#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/02/2010253.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2010253 loop_ _publ_author_name 'Hoveyda, H. R.' 'Orvig, Chris' 'Rettig, Steven J.' _publ_contact_author ; Dr. Steven J. Rettig Department of Chemistry University of British Columbia 2036 Main Mall Vancouver, B.C. Canada V6T 1Z1 ; _publ_section_title ; mer-Tris[2-(5-bromo-2-hydroxyphenyl)-2-oxazolinato]aluminium(III) methanol solvate ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1906 _journal_page_last 1909 _journal_paper_doi 10.1107/S0108270194007729 _journal_volume 50 _journal_year 1994 _chemical_formula_moiety 'C27 H21 Al Br3 N3 O6, C H4 O' _chemical_formula_structural '(Al (C9 H7 Br N O2)3) (C H4 O)' _chemical_formula_sum 'C28 H25 Al Br3 N3 O7' _chemical_formula_weight 782.21 _chemical_name_systematic ; Tris[2-(5'-bromo-2'-hydroxyphenyl)-2-oxazolinato]aluminum(III) methanol solvate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 106.387(8) _cell_angle_beta 106.950(10) _cell_angle_gamma 75.253(6) _cell_formula_units_Z 2 _cell_length_a 11.9780(10) _cell_length_b 13.2165(8) _cell_length_c 10.375(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294.0 _cell_measurement_theta_max 113.9 _cell_measurement_theta_min 109.6 _cell_volume 1480.5(3) _computing_cell_refinement ' MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1985) ; _computing_data_reduction ' TEXSAN (Molecular Structure Corporation, 1992)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _diffrn_ambient_temperature 294.2 _diffrn_measurement_device AFC-6S _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 2.21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6400 _diffrn_reflns_theta_max 77.50 _diffrn_reflns_theta_min 3.5 _diffrn_standards_decay_% none _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.787 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_type ' empirical based on \y scans for 3 reflections' _exptl_absorpt_process_details psi-scan _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.755 _exptl_crystal_description plate _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.66 _refine_diff_density_min -0.78 _refine_ls_extinction_coef 4.0E-6(3) _refine_ls_extinction_method 'Zachariasen type 2, Gaussian isotropic' _refine_ls_goodness_of_fit_obs 3.460 _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 384 _refine_ls_number_reflns 5266 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0390 _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_obs 0.0560 _reflns_number_observed 5266 _reflns_number_total 6400 _reflns_observed_criterion I>=3\s(I) _cod_data_source_file bk1052.cif _cod_data_source_block AlBroz3 