#------------------------------------------------------------------------------ #$Date: 2019-10-07 10:14:40 +0300 (Mon, 07 Oct 2019) $ #$Revision: 219119 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234402.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_7234402 loop_ _publ_author_name 'Min Ren' 'Carlos D. S. Brites' 'Song-Song Bao' 'Rute A. S. Ferreira' 'Li-Min Zheng' 'Luis D. Carlos' _publ_section_title ; A cryogenic luminescent ratiometric thermometer based on a lanthanide phosphonate dimer ; _journal_name_full 'Journal of Materials Chemistry C' _journal_page_first 8480 _journal_page_last 8484 _journal_paper_doi 10.1039/C5TC01468A _journal_volume 3 _journal_year 2015 _chemical_formula_moiety 'C18 H48 Eu2 N8 O26 P6, 8(H2 O)' _chemical_formula_sum 'C18 H64 Eu2 N8 O34 P6' _chemical_formula_weight 1426.51 _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 _cell_angle_alpha 90 _cell_angle_beta 108.570(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.8792(11) _cell_length_b 13.1682(11) _cell_length_c 17.0596(18) _cell_measurement_reflns_used 2190 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 24.92 _cell_measurement_theta_min 3.08 _cell_volume 2316.7(4) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 'phi and omega scans' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type graphite _diffrn_measurement_method 'CCD area detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1026 _diffrn_reflns_av_unetI/netI 0.1041 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13358 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.500 _diffrn_reflns_theta_min 3.077 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 3.002 _exptl_absorpt_correction_T_max 0.714 _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.045 _exptl_crystal_description sheet-like _exptl_crystal_F_000 1432 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.765 _refine_diff_density_min -1.177 _refine_diff_density_rms 0.188 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 310 _refine_ls_number_reflns 4268 _refine_ls_number_restraints 60 _refine_ls_restrained_S_all 0.962 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0437 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0108P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.0609 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2923 _reflns_number_total 4268 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-8480.cif _cod_data_source_block Eu _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7234402 _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 2013-4 _shelx_res_file ; TITL la1 in P2(1)/c CELL 0.71073 10.8792 13.1682 17.0596 90.000 108.570 90.000 ZERR 2.00 0.0011 0.0011 0.0018 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P Eu UNIT 36 128 16 68 12 4 OMIT 0.00 51.00 L.S. 4 ACTA bond $H FMAP 2 PLAN 5 HTAB O5W O3W_$5 HTAB O5W O3 HTAB O4W O5_$10 HTAB O4W O2W_$9 HTAB O4W O10_$3 HTAB O3W O9_$3 HTAB O3W O11_$3 HTAB O2W O9_$8 HTAB O2W O12_$2 HTAB O2W O10_$2 HTAB O2W N4_$2 HTAB O1W O4W_$7 HTAB O1W O5W_$6 HTAB O8 O2W_$5 HTAB O5 O3_$2 HTAB C9 O4W_$4 HTAB C6 O11_$1 HTAB C6 O8 HTAB C6 O2 HTAB C5 O8 HTAB C4 O3W_$4 HTAB C3 O12_$3 HTAB C2 O10_$2 HTAB C1 O2_$1 HTAB N3 O4 HTAB N1 O4 isor 0.002 0.005 o12 o1w simu 0.005 0.01 N4 O10 O11 o12 delu 0.002 0.005 N4 O10 O11 o12 simu 0.005 0.01 N1 C1 C6 C7 delu 0.005 0.01 N1 C1 C6 C7 HTAB CONF HTAB N1 O4 HTAB N3 O4 EQIV $1 -x+1, y-1/2, -z+1/2 HTAB C1 O2_$1 EQIV $2 -x+1, -y+2, -z+1 HTAB C2 O10_$2 EQIV $3 x, y-1, z HTAB C3 O12_$3 EQIV $4 -x, y+1/2, -z+1/2 HTAB C4 O3W_$4 HTAB C5 O8 HTAB C6 O2 HTAB C6 O8 HTAB C6 O11_$1 HTAB C9 O4W_$4 HTAB O5 O3_$2 EQIV $5 -x+1, y+1/2, -z+1/2 HTAB O8 O2W_$5 EQIV $6 x-1, y, z HTAB O1W O5W_$6 EQIV $7 x, y+1, z HTAB O1W O4W_$7 HTAB O2W O12_$2 EQIV $8 x+1, -y+3/2, z+1/2 HTAB O2W O9_$8 HTAB O3W O11_$3 HTAB O3W O9_$3 EQIV $9 -x+1, -y+1, -z+1 HTAB O4W O2W_$9 EQIV $10 -x, -y+1, -z+1 HTAB O4W O5_$10 HTAB O5W O3 EQIV $11 x+1, y, z HTAB O5W O1W_$11 FREE Eu1 P1 FREE Eu1 N4 TEMP -100.150 WGHT 0.010800 FVAR 0.23027 EU1 6 0.373625 1.057624 0.396004 11.00000 0.00927 0.00751 = 0.00718 0.00028 0.00274 -0.00038 P1 5 0.633572 0.971362 0.385805 11.00000 0.01105 0.00715 = 0.00943 -0.00111 0.00649 -0.00028 P2 5 0.328943 0.810873 0.474882 11.00000 0.01098 0.00820 = 0.00976 -0.00022 0.00473 -0.00105 P3 5 0.160073 0.976466 0.178673 11.00000 0.01488 0.01313 = 0.00931 0.00009 0.00245 0.00114 N1 3 0.524576 0.782342 0.323742 11.00000 0.01346 0.00924 = 0.00751 -0.00397 0.00347 0.00222 AFIX 3 H1C 2 0.478847 0.801361 0.356112 11.00000 -1.20000 AFIX 0 N2 3 0.350495 0.657708 0.371547 11.00000 