#------------------------------------------------------------------------------ #$Date: 2020-04-05 13:55:39 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250314 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/29/7702941.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_7702941 loop_ _publ_author_name 'Hou, Xiaomin' 'Yan, Chong-Chong' 'Xu, Xiuling' 'Liang, Ai-Qin' 'Song, Zu-Wei' 'Tang, Si-Fu' _publ_section_title ; Two-dimensional layered lanthanide diphosphonates: synthesis, structures and sensing properties toward Fe3+ and Cr2O72. ; _journal_issue 12 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 3809 _journal_page_last 3815 _journal_paper_doi 10.1039/c9dt03531a _journal_volume 49 _journal_year 2020 _chemical_formula_sum 'C9 H15 Eu O8 P2' _chemical_formula_weight 465.11 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2019-08-16 deposited with the CCDC. 2019-12-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.3360(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.2586(6) _cell_length_b 8.3554(4) _cell_length_c 13.4007(6) _cell_measurement_reflns_used 21835 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.000 _cell_measurement_theta_min 3.344 _cell_volume 1364.19(11) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 17597 _diffrn_reflns_point_group_measured_fraction_full 0.970 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.344 _exptl_absorpt_coefficient_mu 4.865 _exptl_absorpt_correction_T_max 0.839 _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.265 _exptl_crystal_description block _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.036 _refine_diff_density_max 2.120 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.112 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2387 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0216 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+2.2575P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.0541 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2086 _reflns_number_total 2387 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt03531a2.cif _cod_data_source_block 1_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7702940--7702943.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7702941 _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. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL 1 in P2(1)/c CELL 0.71073 12.2586 8.3554 13.4007 90.000 96.336 90.000 ZERR 4.00 0.0006 0.0004 0.0006 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O P EU UNIT 36 60 32 8 4 L.S. 10 BOND acta omit -3 50 OMIT 0 1 1 OMIT 4 0 0 OMIT -1 2 4 OMIT -1 3 1 OMIT -2 1 2 FMAP 2 PLAN 10 WGHT 0.024300 2.257500 FVAR 0.10698 EU1 5 0.480747 0.255519 0.088699 11.00000 0.01923 0.01123 = 0.00806 -0.00028 0.00108 0.00212 P1 4 0.384139 0.397416 0.325644 11.00000 0.01858 0.01103 = 0.00742 -0.00029 0.00211 -0.00053 P2 4 0.309092 -0.131634 0.548339 11.00000 0.02131 0.01453 = 0.01175 -0.00022 0.00215 -0.00328 O1 3 0.429986 0.336552 0.428140 11.00000 0.02627 0.03442 = 0.00974 0.00573 0.00133 0.00241 O1W 3 0.338072 0.050145 0.094092 11.00000 