#------------------------------------------------------------------------------ #$Date: 2025-08-19 15:49:58 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301806 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239070.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_2239070 loop_ _publ_author_name 'Fang, Li' 'Li, Feifei' 'Luo, Xuemei' _publ_section_title ; 1,3,5-Tris(4-methoxyphenyl)-1,3,5-triazinane-2,4,6-trione ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o118 _journal_paper_doi 10.1107/S160053681303482X _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C24 H21 N3 O6' _chemical_formula_moiety 'C24 H21 N3 O6' _chemical_formula_sum 'C24 H21 N3 O6' _chemical_formula_weight 447.44 _chemical_name_systematic ; 1,3,5-Tris(4-methoxyphenyl)-1,3,5-triazinane-2,4,6-trione ; _space_group_IT_number 161 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_space_group_name_H-M 'R 3 c :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 6 _cell_length_a 13.2008(14) _cell_length_b 13.2008(14) _cell_length_c 26.695(3) _cell_measurement_reflns_used 1247 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 20.36 _cell_measurement_theta_min 2.29 _cell_volume 4028.7(8) _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_collection 'SMART (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 6995 _diffrn_reflns_theta_full 25.04 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_min 2.35 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_max 0.9967 _exptl_absorpt_correction_T_min 0.9599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1404 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.160 _refine_diff_density_min -0.116 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1577 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0439 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.1219 _reflns_number_gt 1142 _reflns_number_total 1577 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL s331b_0m in R3c CELL 0.71073 13.2008 13.2008 26.6954 90.000 90.000 120.000 ZERR 6.00 0.0014 0.0014 0.0030 0.000 0.000 0.000 LATT -3 SYMM -y, x-y, z SYMM -x+y, -x, z SYMM -x+y, y, z+1/2 SYMM x, x-y, z+1/2 SYMM -y, -x, z+1/2 SFAC C H N O UNIT 144 126 18 36 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 SIZE 0.51 0.49 .041 WGHT 0.068700 0.000000 FVAR 0.579760 TEMP -73.000 N1 3 0.243174 0.688528 0.063361 11.000000 0.039030 0.040610 = 0.073420 0.003320 0.002860 0.020600 O1 4 0.376279 0.883597 0.061606 11.000000 0.057080 0.048840 = 0.112400 -0.003570 -0.000600 0.030550 O2 4 -0.127513 0.777378 0.062627 11.000000 0.094350 0.157560 = 0.127440 0.023450 0.005620 0.089560 C1 1 0.147039 0.710777 0.065414 11.000000 0.045170 0.045570 = 0.077030 -0.002640 0.001150 0.024230 C2 1 0.086379 0.694231 0.109069 11.000000 0.060780 0.063630 = 0.076200 0.005090 0.007570 0.034960 AFIX 43 H2 2 0.109024 0.670878 0.138706 11.000000 -1.200000 AFIX 0 C3 1 -0.010416 0.712372 0.109441 11.000000 0.059070 0.079880 = 0.089170 0.007500 0.020690 0.033090 AFIX 43 H3 2 -0.056527 0.696978 0.138803 11.000000 -1.200000 AFIX 0 C4 1 -0.036900 0.752451 0.066905 11.000000 0.053800 0.078230 = 0.098320 0.003620 -0.002720 0.042900 C5 1 0.025279 0.770837 0.025136 11.000000 0.071370 0.110580 = 0.093230 0.018680 -0.008420 0.054300 AFIX 43 H5 2 0.004964 0.798278 -0.003934 11.000000 -1.200000 AFIX 0 C6 1 0.116787 0.751374 0.023079 11.000000 0.065370 0.078740 = 0.081330 0.017900 0.003810 0.040970 AFIX 43 H6 2 0.160007 0.765361 -0.007081 11.000000 -1.200000 AFIX 0 C7 1 0.356624 0.783777 0.062249 11.000000 0.046490 0.047160 = 0.075150 -0.002080 0.001170 0.022730 C8 1 -0.206022 0.744610 0.102771 11.000000 0.085220 0.174010 = 0.166060 -0.010660 0.016430 0.088490 AFIX 137 H8A 2 -0.241435 0.660365 0.108690 11.000000 -1.500000 H8B 2 -0.267432 0.763124 0.094792 11.000000 -1.500000 H8C 2 -0.164136 0.787412 0.132922 11.000000 -1.500000 AFIX 0 Q1 1 -0.112600 0.773200 0.118800 11.000000 0.050000 0.16 Q2 1 -0.000500 0.702000 0.147500 11.000000 0.050000 0.12 Q3 1 0.206100 0.770100 0.168700 11.000000 0.050000 0.11 Q4 1 -0.155700 0.819000 0.031900 11.000000 0.050000 0.10 Q5 1 0.083500 0.718900 -0.029600 11.000000 0.050000 0.10 HKLF 4 END ; _cod_data_source_file tk5284sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M ' R 3 c' _cod_database_code 2239070 _cod_database_fobs_code 2239070 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity N N1 0.24317(15) 0.68853(16) 0.06336(8) 0.0507(6) Uani d . 