0.02126 0.00984 = 0.01504 -0.00173 0.00776 0.00131 N3 3 0.218574 0.775387 0.237843 11.00000 0.01546 0.00813 = 0.00812 -0.00312 0.00206 -0.00031 AFIX 3 H3C 2 0.255536 0.801600 0.287964 11.00000 -1.20000 AFIX 0 N4 3 0.304574 1.280159 0.379754 11.00000 0.01708 0.01524 = 0.02051 0.00213 0.00702 0.00175 C1 1 0.548942 0.669325 0.335177 11.00000 0.01841 0.01183 = 0.01436 -0.00217 0.00516 0.00607 AFIX 23 H1A 2 0.643427 0.656269 0.356303 11.00000 -1.20000 H1B 2 0.513266 0.634378 0.281296 11.00000 -1.20000 AFIX 0 C2 1 0.484681 0.627675 0.396238 11.00000 0.02257 0.00746 = 0.01584 0.00021 0.00487 0.00115 AFIX 23 H2A 2 0.490914 0.552655 0.397959 11.00000 -1.20000 H2B 2 0.530304 0.653956 0.452360 11.00000 -1.20000 AFIX 0 C3 1 0.260378 0.602004 0.303108 11.00000 0.01657 0.01167 = 0.01449 -0.00270 0.00007 -0.00378 AFIX 23 H3A 2 0.217644 0.547724 0.325167 11.00000 -1.20000 H3B 2 0.308586 0.569735 0.269333 11.00000 -1.20000 AFIX 0 C4 1 0.157801 0.673986 0.249100 11.00000 0.02164 0.01662 = 0.00932 -0.00144 -0.00328 -0.00748 AFIX 23 H4A 2 0.089793 0.685867 0.275206 11.00000 -1.20000 H4B 2 0.116394 0.642399 0.194358 11.00000 -1.20000 AFIX 0 C5 1 0.323318 0.759021 0.197289 11.00000 0.01322 0.01174 = 0.01319 0.00588 0.00984 0.00307 AFIX 23 H5A 2 0.342367 0.685447 0.198037 11.00000 -1.20000 H5B 2 0.288343 0.780198 0.138674 11.00000 -1.20000 AFIX 0 C6 1 0.447985 0.814569 0.236551 11.00000 0.01426 0.01191 = 0.00967 0.00351 0.00413 -0.00034 AFIX 23 H6A 2 0.428350 0.887903 0.237313 11.00000 -1.20000 H6B 2 0.503774 0.805770 0.201146 11.00000 -1.20000 AFIX 0 C7 1 0.650324 0.841509 0.353593 11.00000 0.01188 0.01239 = 0.00951 -0.00138 0.00199 0.00040 AFIX 23 H7A 2 0.689572 0.843427 0.308624 11.00000 -1.20000 H7B 2 0.711031 0.804715 0.400769 11.00000 -1.20000 AFIX 0 C8 1 0.297822 0.679335 0.439587 11.00000 0.02468 0.01063 = 0.00762 -0.00455 0.00362 -0.00038 AFIX 23 H8A 2 0.338098 0.632892 0.486364 11.00000 -1.20000 H8B 2 0.203189 0.666707 0.420451 11.00000 -1.20000 AFIX 0 C9 1 0.111757 0.846324 0.191240 11.00000 0.01186 0.02419 = 0.01478 -0.00043 0.00193 -0.00275 AFIX 23 H9A 2 0.046029 0.848439 0.220155 11.00000 -1.20000 H9B 2 0.069355 0.817360 0.135609 11.00000 -1.20000 AFIX 0 O1 4 0.590909 0.962313 0.463020 11.00000 0.01290 0.00983 = 0.00465 -0.00052 0.00581 -0.00062 O2 4 0.522944 1.022525 0.320454 11.00000 0.01705 0.01217 = 0.00717 0.00216 0.00760 0.00359 O3 4 0.766290 1.017171 0.401002 11.00000 0.01080 0.01643 = 0.01383 -0.00675 0.00715 -0.00255 O4 4 0.330363 0.872740 0.398964 11.00000 0.01116 0.01225 = 0.01212 0.00120 0.00563 -0.00356 O5 4 0.203604 0.833345 0.498256 11.00000 0.01498 0.01413 = 0.01278 -0.00477 0.00561 -0.00077 AFIX 83 H5C 2 0.216964 0.883089 0.530718 11.00000 -1.20000 AFIX 0 O6 4 0.450155 0.819815 0.548097 11.00000 0.00835 0.01103 = 0.01268 0.00048 0.00205 -0.00161 O7 4 0.244256 1.015003 0.260427 11.00000 0.02146 0.01641 = 0.00927 -0.00272 0.00100 0.00003 O8 4 0.244276 0.967840 0.118326 11.00000 0.02073 0.02528 = 0.00860 0.00725 0.00303 0.00526 H8C 2 0.224567 0.998912 0.078128 11.00000 -1.20000 O9 4 0.035072 1.031369 0.136627 11.00000 0.01288 0.01573 = 0.01702 0.00347 -0.00197 0.00452 O10 4 0.302503 1.238832 0.444476 11.00000 0.01907 0.01998 = 0.01879 0.00148 0.00977 0.00235 O11 4 0.310824 1.223296 0.320513 11.00000 0.01662 0.01710 = 0.01409 0.00259 0.00490 0.00200 O12 4 0.303362 1.373577 0.371473 11.00000 0.04641 0.01650 = 0.04100 0.00482 0.01966 0.00544 O1W 4 0.153946 1.065405 0.399256 11.00000 0.01023 0.01835 = 0.02290 -0.01222 0.00408 -0.00320 AFIX 3 H1WA 2 0.093113 1.023489 0.377767 11.00000 -1.20000 H1WB 2 0.133471 1.105783 0.431943 11.00000 -1.20000 AFIX 0 O2W 4 0.846725 0.566543 0.520472 11.00000 0.02066 0.02734 = 0.01645 -0.00558 0.00294 0.01251 AFIX 3 H2WA 2 0.801653 0.586976 0.549939 11.00000 -1.20000 H2WB 2 0.908823 0.529287 0.548791 11.00000 -1.20000 AFIX 0 O3W 4 0.081811 0.231075 0.172551 11.00000 0.03057 0.02048 = 0.05721 0.01026 0.00978 0.00159 AFIX 3 H3WA 2 0.152148 0.234297 0.212694 11.00000 -1.20000 H3WB 2 0.059394 0.169691 0.160640 11.00000 -1.20000 AFIX 0 O4W 4 0.051590 0.215191 0.482439 11.00000 0.02834 0.03636 = 0.04121 -0.00084 0.02130 0.00165 AFIX 3 H4WA 2 0.103022 0.265621 0.492050 11.00000 -1.20000 H4WB 2 -0.005713 0.223158 0.506086 11.00000 -1.20000 AFIX 0 O5W 4 0.951950 0.940329 0.338511 11.00000 0.02161 0.01758 = 0.04541 -0.00949 0.02082 -0.00402 AFIX 3 H5WB 2 0.907469 0.959117 0.368824 11.00000 -1.20000 H5WA 2 0.966968 0.877237 0.346879 11.00000 -1.20000 AFIX 0 HKLF 4 REM la1 in P2(1)/c REM R1 = 0.0437 for 2923 Fo > 4sig(Fo) and 0.0874 for all 4268 data REM 310 parameters refined using 60 