#------------------------------------------------------------------------------ #$Date: 2019-12-03 05:00:05 +0200 (Tue, 03 Dec 2019) $ #$Revision: 244875 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/29/7702942.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_7702942 loop_ _publ_author_name 'Hou, Xiaomin' 'Yan, Chong-Chong' 'Xu, Xiu ling' 'Liang, Ai-Qin' 'Song, Zuwei' 'Tang, Sifu' _publ_section_title ; Two-dimensional Layered Lanthanide Diphosphonates: Synthesis, Structures and Sensing Properties toward Fe3+ and Cr2O72- ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT03531A _journal_year 2019 _chemical_formula_sum 'C9 H15 Er O8 P2' _chemical_formula_weight 480.41 _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 95.3350(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.2733(5) _cell_length_b 8.2942(3) _cell_length_c 13.2498(5) _cell_measurement_reflns_used 14171 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.996 _cell_measurement_theta_min 2.901 _cell_volume 1342.95(9) _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 0.973 _diffrn_measured_fraction_theta_max 0.998 _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 0.0446 _diffrn_reflns_av_unetI/netI 0.0294 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.998 _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 17103 _diffrn_reflns_point_group_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_min 2.901 _exptl_absorpt_coefficient_mu 6.521 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.376 _exptl_crystal_description block _exptl_crystal_F_000 924 _exptl_crystal_size_max 0.205 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.041 _refine_diff_density_max 2.337 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.149 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 182 _refine_ls_number_reflns 2362 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0269 _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^)+(0.0364P)^2^+2.9506P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.0675 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1838 _reflns_number_total 2362 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt03531a2.cif _cod_data_source_block 1_CCDC2 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7702942 _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 12.2733 8.2942 13.2498 90.000 95.335 90.000 ZERR 4.00 0.0005 0.0003 0.0005 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O P Er UNIT 36 60 32 8 4 L.S. 4 BOND OMIT -3 50 OMIT 0 6 6 OMIT -1 7 4 acta FMAP 2 PLAN 10 WGHT 0.036400 2.950600 FVAR 0.10395 0.10698 ER1 5 0.478448 0.253715 0.091276 11.00000 0.02000 0.00911 = 0.00636 0.00006 0.00131 0.00166 P1 4 0.386020 0.396069 0.329642 11.00000 0.02036 0.00899 = 0.00576 -0.00012 0.00218 -0.00126 P2 4 0.312893 -0.128383 0.550176 11.00000 0.02192 0.01188 = 0.01023 -0.00074 