1 1 O O1 0.37628(17) 0.88360(16) 0.06161(9) 0.0710(6) Uani d . 1 1 O O2 -0.1275(2) 0.7774(3) 0.06263(12) 0.1146(9) Uani d . 1 1 C C1 0.1470(2) 0.7108(2) 0.06541(11) 0.0552(7) Uani d . 1 1 C C2 0.0864(2) 0.6942(2) 0.10907(12) 0.0652(7) Uani d . 1 1 H H2 0.1090 0.6709 0.1387 0.078 Uiso calc R 1 1 C C3 -0.0104(3) 0.7124(3) 0.10944(13) 0.0768(9) Uani d . 1 1 H H3 -0.0565 0.6970 0.1388 0.092 Uiso calc R 1 1 C C4 -0.0369(2) 0.7525(3) 0.06691(14) 0.0724(8) Uani d . 1 1 C C5 0.0253(3) 0.7708(3) 0.02514(15) 0.0878(10) Uani d . 1 1 H H5 0.0050 0.7983 -0.0039 0.105 Uiso calc R 1 1 C C6 0.1168(3) 0.7514(3) 0.02308(12) 0.0729(8) Uani d . 1 1 H H6 0.1600 0.7654 -0.0071 0.088 Uiso calc R 1 1 C C7 0.3566(2) 0.7838(2) 0.06225(11) 0.0566(7) Uani d . 1 1 C C8 -0.2060(4) 0.7446(5) 0.1028(2) 0.1312(17) Uani d . 1 1 H H8A -0.2414 0.6604 0.1087 0.197 Uiso calc R 1 1 H H8B -0.2674 0.7631 0.0948 0.197 Uiso calc R 1 1 H H8C -0.1641 0.7874 0.1329 0.197 Uiso calc R 1 1 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 N1 0.0390(12) 0.0406(12) 0.0734(15) 0.0206(10) 0.0029(11) 0.0033(11) O1 0.0571(12) 0.0488(12) 0.1124(15) 0.0306(10) -0.0006(11) -0.0036(10) O2 0.0943(19) 0.158(3) 0.127(2) 0.0896(19) 0.0056(17) 0.0234(18) C1 0.0452(16) 0.0456(15) 0.0770(18) 0.0242(14) 0.0011(15) -0.0026(14) C2 0.0608(17) 0.0636(18) 0.0762(19) 0.0350(14) 0.0076(14) 0.0051(15) C3 0.0591(18) 0.080(2) 0.089(2) 0.0331(16) 0.0207(15) 0.0075(17) C4 0.0538(16) 0.078(2) 0.098(2) 0.0429(16) -0.0027(18) 0.0036(17) C5 0.071(2) 0.111(3) 0.093(3) 0.054(2) -0.008(2) 0.0187(19) C6 0.0654(19) 0.079(2) 0.081(2) 0.0410(16) 0.0038(16) 0.0179(16) C7 0.0465(16) 0.0472(16) 0.0751(19) 0.0227(11) 0.0012(14) -0.0021(14) C8 0.085(3) 0.174(4) 0.166(4) 0.088(3) 0.016(3) -0.011(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C7 N1 C7 2_665 . 124.2(3) C7 N1 C1 2_665 . 117.35(19) C7 N1 C1 . . 118.43(19) C4 O2 C8 . . 117.0(3) C2 C1 C6 . . 119.7(2) C2 C1 N1 . . 120.3(3) C6 C1 N1 . . 120.0(2) C1 C2 C3 . . 119.1(3) C1 C2 H2 . . 120.5 C3 C2 H2 . . 120.5 C4 C3 C2 . . 119.1(3) C4 C3 H3 . . 120.4 C2 C3 H3 . . 120.4 C5 C4 C3 . . 120.7(3) C5 C4 O2 . . 114.3(3) C3 C4 O2 . . 125.0(3) C4 C5 C6 . . 121.7(3) C4 C5 H5 . . 119.2 C6 C5 H5 . . 119.2 C5 C6 C1 . . 119.6(3) C5 C6 H6 . . 120.2 C1 C6 H6 . . 120.2 O1 C7 N1 . 3_565 122.2(2) O1 C7 N1 . . 122.1(2) N1 C7 N1 3_565 . 115.7(3) O2 C8 H8A . . 109.5 O2 C8 H8B . . 109.5 H8A C8 H8B . . 109.5 O2 C8 H8C . . 109.5 H8A C8 H8C . . 109.5 H8B C8 H8C . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 C7 2_665 1.384(3) N1 C7 . 1.393(3) N1 C1 . 1.440(3) O1 C7 . 1.209(3) O2 C4 . 1.395(4) O2 C8 . 1.400(5) C1 C2 . 1.368(4) C1 C6 . 1.392(4) C2 C3 . 1.413(4) C2 H2 . 0.9500 C3 C4 . 1.370(5) C3 H3 . 0.9500 C4 C5 . 1.333(4) C5 C6 . 1.356(4) C5 H5 . 0.9500 C6 H6 . 0.9500 C7 N1 3_565 1.384(3) C8 H8A . 0.9800 C8 H8B . 0.9800 C8 H8C . 0.9800 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 0.006 14 2 ' ' 2 0.000 0.000 0.223 153 39 ' ' 3 0.000 0.000 0.506 14 2 ' ' 4 0.000 0.000 0.723 153 39 ' ' 5 0.333 0.667 0.390 151 39 ' ' 6 0.333 0.667 0.890 151 39 ' ' 7 0.333 0.667 0.172 14 2 ' ' 8 0.333 0.667 0.672 14 2 ' ' 9 0.667 0.333 0.056 151 39 ' ' 10 0.667 0.333 0.556 151 39 ' ' 11 0.666 0.333 0.339 14 2 ' ' 12 0.666 0.333 0.839 14 2 ' ' loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 199633