restraints END WGHT 0.0151 0.0000 REM Instructions for potential hydrogen bonds HTAB N1 O4 HTAB N3 O4 HTAB C1 O2_$1 HTAB C2 O10_$2 HTAB C3 O12_$3 HTAB C4 O3W_$4 HTAB C5 O8 HTAB C6 O2 HTAB C6 O8 HTAB C6 O11_$1 HTAB C9 O4W_$4 HTAB O5 O3_$2 HTAB O8 O2W_$5 HTAB O1W O5W_$6 HTAB O1W O4W_$7 HTAB O2W N4_$2 HTAB O2W O10_$2 HTAB O2W O12_$2 HTAB O2W O9_$8 HTAB O3W O11_$3 HTAB O3W O9_$3 HTAB O4W O10_$3 HTAB O4W O2W_$9 HTAB O4W O5_$10 HTAB O5W O3 HTAB O5W O3W_$5 REM Highest difference peak 0.765, deepest hole -1.177, 1-sigma level 0.188 Q1 1 0.4443 0.8586 0.1077 11.00000 0.05 0.77 Q2 1 0.5073 0.9789 0.3442 11.00000 0.05 0.75 Q3 1 0.3420 0.6764 0.2455 11.00000 0.05 0.73 Q4 1 0.7409 0.9255 0.4450 11.00000 0.05 0.73 Q5 1 0.5357 0.8811 0.5691 11.00000 0.05 0.71 ; _shelx_res_checksum 79038 _shelx_hkl_file ; 2 0 0 1146.85 32.0233 1 -2 0 0 1210.06 34.6542 1 3 0 0 2266.75 50.7156 1 4 0 0 1783.14 52.1845 1 5 0 0 91.6069 22.3013 1 6 0 0 671.603 45.5142 1 7 0 0 1115.26 58.8486 1 8 0 0 552.167 55.5371 1 9 0 0 246.453 44.1860 1 10 0 0 281.742 50.7342 1 10 0 0 267.004 52.4128 1 11 0 0 240.742 59.8669 1 11 0 0 187.383 61.4227 1 12 0 0 328.353 87.6545 1 12 0 0 493.885 93.1773 1 2 -1 0 108.232 15.2457 1 -2 -1 0 108.395 19.0508 1 2 1 0 99.4259 17.9864 1 -3 -1 0 676.666 37.3687 1 3 -1 0 679.627 33.5164 1 3 1 0 725.902 37.6491 1 -4 -1 0 416.228 36.7369 1 4 -1 0 390.124 34.2697 1 4 1 0 376.413 35.9186 1 5 -1 0 9.40768 17.5352 1 5 1 0 -11.479 19.0430 1 6 -1 0 137.728 26.8255 1 6 1 0 168.889 27.2477 1 7 -1 0 75.6623 27.1408 1 7 1 0 126.760 26.3826 1 8 -1 0 203.189 37.4263 1 9 -1 0 38.0583 39.2512 1 9 -1 0 38.3301 37.9537 1 9 1 0 58.6536 34.3781 1 10 -1 0 357.949 58.5746 1 10 -1 0 393.245 60.9514 1 10 1 0 336.570 53.4150 1 11 -1 0 62.6817 62.9271 1 11 -1 0 162.490 62.3800 1 11 1 0 20.2289 60.4851 1 11 1 0 146.507 55.2803 1 12 -1 0 94.9639 73.6742 1 12 -1 0 79.9118 79.0895 1 12 1 0 -129.48 68.6098 1 12 1 0 -26.577 72.4229 1 0 -2 0 1074.00 16.7565 1 -1 -2 0 63.6989 12.1609 1 -1 2 0 77.5120 7.68726 1 1 2 0 59.8348 12.0554 1 -2 -2 0 -0.8777 16.8037 1 2 -2 0 20.2400 12.0678 1 2 2 0 0.97287 16.5054 1 -3 -2 0 15.7429 19.5926 1 3 -2 0 38.8519 16.5420 1 3 2 0 17.0083 20.4860 1 -4 -2 0 1339.95 53.3986 1 4 -2 0 1244.60 44.7752 1 4 2 0 1261.76 51.4764 1 5 -2 0 2921.69 67.5388 1 5 2 0 2899.13 74.2936 1 6 -2 0 37.0635 22.6415 1 6 2 0 30.7739 23.8213 1 7 -2 0 291.500 37.5481 1 7 2 0 405.918 44.4394 1 8 -2 0 2436.54 88.4034 1 8 -2 0 2552.29 87.2393 1 8 2 0 2425.24 90.0128 1 9 -2 0 1032.30 77.8716 1 9 -2 0 1000.94 79.4736 1 9 2 0 989.916 65.6429 1 10 -2 0 207.285 61.1722 1 10 -2 0 189.348 49.2830 1 11 -2 0 339.675 72.4926 1 11 -2 0 383.384 70.8984 1 11 2 0 316.691 58.4668 1 12 -2 0 356.691 90.3415 1 12 -2 0 231.576 74.0596 1 12 2 0 87.9510 69.8434 1 12 2 0 163.616 77.8961 1 0 -3 0 1.00652 8.56358 1 0 3 0 5.41213 9.43596 1 1 -3 0 1030.32 17.7766 1 -1 -3 0 1082.16 31.4595 1 1 3 0 1070.55 30.6338 1 -1 3 0 1086.45 18.6505 1 2 -3 0 1868.96 31.1409 1 -2 -3 0 1844.13 46.3409 1 2 3 0 1827.66 46.6886 1 -3 -3 0 1634.61 50.3665 1 3 -3 0 1577.43 38.5669 1 3 3 0 1542.43 50.7347 1 4 -3 0 76.8004 19.2266 1 -4 -3 0 84.9180 23.9925 1 4 -3 0 52.5349 18.4109 1 4 3 0 61.3331 23.1346 1 5 -3 0 1426.26 50.3618 1 -5 -3 0 1406.83 57.0518 1 5 -3 0 1436.61 51.4452 1 5 3 0 1356.02 56.4027 1 6 -3 0 2033.57 66.9093 1 6 -3 0 2171.79 66.5053 1 6 3 0 2171.38 73.5607 1 7 -3 0 473.545 50.3743 1 7 -3 0 396.095 43.0495 1 7 3 0 468.285 48.1331 1 8 -3 0 12.2388 33.6005 1 8 -3 0 29.5316 33.9920 1 8 3 0 -17.547 28.9055 1 9 -3 0 514.286 56.7323 1 9 3 0 575.057 56.7668 1 10 -3 0 419.257 63.3099 1 10 -3 0 430.605 66.9010 1 10 3 0 436.015 51.0844 1 11 -3 0 144.449 70.2257 1 11 3 0 89.5416 51.4674 1 12 -3 0 97.8501 74.6386 1 12 -3 0 -15.139 80.2140 1 12 3 0 67.2831 63.1562 1 12 3 0 -33.408 66.8664 1 0 -4 0 2100.04 32.2505 1 0 4 0 2097.33 32.9111 1 1 -4 0 15.6087 8.10874 1 -1 -4 0 -10.295 13.6113 1 1 4 0 16.5305 14.4489 1 -1 4 0 14.5828 8.52399 1 -2 -4 0 54.0174 19.3600 1 2 -4 0 53.6969 10.8539 1 -2 4 0 52.3714 11.3986 1 2 4 0 31.5328 19.1833 1 -3 -4 0 23.7431 18.6951 1 3 -4 0 52.4356 13.6861 1 3 4 0 32.3814 19.2234 1 4 -4 0 19.2729 15.7847 1 4 -4 0 16.4954 16.5332 1 -4 -4 0 13.1715 20.9254 1 4 4 0 38.0027 20.8310 1 -5 -4 0 85.8678 23.7374 1 5 -4 0 49.6727 21.2492 1 5 -4 0 48.8407 21.7482 1 5 4 0 57.2443 22.4484 1 6 -4 0 13.6960 22.6064 1 6 -4 0 39.2563 24.5660 1 6 4 0 4.29920 22.3216 1 7 -4 0 38.4624 27.2714 1 7 -4 0 45.4753 30.6723 1 7 4 0 12.0734 26.4805 1 8 -4 0 22.8608 34.3777 1 8 -4 0 23.4968 32.3835 1 8 4 0 80.6979 32.1441 1 9 -4 0 108.038 44.8547 1 9 4 0 96.5064 40.4187 1 10 -4 0 20.4537 48.3414 1 10 -4 0 