#------------------------------------------------------------------------------ #$Date: 2019-03-30 01:09:10 +0200 (Sat, 30 Mar 2019) $ #$Revision: 214417 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/32/7123232.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7123232 loop_ _publ_author_name 'Schmitt, Wolfgang' 'Martins, Luana' 'Macreadie, Lauren' 'Sensharma, Debobroto' 'Vaesen, Sebastien' 'Zhang, Xia' 'Gough, John' 'O'Doherty, Mariah' 'Zhu, Nianyong' 'Ruether, Manuel' 'O'Brien, John E' 'Bradley, A. Louise' _publ_section_title ; Light-harvesting, 3rd generation MOF with large, tubular channel aperture ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC00206E _journal_year 2019 _chemical_formula_sum 'C62 H33 Co F3 N12 O8 Ru' _chemical_formula_weight 1291.00 _space_group_crystal_system trigonal _space_group_IT_number 163 _space_group_name_Hall '-P 3 2c' _space_group_name_H-M_alt 'P -3 1 c' _symmetry_space_group_name_Hall '-P 3 2c' _symmetry_space_group_name_H-M 'P -3 1 c' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2018-12-19 deposited with the CCDC. 2019-03-29 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 26.645(4) _cell_length_b 26.645(4) _cell_length_c 10.542(2) _cell_measurement_reflns_used 1442 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.47 _cell_measurement_theta_min 3.32 _cell_volume 6481.6(18) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1939 _diffrn_reflns_av_unetI/netI 0.0710 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 54055 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 52.844 _diffrn_reflns_theta_max 52.844 _diffrn_reflns_theta_min 1.915 _exptl_absorpt_coefficient_mu 2.237 _exptl_absorpt_correction_T_max 0.7504 _exptl_absorpt_correction_T_min 0.5395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 0.661 _exptl_crystal_description block _exptl_crystal_F_000 1302 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.239 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 2508 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.1736 _refine_ls_R_factor_gt 0.1010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1498P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2370 _refine_ls_wR_factor_ref 0.2800 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1416 _reflns_number_total 2508 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc00206e2.cif _cod_data_source_block Photo-MOF _cod_original_cell_volume 6482(2) _cod_database_code 7123232 _shelx_shelxl_version_number 2018/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _platon_squeeze_void_probe_radius 1.20 _shelx_res_file ; TITL cu_TCD760_0m_a.res in P-31c shelx.res created by SHELXL-2018/1 at 17:07:49 on 12-Dec-2018 CELL 1.54184 26.6454 26.6454 10.5418 90.000 90.000 120.000 ZERR 2.00 0.0038 0.0038 0.0020 0.000 0.000 0.000 LATT 1 SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SYMM - Y, - X, 1/2 - Z SYMM - X + Y, Y, 1/2 - Z SYMM X, X - Y, 1/2 - Z SFAC RU CO O N C H F UNIT 2 2 16 24 124 66 6 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 5 0 145 TEMP -173.18 WGHT 0.149800 FVAR 0.77059 RU1 1 0.333333 0.666667 0.750000 10.16667 0.09019 0.09019 = 0.08273 0.00000 0.00000 0.04510 CO1 2 0.666667 0.333333 0.750000 10.16667 0.12011 0.12011 = 0.10021 0.00000 0.00000 0.06006 O1 3 0.651518 0.396387 0.668614 11.00000 0.10638 0.11809 = 0.10546 0.02775 0.03368 0.05811 N1 4 0.399192 0.665397 0.649715 11.00000 0.12790 0.08452 = 0.08217 0.00546 -0.02857 0.05500 N2 4 0.499851 0.553018 0.668799 11.00000 0.11052 0.10354 = 0.10119 0.02517 0.02085 0.07035 AFIX 43 H6 6 0.525652 0.566649 0.607356 10.50000 -1.20000 AFIX 0 C1 5 0.430206 0.696177 0.550362 11.00000 0.13166 0.08862 = 0.05481 0.02726 0.01480 0.04395 AFIX 43 H1 6 0.421777 0.723740 0.513896 11.00000 -1.20000 AFIX 0 C2 5 0.473367 0.689701 0.499206 11.00000 0.08970 0.11718 = 0.09788 0.02416 0.02164 0.05261 AFIX 43 H2 6 0.495600 0.714321 0.431474 11.00000 -1.20000 AFIX 0 C3 5 0.485579 0.649195 0.541973 11.00000 0.09303 0.11491 = 0.11385 0.00713 0.00090 0.06636 AFIX 43 H3 6 0.515343 0.644579 0.503931 11.00000 -1.20000 AFIX 0 C4 5 0.453333 0.614278 0.643537 11.00000 0.09546 0.11383 = 0.05901 0.01624 0.01546 0.04859 C5 5 0.409659 0.623312 0.697935 11.00000 0.10755 0.09367 = 0.04256 0.01028 0.00617 0.04873 C6 5 0.462721 0.569341 0.702394 11.00000 0.09956 0.10714 = 0.08962 0.02846 0.01403 0.05253 C7 5 0.488865 0.511135 0.750000 10.50000 0.09737 0.09737 = 0.15235 0.00447 0.00447 0.08081 C8 5 0.519749 0.480251 0.750000 10.50000 0.10465 0.10465 = 0.07319 0.01830 0.01830 0.02819 C9 5 0.509737 0.438109 0.838492 11.00000 0.10049 0.17849 = 0.13293 0.03687 0.04595 0.09879 AFIX 43 H9 6 0.482366 0.430592 0.903977 11.00000 -1.20000 AFIX 0 C10 5 0.537515 0.406709 0.835977 11.00000 0.11740 0.14367 = 0.10298 0.04334 0.03337 0.07600 AFIX 43 H10 6 0.526498 0.375894 0.894699 11.00000 -1.20000 AFIX 0 C11 5 0.581246 0.418754 0.750000 10.50000 0.11739 0.11739 = 0.09843 -0.00639 -0.00639 0.08354 C12 5 0.613291 0.386709 0.750000 10.50000 0.11316 0.11316 = 0.03866 0.03130 0.03130 0.02670 HKLF 4 REM cu_TCD760_0m_a.res in P-31c REM R1 = 0.1010 for 1416 Fo > 4sig(Fo) and 0.1736 for all 2508 data REM 124 parameters refined using 0 restraints END WGHT 0.1498 0.0000 REM Highest difference peak 1.239, deepest hole -0.461, 1-sigma level 0.082 Q1 1 0.3333 0.6667 0.6407 10.33333 0.05 1.24 Q2 1 0.2852 0.6426 0.7500 10.50000 0.05 0.86 Q3 1 0.6667 0.3333 0.6360 10.33333 0.05 0.55 Q4 1 0.6372 0.3628 0.7500 10.50000 0.05 0.43 Q5 1 0.4518 0.5203 0.7258 11.00000 0.05 0.38 Q6 1 0.5493 0.4507 0.7500 10.50000 0.05 0.31 Q7 1 0.4005 0.6665 0.5637 11.00000 0.05 0.30 Q8 1 0.4236 0.7067 0.6414 11.00000 0.05 0.29 Q9 1 0.5082 0.5131 0.6723 11.00000 0.05 0.27 Q10 1 0.4792 0.6596 0.5780 11.00000 0.05 0.27 Q11 1 0.4319 0.6302 0.6094 11.00000 0.05 0.26 Q12 1 0.6050 0.3025 0.7500 10.50000 0.05 0.25 Q13 1 0.4709 0.6108 0.5715 11.00000 0.05 0.25 Q14 1 0.4942 0.5796 0.6267 11.00000 0.05 0.25 Q15 1 0.4698 0.7079 0.6101 11.00000 0.05 0.24 Q16 1 0.5328 0.6593 0.4618 11.00000 0.05 0.22 Q17 1 0.4774 0.4764 0.7372 11.00000 0.05 0.21 Q18 1 0.4914 0.6653 0.4546 11.00000 0.05 0.20 Q19 