0.03672 0.02414 = 0.01496 -0.00106 0.00333 -0.00737 AFIX 3 H1W 2 0.340802 0.006535 0.151622 11.00000 -1.20000 H2W 2 0.336722 -0.031795 0.056382 11.00000 -1.20000 AFIX 0 O2 3 0.424460 0.568311 0.306738 11.00000 0.02766 0.01292 = 0.01409 -0.00065 -0.00043 -0.00575 O2W 3 0.598079 0.464412 0.179425 11.00000 0.03182 0.02231 = 0.02510 -0.00826 0.01318 -0.00297 AFIX 3 H3W 2 0.559049 0.535622 0.203635 11.00000 -1.20000 H4W 2 0.640359 0.506572 0.140625 11.00000 -1.20000 AFIX 0 O3 3 0.407519 0.285945 0.241424 11.00000 0.03147 0.01802 = 0.01533 -0.00449 0.00722 -0.00282 O4 3 0.346186 -0.257178 0.478930 11.00000 0.02616 0.02098 = 0.01784 -0.00277 0.00374 0.00288 O5 3 0.377729 0.017150 0.550218 11.00000 0.03441 0.02303 = 0.02273 0.00302 -0.00318 -0.01415 O6 3 0.306718 -0.205546 0.655109 11.00000 0.03698 0.02215 = 0.01370 0.00028 0.00226 -0.00815 AFIX 83 H6B 2 0.346324 -0.152971 0.696163 11.00000 -1.50000 AFIX 0 C1 1 0.105353 0.021023 0.233522 11.00000 0.01861 0.03307 = 0.02921 -0.00613 0.00138 -0.00291 C2 1 0.111746 -0.062507 0.323382 11.00000 0.02461 0.02191 = 0.04043 -0.00037 0.00450 -0.00511 AFIX 43 H2A 2 0.088935 -0.168673 0.323164 11.00000 -1.20000 AFIX 0 C3 1 0.151500 0.008992 0.413749 11.00000 0.01597 0.02424 = 0.02715 0.00428 0.00459 0.00114 C4 1 0.185551 0.167928 0.412941 11.00000 0.02145 0.02250 = 0.01983 0.00087 0.00223 0.00066 AFIX 43 H4A 2 0.209622 0.218359 0.473239 11.00000 -1.20000 AFIX 0 C5 1 0.184138 0.252505 0.323362 11.00000 0.01485 0.01965 = 0.02671 0.00268 0.00408 0.00269 C6 1 0.143182 0.177923 0.234739 11.00000 0.02091 0.03237 = 0.02086 0.00424 0.00138 -0.00081 AFIX 43 H6A 2 0.140946 0.234144 0.174652 11.00000 -1.20000 AFIX 0 C7 1 0.061682 -0.054631 0.135545 11.00000 0.03820 0.05015 = 0.03438 -0.01429 0.00061 -0.01170 AFIX 33 H7A 2 0.065992 0.020711 0.082037 11.00000 -1.50000 H7B 2 -0.013427 -0.085393 0.138012 11.00000 -1.50000 H7C 2 0.104561 -0.147579 0.123950 11.00000 -1.50000 AFIX 0 C8 1 0.166591 -0.083831 0.510097 11.00000 0.02335 0.02028 = 0.03453 0.00546 0.00868 0.00115 AFIX 23 H8A 2 0.124677 -0.182326 0.501881 11.00000 -1.20000 H8B 2 0.137988 -0.021763 0.562577 11.00000 -1.20000 AFIX 0 C9 1 0.236106 0.415381 0.322764 11.00000 0.02023 0.01586 = 0.02386 0.00263 0.00281 0.00343 AFIX 23 H9A 2 0.218561 0.475766 0.380721 11.00000 -1.20000 H9B 2 0.206891 0.472910 0.262830 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0216 for 2086 Fo > 4sig(Fo) and 0.0270 for all 2387 data REM 181 parameters refined using 0 restraints END WGHT 0.0243 2.2581 REM Highest difference peak 2.120, deepest hole -0.468, 1-sigma level 0.112 Q1 1 0.5243 0.2455 0.4126 11.00000 0.05 2.12 Q2 1 0.2979 0.1290 0.5439 11.00000 0.05 0.51 Q3 1 0.3865 0.6125 0.3317 11.00000 0.05 0.48 Q4 1 -0.0182 -0.0002 0.1019 11.00000 0.05 0.44 Q5 1 0.4279 0.2531 0.2601 11.00000 0.05 0.44 Q6 1 0.3814 0.3766 0.4638 11.00000 0.05 0.40 Q7 1 0.4043 0.4811 0.3108 11.00000 0.05 0.39 Q8 1 0.0305 -0.1710 0.1515 11.00000 0.05 0.38 Q9 1 0.4323 -0.0172 0.5426 11.00000 0.05 0.37 Q10 1 0.2370 -0.1194 0.5277 11.00000 0.05 0.36 ; _shelx_res_checksum 84753 