#------------------------------------------------------------------------------ #$Date: 2016-03-26 17:20:13 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180388 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/57/7205726.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_7205726 loop_ _publ_author_name 'Hou, Ke-Ling' 'Bai, Feng-Ying' 'Xing, Yong-Heng' 'Wang, Jian-Ling' 'Shi, Zhan' _publ_section_title ; A novel family of 3D photoluminescent lanthanide--bta--flexible MOFs constructed from 1,2,4,5-benzenetetracarboxylic acid and different spanning of dicarboxylate acid ligands ; _journal_issue 11 _journal_name_full CrystEngComm _journal_page_first 3884 _journal_paper_doi 10.1039/c0ce00707b _journal_volume 13 _journal_year 2011 _chemical_formula_sum 'C15 H18 Dy2 O17' _chemical_formula_weight 795.29 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _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 113.70(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.805(4) _cell_length_b 7.7577(16) _cell_length_c 14.724(3) _cell_measurement_reflns_used 8505 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.405 _cell_measurement_theta_min 2.995 _cell_volume 1966.8(8) _computing_cell_refinement 'Rgaku R-AXIS RAPID diffractometer Control Software' _computing_data_collection 'Rgaku R-AXIS RAPID diffractometer Control Software' _computing_data_reduction 'Rgaku R-AXIS RAPID diffractometer Control Software' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP' _diffrn_measurement_method '\w 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 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9064 _diffrn_reflns_theta_full 27.40 _diffrn_reflns_theta_max 27.40 _diffrn_reflns_theta_min 3.00 _diffrn_standards_decay_% none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_number none _exptl_absorpt_coefficient_mu 7.634 _exptl_absorpt_correction_T_max 0.5664 _exptl_absorpt_correction_T_min 0.3063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;Higashi, T. (1995). Program for Absorption Correction. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.520 _refine_diff_density_min -1.198 _refine_diff_density_rms 0.112 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2239 _refine_ls_number_restraints 42 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0175 _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^)+(0.0000P)^2^+11.0824P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0382 _reflns_number_gt 2150 _reflns_number_total 2239 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c0ce00707b.txt _cod_data_source_block 1c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_original_cell_volume 1966.7(7) _cod_original_sg_symbol_H-M C2/c _cod_database_code 7205726 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3W O 0.0000 1.0000 0.0000 0.130(3) Uani 1 2 d S . . H2WA H 0.2508(19) 1.279(3) 0.117(3) 0.031(4) Uiso 1 1 d DU . . H1WB H 0.156(2) 1.049(5) 0.2072(16) 0.029(4) Uiso 