9.77005 49.5677 1 10 4 0 -41.253 38.9523 1 11 -4 0 84.8298 69.6514 1 11 4 0 -60.667 50.7698 1 12 -4 0 25.5707 80.8623 1 12 -4 0 -57.363 79.1741 1 0 -5 0 0.96905 11.3763 1 0 5 0 -9.3711 11.3782 1 1 -5 0 3967.77 37.2283 1 -1 -5 0 3914.55 56.9852 1 1 5 0 3848.33 56.8257 1 -1 5 0 3927.16 37.9273 1 2 -5 0 2068.23 29.8044 1 -2 -5 0 2146.18 52.1256 1 2 5 0 2233.09 53.0670 1 -2 5 0 2160.28 30.9163 1 3 -5 0 3049.61 44.4969 1 -3 -5 0 2878.22 65.6807 1 3 5 0 2782.98 64.2373 1 4 -5 0 279.909 27.5377 1 -4 -5 0 237.427 31.5734 1 4 -5 0 299.397 29.4286 1 4 5 0 246.207 30.1866 1 -5 -5 0 1043.80 56.1466 1 5 -5 0 1134.77 45.1757 1 5 -5 0 1066.34 46.3735 1 5 5 0 1086.78 53.5482 1 6 -5 0 1463.29 57.4326 1 6 -5 0 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76.4446 1 6 -1 -19 175.424 72.8344 1 -6 -1 19 100.005 61.4715 1 6 1 -19 110.697 67.0647 1 -6 1 19 184.927 66.1988 1 5 -1 -19 207.917 77.2960 1 -5 -1 19 104.416 63.3568 1 -5 1 19 184.862 66.8277 1 5 1 -19 179.090 62.3872 1 4 -1 -19 580.574 85.1077 1 -4 -1 19 589.365 73.4139 1 4 1 -19 644.321 77.6004 1 -4 1 19 611.632 83.2975 1 -3 -1 19 537.645 68.0890 1 3 -1 -19 531.432 80.3423 1 3 1 -19 587.790 69.4864 1 -3 1 19 274.270 72.5970 1 2 -1 -19 122.061 67.3315 1 -2 -1 19 65.6601 52.5425 1 -2 1 19 109.102 60.5918 1 2 1 -19 109.024 55.1747 1 1 -1 -19 173.370 67.8921 1 -1 -1 19 79.2447 50.0365 1 -1 1 19 -2.1812 65.1420 1 1 1 -19 86.3102 56.2755 1 0 -1 -19 692.714 87.1241 1 0 -1 19 833.786 83.6978 1 0 1 19 754.221 84.8483 1 0 1 -19 811.636 85.2583 1 9 -2 -19 286.598 97.0773 1 -9 2 19 153.587 89.4636 1 8 -2 -19 -167.30 78.7526 1 -8 -2 19 6.35256 71.2395 1 8 2 -19 28.8658 75.4512 1 -8 2 19 134.487 78.2123 1 -7 -2 19 26.5912 65.0162 1 7 -2 -19 185.356 80.2281 1 -7 2 19 11.6220 74.6493 1 7 2 -19 -52.536 68.9873 1 6 -2 -19 201.007 79.2796 1 -6 -2 19 207.830 60.2590 1 6 2 -19 78.2685 64.1776 1 -6 2 19 249.470 76.4090 1 5 -2 -19 263.640 71.2273 1 -5 -2 19 401.195 65.0671 1 5 2 -19 368.761 66.4741 1 -5 2 19 452.551 78.2828 1 -4 -2 19 66.3777 51.1128 1 4 -2 -19 90.0421 72.2097 1 -4 2 19 23.6526 64.5826 1 4 2 -19 38.4557 52.5286 1 -3 -2 19 133.742 52.3956 1 3 -2 -19 58.6699 69.9498 1 3 2 -19 293.543 57.9943 1 -3 2 19 -24.812 61.1162 1 -2 -2 19 76.2005 55.6257 1 2 -2 -19 147.758 73.8297 1 -2 2 19 169.979 67.2004 1 2 2 -19 275.694 65.9155 1 -1 -2 19 80.3185 53.1601 1 1 -2 -19 165.211 76.5009 1 1 2 -19 200.538 56.5649 1 -1 2 19 100.100 72.5817 1 0 -2 19 -39.584 61.6610 1 0 -2 -19 13.9058 69.4121 1 0 2 19 79.9450 73.4247 1 9 -3 -19 -62.750 93.2152 1 -9 3 19 -42.983 88.4017 1 8 -3 -19 -41.420 84.5936 1 -8 3 19 165.363 78.8898 1 7 -3 -19 -5.1633 76.4375 1 -7 -3 19 -47.603 58.9602 1 -7 3 19 166.261 75.6853 1 7 3 -19 30.8588 63.1721 1 6 -3 -19 235.124 79.5234 1 -6 -3 19 113.428 59.3209 1 -6 3 19 251.010 79.2836 1 6 3 -19 157.640 56.7760 1 -5 -3 19 126.515 50.8565 1 5 -3 -19 130.973 75.1509 1 -5 3 19 -18.024 68.9253 1 5 3 -19 103.240 54.1102 1 -4 -3 19 100.276 50.3779 1 4 -3 -19 106.823 76.2672 1 -4 3 19 173.268 73.4873 1 4 3 -19 251.951 58.2599 1 -3 -3 19 225.059 56.2364 1 3 -3 -19 348.698 75.8556 1 3 3 -19 261.010 59.7068 1 -3 3 19 157.109 79.5341 1 -2 -3 19 -73.275 51.8665 1 2 -3 -19 -5.2973 72.0684 1 2 3 -19 101.980 57.8991 1 -2 3 19 86.8132 70.6491 1 -1 -3 19 -66.842 53.1702 1 1 -3 -19 6.17329 70.7932 1 -1 3 19 -116.39 67.2987 1 0 -3 -19 248.424 85.9797 1 0 3 19 257.994 77.2890 1 8 -4 -19 11.2698 86.3318 1 -8 4 19 155.027 80.7464 1 7 -4 -19 19.2016 84.1123 1 -7 4 19 85.8171 83.0226 1 6 -4 -19 758.048 96.9593 1 -6 -4 19 350.745 60.0821 1 -6 4 19 629.545 85.7653 1 6 4 -19 554.065 74.5107 1 5 -4 -19 172.402 79.1339 1 -5 -4 19 232.420 56.6097 1 5 4 -19 229.641 60.9640 1 -5 4 19 246.670 75.7576 1 -4 -4 19 -28.346 56.4047 1 4 -4 -19 -61.323 72.2964 1 4 4 -19 87.5509 55.6358 1 -4 4 19 20.1426 74.9630 1 3 -4 -19 291.875 80.6133 1 -3 -4 19 247.765 55.2497 1 3 4 -19 168.480 66.6185 1 -3 4 19 105.916 74.6329 1 2 -4 -19 251.878 83.5083 1 -2 -4 19 319.617 58.1424 1 -2 4 19 237.683 72.3815 1 2 4 -19 339.768 63.6166 1 1 -4 -19 206.580 81.2642 1 -1 4 19 251.807 88.4227 1 0 -4 -19 118.607 86.6610 1 0 4 19 156.594 84.1395 1 8 -5 -19 -101.92 88.9334 1 -8 5 19 167.146 85.6193 1 7 -5 -19 -14.695 82.0471 1 -7 5 19 29.0875 80.3242 1 6 -5 -19 25.4350 80.8392 1 -6 5 19 55.2799 81.6623 1 -5 -5 19 -19.355 61.1242 1 5 -5 -19 -52.454 77.2296 1 5 5 -19 -67.333 63.0425 1 -5 5 19 67.2404 73.2433 1 4 -5 -19 27.1188 75.5859 1 -4 -5 19 -9.1981 56.3886 1 -4 5 19 -126.96 71.1636 1 4 5 -19 153.864 58.5808 1 3 -5 -19 49.5383 77.0901 1 -3 -5 19 76.1669 55.0380 1 3 5 -19 169.566 65.8431 1 -3 5 19 147.992 80.3170 1 2 -5 -19 -101.76 