#------------------------------------------------------------------------------ #$Date: 2020-02-12 04:25:56 +0200 (Wed, 12 Feb 2020) $ #$Revision: 248063 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557300.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_1557300 loop_ _publ_author_name 'Zhou, Qing' 'Yang, Tianjia' 'Zhong, Zihao' 'Kausar, Fahmeeda' 'Wang, Ziyi' 'Zhang, Yongming' 'Yuan, Wang Zhang' _publ_section_title ; Clustering-triggered emission strategy towards tunable multi-color persistent phosphorescence ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC06518K _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C5 H10 O5' _chemical_formula_sum 'C5 H10 O5' _chemical_formula_weight 150.13 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-06-18 deposited with the CCDC. 2020-02-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.61070(10) _cell_length_b 9.1858(2) _cell_length_c 12.5998(3) _cell_measurement_reflns_used 4612 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 68.13 _cell_measurement_theta_min 3.51 _cell_volume 649.38(2) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4725 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 63.674 _diffrn_reflns_theta_max 63.674 _diffrn_reflns_theta_min 5.961 _exptl_absorpt_coefficient_mu 1.217 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.536 _exptl_crystal_description block _exptl_crystal_F_000 320 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.200 _exptl_transmission_factor_max 0.7530 _exptl_transmission_factor_min 0.6693 _refine_diff_density_max 0.232 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.3(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1065 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.994 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0302 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.1031 _reflns_Friedel_coverage 0.641 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 1061 _reflns_number_total 1065 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06518k6.cif _cod_data_source_block t_a _cod_database_code 1557300 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_min 0.759 _shelx_estimated_absorpt_t_max 0.793 _shelx_res_file ; TITL t_a P 1 R = New: P212121 t_a.res created by SHELXL-2018/3 at 10:34:16 on 11-Apr-2019 CELL 1.54178 5.6107 9.1858 12.5998 90.000 90.000 90.000 ZERR 4 0.0001 0.0002 0.0003 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H O UNIT 20 40 20 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 5 FMAP 2 PLAN -20 ACTA size 0.24 0.22 0.20 conf BOND $H CONF TWIN WGHT 0.100000 BASF 0.34344 FVAR 2.02286 O1 3 0.846643 1.570134 0.508797 11.00000 0.03585 0.02593 = 0.01490 -0.00065 -0.00011 0.00703 O2 3 1.182475 1.438354 0.457126 11.00000 0.02174 0.03415 = 0.02453 0.00904 -0.00146 0.00334 AFIX 3 H2A 2 1.272455 1.412404 0.514656 11.00000 -1.50000 AFIX 0 H7 2 1.015712 1.673811 0.395572 11.00000 0.02324 H6 2 0.774753 1.759316 0.445264 11.00000 0.02830 