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 67 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_cell_volume 1480.4(3) _cod_database_code 2010253 loop_ _symmetry_equiv_pos_as_xyz '+x, +y, +z' '-x, -y, -z' 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 Br(1) 0.0447(2) 0.0825(3) 0.0685(3) -0.0166(2) 0.0217(2) 0.0250(2) Br(2) 0.1073(4) 0.0528(2) 0.0486(3) -0.0201(2) 0.0382(2) -0.0102(2) Br(3) 0.0540(2) 0.0858(3) 0.0720(3) 0.0125(2) 0.0408(2) 0.0214(2) Al(1) 0.0313(4) 0.0281(4) 0.0341(4) -0.0043(3) 0.0120(3) 0.0055(3) O(1) 0.0490(10) 0.0263(10) 0.069(2) -0.0049(9) 0.0240(10) 0.0089(10) O(2) 0.0330(10) 0.0328(10) 0.0540(10) -0.0017(8) 0.0155(9) 0.0158(9) O(3) 0.069(2) 0.0271(10) 0.0420(10) -0.0115(10) 0.0220(10) 0.0065(9) O(4) 0.0430(10) 0.0290(9) 0.0370(10) -0.0013(8) 0.0154(9) 0.0070(8) O(5) 0.0440(10) 0.0620(10) 0.0300(10) -0.0140(10) 0.0047(9) 0.0070(10) O(6) 0.0316(10) 0.0410(10) 0.0300(10) -0.0055(8) 0.0105(8) 0.0040(8) O(7) 0.053(2) 0.060(2) 0.135(3) 0.0030(10) 0.012(2) 0.038(2) N(1) 0.0330(10) 0.0270(10) 0.0390(10) -0.0015(9) 0.0135(10) 0.0022(9) N(2) 0.0340(10) 0.0310(10) 0.0330(10) -0.0060(9) 0.0113(9) 0.0076(9) N(3) 0.0300(10) 0.0370(10) 0.0360(10) -0.0081(10) 0.0051(10) 0.0050(10) C(1) 0.044(2) 0.0290(10) 0.045(2) 0.0000(10) 0.0170(10) -0.0010(10) C(2) 0.051(2) 0.0280(10) 0.045(2) -0.0010(10) 0.0140(10) 0.0040(10) C(3) 0.0380(10) 0.0250(10) 0.041(2) -0.0070(10) 0.0110(10) 0.0050(10) C(4) 0.0310(10) 0.0330(10) 0.046(2) -0.0060(10) 0.0110(10) 0.0060(10) C(5) 0.0310(10) 0.0340(10) 0.051(2) -0.0070(10) 0.0140(10) 0.0080(10) C(6) 0.042(2) 0.040(2) 0.079(3) 0.0000(10) 0.027(2) 0.017(2) C(7) 0.042(2) 0.045(2) 0.076(3) -0.0020(10) 0.031(2) 0.008(2) C(8) 0.035(2) 0.053(2) 0.050(2) -0.0130(10) 0.0140(10) 0.011(2) C(9) 0.0350(10) 0.040(2) 0.046(2) -0.0120(10) 0.0100(10) 0.0110(10) C(10) 0.044(2) 0.0370(10) 0.038(2) -0.0110(10) 0.0130(10) 0.0100(10) C(11) 0.047(2) 0.0380(10) 0.042(2) -0.0090(10) 0.0130(10) 0.0150(10) C(12) 0.0320(10) 0.0270(10) 0.040(2) -0.0060(10) 0.0120(10) 0.0090(10) C(13) 0.0360(10) 0.0320(10) 0.035(2) -0.0080(10) 0.0130(10) 0.0060(10) C(14) 0.0340(10) 0.0330(10) 0.035(2) -0.0070(10) 0.0130(10) 0.0060(10) C(15) 0.059(2) 0.040(2) 0.042(2) -0.0030(10) 0.019(2) 0.0130(10) C(16) 0.072(2) 0.049(2) 0.039(2) -0.007(2) 0.021(2) 0.0120(10) C(17) 0.057(2) 0.044(2) 0.039(2) -0.0120(10) 0.0220(10) -0.0010(10) C(18) 0.052(2) 0.0340(10) 0.042(2) -0.0120(10) 0.0200(10) 0.0010(10) C(19) 0.034(2) 0.069(2) 0.045(2) -0.011(2) 0.0000(10) 0.011(2) C(20) 0.045(2) 0.066(2) 0.042(2) -0.021(2) -0.0010(10) 0.012(2) C(21) 0.040(2) 0.0310(10) 0.0300(10) -0.0100(10) 0.0080(10) 0.0050(10) C(22) 0.0330(10) 0.0320(10) 0.036(2) -0.0040(10) 