75.3157 1 -2 5 19 -100.23 74.9863 1 1 -5 -19 -57.021 81.0206 1 -1 5 19 32.6853 76.7548 1 0 -5 -19 -168.98 89.1811 1 0 5 19 155.693 86.0113 1 7 -6 -19 34.7702 88.1006 1 -7 6 19 -56.283 85.4596 1 6 -6 -19 94.3515 84.2932 1 -6 6 19 250.944 89.5342 1 5 -6 -19 557.203 94.9609 1 -5 6 19 559.385 89.0562 1 4 -6 -19 239.041 88.4093 1 -4 6 19 213.928 87.2128 1 3 -6 -19 162.009 86.0253 1 -3 6 19 -15.140 84.1547 1 2 -6 -19 487.028 98.2179 1 -2 6 19 441.386 88.8951 1 1 -6 -19 280.625 100.006 1 -1 6 19 232.856 93.1146 1 5 -7 -19 77.3594 86.4795 1 -5 7 19 117.697 86.7820 1 4 -7 -19 232.567 91.2492 1 -4 7 19 266.518 90.2679 1 3 -7 -19 14.1628 86.6180 1 -3 7 19 -124.25 87.6981 1 2 -7 -19 -140.66 88.8520 1 -2 7 19 -15.472 87.4429 1 -8 0 20 457.844 98.3796 1 8 0 -20 287.284 99.9649 1 -7 0 20 343.328 90.6677 1 7 0 -20 128.613 82.6947 1 6 0 -20 5.34399 72.1446 1 -6 0 20 189.775 77.9709 1 -5 0 20 418.414 81.0440 1 5 0 -20 562.713 89.9538 1 4 0 -20 352.622 82.4991 1 -4 0 20 220.610 70.6195 1 3 0 -20 3.85200 71.6495 1 -3 0 20 -22.284 68.4431 1 2 0 -20 86.0648 69.7481 1 -2 0 20 -91.506 63.6327 1 8 -1 -20 61.6122 93.1749 1 -8 1 20 38.2392 87.8539 1 7 -1 -20 1.25456 80.7402 1 -7 -1 20 31.6739 74.9186 1 -7 1 20 116.969 82.4277 1 7 1 -20 -4.2776 81.8256 1 6 -1 -20 103.894 79.6965 1 -6 -1 20 63.3294 75.0669 1 6 1 -20 97.1753 78.4325 1 -6 1 20 116.476 80.1679 1 5 -1 -20 1.98057 69.6900 1 -5 -1 20 55.1039 73.1773 1 -5 1 20 88.8811 76.3284 1 5 1 -20 -47.100 75.3893 1 4 -1 -20 -65.954 80.3510 1 -4 -1 20 -43.794 58.0390 1 4 1 -20 -9.3551 65.1409 1 -4 1 20 -21.585 71.6216 1 3 -1 -20 -78.625 73.6270 1 -3 -1 20 61.3840 64.9359 1 3 1 -20 32.1287 69.3436 1 -3 1 20 -152.34 72.2717 1 2 -1 -20 70.0457 78.5472 1 2 1 -20 -21.195 62.1161 1 -2 1 20 34.2516 70.6088 1 8 -2 -20 43.0872 97.6284 1 -8 2 20 209.040 90.6952 1 7 -2 -20 93.2998 88.4393 1 -7 2 20 227.967 85.1964 1 6 -2 -20 -22.657 82.3970 1 -6 -2 20 -30.591 76.5984 1 -6 2 20 101.230 85.3681 1 6 2 -20 -74.468 65.7414 1 5 -2 -20 224.106 89.6115 1 -5 -2 20 264.282 69.7293 1 -5 2 20 158.642 81.4536 1 5 2 -20 150.699 66.0224 1 4 -2 -20 181.222 88.1186 1 -4 -2 20 122.624 60.9135 1 -4 2 20 30.4901 76.8657 1 4 2 -20 4.69570 63.6859 1 3 -2 -20 156.096 78.6346 1 3 2 -20 43.5508 61.7449 1 -3 2 20 -199.70 76.8361 1 2 -2 -20 147.378 81.5231 1 -2 2 20 -19.141 71.3336 1 1 -2 -20 192.944 84.1741 1 7 -3 -20 91.1210 91.7931 1 -7 3 20 236.896 92.7756 1 6 -3 -20 331.803 92.3859 1 -6 3 20 262.251 92.5803 1 5 -3 -20 89.4742 83.3349 1 -5 3 20 8.25593 79.1140 1 4 -3 -20 34.4393 86.1408 1 -4 3 20 110.374 88.1932 1 3 -3 -20 344.999 93.9518 1 -3 3 20 206.049 88.6473 1 2 -3 -20 215.362 84.9273 1 -2 3 20 253.014 91.6900 1 1 -3 -20 -58.702 87.0308 1 -1 3 20 -55.682 88.5585 1 7 -4 -20 -24.451 92.3634 1 -7 4 20 -13.499 87.6377 1 6 -4 -20 -15.656 87.9270 1 -6 4 20 66.6424 87.6645 1 5 -4 -20 -91.891 84.8379 1 -5 4 20 59.2505 82.4584 1 4 -4 -20 82.4361 85.8058 1 -4 4 20 -102.34 84.3175 1 3 -4 -20 -74.968 84.8019 1 -3 4 20 -220.30 77.8475 1 2 -4 -20 -19.576 87.9567 1 -2 4 20 -93.315 80.5068 1 1 -4 -20 -65.317 89.9566 1 -1 4 20 -45.562 91.9372 1 6 -5 -20 170.107 96.5779 1 -6 5 20 215.022 94.3901 1 5 -5 -20 101.404 90.8439 1 -5 5 20 111.205 88.5659 1 4 -5 -20 133.337 95.7281 1 -4 5 20 113.005 98.5734 1 3 -5 -20 320.251 96.3812 1 -3 5 20 7.54944 91.2548 1 2 -5 -20 38.0359 87.6515 1 -2 5 20 138.119 90.6394 1 5 -2 -21 -81.504 94.7427 1 -5 2 21 -72.255 86.4221 1 4 -2 -21 101.064 98.8848 1 -4 2 21 98.6471 93.8157 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 26151 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.37363(3) 1.05762(2) 0.39600(2) 0.00795(8) Uani 1 1 d . . . . . P1 P 0.63357(16) 0.97136(10) 0.38581(10) 0.0084(4) Uani 1 1 d . . . . . P2 P 0.32894(16) 0.81087(11) 0.47488(10) 0.0093(4) Uani 1 1 d . . . . . P3 P 0.16007(17) 0.97647(11) 0.17867(10) 0.0128(4) Uani 1 1 d . . . . . N1 N 0.5246(5) 0.7823(3) 0.3237(3) 0.0100(10) Uani 1 1 d . U . . . H1C H 0.4788 0.8014 0.3561 0.012 Uiso 1 1 d R U . . . N2 N 0.3505(5) 0.6577(3) 0.3715(3) 0.0149(13) Uani 1 1 d . . . . . N3 N 0.2186(5) 0.7754(3) 0.2378(3) 0.0110(12) Uani 1 1 d . . . . . H3C H 0.2555 0.8016 0.2880 0.013 Uiso 1 1 d R U . . . N4 N 0.3046(5) 1.2802(4) 0.3798(3) 0.0174(10) Uani 1 1 d . U . . . C1 C 0.5489(6) 0.6693(4) 0.3352(4) 0.0149(13) Uani 1 1 d . U . . . H1A H 0.6434 0.6563 0.3563 0.018 Uiso 1 1 calc R U . . . H1B H 0.5133 0.6344 0.2813 0.018 Uiso 1 1 calc R U . . . C2 C 0.4847(6) 0.6277(4) 0.3962(4) 0.0156(15) Uani 1 1 d . . . . . H2A H 0.4909 0.5527 0.3980 0.019 Uiso 1 1 calc R U . . . H2B H 0.5303 0.6540 0.4524 0.019 Uiso 1 1 calc R U . . . C3 C 0.2604(6) 0.6020(4) 