O3 3 0.879755 1.213864 0.380451 11.00000 0.02734 0.01742 = 0.02661 0.00378 0.01105 0.00193 AFIX 3 H3A 2 0.997475 1.212924 0.351451 11.00000 -1.50000 AFIX 0 O4 3 0.638406 1.380057 0.225345 11.00000 0.03916 0.03197 = 0.01408 0.00252 -0.00203 -0.01958 AFIX 147 H4A 2 0.676094 1.402300 0.164593 11.00000 -1.50000 AFIX 0 O5 3 0.717757 1.693485 0.236820 11.00000 0.02505 0.02279 = 0.02108 0.00904 0.00444 0.00772 AFIX 3 H5 2 0.595517 1.756665 0.242300 11.00000 -1.50000 AFIX 0 C1 1 0.943207 1.429539 0.486288 11.00000 0.02447 0.02271 = 0.01563 0.00566 0.00016 0.00553 AFIX 13 H1 2 0.930874 1.369560 0.550376 11.00000 -1.20000 AFIX 0 C2 1 0.798255 1.357805 0.398441 11.00000 0.01978 0.01824 = 0.01739 0.00230 0.00600 0.00068 AFIX 13 H2 2 0.633869 1.350421 0.424174 11.00000 -1.20000 AFIX 0 C3 1 0.792410 1.451337 0.298485 11.00000 0.01790 0.01909 = 0.01447 0.00280 0.00120 -0.00300 AFIX 13 H3 2 0.952984 1.458669 0.268349 11.00000 -1.20000 AFIX 0 C4 1 0.702393 1.601600 0.328086 11.00000 0.01587 0.02318 = 0.01423 0.00482 0.00224 0.00276 AFIX 13 H4 2 0.535671 1.594648 0.350715 11.00000 -1.20000 AFIX 0 C5 1 0.850323 1.665566 0.417746 11.00000 0.02684 0.02016 = 0.02031 0.00048 -0.00091 0.00264 HKLF 4 REM t_a P 1 R = New: P212121 REM wR2 = 0.103118, GooF = S = 0.99371, Restrained GooF = 0.99371 for all data REM R1 = 0.030221 for 1061 Fo > 4sig(Fo) and 0.030791 for all 1065 data REM 101 parameters refined using 0 restraints END WGHT 0.0503 0.1687 REM Highest difference peak 0.232, deepest hole -0.210, 1-sigma level 0.042 Q1 1 0.9870 1.4182 0.5745 11.00000 0.05 0.23 Q2 1 0.8039 1.3996 0.3437 11.00000 0.05 0.20 Q3 1 0.8535 1.3943 0.4365 11.00000 0.05 0.20 Q4 1 0.7719 1.6232 0.3729 11.00000 0.05 0.15 Q5 1 0.7639 1.5337 0.3039 11.00000 0.05 0.14 Q6 1 0.8856 1.6188 0.4626 11.00000 0.05 0.14 Q7 1 0.8472 1.7680 0.4327 11.00000 0.05 0.14 Q8 1 0.9681 1.6873 0.3822 11.00000 0.05 0.12 Q9 1 1.2303 1.1842 0.3250 11.00000 0.05 0.12 Q10 1 0.8752 1.6038 0.5596 11.00000 0.05 0.12 Q11 1 0.5603 1.5768 0.5265 11.00000 0.05 0.12 Q12 1 0.2878 1.5089 0.2574 11.00000 0.05 0.10 Q13 1 1.0707 1.7956 0.4590 11.00000 0.05 0.10 Q14 1 0.7228 1.4242 0.2407 11.00000 0.05 0.10 Q15 1 0.9235 1.2308 0.5585 11.00000 0.05 0.10 Q16 1 0.7028 1.7808 0.2573 11.00000 0.05 0.10 Q17 1 0.8865 1.7478 0.5798 11.00000 0.05 0.09 Q18 1 0.5487 1.5579 0.3167 11.00000 0.05 0.09 Q19 1 0.6436 1.2084 0.2779 11.00000 0.05 0.09 Q20 1 0.7505 1.8683 0.1940 11.00000 0.05 0.09 ; _shelx_res_checksum 22044 loop_ _space_group_symop_operation_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' 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 O1 O 0.8466(3) 1.57013(16) 0.50880(11) 0.0256(5) Uani 1 1 d . . O2 O 1.1825(3) 1.43835(18) 0.45713(13) 0.0268(4) Uani 1 1 d . . H2A H 1.272455 1.412404 0.514656 0.040 Uiso 1 1 d R U H7 H 1.016(5) 1.674(3) 0.396(2) 0.023(6) Uiso 1 1 d . . H6 H 0.775(5) 1.759(3) 0.445(2) 0.028(7) Uiso 1 1 d . . O3 O 0.8798(3) 1.21386(15) 0.38045(12) 0.0238(5) Uani 1 1 d . . H3A H 