#------------------------------------------------------------------------------ #$Date: 2020-04-05 13:34:19 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250250 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557299.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_1557299 loop_ _publ_author_name 'Zhou, Qing' 'Yang, Tianjia' 'Zhong, Zihao' 'Kausar, Fahmeeda' 'Wang, Ziyi' 'Zhang, Yongming' 'Yuan, Wang Zhang' _publ_section_title ; A clustering-triggered emission strategy for tunable multicolor persistent phosphorescence ; _journal_issue 11 _journal_name_full 'Chemical Science' _journal_page_first 2926 _journal_paper_doi 10.1039/C9SC06518K _journal_volume 11 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C5 H12 O4' _chemical_formula_sum 'C5 H12 O4' _chemical_formula_weight 136.15 _space_group_crystal_system tetragonal _space_group_IT_number 82 _space_group_name_Hall 'I -4' _space_group_name_H-M_alt 'I -4' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _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 2 _cell_length_a 6.0826(12) _cell_length_b 6.0826(12) _cell_length_c 8.792(2) _cell_measurement_reflns_used 1577 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 67.62 _cell_measurement_theta_min 8.87 _cell_volume 325.29(12) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _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 0.0423 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1675 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.944 _diffrn_reflns_theta_min 8.865 _exptl_absorpt_coefficient_mu 1.029 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.390 _exptl_crystal_description block _exptl_crystal_F_000 148 _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 0.6324 _refine_diff_density_max 0.115 _refine_diff_density_min -0.112 _refine_diff_density_rms 0.031 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.1(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 24 _refine_ls_number_reflns 304 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0587P)^2^+0.0457P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.0836 _reflns_Friedel_coverage 0.855 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 290 _reflns_number_total 304 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06518k6.cif _cod_data_source_block a_a _cod_depositor_comments 'Adding full bibliography for 1557298--1557301.cif.' _cod_original_cell_volume 325.31(15) _cod_database_code 1557299 _shelx_shelxl_version_number 2016/6 _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 0.790 _shelx_estimated_absorpt_t_max 0.821 _shelx_res_file ; TITL a_a.res in I-4 a_a.res created by SHELXL-2016/6 at 09:50:07 on 30-Sep-2018 REM Old TITL a in I-4 REM SHELXT solution in I-4 REM R1 0.183, Rweak 0.018, Alpha 0.002, Orientation as input REM Flack x = 0.499 ( 0.287 ) from Parsons' quotients REM Formula found by SHELXT: C5 O4 CELL 1.54178 6.0826 6.0826 8.7925 90.000 90.000 90.000 ZERR 2.000 0.0012 0.0012 0.0021 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SFAC C H O UNIT 10 24 8 ACTA size 0.24 0.22 0.20 conf twin TEMP 25.100 L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 20 