0.4350(2) 0.3587(2) 0.1976(2) 0.0363(6) Uani 1.00 d . . . O(12) O 0.4142(3) 0.3910(3) 0.3404(2) 0.0521(8) Uani 1.00 d . . . O(13) O 0.6497(3) 0.6454(3) 0.2383(3) 0.070(1) Uani 1.00 d . . . O(14) O 0.5844(2) 0.4616(2) -0.0348(2) 0.0370(6) Uani 1.00 d . . . O(15) O 0.0182(3) 0.1894(3) 0.5427(2) 0.0450(7) Uani 1.00 d . . . O(16) O 0.0423(4) 0.3572(3) 0.5684(3) 0.067(1) Uani 1.00 d . . . O(17) O 0.0175(4) 0.4301(4) 0.3162(3) 0.071(1) Uani 1.00 d . . . O(18) O 0.2288(3) 0.0538(3) 0.5766(2) 0.0430(7) Uani 1.00 d . . . O(19) O 0.4114(3) -0.0342(3) 0.6251(2) 0.0573(9) Uani 1.00 d . . . O(20a) O 0.374(1) -0.2429(9) 0.4399(7) 0.082(3) Uani 0.50 d P . . O(20b) O 0.287(1) -0.2797(8) 0.4862(8) 0.090(3) Uani 0.50 d P . . O(21) O -0.0285(2) 0.0545(2) 0.4223(2) 0.0398(6) Uani 1.00 d . . . O(22) O 0.8028(4) 0.5041(6) 0.3968(4) 0.104(2) Uani 1.00 d . . . O(23) O 0.4365(10) 0.1812(7) 0.6707(7) 0.190(4) Uani 1.00 d . . . O(24) O 0.590(2) 0.533(3) 0.508(1) 0.67(2) Uani 1.00 d . . . N(1) N 0.0981(3) 0.2417(3) -0.0027(2) 0.0335(7) Uani 1.00 d . . . N(2) N 0.0071(2) 0.1828(3) -0.1515(2) 0.0320(6) Uani 1.00 d . . . N(3) N 0.6207(3) 0.2419(3) 0.1108(2) 0.0356(7) Uani 1.00 d . . . N(4) N 0.6330(3) 0.4502(3) 0.1544(2) 0.0350(7) Uani 1.00 d . . . N(5) N 0.1541(3) 0.2071(3) 0.3972(2) 0.0355(7) Uani 1.00 d . . . N(6) N 0.2245(3) -0.0270(3) 0.4292(2) 0.0392(8) Uani 1.00 d . . . C(1) C 0.1073(4) 0.3224(4) -0.0986(3) 0.0439(10) Uani 1.00 d . . . C(2) C 0.1115(3) 0.2486(4) -0.1682(3) 0.0402(9) Uani 1.00 d . . . C(3) C 0.0052(3) 0.1944(3) 0.1527(2) 0.0310(7) Uani 1.00 d . . . C(4) C 0.0521(3) 0.2941(3) 0.0741(2) 0.0323(7) Uani 1.00 d . . . C(5) C 0.1378(4) 0.3565(4) 0.1122(3) 0.0432(10) Uani 1.00 d . . . C(6) C -0.1803(3) 0.2950(3) -0.1194(2) 0.0355(8) Uani 1.00 d . . . C(7) C -0.1043(3) 0.2562(3) -0.1954(2) 0.0375(8) Uani 1.00 d . . . C(8) C -0.1777(4) 0.1874(4) -0.2411(3) 0.046(1) Uani 1.00 d . . . C(9) C 0.6999(3) 0.2383(3) 0.1909(3) 0.0390(9) Uani 1.00 d . . . C(10) C 0.7395(3) 0.3594(4) 0.1696(3) 0.0412(9) Uani 1.00 d . . . C(11) C 0.4320(3) 0.1962(3) 0.0647(3) 0.0396(9) Uani 1.00 d . . . C(12) C 0.5446(3) 0.1470(3) 0.1280(3) 0.0391(9) Uani 1.00 d . . . C(13) C 0.6077(4) 0.0339(4) 0.1122(4) 0.053(1) Uani 1.00 d . . . C(14) C 0.4655(3) 0.4017(3) 0.2643(2) 0.0351(8) Uani 1.00 d . . . C(15) C 0.5753(3) 0.4653(3) 0.2441(3) 0.0379(9) Uani 1.00 d . . . C(16) C 0.5433(4) 0.5937(4) 0.2405(3) 0.050(1) Uani 1.00 d . . . C(17) C 0.2697(4) 0.1719(4) 0.3557(3) 0.0427(9) Uani 1.00 d . . . C(18) C 0.2600(4) 0.0537(4) 0.3392(3) 0.0424(9) Uani 1.00 d . . . C(19) C 0.0644(4) 0.2860(4) 0.5236(3) 0.0441(10) Uani 1.00 d . . . C(20) C 0.1531(4) 0.3046(4) 0.4404(3) 0.0415(9) Uani 1.00 d . . . C(21) C 0.1229(5) 0.4259(4) 