0.00195 -0.00291 O1 3 0.430055 0.332523 0.432360 11.00000 0.02540 0.02931 = 0.00773 0.00627 0.00080 -0.00067 O1W 3 0.340214 0.051431 0.097213 11.00000 0.03865 0.02185 = 0.01285 0.00048 0.00431 -0.01129 AFIX 3 H1W 2 0.342944 0.007821 0.154743 11.00000 -1.20000 H2W 2 0.338864 -0.030509 0.059503 11.00000 -1.20000 AFIX 0 O2 3 0.428087 0.567753 0.310654 11.00000 0.02809 0.01186 = 0.01104 -0.00096 -0.00095 -0.00256 O2W 3 0.591374 0.461296 0.175754 11.00000 0.03116 0.02166 = 0.02446 -0.00827 0.01473 -0.00313 AFIX 3 H3W 2 0.552344 0.532506 0.199964 11.00000 -1.20000 H4W 2 0.633654 0.503456 0.136954 11.00000 -1.20000 AFIX 0 O3 3 0.409950 0.283665 0.244036 11.00000 0.03097 0.01188 = 0.01065 -0.00225 0.00743 -0.00008 O4 3 0.355414 -0.251266 0.479540 11.00000 0.02867 0.02048 = 0.01307 -0.00435 0.00318 0.00158 O5 3 0.375691 0.026748 0.553342 11.00000 0.03719 0.01637 = 0.01808 0.00151 -0.00365 -0.00846 O6 3 0.310723 -0.205578 0.658102 11.00000 0.04081 0.01679 = 0.01382 0.00039 0.00199 -0.00644 AFIX 83 H6B 2 0.350224 -0.153373 0.699384 11.00000 -1.50000 AFIX 0 C1 1 0.105433 0.024293 0.235310 11.00000 0.01803 0.02882 = 0.03010 -0.00825 0.00027 -0.00501 C2 1 0.113010 -0.062945 0.324890 11.00000 0.02083 0.01904 = 0.03504 -0.00024 0.00287 -0.00808 AFIX 43 H2A 2 0.090564 -0.170077 0.323731 11.00000 -1.20000 AFIX 0 C3 1 0.153175 0.005638 0.415944 11.00000 0.01361 0.02038 = 0.02456 0.00235 0.00317 -0.00117 C4 1 0.186571 0.167395 0.415847 11.00000 0.02035 0.02134 = 0.01779 0.00224 0.00182 0.00107 AFIX 43 H4A 2 0.210597 0.216589 0.476970 11.00000 -1.20000 AFIX 0 C5 1 0.184642 0.255169 0.327398 11.00000 0.01621 0.01836 = 0.02057 0.00234 -0.00074 0.00246 C6 1 0.144274 0.181902 0.237364 11.00000 0.02037 0.02682 = 0.02129 0.00441 0.00305 0.00243 AFIX 43 H6A 2 0.143182 0.239522 0.177066 11.00000 -1.20000 AFIX 0 C7 1 0.060396 -0.050147 0.136398 11.00000 0.03850 0.04963 = 0.03121 -0.01596 0.00533 -0.01050 AFIX 33 H7A 2 0.064915 0.026369 0.082584 11.00000 -1.50000 H7B 2 -0.014664 -0.079908 0.140430 11.00000 -1.50000 H7C 2 0.102237 -0.144336 0.123150 11.00000 -1.50000 AFIX 0 C8 1 0.169656 -0.090096 0.512374 11.00000 0.02673 0.02092 = 0.02489 0.00369 0.00758 -0.00187 AFIX 23 H8A 2 0.131398 -0.192119 0.503103 11.00000 -1.20000 H8B 2 0.138120 -0.031705 0.566028 11.00000 -1.20000 AFIX 0 C9 1 0.238703 0.417332 0.326548 11.00000 0.02368 0.01610 = 0.01532 0.00456 0.00292 0.00335 AFIX 23 H9A 2 0.220699 0.479110 0.384900 11.00000 -1.20000 H9B 2 0.211416 0.475587 0.265920 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0269 for 1838 Fo > 4sig(Fo) and 0.0406 for all 2362 data REM 182 parameters refined using 0 restraints END WGHT 0.0366 2.9034 REM Highest difference peak 2.337, deepest hole -0.657, 1-sigma level 0.149 Q1 1 0.5621 0.2529 0.1012 11.00000 0.05 2.34 Q2 1 0.3999 0.2522 0.0782 11.00000 0.05 2.13 Q3 1 0.5203 0.2430 0.4030 11.00000 