0.0110(10) 0.0050(10) C(23) 0.0330(10) 0.0270(10) 0.037(2) -0.0040(10) 0.0130(10) 0.0050(10) C(24) 0.0340(10) 0.041(2) 0.038(2) -0.0040(10) 0.0080(10) 0.0090(10) C(25) 0.033(2) 0.042(2) 0.055(2) -0.0020(10) 0.0120(10) 0.0120(10) C(26) 0.039(2) 0.045(2) 0.049(2) 0.0040(10) 0.0260(10) 0.0090(10) C(27) 0.043(2) 0.045(2) 0.037(2) -0.0040(10) 0.0160(10) 0.0070(10) C(28) 0.066(3) 0.139(7) 0.124(6) 0.003(4) -0.002(3) 0.029(5) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Br(1) 0.53439(4) 0.34713(4) -0.21242(5) 0.06060(10) Uani ? ? Br(2) 0.20419(5) -0.14550(4) -0.53171(5) 0.06870(10) Uani ? ? Br(3) -0.35934(4) 0.42750(4) 0.48365(5) 0.06880(10) Uani ? ? Al(1) 0.13485(7) 0.24979(6) 0.11986(9) 0.0307(3) Uani ? ? O(1) 0.2165(2) 0.5330(2) 0.1050(3) 0.0466(6) Uani ? ? O(2) 0.3003(2) 0.2178(2) 0.1421(2) 0.0384(5) Uani ? ? O(3) 0.1674(2) -0.0825(2) -0.0104(2) 0.0440(6) Uani ? ? O(4) 0.1062(2) 0.2296(2) -0.0688(2) 0.0360(5) Uani ? ? O(5) 0.1091(2) 0.3428(2) 0.5322(2) 0.0462(6) Uani ? ? O(6) -0.0264(2) 0.2871(2) 0.1047(2) 0.0345(5) Uani ? ? O(7) 0.4085(3) 0.0319(3) 0.2408(5) 0.0840(10) Uani ? ? N(1) 0.1472(2) 0.4037(2) 0.1400(3) 0.0339(6) Uani ? ? N(2) 0.1400(2) 0.0920(2) 0.0949(3) 0.0317(6) Uani ? ? N(3) 0.1572(2) 0.2796(2) 0.3268(3) 0.0351(6) Uani ? ? C(1) 0.0668(3) 0.5035(2) 0.1862(3) 0.0406(8) Uani ? ? C(2) 0.1201(3) 0.5919(2) 0.1723(4) 0.0431(9) Uani ? ? C(3) 0.2246(3) 0.4289(2) 0.0979(3) 0.0344(8) Uani ? ? C(4) 0.3206(3) 0.3529(2) 0.0423(3) 0.0370(8) Uani ? ? C(5) 0.3542(3) 0.2494(2) 0.0693(4) 0.0379(8) Uani ? ? C(6) 0.4481(3) 0.1798(3) 0.0162(5) 0.0520(10) Uani ? ? C(7) 0.5007(3) 0.2093(3) -0.0658(5) 0.0530(10) Uani ? ? C(8) 0.4632(3) 0.3102(3) -0.0946(4) 0.0444(9) Uani ? ? C(9) 0.3755(3) 0.3831(3) -0.0392(3) 0.0391(8) Uani ? ? C(10) 0.1363(3) 0.0362(2) 0.1982(3) 0.0377(8) Uani ? ? C(11) 0.1625(3) -0.0819(3) 0.1283(3) 0.0399(8) Uani ? ? C(12) 0.1558(2) 0.0203(2) -0.0150(3) 0.0317(7) Uani ? ? C(13) 0.1573(3) 0.0390(2) -0.1459(3) 0.0334(8) Uani ? ? C(14) 0.1284(3) 0.1448(2) -0.1648(3) 0.0329(8) Uani ? ? C(15) 0.1201(3) 0.1594(3) -0.2972(4) 0.0454(9) Uani ? ? C(16) 0.1406(4) 0.0738(3) -0.4032(4) 0.0520(10) Uani ? ? C(17) 0.1700(3) -0.0295(3) -0.3825(4) 0.0456(9) Uani ? ? C(18) 0.1780(3) -0.0483(2) -0.2561(3) 0.0412(8) Uani ? ? C(19) 0.2726(3) 0.2812(3) 0.4300(4) 0.0520(10) Uani ? ? C(20) 0.2383(3) 0.3263(3) 0.5674(4) 0.0520(10) Uani ? ? C(21) 0.0746(3) 0.3150(2) 0.3933(3) 0.0335(8) Uani ? ? C(22) -0.0528(3) 0.3306(2) 0.3348(3) 0.0336(7) Uani ? ? C(23) -0.0962(3) 0.3159(2) 0.1900(3) 0.0321(7) Uani ? ? C(24) -0.2200(3) 0.3354(3) 0.1379(3) 0.0384(8) Uani ? ? C(25) -0.2966(3) 0.3665(3) 0.2236(4) 0.0441(9) Uani ? ? C(26) -0.2521(3) 0.3803(3) 0.3655(4) 