1 1 d DU . . H1WA H 0.168(2) 1.132(3) 0.133(3) 0.033(4) Uiso 1 1 d DU . . H2WB H 0.3050(14) 1.180(5) 0.098(3) 0.031(4) Uiso 1 1 d DU . . Dy1 Dy 0.246511(7) 0.866296(17) 0.115480(9) 0.01140(5) Uani 1 1 d . . . C1 C 0.57552(16) 1.0172(4) 0.0740(2) 0.0149(6) Uani 1 1 d . . . C2 C 0.43776(16) 0.9620(4) 0.0261(2) 0.0153(6) Uani 1 1 d . . . C3 C 0.51330(16) 0.9803(4) 0.0990(2) 0.0162(6) Uani 1 1 d . . . H3 H 0.5220 0.9674 0.1654 0.019 Uiso 1 1 calc RU . . C5 C 0.37426(17) 0.9272(4) 0.0604(2) 0.0163(6) Uani 1 1 d . . . C6 C 0.36459(16) 0.5289(4) 0.1240(2) 0.0171(6) Uani 1 1 d . . . C7 C 0.42989(17) 0.4143(4) 0.1897(2) 0.0204(6) Uani 1 1 d . . . H7A H 0.4438 0.3333 0.1494 0.024 Uiso 1 1 calc RU . . H7B H 0.4133 0.3492 0.2340 0.024 Uiso 1 1 calc RU . . C8 C 0.5000 0.5256(6) 0.2500 0.0214(9) Uani 1 2 d S . . H8A H 0.5129 0.5991 0.2055 0.026 Uiso 0.50 1 calc PRU . . H8B H 0.4871 0.5991 0.2945 0.026 Uiso 0.50 1 calc PRU . . O1W O 0.15205(13) 1.0392(3) 0.14866(17) 0.0231(5) Uani 1 1 d D . . O2W O 0.26256(17) 1.1841(4) 0.0994(2) 0.0344(6) Uani 1 1 d D . . O3 O 0.38521(13) 0.9493(3) 0.14828(16) 0.0273(5) Uani 1 1 d . . . O4 O 0.30737(11) 0.8778(3) -0.00293(15) 0.0185(4) Uani 1 1 d . . . O6 O 0.32857(12) 0.6169(3) 0.16449(16) 0.0202(5) Uani 1 1 d . . . O5 O 0.35181(13) 0.5353(3) 0.03357(16) 0.0259(5) Uani 1 1 d . . . C4 C 0.65387(15) 1.0409(4) 0.1607(2) 0.0135(6) Uani 1 1 d . . . O1 O 0.67932(12) 1.1923(3) 0.18184(16) 0.0191(4) Uani 1 1 d . . . O2 O 0.68527(12) 0.9105(3) 0.21095(16) 0.0198(4) 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 O3W 0.036(3) 0.246(11) 0.101(6) -0.031(6) 0.021(3) 0.006(5) Dy1 0.00923(7) 0.01641(8) 0.00874(7) -0.00022(5) 0.00379(5) -0.00119(5) C1 0.0099(12) 0.0188(14) 0.0150(14) 0.0005(11) 0.0040(11) -0.0013(11) C2 0.0117(13) 0.0201(15) 0.0149(14) 0.0012(11) 0.0063(11) -0.0026(11) C3 0.0119(13) 0.0253(16) 0.0119(13) 0.0016(11) 0.0051(11) -0.0034(12) C5 0.0136(13) 0.0210(15) 0.0148(14) 0.0012(11) 0.0064(11) -0.0025(12) C6 0.0119(13) 0.0238(16) 0.0147(14) -0.0011(11) 0.0044(11) -0.0038(12) C7 0.0154(14) 0.0217(15) 0.0205(16) -0.0015(12) 0.0034(12) 0.0001(12) C8 0.0133(19) 0.025(2) 0.021(2) 0.000 0.0017(17) 0.000 O1W 0.0251(12) 0.0295(13) 0.0182(11) -0.0019(9) 0.0123(10) 0.0029(10) O2W 0.0441(16) 0.0255(13) 0.0389(16) -0.0003(11) 0.0223(14) -0.0030(12) O3 0.0183(11) 0.0509(16) 0.0148(11) -0.0038(10) 0.0088(9) -0.0122(11) O4 0.0103(9) 0.0308(12) 0.0145(10) -0.0032(9) 0.0049(8) -0.0052(9) O6 0.0172(10) 0.0283(12) 0.0147(11) 0.0022(9) 0.0061(9) 0.0051(9) O5 0.0215(11) 0.0412(14) 0.0136(11) 0.0003(9) 0.0055(9) 0.0082(10) C4 0.0073(12) 0.0238(15) 0.0117(13) 0.0020(11) 0.0063(10) -0.0011(11) O1 0.0177(10) 0.0221(11) 0.0179(11) -0.0031(8) 0.0076(9) -0.0072(9) O2 0.0175(10) 0.0247(11) 0.0147(10) 0.0048(9) 0.0037(8) 0.0032(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 _geom_angle_publ_flag O1 Dy1 O5 103.00(8) 3_445 7_565 ? O1 Dy1 O2 77.35(8) 3_445 2_655 ? O5 Dy1 O2 146.72(8) 7_565 2_655 ? O1 Dy1 O6 78.29(8) 3_445 . ? O5 Dy1 O6 135.29(8) 7_565 . ? O2 Dy1 O6 77.83(8) 2_655 . ? O1 Dy1 O1W 70.72(8) 3_445 . ? O5 Dy1 O1W 69.19(8) 7_565 . ? O2 Dy1 O1W 80.00(8) 2_655 . ? O6 Dy1 O1W 145.08(8) . . ? O1 Dy1 O4 144.51(8) 3_445 . ? O5 Dy1 O4 74.97(8) 7_565 . ? O2 Dy1 O4 123.82(7) 2_655 . ? O6 Dy1 O4 79.32(7) . . ? O1W Dy1 O4 135.61(8) . . ? O1 Dy1 O4 71.80(7) 3_445 7_565 ? O5 Dy1 O4 70.40(8) 7_565 7_565 ? O2 Dy1 O4 137.35(8) 2_655 7_565 ? O6 Dy1 O4 67.75(8) . 7_565 ? O1W Dy1 O4 115.21(8) . 7_565 ? O4 Dy1 O4 74.37(8) . 7_565 ? O1 Dy1 O2W 136.04(9) 3_445 . ? O5 Dy1 O2W 70.89(9) 7_565 . ? O2 Dy1 O2W 85.76(9) 2_655 . ? O6 Dy1 O2W 137.28(9) . . ? O1W Dy1 O2W 66.48(9) . . ? O4 Dy1 O2W 77.75(8) . . ? O4 Dy1 O2W 136.78(8) 7_565 . ? O1 Dy1 O3 139.54(8) 3_445 . ? O5 Dy1 O3 117.17(8) 7_565 . ? O2 Dy1 O3 71.93(8) 2_655 . ? O6 Dy1 O3 70.09(8) . . ? O1W Dy1 O3 126.94(8) . . ? O4 Dy1 O3 52.09(7) . . ? O4 Dy1 O3 116.01(8) 7_565 . ? O2W Dy1 O3 67.35(9) . . ? O1 Dy1 C5 151.22(8) 3_445 . ? O5 Dy1 C5 96.66(8) 7_565 . ? O2 Dy1 C5 97.40(8) 2_655 . ? O6 Dy1 C5 72.96(8) . . ? O1W Dy1 C5 136.90(9) . . ? O4 Dy1 C5 26.53(8) . . ? O4 Dy1 C5 95.83(8) 7_565 . ? O2W Dy1 C5 70.42(9) . . ? O3 Dy1 C5 25.56(8) . . ? O1 Dy1 Dy1 108.27(6) 3_445 7_565 ? O5 Dy1 Dy1 68.08(6) 7_565 7_565 ? O2 Dy1 Dy1 144.21(5) 2_655 7_565 ? O6 Dy1 Dy1 69.25(5) . 7_565 ? O1W Dy1 Dy1 135.68(6) . 7_565 ? O4 Dy1 Dy1 37.27(5) . 7_565 ? O4 Dy1 Dy1 37.10(5) 7_565 7_565 ? O2W Dy1 Dy1 108.99(7) . 7_565 ? O3 Dy1 Dy1 83.74(6) . 7_565 ? C5 Dy1 Dy1 60.23(6) . 7_565 ? C3 C1 C2 119.3(3) . 5_675 ? C3 C1 C4 115.9(2) . . ? C2 C1 C4 124.8(3) 5_675 . ? C3 C2 C1 119.4(3) . 5_675 ? C3 C2 C5 117.5(3) . . ? C1 C2 C5 123.1(3) 5_675 . ? C1 C3 C2 121.4(3) . . ? O3 C5 O4 120.1(3) . . ? O3 C5 C2 120.5(3) . . ? O4 C5 C2 119.3(3) . . ? O3 C5 Dy1 62.17(16) . . ? O4 C5 Dy1 57.97(14) . . ? C2 C5 Dy1 176.8(2) . . ? O5 C6 O6 124.6(3) . . ? O5 C6 C7 117.6(3) . . ? O6 C6 C7 117.8(3) . . ? C6 C7 C8 109.2(3) . . ? C7 C8 C7 111.1(4) 2_655 . ? C5 O3 Dy1 92.27(18) . . ? C5 O4 Dy1 95.50(17) . . ? C5 O4 Dy1 137.55(19) . 7_565 ? Dy1 O4 Dy1 105.63(8) . 7_565 ? C6 O6 Dy1 134.0(2) . . ? C6 O5 Dy1 138.1(2) . 7_565 ? O2 C4 O1 124.4(3) . . ? O2 C4 C1 117.7(3) . . ? O1 C4 C1 117.6(3) . . ? C4 O1 Dy1 131.06(19) . 3 ? C4 O2 Dy1 132.4(2) . 2_655 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.316(2) 3_445 ? Dy1 O5 2.357(2) 7_565 ? Dy1 O2 2.379(2) 2_655 ? Dy1 O6 2.398(2) . ? Dy1 O1W 2.427(2) . ? Dy1 O4 2.442(2) . ? Dy1 O4 2.451(2) 7_565 ? Dy1 O2W 2.506(3) . ? Dy1 O3 2.537(2) . ? Dy1 C5 2.867(3) . ? Dy1 Dy1 3.8981(7) 7_565 ? C1 C3 1.390(4) . ? C1 C2 1.403(4) 5_675 ? C1 C4 1.524(4) . ? C2 C3 1.401(4) . ? C2 C1 1.403(4) 5_675 ? C2 C5 1.496(4) . ? C5 O3 1.238(4) . ? C5 O4 1.286(4) . ? C6 O5 1.255(4) . ? C6 O6 1.267(4) . ? C6 C7 1.510(4) . ? C7 C8 1.527(4) . ? C8 C7 1.527(4) 2_655 ? O4 Dy1 2.451(2) 7_565 ? O5 Dy1 2.357(2) 7_565 ? C4 O2 1.252(4) . ? C4 O1 1.259(4) . ? O1 Dy1 2.317(2) 3 ? O2 Dy1 2.379(2) 2_655 ?