0.3679(3) 0.051(1) Uani 1.00 d . . . C(22) C 0.3249(4) -0.0180(4) 0.5726(3) 0.0444(10) Uani 1.00 d . . . C(23) C 0.3261(5) -0.0786(5) 0.4954(3) 0.057(1) Uani 1.00 d . . . C(24) C 0.327(1) -0.2101(5) 0.5362(6) 0.145(4) Uani 1.00 d . . . H(1) H 0.2044 -0.0247 0.0037 0.0585 Uiso 1.00 calc . . . H(2) H 0.1768 0.1994 0.0158 0.0368 Uiso 1.00 calc . . . H(3) H 0.1772 0.3603 -0.1030 0.0486 Uiso 1.00 calc . . . H(4) H 0.0387 0.3808 -0.1107 0.0486 Uiso 1.00 calc . . . H(5) H 0.1844 0.1922 -0.1570 0.0460 Uiso 1.00 calc . . . H(6) H 0.1127 0.2958 -0.2316 0.0460 Uiso 1.00 calc . . . H(7) H 0.0222 0.1164 -0.1771 0.0355 Uiso 1.00 calc . . . H(8) H -0.0153 0.3513 0.0479 0.0374 Uiso 1.00 calc . . . H(9) H 0.2107 0.3045 0.1314 0.0467 Uiso 1.00 calc . . . H(10) H 0.1040 0.3783 0.1664 0.0467 Uiso 1.00 calc . . . H(11) H 0.2162 0.4975 0.0823 0.0585 Uiso 1.00 calc . . . H(12) H -0.0840 0.3229 -0.2432 0.0418 Uiso 1.00 calc . . . H(13) H -0.2133 0.1327 -0.1911 0.0513 Uiso 1.00 calc . . . H(14) H -0.2357 0.2395 -0.2806 0.0513 Uiso 1.00 calc . . . H(15) H -0.0568 0.1734 -0.3538 0.0585 Uiso 1.00 calc . . . H(16) H 0.6251 0.4169 -0.0656 0.0585 Uiso 1.00 calc . . . H(17) H 0.6700 0.2388 0.0569 0.0381 Uiso 1.00 calc . . . H(18) H 0.7694 0.1797 0.1938 0.0447 Uiso 1.00 calc . . . H(19) H 0.6595 0.2190 0.2495 0.0447 Uiso 1.00 calc . . . H(20) H 0.7873 0.3734 0.1141 0.0461 Uiso 1.00 calc . . . H(21) H 0.7844 0.3638 0.2221 0.0461 Uiso 1.00 calc . . . H(22) H 0.6545 0.5240 0.1176 0.0377 Uiso 1.00 calc . . . H(23) H 0.5191 0.1300 0.1926 0.0431 Uiso 1.00 calc . . . H(24) H 0.6745 0.0057 0.1561 0.0579 Uiso 1.00 calc . . . H(25) H 0.5551 -0.0237 0.1254 0.0579 Uiso 1.00 calc . . . H(26) H 0.6129 -0.0095 -0.0160 0.0585 Uiso 1.00 calc . . . H(27) H 0.6312 0.4306 0.2945 0.0412 Uiso 1.00 calc . . . H(28) H 0.4961 0.6347 0.1841 0.0568 Uiso 1.00 calc . . . H(29) H 0.4961 0.6015 0.2945 0.0568 Uiso 1.00 calc . . . H(30) H 0.6078 0.7196 0.2555 0.0585 Uiso 1.00 calc . . . H(31) H -0.0345 0.0821 0.3482 0.0585 Uiso 1.00 calc . . . H(32) H 0.0967 0.2328 0.3474 0.0360 Uiso 1.00 calc . . . H(33) H 0.2855 0.2273 0.2983 0.0459 Uiso 1.00 calc . . . H(34) H 0.3342 0.1616 0.3997 0.0459 Uiso 1.00 calc . . . H(35) H 0.1986 0.0662 0.2913 0.0480 Uiso 1.00 calc . . . H(36) H 0.3327 0.0235 0.3166 0.0480 Uiso 1.00 calc . . . H(37) H 0.1900 -0.0900 0.4157 0.0421 Uiso 1.00 calc . . . H(38) H 0.2302 0.2990 0.4668 0.0453 Uiso 1.00 calc . . . H(39) H 0.1155 0.4861 0.4000 0.0585 Uiso 1.00 calc . . . H(40) H 0.1889 0.4394 0.3237 0.0585 Uiso 1.00 calc . . . H(41) H -0.0624 0.4721 0.3506 0.0585 Uiso 1.00 calc . . . H(42) H 0.3999 -0.0645 0.4592 0.0654 Uiso 1.00 calc . . . H(43a) H 0.2557 -0.2325 0.5554 0.1692 Uiso 0.50 calc P . . H(43b) H 0.2892 -0.2224 0.5929 0.1692 Uiso 0.50 calc P . . H(44a) H 0.3881 -0.2416 0.5847 0.1692 Uiso 0.50 calc P . . H(44b) H 0.4137 -0.2393 0.5467 0.1692 Uiso 0.50 calc P . . H(45a) H 0.3953 -0.3269 0.4718 0.0882 Uiso 0.50 calc P . . H(45b) H 0.3421 -0.2895 0.4243 0.1030 Uiso 0.50 calc P . . H(46) H 0.7275 0.5055 0.4409 0.0649 Uiso 1.00 calc . . . H(47) H 0.7878 0.5209 0.3295 0.0649 Uiso 1.00 calc . . . H(48) H 0.3632 0.2236 0.6978 0.1399 Uiso 1.00 calc . . . H(49) H 0.4579 0.0952 0.6963 0.1399 Uiso 1.00 calc . . . H(50) H 0.6204 0.5050 0.5858 0.3985 Uiso 1.00 calc . . . H(51) H 0.5636 0.4572 0.5297 0.3985 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al(1) 0.0305(4) 0.0316(5) 0.0291(4) -0.0073(4) 0.0020(3) -0.0119(3) Al(2) 0.0312(5) 0.0314(5) 0.0310(5) -0.0046(4) 0.0019(3) -0.0114(3) Al(3) 0.0388(5) 0.0377(5) 0.0286(5) -0.0102(5) -0.0010(4) -0.0081(4) O(1) 0.042(1) 0.036(1) 0.029(1) -0.008(1) 0.0018(9) -0.0088(8) O(2) 0.046(1) 0.056(2) 0.028(1) -0.010(1) -0.0012(10) -0.015(1) O(3) 0.061(2) 0.049(2) 0.068(2) -0.021(2) -0.007(2) -0.013(1) O(4) 0.037(1) 0.035(1) 0.028(1) -0.004(1) 0.0031(8) -0.0132(8) O(5) 0.057(2) 0.075(2) 0.043(2) 0.034(2) -0.007(1) -0.025(1) O(6) 0.061(2) 0.060(2) 0.041(1) -0.012(2) 0.007(1) -0.029(1) O(7) 0.030(1) 0.035(1) 0.044(1) -0.009(1) 0.0017(9) -0.0152(10) O(8) 0.037(1) 0.039(1) 0.044(1) -0.006(1) -0.0048(10) -0.018(1) O(9) 0.043(2) 0.050(2) 0.089(2) -0.013(1) -0.002(1) -0.038(2) O(10) 0.046(2) 0.057(2) 0.093(3) -0.016(2) 0.019(2) -0.048(2) O(11) 0.037(1) 0.043(1) 0.033(1) -0.015(1) 0.0046(9) -0.0122(9) O(12) 0.058(2) 0.067(2) 0.038(1) -0.023(2) 0.014(1) -0.020(1) O(13) 0.058(2) 0.069(2) 0.106(3) -0.033(2) 0.025(2) -0.052(2) O(14) 0.040(1) 0.038(1) 0.035(1) -0.005(1) 0.0085(9) -0.0146(9) O(15) 0.048(2) 0.042(1) 0.044(1) -0.003(1) 0.011(1) -0.014(1) O(16) 0.092(3) 0.056(2) 0.060(2) -0.003(2) 0.015(2) -0.032(2) O(17) 0.074(2) 0.075(2) 0.056(2) 0.009(2) -0.011(2) -0.010(2) O(18) 0.046(1) 0.052(2) 0.035(1) -0.010(1) -0.005(1) -0.016(1) O(19) 0.053(2) 0.069(2) 0.049(2) -0.006(2) -0.018(1) -0.014(1) O(20a) 0.103(7) 0.078(6) 0.074(5) 0.008(6) -0.009(5) -0.042(4) O(20b) 0.118(8) 0.070(5) 0.088(7) 0.014(6) -0.028(6) -0.040(5) O(21) 0.042(1) 0.046(1) 0.029(1) -0.016(1) -0.0053(9) -0.0024(9) O(22) 0.080(3) 0.162(5) 0.090(3) -0.031(3) 0.008(3) -0.060(4) O(23) 0.29(1) 0.145(6) 0.200(8) -0.111(7) 0.111(8) -0.124(6) O(24) 0.68(4) 1.42(7) 0.30(2) -0.87(5) 0.36(2) -0.58(3) N(1) 0.035(1) 0.040(1) 0.030(1) -0.013(1) 0.0046(10) -0.014(1) N(2) 0.034(1) 0.035(1) 0.029(1) -0.005(1) 0.0014(10) -0.0133(10) N(3) 0.037(1) 0.038(1) 0.035(1) -0.010(1) 0.003(1) -0.012(1) N(4) 0.036(1) 0.034(1) 0.037(1) -0.008(1) 0.004(1) -0.013(1) N(5) 0.039(1) 0.038(1) 0.031(1) -0.007(1) 