0.3031(4) 0.0154(15) Uani 1 1 d . . . . . H3A H 0.2176 0.5477 0.3252 0.018 Uiso 1 1 calc R U . . . H3B H 0.3086 0.5697 0.2693 0.018 Uiso 1 1 calc R U . . . C4 C 0.1578(6) 0.6740(4) 0.2491(4) 0.0178(16) Uani 1 1 d . . . . . H4A H 0.0898 0.6859 0.2752 0.021 Uiso 1 1 calc R U . . . H4B H 0.1164 0.6424 0.1944 0.021 Uiso 1 1 calc R U . . . C5 C 0.3233(6) 0.7590(4) 0.1973(4) 0.0114(14) Uani 1 1 d . . . . . H5A H 0.3424 0.6854 0.1980 0.014 Uiso 1 1 calc R U . . . H5B H 0.2883 0.7802 0.1387 0.014 Uiso 1 1 calc R U . . . C6 C 0.4480(6) 0.8146(4) 0.2366(4) 0.0119(13) Uani 1 1 d . U . . . H6A H 0.4283 0.8879 0.2373 0.014 Uiso 1 1 calc R U . . . H6B H 0.5038 0.8058 0.2011 0.014 Uiso 1 1 calc R U . . . C7 C 0.6503(6) 0.8415(4) 0.3536(4) 0.0116(13) Uani 1 1 d . U . . . H7A H 0.6896 0.8434 0.3086 0.014 Uiso 1 1 calc R U . . . H7B H 0.7110 0.8047 0.4008 0.014 Uiso 1 1 calc R U . . . C8 C 0.2978(6) 0.6793(4) 0.4396(4) 0.0147(15) Uani 1 1 d . . . . . H8A H 0.3381 0.6329 0.4864 0.018 Uiso 1 1 calc R U . . . H8B H 0.2032 0.6667 0.4205 0.018 Uiso 1 1 calc R U . . . C9 C 0.1118(6) 0.8463(4) 0.1912(4) 0.0175(16) Uani 1 1 d . . . . . H9A H 0.0460 0.8484 0.2202 0.021 Uiso 1 1 calc R U . . . H9B H 0.0694 0.8174 0.1356 0.021 Uiso 1 1 calc R U . . . O1 O 0.5909(4) 0.9623(3) 0.4630(2) 0.0084(9) Uani 1 1 d . . . . . O2 O 0.5229(4) 1.0225(3) 0.3205(2) 0.0112(10) Uani 1 1 d . . . . . O3 O 0.7663(4) 1.0172(3) 0.4010(2) 0.0129(10) Uani 1 1 d . . . . . O4 O 0.3304(4) 0.8727(3) 0.3990(3) 0.0114(10) Uani 1 1 d . . . . . O5 O 0.2036(4) 0.8333(3) 0.4983(2) 0.0137(10) Uani 1 1 d . . . . . H5C H 0.2170 0.8831 0.5307 0.016 Uiso 1 1 calc R U . . . O6 O 0.4502(4) 0.8198(3) 0.5481(2) 0.0110(10) Uani 1 1 d . . . . . O7 O 0.2443(4) 1.0150(3) 0.2604(2) 0.0166(10) Uani 1 1 d . . . . . O8 O 0.2443(4) 0.9678(3) 0.1183(3) 0.0186(12) Uani 1 1 d . . . . . H8C H 0.225(7) 0.999(5) 0.078(4) 0.022 Uiso 1 1 d . U . . . O9 O 0.0351(4) 1.0314(3) 0.1366(3) 0.0168(10) Uani 1 1 d . . . . . O10 O 0.3025(4) 1.2388(3) 0.4445(3) 0.0184(10) Uani 1 1 d . U . . . O11 O 0.3108(4) 1.2233(3) 0.3205(3) 0.0159(9) Uani 1 1 d . U . . . O12 O 0.3034(5) 1.3736(3) 0.3715(3) 0.0333(12) Uani 1 1 d . U . . . O1W O 0.1539(4) 1.0654(3) 0.3993(2) 0.0174(10) Uani 1 1 d . U . . . H1WA H 0.0931 1.0235 0.3778 0.021 Uiso 1 1 d R U . . . H1WB H 0.1335 1.1058 0.4319 0.021 Uiso 1 1 d R U . . . O2W O 0.8467(4) 0.5665(3) 0.5205(2) 0.0222(10) Uani 1 1 d . . . . . H2WA H 0.8017 0.5870 0.5499 0.027 Uiso 1 1 d R U . . . H2WB H 0.9088 0.5293 0.5488 0.027 Uiso 1 1 d R U . . . O3W O 0.0818(5) 0.2311(3) 0.1726(3) 0.0371(14) Uani 1 1 d . . . . . H3WA H 0.1521 0.2343 0.2127 0.044 Uiso 1 1 d R U . . . H3WB H 0.0594 0.1697 0.1606 0.044 Uiso 1 1 d R U . . . O4W O 0.0516(5) 0.2152(3) 0.4824(3) 0.0329(13) Uani 1 1 d . . . . . H4WA H 0.1030 0.2656 0.4920 0.039 Uiso 1 1 d R U . . . H4WB H -0.0057 0.2232 0.5061 0.039 Uiso 1 1 d R U . . . O5W O 0.9520(4) 0.9403(3) 0.3385(3) 0.0258(11) Uani 1 1 d . . . . . H5WB H 0.9075 0.9591 0.3688 0.031 Uiso 1 1 d R U . . . H5WA H 0.9670 0.8772 0.3469 0.031 Uiso 1 1 d 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 0.00927(16) 0.00751(14) 0.00718(15) 0.00028(16) 0.00274(12) -0.00038(17) P1 0.0111(9) 0.0071(8) 0.0094(9) -0.0011(6) 0.0065(7) -0.0003(6) P2 0.0110(10) 0.0082(8) 0.0098(9) -0.0002(7) 0.0047(8) -0.0010(7) P3 0.0149(10) 0.0131(8) 0.0093(9) 0.0001(7) 0.0024(8) 0.0011(7) N1 0.013(2) 0.009(2) 0.008(2) -0.0040(18) 0.0035(19) 0.0022(18) N2 0.021(4) 0.010(3) 0.015(3) -0.002(2) 0.008(3) 0.001(2) N3 0.015(3) 0.008(3) 0.008(3) -0.003(2) 0.002(3) 0.000(2) N4 0.017(2) 0.0152(18) 0.021(2) 0.0021(16) 0.007(2) 0.002(2) C1 0.018(3) 0.012(3) 0.014(3) -0.002(2) 0.005(3) 0.006(2) C2 0.023(4) 0.007(3) 0.016(4) 0.000(3) 0.005(3) 0.001(3) C3 0.017(4) 0.012(3) 0.014(4) -0.003(3) 0.000(3) -0.004(3) C4 0.022(4) 0.017(3) 0.009(4) -0.001(3) -0.003(3) -0.007(3) C5 0.013(4) 0.012(3) 0.013(4) 0.006(3) 0.010(3) 0.003(3) C6 0.014(3) 0.012(3) 0.010(3) 0.004(2) 0.004(2) 0.000(2) C7 0.012(3) 0.012(3) 0.010(3) -0.001(2) 0.002(3) 0.000(2) C8 0.025(4) 0.011(3) 0.008(4) -0.005(3) 0.004(3) 0.000(3) C9 0.012(4) 0.024(4) 0.015(4) 0.000(3) 0.002(3) -0.003(3) O1 0.013(2) 0.010(2) 0.005(2) -0.0005(17) 0.0058(18) -0.0006(18) O2 0.017(3) 0.012(2) 0.007(2) 0.0022(17) 0.008(2) 0.0036(18) O3 0.011(2) 0.016(2) 0.014(2) -0.0067(18) 0.007(2) -0.0026(18) O4 0.011(3) 0.012(2) 0.012(2) 0.0012(19) 0.006(2) -0.0036(18) O5 0.015(3) 0.014(2) 0.013(3) -0.0048(18) 0.006(2) -0.0008(19) O6 0.008(2) 0.011(2) 0.013(2) 0.0005(18) 0.002(2) -0.0016(19) O7 0.021(3) 0.016(2) 0.009(2) -0.0027(18) 0.001(2) 0.000(2) O8 0.021(3) 0.025(3) 0.009(3) 