1 0.5097 0.4092 0.9175 11.00000 0.05 0.20 Q20 1 0.6284 0.4197 0.7075 11.00000 0.05 0.20 ; _shelx_res_checksum 42369 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Ru1 Ru 0.333333 0.666667 0.750000 0.0877(8) Uani 1 6 d S T P Co1 Co 0.666667 0.333333 0.750000 0.1135(14) Uani 1 6 d S T P O1 O 0.6515(3) 0.3964(3) 0.6686(6) 0.109(2) Uani 1 1 d . . . N1 N 0.3992(3) 0.6654(3) 0.6497(7) 0.097(2) Uani 1 1 d . . . N2 N 0.4999(4) 0.5530(3) 0.6688(7) 0.098(2) Uani 1 1 d . . . H6 H 0.525652 0.566649 0.607356 0.117 Uiso 0.5 1 calc R U P C1 C 0.4302(5) 0.6962(4) 0.5504(8) 0.097(3) Uani 1 1 d . . . H1 H 0.421777 0.723740 0.513896 0.116 Uiso 1 1 calc R U . C2 C 0.4734(4) 0.6897(4) 0.4992(9) 0.101(3) Uani 1 1 d . . . H2 H 0.495600 0.714321 0.431474 0.121 Uiso 1 1 calc R U . C3 C 0.4856(4) 0.6492(4) 0.5420(10) 0.101(3) Uani 1 1 d . . . H3 H 0.515343 0.644579 0.503931 0.121 Uiso 1 1 calc R U . C4 C 0.4533(4) 0.6143(4) 0.6435(8) 0.091(3) Uani 1 1 d . . . C5 C 0.4097(4) 0.6233(4) 0.6979(6) 0.082(2) Uani 1 1 d . . . C6 C 0.4627(4) 0.5693(4) 0.7024(8) 0.098(3) Uani 1 1 d . . . C7 C 0.4889(3) 0.5111(3) 0.750000 0.101(5) Uani 1 2 d S T P C8 C 0.5197(4) 0.4803(4) 0.750000 0.105(5) Uani 1 2 d S T P C9 C 0.5097(4) 0.4381(5) 0.8385(10) 0.124(4) Uani 1 1 d . . . H9 H 0.482366 0.430592 0.903977 0.149 Uiso 1 1 calc R U . C10 C 0.5375(5) 0.4067(5) 0.8360(9) 0.117(3) Uani 1 1 d . . . H10 H 0.526498 0.375894 0.894699 0.140 Uiso 1 1 calc R U . C11 C 0.5812(3) 0.4188(3) 0.750000 0.100(4) Uani 1 2 d S T P C12 C 0.6133(4) 0.3867(4) 0.750000 0.102(5) Uani 1 2 d S T P 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 Ru1 0.0902(10) 0.0902(10) 0.0827(13) 0.000 0.000 0.0451(5) Co1 0.120(2) 0.120(2) 0.100(3) 0.000 0.000 0.0601(10) O1 0.106(5) 0.118(5) 0.105(5) 0.028(4) 0.034(4) 0.058(4) N1 0.128(6) 0.085(5) 0.082(5) 0.005(5) -0.029(5) 0.055(5) N2 0.111(6) 0.104(6) 0.101(6) 0.025(5) 0.021(5) 0.070(6) C1 0.132(9) 0.089(7) 0.055(5) 0.027(5) 0.015(6) 0.044(7) C2 0.090(7) 0.117(9) 0.098(7) 0.024(6) 0.022(6) 0.053(7) C3 0.093(7) 0.115(8) 0.114(8) 0.007(6) 0.001(6) 0.066(7) C4 0.095(7) 0.114(8) 0.059(5) 0.016(6) 0.015(5) 0.049(6) C5 0.108(7) 0.094(7) 0.043(5) 0.010(4) 0.006(4) 0.049(6) C6 0.100(8) 0.107(8) 0.090(7) 0.028(6) 0.014(5) 0.053(7) C7 0.097(9) 0.097(9) 0.152(14) 0.004(9) 0.004(9) 0.081(10) C8 0.105(8) 0.105(8) 0.073(9) 0.018(7) 0.018(7) 0.028(10) C9 0.100(8) 0.178(12) 0.133(9) 0.037(8) 0.046(7) 0.099(9) C10 0.117(9) 0.144(10) 0.103(8) 0.043(7) 0.033(7) 0.076(8) C11 0.117(9) 0.117(9) 0.098(11) -0.006(8) -0.006(8) 0.084(11) C12 0.113(7) 0.113(7) 0.039(7) 0.031(6) 0.031(6) 0.027(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 Ru1 N1 85.1(4) 5_556 2_665 N1 Ru1 N1 96.1(2) 5_556 6_566 N1 Ru1 N1 82.7(4) 2_665 6_566 N1 Ru1 N1 82.7(4) 5_556 3_565 N1 Ru1 N1 96.1(3) 2_665 3_565 N1 Ru1 N1 178.4(4) 6_566 3_565 N1 Ru1 N1 96.1(3) 5_556 4_666 N1 Ru1 N1 178.4(4) 2_665 4_666 N1 Ru1 N1 96.1(2) 6_566 4_666 N1 Ru1 N1 85.1(4) 3_565 4_666 N1 Ru1 N1 178.4(4) 5_556 . N1 Ru1 N1 96.1(3) 2_665 . N1 Ru1 N1 85.1(4) 6_566 . N1 Ru1 N1 96.1(2) 3_565 . N1 Ru1 N1 82.7(4) 4_666 . O1 Co1 O1 61.3(3) 4_666 . O1 Co1 O1 104.4(2) 4_666 5_656 O1 Co1 O1 92.2(3) . 