#------------------------------------------------------------------------------
#$Date: 2024-07-11 04:50:02 +0300 (Thu, 11 Jul 2024) $
#$Revision: 293365 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312547.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312547
loop_
_publ_author_name
'Araujo Junior, Cleber R.'
'Oliveira, Willian X. C.'
'Pinheiro, Carlos B.'
'Pedroso, Emerson F.'
'Nunes, Wallace C.'
'Almeida, Adriele A de'
'Knobel, Marcelo'
'Julve, Miguel'
'Pereira, Cynthia L. M.'
_publ_section_title
;
Crystal structure and cryomagnetic study of a mononuclear erbium(III)
oxamate inclusion complex.
;
_journal_coeditor_code DG3058
_journal_issue 8
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624005977
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac
'(C16 H36 N1) [Er (C11 H12 N1 O3)4 (H2 O1)], 3C2 H6 O S, 1.5H2 O1'
_chemical_formula_moiety
'C16 H36 N1 +, C44 H50 Er N4 O13 -, 3(C2 H6 O S), 1.5(H2 O1)'
_chemical_formula_sum 'C66 H106 Er N5 O17.5 S3'
_chemical_formula_weight 1512.99
_chemical_name_systematic
'Tetrabutylammonium aqua[N-(2,4,6-trimethylphenyl)oxamato]erbium(III)--dimethylsulfoxide--water (1/3/1.5)'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90.1720(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 15.39670(10)
_cell_length_b 30.6741(2)
_cell_length_c 16.06120(10)
_cell_measurement_reflns_used 55180
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 78.8230
_cell_measurement_theta_min 2.8810
_cell_volume 7585.35(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury software (Macrae et al., 2020) and
Vesta (Momma & Izumi, 2011)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature 220(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0606
_diffrn_reflns_av_unetI/netI 0.0356
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 36
_diffrn_reflns_limit_k_min -36
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 103272
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 68.248
_diffrn_reflns_theta_min 2.881
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 3.364
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.135
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2022)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.325
_exptl_crystal_description plate
_exptl_crystal_F_000 3172
_exptl_crystal_size_max 0.442
_exptl_crystal_size_mid 0.242
_exptl_crystal_size_min 0.044
_refine_diff_density_max 1.320
_refine_diff_density_min -1.038
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 843
_refine_ls_number_reflns 13894
_refine_ls_number_restraints 7
_refine_ls_restrained_S_all 1.043
_refine_ls_R_factor_all 0.0424
_refine_ls_R_factor_gt 0.0372
_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^)+(0.0501P)^2^+7.8003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0962
_refine_ls_wR_factor_ref 0.1005
_reflns_number_gt 12290
_reflns_number_total 13894
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dg3058sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C66 H106 Er N5 O17.50 S3'
_cod_database_code 2312547
_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.
;
_shelx_hkl_file
;
0 0 1 16.2225 16.2933 39
0 0 2 55425.3 3310.90 42