0.0073(19) 0.003(2) 0.005(2) O9 0.013(3) 0.016(2) 0.017(2) 0.0035(18) -0.002(2) 0.0045(19) O10 0.019(3) 0.020(2) 0.019(2) 0.0015(17) 0.010(2) 0.0023(19) O11 0.017(2) 0.017(2) 0.014(2) 0.0026(16) 0.005(2) 0.0020(19) O12 0.046(3) 0.0165(17) 0.041(3) 0.0048(19) 0.020(2) 0.005(2) O1W 0.010(2) 0.018(2) 0.023(2) -0.012(2) 0.0041(18) -0.003(2) O2W 0.021(3) 0.027(2) 0.016(2) -0.006(2) 0.003(2) 0.013(2) O3W 0.031(3) 0.020(3) 0.057(4) 0.010(2) 0.010(3) 0.002(2) O4W 0.028(3) 0.036(3) 0.041(3) -0.001(3) 0.021(3) 0.002(2) O5W 0.022(3) 0.018(2) 0.045(3) -0.009(3) 0.021(2) -0.004(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' 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' 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 O7 146.83(13) 3_676 . O1 Eu1 O1W 79.64(13) 3_676 . O7 Eu1 O1W 75.31(14) . . O1 Eu1 O2 127.67(13) 3_676 . O7 Eu1 O2 74.00(14) . . O1W Eu1 O2 149.29(13) . . O1 Eu1 O6 79.67(13) 3_676 3_676 O7 Eu1 O6 133.25(13) . 3_676 O1W Eu1 O6 128.36(13) . 3_676 O2 Eu1 O6 76.03(13) . 3_676 O1 Eu1 O4 80.70(12) 3_676 . O7 Eu1 O4 74.28(13) . . O1W Eu1 O4 81.11(13) . . O2 Eu1 O4 89.27(12) . . O6 Eu1 O4 140.03(13) 3_676 . O1 Eu1 O11 123.77(13) 3_676 . O7 Eu1 O11 74.01(13) . . O1W Eu1 O11 82.26(13) . . O2 Eu1 O11 90.68(12) . . O6 Eu1 O11 71.32(13) 3_676 . O4 Eu1 O11 146.99(14) . . O1 Eu1 O1 70.27(13) 3_676 . O7 Eu1 O1 119.43(12) . . O1W Eu1 O1 141.29(12) . . O2 Eu1 O1 58.04(12) . . O6 Eu1 O1 70.00(12) 3_676 . O4 Eu1 O1 70.68(12) . . O11 Eu1 O1 134.85(12) . . O1 Eu1 O10 75.76(12) 3_676 . O7 Eu1 O10 111.61(13) . . O1W Eu1 O10 64.86(13) . . O2 Eu1 O10 129.40(12) . . O6 Eu1 O10 64.36(13) 3_676 . O4 Eu1 O10 141.31(12) . . O11 Eu1 O10 48.46(13) . . O1 Eu1 O10 126.71(12) . . O1 Eu1 Eu1 37.36(9) 3_676 3_676 O7 Eu1 Eu1 143.12(9) . 3_676 O1W Eu1 Eu1 113.53(9) . 3_676 O2 Eu1 Eu1 90.66(10) . 3_676 O6 Eu1 Eu1 71.10(9) 3_676 3_676 O4 Eu1 Eu1 72.15(10) . 3_676 O11 Eu1 Eu1 140.85(10) . 3_676 O1 Eu1 Eu1 32.91(7) . 3_676 O10 Eu1 Eu1 104.08(9) . 3_676 O3 P1 O2 116.2(2) . . O3 P1 O1 114.7(2) . . O2 P1 O1 106.3(2) . . O3 P1 C7 104.2(2) . . O2 P1 C7 109.1(3) . . O1 P1 C7 105.8(2) . . O6 P2 O4 114.7(2) . . O6 P2 O5 112.2(2) . . O4 P2 O5 111.0(2) . . O6 P2 C8 111.6(3) . . O4 P2 C8 106.0(2) . . O5 P2 C8 100.2(3) . . O7 P3 O9 118.3(2) . . O7 P3 O8 108.8(3) . . O9 P3 O8 110.3(2) . . O7 P3 C9 108.9(3) . . O9 P3 C9 104.9(3) . . O8 P3 C9 104.9(3) . . C1 N1 C7 111.1(4) . . C1 N1 C6 114.9(4) . . C7 N1 C6 110.0(4) . . C1 N1 H1C 107.9 . . C7 N1 H1C 105.7 . . C6 N1 H1C 106.8 . . C2 N2 C3 117.1(5) . . C2 N2 C8 115.7(5) . . C3 N2 C8 113.3(5) . . C9 N3 C5 114.2(5) . . C9 N3 C4 108.4(5) . . C5 N3 C4 110.4(4) . . C9 N3 H3C 107.6 . . C5 N3 H3C 108.4 . . C4 N3 H3C 107.4 . . O12 N4 O10 122.4(5) . . O12 N4 O11 119.6(5) . . O10 N4 O11 118.0(5) . . N1 C1 C2 109.9(4) . . N1 C1 H1A 109.7 . . C2 C1 H1A 109.7 . . N1 C1 H1B 109.7 . . C2 C1 H1B 109.7 . . H1A C1 H1B 108.2 . . N2 C2 C1 110.1(5) . . N2 C2 H2A 109.6 . . C1 C2 H2A 109.6 . . N2 C2 H2B 109.6 . . C1 C2 H2B 109.6 . . H2A C2 H2B 108.2 . . N2 C3 C4 110.2(5) . . N2 C3 H3A 109.6 . . C4 C3 H3A 109.6 . . N2 C3 H3B 109.6 . . C4 C3 H3B 109.6 . . H3A C3 H3B 108.1 . . C3 C4 N3 110.8(5) . . C3 C4 H4A 109.5 . . N3 C4 H4A 109.5 . . C3 C4 H4B 109.5 . . N3 C4 H4B 109.5 . . H4A C4 H4B 108.1 . . C6 C5 N3 115.4(5) . . C6 C5 H5A 108.4 . . N3 C5 H5A 108.4 . . C6 C5 H5B 108.4 . . N3 C5 H5B 108.4 . . H5A C5 H5B 107.5 . . C5 C6 N1 116.0(5) . . C5 C6 H6A 108.3 . . N1 C6 H6A 108.3 . . C5 C6 H6B 108.3 . . N1 C6 H6B 108.3 . . H6A C6 H6B 107.4 . . N1 C7 P1 114.7(4) . . N1 C7 H7A 108.6 . . P1 C7 H7A 108.6 . . N1 C7 H7B 108.6 . . P1 C7 H7B 108.6 . . H7A C7 H7B 107.6 . . N2 C8 P2 111.3(4) . . N2 C8 H8A 109.4 . . P2 C8 H8A 109.4 . . N2 C8 H8B 109.4 . . P2 C8 H8B 109.4 . . H8A C8 H8B 108.0 . . N3 C9 P3 116.2(4) . . N3 C9 H9A 108.2 . . P3 C9 H9A 108.2 . . N3 C9 H9B 108.2 . . P3 C9 H9B 108.2 . . H9A C9 H9B 107.4 . . P1 O1 Eu1 154.2(2) . 3_676 P1 O1 Eu1 93.80(17) . . Eu1 O1 Eu1 109.73(13) 3_676 . P1 O2 Eu1 101.77(19) . . P2 O4 Eu1 126.2(2) . . P2 O5 H5C 109.5 . . P2 O6 Eu1 138.0(2) . 