0.05 1.10 Q4 1 0.3619 -0.2421 0.3923 11.00000 0.05 0.72 Q5 1 0.3122 0.3925 0.3221 11.00000 0.05 0.67 Q6 1 0.3211 0.2516 0.0688 11.00000 0.05 0.67 Q7 1 0.1224 -0.0324 0.0846 11.00000 0.05 0.57 Q8 1 0.2297 -0.1188 0.5383 11.00000 0.05 0.53 Q9 1 0.3747 0.2837 0.4384 11.00000 0.05 0.51 Q10 1 0.3999 0.1078 0.0816 11.00000 0.05 0.46 ; _shelx_res_checksum 71236 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 Er1 Er 0.47845(2) 0.25371(3) 0.09128(2) 0.01182(10) Uani 1 1 d . . P1 P 0.38602(11) 0.39607(15) 0.32964(9) 0.0116(3) Uani 1 1 d . . P2 P 0.31289(12) -0.12838(16) 0.55018(10) 0.0146(3) Uani 1 1 d . . O1 O 0.4301(3) 0.3325(5) 0.4324(3) 0.0209(9) Uani 1 1 d . . O1W O 0.3402(3) 0.0514(4) 0.0972(3) 0.0243(9) Uani 1 1 d . . H1W H 0.3429 0.0078 0.1547 0.029 Uiso 1 1 d R U H2W H 0.3389 -0.0305 0.0595 0.029 Uiso 1 1 d R U O2 O 0.4281(3) 0.5678(4) 0.3107(3) 0.0172(8) Uani 1 1 d . . O2W O 0.5914(3) 0.4613(4) 0.1758(3) 0.0250(9) Uani 1 1 d . . H3W H 0.5523 0.5325 0.2000 0.030 Uiso 1 1 d R U H4W H 0.6337 0.5035 0.1370 0.030 Uiso 1 1 d R U O3 O 0.4100(3) 0.2837(4) 0.2440(3) 0.0175(8) Uani 1 1 d . . O4 O 0.3554(3) -0.2513(4) 0.4795(3) 0.0207(9) Uani 1 1 d . . O5 O 0.3757(3) 0.0267(4) 0.5533(3) 0.0243(9) Uani 1 1 d . . O6 O 0.3107(3) -0.2056(4) 0.6581(3) 0.0238(9) Uani 1 1 d . . H6B H 0.3502 -0.1534 0.6994 0.036 Uiso 1 1 calc R U C1 C 0.1054(5) 0.0243(7) 0.2353(4) 0.0258(14) Uani 1 1 d . . C2 C 0.1130(5) -0.0629(7) 0.3249(4) 0.0250(14) Uani 1 1 d . . H2A H 0.0906 -0.1701 0.3237 0.030 Uiso 1 1 calc R U C3 C 0.1532(4) 0.0056(6) 0.4159(4) 0.0194(12) Uani 1 1 d . . C4 C 0.1866(4) 0.1674(7) 0.4158(4) 0.0198(12) Uani 1 1 d . . H4A H 0.2106 0.2166 0.4770 0.024 Uiso 1 1 calc R U C5 C 0.1846(4) 0.2552(6) 0.3274(4) 0.0185(12) Uani 1 1 d . . C6 C 0.1443(4) 0.1819(7) 0.2374(4) 0.0228(13) Uani 1 1 d . . H6A H 0.1432 0.2395 0.1771 0.027 Uiso 1 1 calc R U C7 C 0.0604(5) -0.0501(9) 0.1364(5) 0.0397(17) Uani 1 1 d . . H7A H 0.0649 0.0264 0.0826 0.059 Uiso 1 1 calc R U H7B H -0.0147 -0.0799 0.1404 0.059 Uiso 1 1 calc R U H7C H 0.1022 -0.1443 0.1232 0.059 Uiso 1 1 calc R U C8 C 0.1697(5) -0.0901(7) 0.5124(4) 0.0239(13) Uani 1 1 d . . H8A H 0.1314 -0.1921 0.5031 0.029 Uiso 1 1 calc R U H8B H 0.1381 -0.0317 0.5660 0.029 Uiso 1 1 calc R U C9 C 0.2387(4) 0.4173(6) 0.3265(4) 0.0183(12) Uani 1 1 d . . H9A H 0.2207 0.4791 0.3849 0.022 Uiso 1 1 calc R U H9B H 0.2114 0.4756 0.2659 0.022 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 Er1 0.02000(16) 0.00911(15) 0.00636(15) 0.00006(9) 0.00131(9) 0.00166(11) P1 0.0204(8) 0.0090(7) 0.0058(6) -0.0001(5) 0.0022(5) -0.0013(6) P2 0.0219(8) 0.0119(7) 0.0102(7) -0.0007(5) 0.0019(6) -0.0029(6) O1 0.025(2) 0.029(2) 0.0077(19) 0.0063(16) 0.0008(16) -0.0007(18) O1W 0.039(3) 0.022(2) 0.013(2) 0.0005(16) 0.0043(18) -0.0113(19) O2 0.028(2) 0.0119(18) 0.0110(19) -0.0010(15) -0.0010(16) -0.0026(16) O2W 0.031(2) 