0.001(1) -0.010(1) N(6) 0.045(2) 0.039(2) 0.036(1) -0.003(1) -0.008(1) -0.014(1) C(1) 0.050(2) 0.049(2) 0.036(2) -0.024(2) 0.006(1) -0.010(1) C(2) 0.037(2) 0.052(2) 0.033(2) -0.010(2) 0.007(1) -0.013(1) C(3) 0.031(1) 0.035(2) 0.029(1) -0.002(1) -0.002(1) -0.011(1) C(4) 0.033(1) 0.032(1) 0.034(1) -0.003(1) -0.001(1) -0.011(1) C(5) 0.044(2) 0.050(2) 0.043(2) -0.013(2) 0.001(1) -0.020(2) C(6) 0.037(2) 0.036(2) 0.034(2) 0.006(2) -0.005(1) -0.014(1) C(7) 0.042(2) 0.042(2) 0.029(1) -0.005(2) 0.002(1) -0.013(1) C(8) 0.041(2) 0.064(3) 0.040(2) -0.006(2) -0.002(1) -0.027(2) C(9) 0.033(2) 0.042(2) 0.042(2) -0.006(2) -0.003(1) -0.012(1) C(10) 0.031(2) 0.049(2) 0.047(2) -0.008(2) 0.002(1) -0.019(2) C(11) 0.043(2) 0.037(2) 0.048(2) -0.011(2) 0.005(1) -0.025(1) C(12) 0.042(2) 0.034(2) 0.045(2) -0.009(2) 0.004(1) -0.015(1) C(13) 0.051(2) 0.034(2) 0.078(3) -0.009(2) -0.001(2) -0.018(2) C(14) 0.036(2) 0.037(2) 0.033(2) -0.007(1) 0.004(1) -0.012(1) C(15) 0.037(2) 0.044(2) 0.037(2) -0.008(2) 0.001(1) -0.018(1) C(16) 0.048(2) 0.053(2) 0.063(3) -0.019(2) 0.012(2) -0.033(2) C(17) 0.043(2) 0.048(2) 0.040(2) -0.014(2) 0.007(1) -0.015(1) C(18) 0.044(2) 0.048(2) 0.037(2) -0.005(2) 0.001(1) -0.015(1) C(19) 0.049(2) 0.041(2) 0.042(2) 0.003(2) -0.001(2) -0.015(1) C(20) 0.045(2) 0.041(2) 0.041(2) -0.009(2) -0.002(1) -0.014(1) C(21) 0.063(3) 0.031(2) 0.055(2) 0.004(2) 0.002(2) -0.011(2) C(22) 0.048(2) 0.050(2) 0.035(2) -0.016(2) -0.007(1) -0.006(1) C(23) 0.060(3) 0.064(3) 0.048(2) 0.017(2) -0.018(2) -0.025(2) C(24) 0.26(1) 0.050(3) 0.116(6) 0.062(6) -0.130(8) -0.042(4) #------------------------------------------------------------------------------ _computing_data_collection 'RAPID-AUTO ver.1.06' _computing_cell_refinement 'RAPID-AUTO ver.1.06' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics 'teXsan Ver. 1.11' #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al(1) O(1) 1.860(2) . . yes Al(1) O(4) 1.909(3) . . yes Al(1) O(7) 1.858(3) . . yes Al(1) O(7) 1.842(2) . 2_555 yes Al(1) N(1) 2.050(3) . . yes Al(1) N(2) 2.062(3) . . yes Al(2) O(8) 1.878(3) . . yes Al(2) O(11) 1.874(3) . . yes Al(2) O(14) 1.849(3) . . yes Al(2) O(14) 1.822(3) . 2_665 yes Al(2) N(3) 2.039(3) . . yes Al(2) N(4) 2.085(3) . . yes Al(3) O(15) 1.885(3) . . yes Al(3) O(18) 1.884(3) . . yes Al(3) O(21) 1.866(3) . . yes Al(3) O(21) 1.853(3) . 