0.0438(9) Uani ? ? C(27) -0.1319(3) 0.3626(3) 0.4218(3) 0.0417(9) Uani ? ? C(28) 0.5219(6) 0.0412(7) 0.3220(8) 0.119(3) Uani ? ? H(1) -0.0129 0.5041 0.1278 0.0487 Uani ? ? H(2) 0.0648 0.5118 0.2814 0.0487 Uani ? ? H(3) 0.1504 0.6354 0.2624 0.0517 Uani ? ? H(4) 0.0617 0.6374 0.1158 0.0517 Uani ? ? H(5) 0.4766 0.1095 0.0376 0.0620 Uani ? ? H(6) 0.5643 0.1592 -0.1034 0.0634 Uani ? ? H(7) 0.3519 0.4549 -0.0564 0.0469 Uani ? ? H(8) 0.1962 0.0531 0.2829 0.0452 Uani ? ? H(9) 0.0585 0.0555 0.2185 0.0452 Uani ? ? H(10) 0.0998 -0.1175 0.1247 0.0479 Uani ? ? H(11) 0.2378 -0.1172 0.1771 0.0479 Uani ? ? H(12) 0.0994 0.2315 -0.3131 0.0545 Uani ? ? H(13) 0.1346 0.0855 -0.4934 0.0620 Uani ? ? H(14) 0.1978 -0.1212 -0.2430 0.0494 Uani ? ? H(15) 0.3196 0.2093 0.4260 0.0619 Uani ? ? H(16) 0.3170 0.3270 0.4148 0.0619 Uani ? ? H(17) 0.2652 0.3937 0.6132 0.0619 Uani ? ? H(18) 0.2722 0.2757 0.6269 0.0619 Uani ? ? H(19) -0.2520 0.3267 0.0389 0.0461 Uani ? ? H(20) -0.3817 0.3787 0.1851 0.0529 Uani ? ? H(21) -0.1018 0.3722 0.5211 0.0500 Uani ? ? H(22) 0.373(6) 0.080(5) 0.215(7) 0.11(2) Uani ? ? H(23) 0.5607 -0.0256 0.3504 0.1425 Uani ? ? H(24) 0.5677 0.0567 0.2690 0.1425 Uani ? ? H(25) 0.5165 0.0990 0.4031 0.1425 Uani ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br -0.676 1.280 'International Tables' Al 0.213 0.246 'International Tables' O 0.049 0.032 'International Tables' N 0.031 0.018 'International Tables' C 0.018 0.009 'International Tables' H 0.000 0.000 'International Tables' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(2) Al(1) O(4) 93.00(10) yes O(2) Al(1) O(6) 177.20(10) yes O(2) Al(1) N(1) 86.19(10) yes O(2) Al(1) N(2) 87.93(10) yes O(2) Al(1) N(3) 90.00(10) yes O(4) Al(1) O(6) 88.82(10) yes O(4) Al(1) N(1) 89.20(10) yes O(4) Al(1) N(2) 89.10(10) yes O(4) Al(1) N(3) 176.40(10) yes O(6) Al(1) N(1) 91.68(10) yes O(6) Al(1) N(2) 94.20(10) yes O(6) Al(1) N(3) 88.17(10) yes N(1) Al(1) N(2) 173.80(10) yes N(1) Al(1) N(3) 88.90(10) yes N(2) Al(1) N(3) 93.10(10) yes C(2) O(1) C(3) 107.0(2) yes Al(1) O(2) C(5) 122.7(2) yes C(11) O(3) C(12) 106.8(2) yes Al(1) O(4) C(14) 131.9(2) yes C(20) O(5) C(21) 106.7(3) yes Al(1) O(6) C(23) 135.9(2) yes Al(1) N(1) C(1) 129.1(2) yes Al(1) N(1) C(3) 123.0(2) yes C(1) N(1) C(3) 107.5(2) yes Al(1) N(2) C(10) 127.8(2) yes Al(1) N(2) C(12) 124.3(2) yes C(10) N(2) C(12) 107.8(2) yes Al(1) N(3) C(19) 125.5(2) yes Al(1) N(3) C(21) 126.3(2) yes C(19) N(3) C(21) 107.5(3) yes N(1) C(1) C(2) 104.3(3) yes O(1) C(2) C(1) 103.5(2) yes O(1) C(3) N(1) 117.2(3) yes O(1) C(3) C(4) 117.6(3) yes N(1) C(3) C(4) 125.2(3) yes C(3) C(4) C(5) 119.1(3) yes C(3) C(4) C(9) 119.7(3) yes C(5) C(4) C(9) 121.2(3) yes O(2) C(5) C(4) 122.2(3) yes