3_676 P3 O7 Eu1 173.4(2) . . P3 O8 H8C 119(5) . . N4 O10 Eu1 91.5(3) . . N4 O11 Eu1 100.2(3) . . Eu1 O1W H1WA 127.2 . . Eu1 O1W H1WB 120.7 . . H1WA O1W H1WB 111.0 . . H2WA O2W H2WB 110.5 . . H3WA O3W H3WB 110.9 . . H4WA O4W H4WB 110.4 . . H5WB O5W H5WA 107.4 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Eu1 O1 2.326(4) 3_676 Eu1 O7 2.361(4) . Eu1 O1W 2.410(4) . Eu1 O2 2.418(4) . Eu1 O6 2.455(4) 3_676 Eu1 O4 2.483(3) . Eu1 O11 2.515(4) . Eu1 O1 2.598(4) . Eu1 O10 2.717(4) . Eu1 Eu1 4.0299(7) 3_676 P1 O3 1.509(4) . P1 O2 1.514(4) . P1 O1 1.534(4) . P1 C7 1.823(5) . P2 O6 1.505(4) . P2 O4 1.534(4) . P2 O5 1.566(4) . P2 C8 1.830(5) . P3 O7 1.493(4) . P3 O9 1.505(4) . P3 O8 1.585(4) . P3 C9 1.825(6) . N1 C1 1.513(6) . N1 C7 1.515(7) . N1 C6 1.516(7) . N1 H1C 0.8889 . N2 C2 1.440(8) . N2 C3 1.461(7) . N2 C8 1.477(7) . N3 C9 1.506(7) . N3 C5 1.525(7) . N3 C4 1.529(7) . N3 H3C 0.8905 . N4 O12 1.238(6) . N4 O10 1.238(6) . N4 O11 1.277(6) . C1 C2 1.529(8) . C1 H1A 0.9900 . C1 H1B 0.9900 . C2 H2A 0.9900 . C2 H2B 0.9900 . C3 C4 1.529(8) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 C6 1.498(8) . C5 H5A 0.9900 . C5 H5B 0.9900 . C6 H6A 0.9900 . C6 H6B 0.9900 . C7 H7A 0.9900 . C7 H7B 0.9900 . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 H9A 0.9900 . C9 H9B 0.9900 . O1 Eu1 2.326(4) 3_676 O5 H5C 0.8400 . O6 Eu1 2.455(4) 3_676 O8 H8C 0.77(6) . O1W H1WA 0.8500 . O1W H1WB 0.8499 . O2W H2WA 0.8500 . O2W H2WB 0.8501 . O3W H3WA 0.8500 . O3W H3WB 0.8500 . O4W H4WA 0.8500 . O4W H4WB 0.8500 . O5W H5WB 0.8498 . O5W H5WA 0.8500 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5W H5WA O3W 0.85 2.00 2.778(6) 152.6 2_655 O5W H5WB O3 0.85 1.94 2.759(5) 160.1 . O4W H4WB O5 0.85 2.26 2.968(6) 141.3 3_566 O4W H4WA O2W 0.85 2.30 3.086(6) 153.3 3_666 O4W H4WA O10 0.85 2.57 3.016(6) 113.7 1_545 O3W H3WB O9 0.85 1.87 2.711(5) 171.8 1_545 O3W H3WA O11 0.85 2.09 2.930(7) 170.3 1_545 O2W H2WB O9 0.85 1.86 2.684(6) 162.8 4_676 O2W H2WA O12 0.85 2.09 2.933(6) 175.2 3_676 O2W H2WA O10 0.85 2.57 3.191(5) 130.4 3_676 O2W H2WA N4 0.85 2.59 3.386(6) 156.0 3_676 O1W H1WB O4W 0.85 2.02 2.855(6) 165.2 1_565 O1W H1WA O5W 0.85 1.83 2.677(6) 173.5 1_455 O8 H8C O2W 0.77(6) 1.84(6) 2.604(6) 172(7) 2_655 O5 H5C O3 0.84 1.73 2.565(5) 175.6 3_676 C9 H9B O4W 0.99 2.43 3.401(8) 166.3 2 C6 H6B O11 0.99 2.42 3.302(7) 148.0 2_645 C6 H6A O8 0.99 2.58 3.195(7) 120.3 . C6 H6A O2 0.99 2.30 3.077(7) 134.8 . C5 H5B O8 0.99 2.52 3.062(7) 114.2 . C4 H4A O3W 0.99 2.39 3.371(8) 173.3 2 C3 H3A O12 0.99 2.51 3.206(7) 127.4 1_545 C2 H2B O10 0.99 2.52 3.439(8) 154.0 3_676 C1 H1B O2 0.99 2.21 3.174(7) 163.0 2_645 N3 H3C O4 0.89 2.04 2.924(6) 174.9 . N1 H1C O4 0.89 2.19 3.042(6) 161.5 . N1 H1C O4 0.89 2.19 3.042(6) 161.5 . N3 H3C O4 0.89 2.04 2.924(6) 174.9 . C1 H1B O2 0.99 2.21 3.174(7) 163.0 2_645 C2 H2B O10 0.99 2.52 3.439(8) 154.0 3_676 C3 H3A O12 0.99 2.51 3.206(7) 127.4 1_545 C4 H4A O3W 0.99 2.39 3.371(8) 173.3 2 C5 H5B O8 0.99 2.52 3.062(7) 114.2 . C6 H6A O2 0.99 2.30 3.077(7) 134.8 . C6 H6A O8 0.99 2.58 3.195(7) 120.3 . C6 H6B O11 0.99 2.42 3.302(7) 148.0 2_645 C9 H9B O4W 0.99 2.43 3.401(8) 166.3 2 O5 H5C O3 0.84 1.73 2.565(5) 175.6 3_676 O8 H8C O2W 0.77(6) 1.84(6) 2.604(6) 172(7) 2_655 O1W H1WA O5W 0.85 1.83 2.677(6) 173.5 1_455 O1W H1WB O4W 0.85 2.02 2.855(6) 165.2 1_565 O2W H2WA O12 0.85 2.09 2.933(6) 175.2 3_676 O2W H2WB O9 0.85 1.86 2.684(6) 162.8 4_676 O3W H3WA O11 0.85 2.09 2.930(7) 170.3 1_545 O3W H3WB O9 0.85 1.87 2.711(5) 171.8 1_545 O4W H4WA O2W 0.85 2.30 3.086(6) 153.3 3_666 O4W H4WB O5 0.85 2.26 2.968(6) 141.3 3_566 O5W H5WB O3 0.85 1.94 2.759(5) 160.1 . 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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C7 N1 C1 C2 116.6(5) . . . . C6 N1 C1 C2 -117.8(6) . . . . C3 N2 C2 C1 77.2(6) . . . . C8 N2 C2 C1 -145.0(5) . . . . N1 C1 C2 N2 51.9(7) . . . . C2 N2 C3 C4 -142.9(5) . . . . C8 N2 C3 C4 78.3(6) . . . . N2 C3 C4 N3 40.4(7) . . . . C9 N3 C4 C3 -174.7(5) . . . . C5 N3 C4 C3 59.4(6) . . . . C9 N3 C5 C6 103.6(6) . . . . C4 N3 C5 C6 -133.9(5) . . . . N3 C5 C6 N1 65.5(7) . . . . C1 N1 C6 C5 51.2(7) . . . . C7 N1 C6 C5 177.4(5) . . . . C1 N1 C7 P1 -154.2(4) . . . . C6 N1 C7 P1 77.4(5) . . . . O3 P1 C7 N1 -172.5(4) . . . . O2 P1 C7 N1 -47.8(5) . . . . O1 P1 C7 N1 66.2(5) . . . . C2 N2 C8 P2 86.0(5) . . . . C3 N2 C8 P2 -134.7(4) . . . . O6 P2 C8 N2 -95.1(4) . . . . O4 P2 C8 N2 30.4(5) . . . . O5 P2 C8 N2 145.9(4) . . . . C5 N3 C9 P3 -61.8(6) . . . . C4 N3 C9 P3 174.6(4) . . . . O7 P3 C9 N3 -48.2(5) . . . . O9 P3 C9 N3 -175.7(4) . . . . O8 P3 C9 N3 68.1(5) . . . . O3 P1 O1 Eu1 -29.6(6) . . . 3_676 O2 P1 O1 Eu1 -159.4(5) . . . 3_676 C7 P1 O1 Eu1 84.6(5) . . . 3_676 O3 P1 O1 Eu1 126.68(19) . . . . O2 P1 O1 Eu1 -3.1(2) . . . . C7 P1 O1 Eu1 -119.1(2) . . . . O3 P1 O2 Eu1 -125.5(2) . . . . O1 P1 O2 Eu1 3.4(2) . . . . C7 P1 O2 Eu1 117.1(2) . . . . O6 P2 O4 Eu1 -54.3(3) . . . . O5 P2 O4 Eu1 74.2(3) . . . . C8 P2 O4 Eu1 -177.9(3) . . . . O4 P2 O6 Eu1 25.6(4) . . . 3_676 O5 P2 O6 Eu1 -102.3(3) . . . 3_676 C8 P2 O6 Eu1 146.1(3) . . . 3_676 O12 N4 O10 Eu1 -165.6(5) . . . . O11 N4 O10 Eu1 12.9(5) . . . . O12 N4 O11 Eu1 164.4(5) . . . . O10 N4 O11 Eu1 -14.2(6) . . . .