2_556 yes Al(3) N(5) 2.038(3) . . yes Al(3) N(6) 2.090(4) . . yes O(1) C(3) 1.285(4) . . yes O(2) C(3) 1.228(4) . . yes O(3) C(5) 1.408(5) . . yes O(3) H(11) 1.120 . . no O(4) C(6) 1.281(4) . . yes O(5) C(6) 1.235(5) . . yes O(6) C(8) 1.422(5) . . yes O(6) H(15) 1.088 . . no O(7) H(1) 1.129 . . no O(8) C(11) 1.282(4) . . yes O(9) C(11) 1.234(4) . . yes O(10) C(13) 1.417(6) . . yes O(10) H(26) 1.155 . . no O(11) C(14) 1.299(4) . . yes O(12) C(14) 1.220(4) . . yes O(13) C(16) 1.422(5) . . yes O(13) H(30) 1.038 . . no O(14) H(16) 0.870 . . no O(15) C(19) 1.289(5) . . yes O(16) C(19) 1.210(5) . . yes O(17) C(21) 1.419(6) . . yes O(17) H(41) 1.143 . . no O(18) C(22) 1.298(5) . . yes O(19) C(22) 1.223(5) . . yes O(20a) C(24) 1.62(1) . . yes O(20a) H(45a) 0.980 . . no O(20b) C(24) 1.38(1) . . yes O(20b) H(45b) 1.103 . . no O(21) H(31) 1.042 . . no O(22) H(46) 1.051 . . no O(22) H(47) 0.964 . . no O(23) H(48) 1.037 . . no O(23) H(49) 0.988 . . no O(24) H(50) 1.138 . . no O(24) H(51) 0.957 . . no N(1) C(1) 1.472(5) . . yes N(1) C(4) 1.480(4) . . yes N(1) H(2) 0.966 . . no N(2) C(2) 1.483(4) . . yes N(2) C(7) 1.482(5) . . yes N(2) H(7) 0.961 . . no N(3) C(9) 1.485(4) . . yes N(3) C(12) 1.479(4) . . yes N(3) H(17) 0.956 . . no N(4) C(10) 1.482(5) . . yes N(4) C(15) 1.490(4) . . yes N(4) H(22) 0.954 . . no N(5) C(17) 1.479(5) . . yes N(5) C(20) 1.475(5) . . yes N(5) H(32) 0.947 . . no N(6) C(18) 1.476(5) . . yes N(6) C(23) 1.476(5) . . yes N(6) H(37) 0.964 . . no C(1) C(2) 1.520(5) . . yes C(1) H(3) 0.954 . . no C(1) H(4) 0.954 . . no C(2) H(5) 0.977 . . no C(2) H(6) 0.941 . . no C(3) C(4) 1.544(4) . . yes C(4) C(5) 1.508(5) . . yes C(4) H(8) 0.960 . . no C(5) H(9) 0.958 . . no C(5) H(10) 0.954 . . no C(6) C(7) 1.518(5) . . yes C(7) C(8) 1.533(5) . . yes C(7) H(12) 0.950 . . no C(8) H(13) 0.953 . . no C(8) H(14) 0.928 . . no C(9) C(10) 1.521(6) . . yes C(9) H(18) 0.970 . . no C(9) H(19) 0.942 . . no C(10) H(20) 0.947 . . no C(10) H(21) 0.951 . . no C(11) C(12) 1.545(6) . . yes C(12) C(13) 1.513(6) . . yes C(12) H(23) 0.952 . . no C(13) H(24) 0.967 . . no C(13) H(25) 0.946 . . no C(14) C(15) 1.521(5) . . yes C(15) C(16) 1.515(6) . . yes C(15) H(27) 0.950 . . no C(16) H(28) 0.966 . . no C(16) H(29) 0.957 . . no C(17) C(18) 1.519(6) . . yes C(17) H(33) 0.941 . . no C(17) H(34) 0.961 . . no C(18) H(35) 0.969 . . no C(18) H(36) 0.938 . . no C(19) C(20) 1.536(6) . . yes C(20) C(21) 1.538(6) . . yes C(20) H(38) 0.951 . . no C(21) H(39) 0.959 . . no C(21) H(40) 0.970 . . no C(22) C(23) 1.503(6) . . yes C(23) C(24) 1.516(9) . . yes C(23) H(42) 0.981 . . no C(24) H(43a) 0.893 . . no C(24) H(44a) 0.968 . . no C(24) H(43b) 0.902 . . no C(24) H(44b) 0.997 . . no Al(1) Al(1) 2.868(2) . 2_555 yes Al(2) Al(2) 2.838(2) . 2_665 yes Al(3) Al(3) 2.890(2) . 2_556 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Al(1) O(4) 89.9(1) . . . yes O(1) Al(1) O(7) 97.6(1) . . . yes O(1) Al(1) O(7) 96.7(1) . . 2_555 yes O(1) Al(1) N(1) 82.4(1) . . . yes O(1) Al(1) N(2) 163.6(1) . . . yes O(4) Al(1) O(7) 170.0(1) . . . yes O(4) Al(1) O(7) 94.1(1) . . 