O(2) C(5) C(6) 120.6(3) yes C(4) C(5) C(6) 117.2(3) yes C(5) C(6) C(7) 121.3(3) yes C(6) C(7) C(8) 120.1(3) yes Br(1) C(8) C(7) 119.2(3) yes Br(1) C(8) C(9) 120.2(3) yes C(7) C(8) C(9) 120.6(3) yes C(4) C(9) C(8) 119.4(3) yes N(2) C(10) C(11) 103.7(2) yes O(3) C(11) C(10) 104.7(2) yes O(3) C(12) N(2) 116.8(3) yes O(3) C(12) C(13) 116.3(3) yes N(2) C(12) C(13) 126.9(3) yes C(12) C(13) C(14) 119.4(3) yes C(12) C(13) C(18) 120.1(3) yes C(14) C(13) C(18) 120.3(3) yes O(4) C(14) C(13) 124.0(3) yes O(4) C(14) C(15) 118.1(3) yes C(13) C(14) C(15) 117.9(3) yes C(14) C(15) C(16) 121.1(3) yes C(15) C(16) C(17) 120.2(3) yes Br(2) C(17) C(16) 118.4(3) yes Br(2) C(17) C(18) 120.5(3) yes C(16) C(17) C(18) 121.1(3) yes C(13) C(18) C(17) 119.4(3) yes N(3) C(19) C(20) 104.0(3) yes O(5) C(20) C(19) 104.7(3) yes O(5) C(21) N(3) 116.9(3) yes O(5) C(21) C(22) 116.0(3) yes N(3) C(21) C(22) 127.1(3) yes C(21) C(22) C(23) 119.4(3) yes C(21) C(22) C(27) 120.2(3) yes C(23) C(22) C(27) 120.4(3) yes O(6) C(23) C(22) 122.8(3) yes O(6) C(23) C(24) 119.6(3) yes C(22) C(23) C(24) 117.6(3) yes C(23) C(24) C(25) 121.6(3) yes C(24) C(25) C(26) 119.9(3) yes Br(3) C(26) C(25) 119.4(2) yes Br(3) C(26) C(27) 119.7(3) yes C(25) C(26) C(27) 120.9(3) yes C(22) C(27) C(26) 119.6(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br(1) C(8) ? ? 1.901(3) yes Br(2) C(17) ? ? 1.905(3) yes Br(3) C(26) ? ? 1.903(3) yes Al(1) O(2) ? ? 1.876(2) yes Al(1) O(4) ? ? 1.839(2) yes Al(1) O(6) ? ? 1.839(2) yes Al(1) N(1) ? ? 2.024(3) yes Al(1) N(2) ? ? 2.015(3) yes Al(1) N(3) ? ? 2.019(3) yes O(1) C(2) ? ? 1.461(4) yes O(1) C(3) ? ? 1.336(3) yes O(2) C(5) ? ? 1.327(4) yes O(3) C(11) ? ? 1.455(4) yes O(3) C(12) ? ? 1.343(3) yes O(4) C(14) ? ? 1.301(3) yes O(5) C(20) ? ? 1.456(4) yes O(5) C(21) ? ? 1.347(4) yes O(6) C(23) ? ? 1.307(3) yes O(7) C(28) ? ? 1.388(7) yes N(1) C(1) ? ? 1.470(4) yes N(1) C(3) ? ? 1.280(4) yes N(2) C(10) ? ? 1.477(4) yes N(2) C(12) ? ? 1.288(4) yes N(3) C(19) ? ? 1.482(4) yes N(3) C(21) ? ? 1.286(4) yes C(1) C(2) ? ? 1.523(5) yes C(3) C(4) ? ? 1.461(4) yes C(4) C(5) ? ? 1.408(4) yes C(4) C(9) ? ? 1.397(4) yes C(5) C(6) ? ? 1.401(4) yes C(6) C(7) ? ? 1.379(5) yes C(7) C(8) ? ? 1.382(5) yes C(8) C(9) ? ? 1.374(5) yes C(10) C(11) ? ? 1.518(4) yes C(12) C(13) ? ? 1.453(4) yes C(13) C(14) ? ? 1.408(4) yes C(13) C(18) ? ? 1.405(4) yes C(14) C(15) ? ? 1.412(4) yes C(15) C(16) ? ? 1.365(5) yes C(16) C(17) ? ? 1.383(5) yes C(17) C(18) ? ? 1.375(5) yes C(19) C(20) ? ? 1.514(5) yes C(21) C(22) ? ? 1.453(4) yes C(22) C(23) ? ? 1.413(4) yes C(22) C(27) ? ? 1.403(4) yes C(23) C(24) ? ? 1.405(4) yes C(24) C(25) ? ? 1.371(5) yes C(25) C(26) ? ? 1.388(5) yes C(26) C(27) ? ? 1.373(5) yes