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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 Eu1 Eu 0.48075(2) 0.25552(2) 0.08870(2) 0.01287(8) Uani 1 1 d . . P1 P 0.38414(7) 0.39742(10) 0.32564(6) 0.01229(19) Uani 1 1 d . . P2 P 0.30909(8) -0.13163(11) 0.54834(7) 0.0158(2) Uani 1 1 d . . O1 O 0.4300(2) 0.3366(3) 0.42814(17) 0.0235(6) Uani 1 1 d . . O1W O 0.3381(2) 0.0501(3) 0.09409(19) 0.0252(6) Uani 1 1 d . . H1W H 0.3408 0.0065 0.1516 0.030 Uiso 1 1 d R U H2W H 0.3367 -0.0318 0.0564 0.030 Uiso 1 1 d R U O2 O 0.4245(2) 0.5683(3) 0.30674(18) 0.0184(5) Uani 1 1 d . . O2W O 0.5981(2) 0.4644(3) 0.17943(19) 0.0257(6) Uani 1 1 d . . H3W H 0.5590 0.5356 0.2036 0.031 Uiso 1 1 d R U H4W H 0.6404 0.5066 0.1406 0.031 Uiso 1 1 d R U O3 O 0.4075(2) 0.2859(3) 0.24142(19) 0.0213(6) Uani 1 1 d . . O4 O 0.3462(2) -0.2572(3) 0.4789(2) 0.0216(6) Uani 1 1 d . . O5 O 0.3777(2) 0.0171(3) 0.55022(19) 0.0272(6) Uani 1 1 d . . O6 O 0.3067(2) -0.2055(3) 0.65511(19) 0.0243(6) Uani 1 1 d . . H6B H 0.3463 -0.1530 0.6962 0.036 Uiso 1 1 calc R U C1 C 0.1054(3) 0.0210(5) 0.2335(3) 0.0271(9) Uani 1 1 d . . C2 C 0.1117(3) -0.0625(5) 0.3234(3) 0.0289(10) Uani 1 1 d . . H2A H 0.0889 -0.1687 0.3232 0.035 Uiso 1 1 calc R U C3 C 0.1515(3) 0.0090(4) 0.4137(3) 0.0223(8) Uani 1 1 d . . C4 C 0.1856(3) 0.1679(4) 0.4129(3) 0.0213(8) Uani 1 1 d . . H4A H 0.2096 0.2184 0.4732 0.026 Uiso 1 1 calc R U C5 C 0.1841(3) 0.2525(4) 0.3234(3) 0.0203(8) Uani 1 1 d . . C6 C 0.1432(3) 0.1779(5) 0.2347(3) 0.0248(9) Uani 1 1 d . . H6A H 0.1409 0.2341 0.1747 0.030 Uiso 1 1 calc R U C7 C 0.0617(4) -0.0546(6) 0.1355(3) 0.0412(12) Uani 1 1 d . . H7A H 0.0660 0.0207 0.0820 0.062 Uiso 1 1 calc R U H7B H -0.0134 -0.0854 0.1380 0.062 Uiso 1 1 calc R U H7C H 0.1046 -0.1476 0.1240 0.062 Uiso 1 1 calc R U C8 C 0.1666(3) -0.0838(5) 0.5101(3) 0.0256(9) Uani 1 1 d . . H8A H 0.1247 -0.1823 0.5019 0.031 Uiso 1 1 calc R U H8B H 0.1380 -0.0218 0.5626 0.031 Uiso 1 1 calc R U C9 C 0.2361(3) 0.4154(4) 0.3228(3) 0.0200(8) Uani 1 1 d . . H9A H 0.2186 0.4758 0.3807 0.024 Uiso 1 1 calc R U H9B H 0.2069 0.4729 0.2628 0.024 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 Eu1 0.01923(12) 0.01123(11) 0.00806(12) -0.00028(6) 0.00108(8) 0.00212(7) P1 0.0186(5) 0.0110(4) 0.0074(4) -0.0003(3) 0.0021(4) -0.0005(4) P2 0.0213(5) 0.0145(5) 0.0117(5) -0.0002(4) 0.0021(4) -0.0033(4) O1 0.0263(14) 0.0344(16) 0.0097(13) 0.0057(11) 0.0013(11) 0.0024(12) O1W 0.0367(16) 0.0241(14) 0.0150(13) -0.0011(11) 0.0033(12) -0.0074(12) O2 0.0277(14) 0.0129(12) 0.0141(13) -0.0006(10) -0.0004(11) -0.0057(10) O2W 0.0318(16) 0.0223(14) 0.0251(15) -0.0083(12) 0.0132(12) -0.0030(12) O3 0.0315(15) 0.0180(13) 0.0153(14) -0.0045(10) 0.0072(12) -0.0028(11) O4 0.0262(15) 0.0210(14) 0.0178(14) -0.0028(10) 0.0037(12) 0.0029(10) O5 0.0344(16) 0.0230(14) 0.0227(14) 0.0030(12) -0.0032(12) -0.0142(12) O6 0.0370(16) 0.0222(14) 0.0137(14) 0.0003(11) 0.0023(12) -0.0082(12) C1 0.019(2) 0.033(2) 0.029(2) -0.0061(18) 0.0014(17) -0.0029(17) C2 0.025(2) 0.022(2) 0.040(3) -0.0004(18) 0.0045(19) -0.0051(17) C3 0.0160(19) 0.024(2) 0.027(2) 0.0043(17) 0.0046(16) 0.0011(15) C4 0.021(2) 