2_555 yes O(4) Al(1) N(1) 91.7(1) . . . yes O(4) Al(1) N(2) 82.0(1) . . . yes O(7) Al(1) O(7) 78.4(1) . . 2_555 yes O(7) Al(1) N(1) 96.0(1) . . . yes O(7) Al(1) N(2) 92.3(1) . . . yes O(7) Al(1) N(1) 174.1(1) 2_555 . . yes O(7) Al(1) N(2) 98.1(1) 2_555 . . yes N(1) Al(1) N(2) 83.7(1) . . . yes O(8) Al(2) O(11) 91.5(1) . . . yes O(8) Al(2) O(14) 97.5(1) . . . yes O(8) Al(2) O(14) 96.7(1) . . 2_665 yes O(8) Al(2) N(3) 81.7(1) . . . yes O(8) Al(2) N(4) 164.2(1) . . . yes O(11) Al(2) O(14) 169.3(1) . . . yes O(11) Al(2) O(14) 94.4(1) . . 2_665 yes O(11) Al(2) N(3) 92.3(1) . . . yes O(11) Al(2) N(4) 82.1(1) . . . yes O(14) Al(2) O(14) 78.7(1) . . 2_665 yes O(14) Al(2) N(3) 94.9(1) . . . yes O(14) Al(2) N(4) 90.7(1) . . . yes O(14) Al(2) N(3) 173.2(1) 2_665 . . yes O(14) Al(2) N(4) 98.1(1) 2_665 . . yes N(3) Al(2) N(4) 84.1(1) . . . yes O(15) Al(3) O(18) 89.9(1) . . . yes O(15) Al(3) O(21) 97.0(1) . . . yes O(15) Al(3) O(21) 97.1(1) . . 2_556 yes O(15) Al(3) N(5) 81.3(1) . . . yes O(15) Al(3) N(6) 161.2(1) . . . yes O(18) Al(3) O(21) 170.7(1) . . . yes O(18) Al(3) O(21) 95.0(1) . . 2_556 yes O(18) Al(3) N(5) 92.0(1) . . . yes O(18) Al(3) N(6) 81.7(1) . . . yes O(21) Al(3) O(21) 78.0(1) . . 2_556 yes O(21) Al(3) N(5) 95.2(1) . . . yes O(21) Al(3) N(6) 93.4(1) . . . yes O(21) Al(3) N(5) 172.9(1) 2_556 . . yes O(21) Al(3) N(6) 100.4(1) 2_556 . . yes N(5) Al(3) N(6) 82.2(1) . . . yes Al(1) O(1) C(3) 118.6(2) . . . yes C(5) O(3) H(11) 100.1 . . . no Al(1) O(4) C(6) 119.5(2) . . . yes C(8) O(6) H(15) 115.7 . . . no Al(1) O(7) Al(1) 101.6(1) . . 2_555 yes Al(1) O(7) H(1) 140.1 . . . no Al(1) O(7) H(1) 118.0 2_555 . . no Al(2) O(8) C(11) 118.2(2) . . . yes C(13) O(10) H(26) 107.6 . . . no Al(2) O(11) C(14) 119.9(2) . . . yes C(16) O(13) H(30) 94.9 . . . no Al(2) O(14) Al(2) 101.3(1) . . 2_665 yes Al(2) O(14) H(16) 120.8 . . . no Al(2) O(14) H(16) 130.5 2_665 . . no Al(3) O(15) C(19) 117.4(3) . . . yes C(21) O(17) H(41) 109.1 . . . no Al(3) O(18) C(22) 120.4(2) . . . yes C(24) O(20a) H(45a) 94.5 . . . no C(24) O(20b) H(45b) 115.7 . . . no Al(3) O(21) Al(3) 102.0(1) . . 2_556 yes Al(3) O(21) H(31) 126.4 . . . no Al(3) O(21) H(31) 127.0 2_556 . . no H(46) O(22) H(47) 116.7 . . . no H(48) O(23) H(49) 119.7 . . . no H(50) O(24) H(51) 79.5 . . . no Al(1) N(1) C(1) 109.6(2) . . . yes Al(1) N(1) C(4) 105.3(2) . . . yes Al(1) N(1) H(2) 108.6 . . . no C(1) N(1) C(4) 117.3(3) . . . yes C(1) N(1) H(2) 107.7 . . . no C(4) N(1) H(2) 108.1 . . . no Al(1) N(2) C(2) 107.3(2) . . . yes Al(1) N(2) C(7) 109.4(2) . . . yes Al(1) N(2) H(7) 108.9 . . . no C(2) N(2) C(7) 112.7(3) . . . yes C(2) N(2) H(7) 110.0 . . . no C(7) N(2) H(7) 108.4 . . . no Al(2) N(3) C(9) 108.7(2) . . . yes Al(2) N(3) C(12) 107.0(2) . . . yes Al(2) N(3) H(17) 108.8 . . . no