0.997475 1.212924 0.351451 0.036 Uiso 1 1 d R U O4 O 0.6384(3) 1.38006(19) 0.22535(11) 0.0284(5) Uani 1 1 d . . H4A H 0.676094 1.402300 0.164593 0.043 Uiso 1 1 calc R U O5 O 0.7178(3) 1.69349(16) 0.23682(11) 0.0230(4) Uani 1 1 d . . H5 H 0.595517 1.756665 0.242300 0.034 Uiso 1 1 d R U C1 C 0.9432(4) 1.4295(2) 0.48629(16) 0.0209(5) Uani 1 1 d . . H1 H 0.930874 1.369560 0.550376 0.025 Uiso 1 1 calc R U C2 C 0.7983(4) 1.3578(2) 0.39844(15) 0.0185(5) Uani 1 1 d . . H2 H 0.633869 1.350421 0.424174 0.022 Uiso 1 1 calc R U C3 C 0.7924(3) 1.4513(2) 0.29849(16) 0.0172(5) Uani 1 1 d . . H3 H 0.952984 1.458669 0.268349 0.021 Uiso 1 1 calc R U C4 C 0.7024(3) 1.6016(2) 0.32809(15) 0.0178(5) Uani 1 1 d . . H4 H 0.535671 1.594648 0.350715 0.021 Uiso 1 1 calc R U C5 C 0.8503(4) 1.6656(2) 0.41775(17) 0.0224(5) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0358(9) 0.0259(9) 0.0149(8) -0.0006(6) -0.0001(6) 0.0070(7) O2 0.0217(8) 0.0342(9) 0.0245(8) 0.0090(6) -0.0015(5) 0.0033(7) O3 0.0273(8) 0.0174(8) 0.0266(9) 0.0038(6) 0.0111(7) 0.0019(6) O4 0.0392(9) 0.0320(9) 0.0141(8) 0.0025(6) -0.0020(6) -0.0196(7) O5 0.0251(8) 0.0228(8) 0.0211(8) 0.0090(6) 0.0044(6) 0.0077(6) C1 0.0245(11) 0.0227(10) 0.0156(9) 0.0057(8) 0.0002(8) 0.0055(9) C2 0.0198(10) 0.0182(10) 0.0174(10) 0.0023(8) 0.0060(8) 0.0007(8) C3 0.0179(9) 0.0191(10) 0.0145(9) 0.0028(8) 0.0012(7) -0.0030(8) C4 0.0159(9) 0.0232(10) 0.0142(9) 0.0048(8) 0.0022(8) 0.0028(8) C5 0.0268(12) 0.0202(10) 0.0203(10) 0.0005(9) -0.0009(9) 0.0026(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0492 0.0322 '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 C1 O1 C5 112.68(14) C1 O2 H2A 107.9 C2 O3 H3A 111.7 C3 O4 H4A 109.5 C4 O5 H5 105.8 O2 C1 O1 111.40(19) O2 C1 C2 110.35(17) O1 C1 C2 109.43(17) O2 C1 H1 108.5 O1 C1 H1 108.5 C2 C1 H1 108.5 O3 C2 C1 110.33(17) O3 C2 C3 113.61(16) C1 C2 C3 111.58(17) O3 C2 H2 107.0 C1 C2 H2 107.0 C3 C2 H2 107.0 O4 C3 C4 112.08(18) O4 C3 C2 106.78(16) C4 C3 C2 108.47(16) O4 C3 H3 109.8 C4 C3 H3 109.8 C2 C3 H3 109.8 O5 C4 C3 108.64(15) O5 C4 C5 109.68(17) C3 C4 C5 110.66(17) O5 C4 H4 109.3 C3 C4 H4 109.3 C5 C4 H4 109.3 O1 C5 C4 110.37(17) O1 C5 H7 106.8(15) C4 C5 H7 109.7(15) O1 C5 H6 103.7(17) C4 C5 H6 110.6(16) H7 C5 H6 115(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.429(3) O1 C5 1.444(2) O2 C1 1.394(3) O2 H2A 0.9149 O3 C2 1.417(3) O3 H3A 0.7549 O4 C3 1.423(3) O4 H4A 0.8200 O5 C4 1.429(2) O5 H5 0.9011 C1 C2 1.523(3) C1 H1 0.9800 C2 C3 1.525(3) C2 H2 0.9800 C3 C4 1.516(3) C3 H3 0.9800 C4 C5 1.520(3) C4 H4 0.9800 C5 H7 0.97(3) C5 H6 1.02(3) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C5 O1 C1 O2 62.3(2) C5 O1 C1 C2 -60.0(2) O2 C1 C2 O3 61.5(2) O1 C1 C2 O3 -175.57(14) O2 C1 C2 C3 -65.8(2) O1 C1 C2 C3 57.1(2) O3 C2 C3 O4 58.9(2) C1 C2 C3 O4 -175.56(16) O3 C2 C3 C4 179.92(16) C1 C2 C3 C4 -54.6(2) O4 C3 C4 O5 -67.7(2) C2 C3 C4 O5 174.63(14) O4 C3 C4 C5 171.81(16) C2 C3 C4 C5 54.2(2) C1 O1 C5 C4 60.6(2) O5 C4 C5 O1 -177.04(14) C3 C4 C5 O1 -57.2(2)