0.022(2) 0.020(2) 0.0009(16) 0.0022(16) 0.0007(16) C5 0.0149(19) 0.020(2) 0.027(2) 0.0027(15) 0.0041(17) 0.0027(15) C6 0.021(2) 0.032(2) 0.021(2) 0.0042(18) 0.0014(17) -0.0008(18) C7 0.038(3) 0.050(3) 0.034(3) -0.014(2) 0.001(2) -0.012(2) C8 0.023(2) 0.020(2) 0.035(2) 0.0055(17) 0.0087(18) 0.0011(16) C9 0.0202(19) 0.0159(18) 0.024(2) 0.0026(15) 0.0028(16) 0.0034(15) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 O1 Eu1 O5 88.93(9) 4_565 4_565 O1 Eu1 O2 113.81(9) 4_565 2_645 O5 Eu1 O2 156.02(9) 4_565 2_645 O1 Eu1 O3 139.76(9) 4_565 . O5 Eu1 O3 81.52(9) 4_565 . O2 Eu1 O3 76.12(9) 2_645 . O1 Eu1 O4 77.97(9) 4_565 2_655 O5 Eu1 O4 115.90(9) 4_565 2_655 O2 Eu1 O4 78.10(9) 2_645 2_655 O3 Eu1 O4 140.93(9) . 2_655 O1 Eu1 O1W 71.01(9) 4_565 . O5 Eu1 O1W 101.99(9) 4_565 . O2 Eu1 O1W 79.77(9) 2_645 . O3 Eu1 O1W 72.95(9) . . O4 Eu1 O1W 129.95(8) 2_655 . O1 Eu1 O2W 140.46(9) 4_565 . O5 Eu1 O2W 78.73(9) 4_565 . O2 Eu1 O2W 87.36(9) 2_645 . O3 Eu1 O2W 75.72(9) . . O4 Eu1 O2W 74.24(8) 2_655 . O1W Eu1 O2W 148.15(8) . . O1 Eu1 P2 74.65(7) 4_565 2_655 O5 Eu1 P2 94.49(7) 4_565 2_655 O2 Eu1 P2 98.72(6) 2_645 2_655 O3 Eu1 P2 144.72(6) . 2_655 O4 Eu1 P2 21.46(6) 2_655 2_655 O1W Eu1 P2 141.35(6) . 2_655 O2W Eu1 P2 69.15(6) . 2_655 O1 Eu1 P1 95.10(7) 4_565 2_645 O5 Eu1 P1 172.17(7) 4_565 2_645 O2 Eu1 P1 18.75(6) 2_645 2_645 O3 Eu1 P1 91.10(6) . 2_645 O4 Eu1 P1 71.60(6) 2_655 2_645 O1W Eu1 P1 73.14(6) . 2_645 O2W Eu1 P1 102.07(6) . 2_645 P2 Eu1 P1 93.05(2) 2_655 2_645 O1 P1 O3 112.81(15) . . O1 P1 O2 111.52(15) . . O3 P1 O2 110.90(14) . . O1 P1 C9 108.48(16) . . O3 P1 C9 107.79(17) . . O2 P1 C9 104.93(15) . . O1 P1 Eu1 82.90(11) . 2_655 O3 P1 Eu1 129.75(11) . 2_655 O2 P1 Eu1 28.99(9) . 2_655 C9 P1 Eu1 111.51(12) . 2_655 O5 P2 O4 112.39(16) . . O5 P2 O6 112.31(15) . . O4 P2 O6 109.15(15) . . O5 P2 C8 110.12(17) . . O4 P2 C8 109.07(18) . . O6 P2 C8 103.40(17) . . O5 P2 Eu1 77.60(11) . 2_645 O4 P2 Eu1 35.68(11) . 2_645 O6 P2 Eu1 117.99(11) . 2_645 C8 P2 Eu1 131.49(13) . 2_645 P1 O1 Eu1 173.84(16) . 4_566 P1 O2 Eu1 132.27(14) . 2_655 P1 O3 Eu1 147.31(15) . . P2 O4 Eu1 122.86(14) . 2_645 P2 O5 Eu1 168.02(17) . 4_566 C2 C1 C6 118.5(4) . . C2 C1 C7 121.9(4) . . C6 C1 C7 119.6(4) . . C1 C2 C3 121.4(4) . . C2 C3 C4 118.7(4) . . C2 C3 C8 121.7(4) . . C4 C3 C8 119.4(3) . . C5 C4 C3 121.1(4) . . C6 C5 C4 118.7(3) . . C6 C5 C9 121.1(4) . . C4 C5 C9 120.0(4) . . C5 C6 C1 121.5(4) . . C3 C8 P2 112.4(3) . . C5 C9 P1 110.4(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Eu1 O1 2.305(2) 4_565 Eu1 O5 2.308(2) 4_565 Eu1 O2 2.324(2) 2_645 Eu1 O3 2.338(2) . Eu1 O4 2.400(3) 2_655 Eu1 O1W 2.457(2) . Eu1 O2W 2.491(2) . Eu1 P2 3.4559(9) 2_655 Eu1 P1 3.5488(9) 2_645 P1 O1 1.513(2) . P1 O3 1.515(3) . P1 O2 1.541(2) . P1 C9 1.817(4) . P1 Eu1 3.5488(9) 2_655 P2 O5 1.500(3) . P2 O4 1.505(3) . P2 O6 1.562(3) . P2 C8 1.810(4) . P2 Eu1 3.4559(9) 2_645 O1 Eu1 2.305(2) 4_566 O2 Eu1 2.324(2) 2_655 O4 Eu1 2.400(3) 2_645 O5 Eu1 2.308(2) 4_566 C1 C2 1.387(6) . C1 C6 1.390(6) . C1 C7 1.502(6) . C2 C3 1.389(6) . C3 C4 1.392(5) . C3 C8 1.500(5) . C4 C5 1.391(5) . C5 C6 1.385(6) . C5 C9 1.503(5) .