C(9) N(3) C(12) 116.1(3) . . . yes C(9) N(3) H(17) 108.0 . . . no C(12) N(3) H(17) 108.1 . . . no Al(2) N(4) C(10) 106.8(2) . . . yes Al(2) N(4) C(15) 108.2(2) . . . yes Al(2) N(4) H(22) 109.3 . . . no C(10) N(4) C(15) 114.1(3) . . . yes C(10) N(4) H(22) 109.7 . . . no C(15) N(4) H(22) 108.7 . . . no Al(3) N(5) C(17) 111.0(2) . . . yes Al(3) N(5) C(20) 108.7(2) . . . yes Al(3) N(5) H(32) 107.5 . . . no C(17) N(5) C(20) 115.1(3) . . . yes C(17) N(5) H(32) 107.7 . . . no C(20) N(5) H(32) 106.6 . . . no Al(3) N(6) C(18) 108.4(2) . . . yes Al(3) N(6) C(23) 108.1(2) . . . yes Al(3) N(6) H(37) 109.5 . . . no C(18) N(6) C(23) 112.6(3) . . . yes C(18) N(6) H(37) 109.5 . . . no C(23) N(6) H(37) 108.6 . . . no N(1) C(1) C(2) 106.7(3) . . . yes N(1) C(1) H(3) 110.3 . . . no N(1) C(1) H(4) 109.2 . . . no C(2) C(1) H(3) 111.6 . . . no C(2) C(1) H(4) 110.3 . . . no H(3) C(1) H(4) 108.8 . . . no N(2) C(2) C(1) 109.1(3) . . . yes N(2) C(2) H(5) 108.6 . . . no N(2) C(2) H(6) 110.9 . . . no C(1) C(2) H(5) 109.1 . . . no C(1) C(2) H(6) 111.1 . . . no H(5) C(2) H(6) 107.9 . . . no O(1) C(3) O(2) 124.5(3) . . . yes O(1) C(3) C(4) 114.6(3) . . . yes O(2) C(3) C(4) 120.8(3) . . . yes N(1) C(4) C(3) 106.3(3) . . . yes N(1) C(4) C(5) 116.2(3) . . . yes N(1) C(4) H(8) 106.5 . . . no C(3) C(4) C(5) 112.6(3) . . . yes C(3) C(4) H(8) 107.6 . . . no C(5) C(4) H(8) 107.2 . . . no O(3) C(5) C(4) 109.4(3) . . . yes O(3) C(5) H(9) 109.9 . . . no O(3) C(5) H(10) 109.8 . . . no C(4) C(5) H(9) 109.3 . . . no C(4) C(5) H(10) 109.9 . . . no H(9) C(5) H(10) 108.5 . . . no O(4) C(6) O(5) 125.5(3) . . . yes O(4) C(6) C(7) 116.5(3) . . . yes O(5) C(6) C(7) 118.0(3) . . . yes N(2) C(7) C(6) 109.5(3) . . . yes N(2) C(7) C(8) 111.2(3) . . . yes N(2) C(7) H(12) 109.0 . . . no C(6) C(7) C(8) 108.2(3) . . . yes C(6) C(7) H(12) 110.0 . . . no C(8) C(7) H(12) 108.9 . . . no O(6) C(8) C(7) 111.6(3) . . . yes O(6) C(8) H(13) 107.5 . . . no O(6) C(8) H(14) 109.9 . . . no C(7) C(8) H(13) 107.7 . . . no C(7) C(8) H(14) 109.2 . . . no H(13) C(8) H(14) 110.9 . . . no N(3) C(9) C(10) 106.5(3) . . . yes N(3) C(9) H(18) 110.0 . . . no N(3) C(9) H(19) 111.1 . . . no C(10) C(9) H(18) 109.5 . . . no C(10) C(9) H(19) 111.3 . . . no H(18) C(9) H(19) 108.5 . . . no N(4) C(10) C(9) 109.6(3) . . . yes N(4) C(10) H(20) 109.3 . . . no N(4) C(10) H(21) 109.0 . . . no C(9) C(10) H(20) 109.9 . . . no C(9) C(10) H(21) 109.6 . . . no H(20) C(10) H(21) 109.5 . . . no O(8) C(11) O(9) 124.3(4) . . . yes O(8) C(11) C(12) 115.1(3) . . . yes O(9) C(11) C(12) 120.6(3) . . . yes N(3) C(12) C(11) 107.3(3) . . . yes N(3) C(12) C(13) 113.9(3) . . . yes N(3) C(12) H(23) 108.0 . . . no C(11) C(12) C(13) 112.4(3) . . . yes C(11) C(12) H(23) 107.4 . . . no