5_656 O1 Co1 O1 92.2(3) 4_666 2_655 O1 Co1 O1 104.4(2) . 2_655 O1 Co1 O1 160.8(3) 5_656 2_655 O1 Co1 O1 160.8(3) 4_666 3_665 O1 Co1 O1 104.4(2) . 3_665 O1 Co1 O1 61.3(3) 5_656 3_665 O1 Co1 O1 104.4(2) 2_655 3_665 O1 Co1 O1 104.4(2) 4_666 6_556 O1 Co1 O1 160.8(3) . 6_556 O1 Co1 O1 104.4(2) 5_656 6_556 O1 Co1 O1 61.3(3) 2_655 6_556 O1 Co1 O1 92.2(3) 3_665 6_556 O1 Co1 C12 30.65(17) 4_666 . O1 Co1 C12 30.65(17) . . O1 Co1 C12 99.60(16) 5_656 . O1 Co1 C12 99.60(16) 2_655 . O1 Co1 C12 133.92(17) 3_665 . O1 Co1 C12 133.92(17) 6_556 . O1 Co1 C12 99.59(17) 4_666 2_655 O1 Co1 C12 133.92(17) . 2_655 O1 Co1 C12 133.92(17) 5_656 2_655 O1 Co1 C12 30.65(17) 2_655 2_655 O1 Co1 C12 99.59(16) 3_665 2_655 O1 Co1 C12 30.65(17) 6_556 2_655 C12 Co1 C12 120.000(1) . 2_655 O1 Co1 C12 133.92(17) 4_666 3_665 O1 Co1 C12 99.59(17) . 3_665 O1 Co1 C12 30.65(17) 5_656 3_665 O1 Co1 C12 133.92(17) 2_655 3_665 O1 Co1 C12 30.65(17) 3_665 3_665 O1 Co1 C12 99.59(16) 6_556 3_665 C12 Co1 C12 120.000(2) . 3_665 C12 Co1 C12 120.000(1) 2_655 3_665 C12 O1 Co1 91.0(8) . . C1 N1 C5 118.3(8) . . C1 N1 Ru1 131.6(7) . . C5 N1 Ru1 110.1(6) . . C6 N2 C7 102.7(9) . . C6 N2 H6 128.6 . . C7 N2 H6 128.6 . . N1 C1 C2 122.6(9) . . N1 C1 H1 118.7 . . C2 C1 H1 118.7 . . C3 C2 C1 121.8(9) . . C3 C2 H2 119.1 . . C1 C2 H2 119.1 . . C2 C3 C4 118.3(9) . . C2 C3 H3 120.8 . . C4 C3 H3 120.8 . . C3 C4 C5 118.6(9) . . C3 C4 C6 124.4(9) . . C5 C4 C6 116.9(8) . . N1 C5 C5 118.6(5) . 4_666 N1 C5 C4 120.3(7) . . C5 C5 C4 121.2(5) 4_666 . N2 C6 C6 110.0(5) . 4_666 N2 C6 C4 128.1(8) . . C6 C6 C4 121.9(5) 4_666 . N2 C7 N2 114.5(11) 4_666 . N2 C7 C8 122.7(6) 4_666 . N2 C7 C8 122.7(6) . . C9 C8 C9 115.0(15) 4_666 . C9 C8 C7 122.5(8) 4_666 . C9 C8 C7 122.5(8) . . C10 C9 C8 122.8(11) . . C10 C9 H9 118.6 . . C8 C9 H9 118.6 . . C9 C10 C11 121.5(10) . . C9 C10 H10 119.2 . . C11 C10 H10 119.2 . . C10 C11 C10 116.1(13) . 4_666 C10 C11 C12 122.0(7) . . C10 C11 C12 122.0(7) 4_666 . O1 C12 O1 116.7(16) . 4_666 O1 C12 C11 121.6(8) . . O1 C12 C11 121.6(8) 4_666 . O1 C12 Co1 58.4(8) . . O1 C12 Co1 58.4(8) 4_666 . C11 C12 Co1 180.0(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ru1 N1 2.063(8) 5_556 Ru1 N1 2.063(8) 2_665 Ru1 N1 2.063(9) 6_566 Ru1 N1 2.063(8) 3_565 Ru1 N1 2.063(8) 4_666 Ru1 N1 2.063(8) . Co1 O1 2.097(6) 4_666 Co1 O1 2.098(6) . Co1 O1 2.098(6) 5_656 Co1 O1 2.098(6) 2_655 Co1 O1 2.098(6) 3_665 Co1 O1 2.098(6) 6_556 Co1 C12 2.463(19) . Co1 C12 2.463(19) 2_655 Co1 C12 2.463(19) 3_665 O1 C12 1.256(10) . N1 C1 1.332(10) . N1 C5 1.381(10) . N2 C6 1.313(10) . N2 C7 1.318(8) . N2 H6 0.8800 . C1 C2 1.357(12) . C1 H1 0.9500 . C2 C3 1.351(12) . C2 H2 0.9500 . C3 C4 1.397(11) . C3 H3 0.9500 . C4 C5 1.422(11) . C4 C6 1.477(12) . C5 C5 1.406(15) 4_666 C6 C6 1.318(16) 4_666 C7 C8 1.425(19) . C8 C9 1.379(13) 4_666 C8 C9 1.379(13) . C9 C10 1.367(12) . C9 H9 0.9500 . C10 C11 1.381(11) . C10 H10 0.9500 . C11 C12 1.479(19) . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.012 4393 1549 ' '