WGHT 0.058700 0.045700 BASF 0.09210 FVAR 2.94467 O1 3 0.253280 0.817805 0.480552 11.00000 0.02996 0.02853 = 0.09565 0.00042 0.00381 0.00532 AFIX 148 H1 2 0.136920 0.773093 0.497586 11.00000 -1.50000 AFIX 0 C1 1 0.500000 0.500000 0.500000 10.25000 0.02516 0.02516 = 0.03488 0.00000 0.00000 0.00000 C2 1 0.374078 0.658286 0.396596 11.00000 0.03294 0.03564 = 0.04866 0.00603 -0.00265 0.00452 AFIX 23 H2A 2 0.477291 0.732792 0.330144 11.00000 -1.20000 H2B 2 0.273478 0.574971 0.333308 11.00000 -1.20000 AFIX 0 HKLF 4 REM a_a.res in I-4 REM R1 = 0.0297 for 290 Fo > 4sig(Fo) and 0.0354 for all 304 data REM 24 parameters refined using 0 restraints END WGHT 0.0527 0.0490 REM Highest difference peak 0.115, deepest hole -0.112, 1-sigma level 0.031 Q1 1 0.5000 1.0000 0.4604 10.50000 0.05 0.11 Q2 1 0.0000 1.0000 0.4317 10.50000 0.05 0.11 Q3 1 0.1403 0.5152 0.4365 11.00000 0.05 0.09 Q4 1 0.1403 0.6099 0.5778 11.00000 0.05 0.09 Q5 1 0.1794 0.7227 0.2296 11.00000 0.05 0.06 Q6 1 0.5000 1.0000 0.2500 10.25000 0.05 0.06 Q7 1 0.2711 0.3479 0.2559 11.00000 0.05 0.06 Q8 1 0.2967 0.7497 0.5576 11.00000 0.05 0.05 Q9 1 0.2485 0.9522 0.5766 11.00000 0.05 0.05 Q10 1 0.4031 0.8630 0.2407 11.00000 0.05 0.05 Q11 1 0.1430 0.8540 0.6066 11.00000 0.05 0.04 Q12 1 0.1752 0.8037 0.6463 11.00000 0.05 0.04 Q13 1 0.1524 0.8944 0.4195 11.00000 0.05 0.03 Q14 1 0.4141 0.5732 0.4509 11.00000 0.05 0.03 Q15 1 0.4310 0.6412 0.2518 11.00000 0.05 0.03 Q16 1 0.3038 0.5525 0.2000 11.00000 0.05 0.03 Q17 1 0.2819 0.7411 0.4234 11.00000 0.05 0.03 Q18 1 0.3770 0.5222 0.1719 11.00000 0.05 0.03 Q19 1 0.3227 0.7418 0.2526 11.00000 0.05 0.02 Q20 1 0.5243 0.8791 0.1920 11.00000 0.05 0.02 ; _shelx_res_checksum 21594 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+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 _atom_site_refinement_flags_occupancy O1 O 0.2533(2) 0.81780(18) 0.4806(2) 0.0514(6) Uani 1 1 d . . . H1 H 0.137(6) 0.773(3) 0.498(4) 0.077 Uiso 1 1 calc R U . C1 C 0.500000 0.500000 0.500000 0.0284(8) Uani 1 4 d S T P C2 C 0.3741(3) 0.6583(3) 0.3966(2) 0.0391(6) Uani 1 1 d . . . H2A H 0.477291 0.732792 0.330144 0.047 Uiso 1 1 calc R U . H2B H 0.273478 0.574971 0.333308 0.047 Uiso 1 1 calc R U . 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 0.0300(8) 0.0285(8) 0.0956(12) 0.0004(8) 0.0038(7) 0.0053(6) C1 0.0252(10) 0.0252(10) 0.0349(16) 0.000 0.000 0.000 C2 0.0329(10) 0.0356(10) 0.0487(11) 0.0060(7) -0.0027(7) 0.0045(8) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C2 O1 H1 109.5 . . C2 C1 C2 110.68(8) 3_566 2_665 C2 C1 C2 107.07(16) 3_566 4_656 C2 C1 C2 110.68(8) 2_665 4_656 C2 C1 C2 110.68(8) 3_566 . C2 C1 C2 107.07(16) 2_665 . C2 C1 C2 110.68(8) 4_656 . O1 C2 C1 112.29(15) . . O1 C2 H2A 109.1 . . C1 C2 H2A 109.1 . . O1 C2 H2B 109.1 . . C1 C2 H2B 109.1 . . H2A C2 H2B 107.9 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C2 1.423(2) . O1 H1 0.77(4) . C1 C2 1.5298(19) 3_566 C1 C2 1.5298(19) 2_665 C1 C2 1.5298(19) 4_656 C1 C2 1.5298(19) . C2 H2A 0.9700 . C2 H2B 0.9700 . 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 _geom_torsion_site_symmetry_1 C2 C1 C2 O1 -58.01(18) 3_566 C2 C1 C2 O1 -178.74(18) 2_665 C2 C1 C2 O1 60.54(18) 4_656