C(13) C(12) H(23) 107.6 . . . no O(10) C(13) C(12) 110.1(4) . . . yes O(10) C(13) H(24) 109.1 . . . no O(10) C(13) H(25) 110.9 . . . no C(12) C(13) H(24) 108.2 . . . no C(12) C(13) H(25) 110.0 . . . no H(24) C(13) H(25) 108.4 . . . no O(11) C(14) O(12) 124.4(3) . . . yes O(11) C(14) C(15) 115.7(3) . . . yes O(12) C(14) C(15) 119.8(3) . . . yes N(4) C(15) C(14) 109.8(3) . . . yes N(4) C(15) C(16) 112.1(3) . . . yes N(4) C(15) H(27) 107.7 . . . no C(14) C(15) C(16) 111.0(3) . . . yes C(14) C(15) H(27) 108.6 . . . no C(16) C(15) H(27) 107.5 . . . no O(13) C(16) C(15) 109.5(3) . . . yes O(13) C(16) H(28) 109.4 . . . no O(13) C(16) H(29) 110.0 . . . no C(15) C(16) H(28) 109.9 . . . no C(15) C(16) H(29) 110.6 . . . no H(28) C(16) H(29) 107.4 . . . no N(5) C(17) C(18) 105.8(3) . . . yes N(5) C(17) H(33) 111.8 . . . no N(5) C(17) H(34) 110.8 . . . no C(18) C(17) H(33) 110.8 . . . no C(18) C(17) H(34) 108.4 . . . no H(33) C(17) H(34) 109.1 . . . no N(6) C(18) C(17) 108.8(3) . . . yes N(6) C(18) H(35) 109.6 . . . no N(6) C(18) H(36) 111.5 . . . no C(17) C(18) H(35) 107.6 . . . no C(17) C(18) H(36) 110.4 . . . no H(35) C(18) H(36) 108.9 . . . no O(15) C(19) O(16) 123.2(4) . . . yes O(15) C(19) C(20) 115.4(3) . . . yes O(16) C(19) C(20) 121.3(4) . . . yes N(5) C(20) C(19) 108.0(3) . . . yes N(5) C(20) C(21) 112.6(3) . . . yes N(5) C(20) H(38) 107.9 . . . no C(19) C(20) C(21) 111.8(3) . . . yes C(19) C(20) H(38) 107.0 . . . no C(21) C(20) H(38) 109.3 . . . no O(17) C(21) C(20) 110.6(4) . . . yes O(17) C(21) H(39) 111.7 . . . no O(17) C(21) H(40) 109.0 . . . no C(20) C(21) H(39) 109.7 . . . no C(20) C(21) H(40) 108.6 . . . no H(39) C(21) H(40) 107.1 . . . no O(18) C(22) O(19) 123.7(4) . . . yes O(18) C(22) C(23) 115.3(3) . . . yes O(19) C(22) C(23) 120.9(4) . . . yes N(6) C(23) C(22) 111.0(4) . . . yes N(6) C(23) C(24) 110.8(5) . . . yes N(6) C(23) H(42) 107.6 . . . no C(22) C(23) C(24) 111.7(4) . . . yes C(22) C(23) H(42) 106.9 . . . no C(24) C(23) H(42) 108.6 . . . no O(20a) C(24) C(23) 95.5(7) . . . yes O(20a) C(24) H(43a) 113.5 . . . no O(20a) C(24) H(44a) 108.5 . . . no C(23) C(24) H(43a) 115.0 . . . no C(23) C(24) H(44a) 110.2 . . . no H(43a) C(24) H(44a) 112.8 . . . no O(20b) C(24) C(23) 123.2(6) . . . yes O(20b) C(24) H(43b) 108.9 . . . no O(20b) C(24) H(44b) 104.3 . . . no C(23) C(24) H(43b) 107.6 . . . no C(23) C(24) H(44b) 102.6 . . . no H(43b) C(24) H(44b) 109.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Al(1) Al(1) 2.868(2) . 2_555 ? Al(2) Al(2) 2.838(2) . 2_665 ? Al(3) Al(3) 2.890(2) . 2_556 ? #------------------------------------------------------------------------------ # END of CIF #------------------------------------------------------------------------------