0.022(2) 0.024(2) -0.0083(18) 0.0147(18) -0.0031(18) O3 0.031(2) 0.0119(19) 0.0107(19) -0.0022(14) 0.0074(16) -0.0001(16) O4 0.029(2) 0.020(2) 0.013(2) -0.0044(15) 0.0032(16) 0.0016(17) O5 0.037(3) 0.016(2) 0.018(2) 0.0015(16) -0.0037(18) -0.0085(18) O6 0.041(3) 0.017(2) 0.014(2) 0.0004(16) 0.0020(18) -0.0064(18) C1 0.018(3) 0.029(3) 0.030(4) -0.008(3) 0.000(3) -0.005(3) C2 0.021(3) 0.019(3) 0.035(4) 0.000(3) 0.003(3) -0.008(3) C3 0.014(3) 0.020(3) 0.025(3) 0.002(2) 0.003(2) -0.001(2) C4 0.020(3) 0.021(3) 0.018(3) 0.002(2) 0.002(2) 0.001(3) C5 0.016(3) 0.018(3) 0.021(3) 0.002(2) -0.001(2) 0.002(2) C6 0.020(3) 0.027(3) 0.021(3) 0.004(3) 0.003(2) 0.002(3) C7 0.039(4) 0.050(4) 0.031(4) -0.016(3) 0.005(3) -0.011(3) C8 0.027(3) 0.021(3) 0.025(3) 0.004(2) 0.008(3) -0.002(3) C9 0.024(3) 0.016(3) 0.015(3) 0.005(2) 0.003(2) 0.003(2) 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' Er Er -0.2586 4.9576 '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 O5 Er1 O1 87.39(13) 4_565 4_565 O5 Er1 O2 157.95(13) 4_565 2_645 O1 Er1 O2 113.38(13) 4_565 2_645 O5 Er1 O3 82.20(13) 4_565 . O1 Er1 O3 141.21(14) 4_565 . O2 Er1 O3 76.87(13) 2_645 . O5 Er1 O4 114.83(13) 4_565 2_655 O1 Er1 O4 77.39(13) 4_565 2_655 O2 Er1 O4 78.60(13) 2_645 2_655 O3 Er1 O4 140.51(13) . 2_655 O5 Er1 O1W 101.00(14) 4_565 . O1 Er1 O1W 71.44(13) 4_565 . O2 Er1 O1W 79.98(13) 2_645 . O3 Er1 O1W 74.08(12) . . O4 Er1 O1W 130.74(13) 2_655 . O5 Er1 O2W 79.17(13) 4_565 . O1 Er1 O2W 138.52(13) 4_565 . O2 Er1 O2W 88.93(13) 2_645 . O3 Er1 O2W 75.76(12) . . O4 Er1 O2W 73.31(12) 2_655 . O1W Er1 O2W 149.49(12) . . O1 P1 O3 112.4(2) . . O1 P1 O2 111.8(2) . . O3 P1 O2 110.7(2) . . O1 P1 C9 109.1(2) . . O3 P1 C9 107.7(2) . . O2 P1 C9 104.7(2) . . O5 P2 O4 113.0(2) . . O5 P2 O6 112.2(2) . . O4 P2 O6 109.0(2) . . O5 P2 C8 109.9(2) . . O4 P2 C8 109.3(3) . . O6 P2 C8 103.0(2) . . P1 O1 Er1 173.8(2) . 4_566 P1 O2 Er1 134.1(2) . 2_655 P1 O3 Er1 147.6(2) . . P2 O4 Er1 127.3(2) . 2_645 P2 O5 Er1 168.4(2) . 4_566 C2 C1 C6 118.6(5) . . C2 C1 C7 121.4(5) . . C6 C1 C7 120.0(6) . . C3 C2 C1 121.5(5) . . C2 C3 C4 118.2(5) . . C2 C3 C8 122.3(5) . . C4 C3 C8 119.3(5) . . C5 C4 C3 121.6(5) . . C4 C5 C6 118.4(5) . . C4 C5 C9 120.5(5) . . C6 C5 C9 120.6(5) . . C5 C6 C1 121.5(5) . . C3 C8 P2 112.2(4) . . C5 C9 P1 110.7(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Er1 O5 2.245(4) 4_565 Er1 O1 2.251(3) 4_565 Er1 O2 2.260(3) 2_645 Er1 O3 2.276(3) . Er1 O4 2.323(4) 2_655 Er1 O1W 2.393(4) . Er1 O2W 2.419(4) . P1 O1 1.512(4) . P1 O3 1.518(4) . P1 O2 1.543(4) . P1 C9 1.813(5) . P2 O5 1.498(4) . P2 O4 1.509(4) . P2 O6 1.569(4) . P2 C8 1.811(6) . O1 Er1 2.251(3) 4_566 O2 Er1 2.260(3) 2_655 O4 Er1 2.323(4) 2_645 O5 Er1 2.245(4) 4_566 C1 C2 1.386(8) . C1 C6 1.391(8) . C1 C7 1.507(8) . C2 C3 1.383(8) . C3 C4 1.403(8) . C3 C8 1.502(7) . C4 C5 1.378(8) . C5 C6 1.389(8) . C5 C9 1.500(7) .