0 0 2 50289.5 3252.25 31
0 0 2 54877.6 3299.28 39
0 0 3 39.2673 66.9667 42
0 0 3 16.5542 51.5534 39
0 0 4 6576.34 559.815 42
0 0 4 7089.68 546.443 39
0 0 5 29.2638 81.4787 8
0 0 5-35.4999 102.876 1
0 0 5 29.0157 90.3229 39
0 0 5-34.3454 106.913 42
0 0 6 55188.1 3798.08 42
0 0 6 56298.5 3809.25 1
0 0 6 59898.5 3781.35 8
0 0 7-43.8976 117.028 8
0 0 7-51.5741 165.813 42
0 0 7 53.3742 148.613 1
0 0 8 196121. 12840.1 1
0 0 8 206399. 12837.1 42
0 0 8 196631. 12561.4 35
0 0 8 211567. 12789.5 8
0 0 9 60.9923 155.020 8
0 0 9-71.7045 207.791 42
0 0 9 42.4836 61.3008 35
0 0 9-74.5312 189.430 1
0 0 10 1320.33 339.086 42
0 0 10 1121.48 324.891 1
0 0 11-69.0095 109.491 2
0 0 11-97.8579 222.512 1
0 0 11-18.6709 83.7001 3
0 0 11-237.490 220.459 8
0 0 12 902.129 126.697 11
0 0 12 971.442 129.295 9
0 0 12 1122.55 148.606 10
0 0 12 1083.38 180.999 2
0 0 12 1079.55 351.695 1
0 0 12 796.722 118.666 4
0 0 12 875.811 140.897 3
0 0 12 677.160 144.629 6
0 0 12 753.913 132.211 7
0 0 12 1305.35 310.136 8
0 0 12 1065.61 140.402 5
0 0 13-16.7001 79.4465 9
0 0 13 95.6138 76.8878 10
0 0 13-68.0780 93.8113 11
0 0 13-31.0204 66.0111 4
0 0 13-26.8327 123.912 2
0 0 13-231.347 383.328 1
0 0 13-86.0790 99.3887 3
0 0 13-168.881 121.192 6
0 0 13 41.0556 77.4260 7
0 0 13-92.5427 128.851 8
0 0 13 34.6726 63.9010 5
0 0 14 23339.0 1709.03 2
0 0 14 25010.9 1686.20 3
0 0 14 23708.2 1653.35 4
0 0 14 24384.9 1665.29 11
0 0 14 27058.1 1667.62 9
0 0 14 25936.7 1675.49 10
0 0 14 26427.9 1693.90 6
0 0 14 25665.6 1665.69 5
0 0 14 24259.2 1679.26 7
0 0 15-85.1127 104.065 3
0 0 15-26.8172 131.136 2
0 0 15-47.7559 92.3047 4
0 0 15-131.978 101.692 11
0 0 15-36.6898 64.3330 10
0 0 15 20.7251 91.2806 6
0 0 15-40.3576 74.3767 7
0 0 15-16.3145 62.9504 5
0 0 16 15743.9 1037.41 4
0 0 16 14263.1 1050.55 3
0 0 16 13956.5 1074.95 2
0 0 16 14879.6 1035.20 11
0 0 16 15719.5 1040.10 10
0 0 16 15948.9 1035.56 9
0 0 16 15687.6 1057.91 6
0 0 17 63.5839 109.105 2
0 0 17-80.9557 86.1125 4
0 0 17-22.5548 67.8772 11
0 0 17-36.3196 53.3578 9
0 0 17-37.1723 55.5081 10
0 0 17-76.2086 90.8856 6
0 0 18 88.9818 76.9638 6
0 0 18 334.287 79.1525 4
0 1 1 5706.74 379.070 42
0 -1 1 5380.34 373.862 8
0 -1 1 5367.78 373.746 39
0 1 1 5739.58 380.324 1
0 1 2 25503.7 1586.35 1
0 1 2 26028.9 1585.61 42
0 1 2 23143.0 1534.00 32
0 1 2 23677.9 1536.11 33
0 -1 2 24206.3 1573.43 8
0 -1 2 26878.0 1579.26 39
0 -1 3 1082.79 133.301 39
0 1 3 1190.34 145.803 42
0 1 3 751.428 75.0134 32
0 1 3 811.165 74.1502 31
0 -1 4 13281.9 931.436 39
0 1 4 12540.3 935.267 42
0 1 5 3534.12 390.336 42
0 -1 5 4153.88 384.800 39
0 -1 5 4192.27 385.108 8
0 1 5 3491.79 386.373 1
0 1 6 25595.7 1808.08 42
0 1 6 26572.3 1820.37 1
0 -1 6 24716.7 1780.82 8
0 -1 7 1092.45 214.913 8
0 1 7 727.268 212.718 42
0 1 7 1471.72 266.074 1
0 1 8 5580.28 598.221 42
0 -1 8 5272.45 403.711 35
0 -1 8 6179.22 585.420 8
0 1 8 5489.28 604.518 1
0 -1 9 242.851 170.612 8
0 -1 9 399.501 86.6342 35
0 1 9 705.178 227.884 1
0 1 9 201.578 180.600 42
0 -1 10 11891.9 1054.34 8
0 1 10 11112.6 1065.21 42
0 1 10 11801.7 1096.80 1
0 -1 11 2508.04 250.185 3
0 1 11 2356.60 262.824 2
0 1 11 2396.83 471.501 1
0 -1 11 2594.32 226.059 4
0 -1 11 2680.63 444.241 8
0 -1 12 10609.6 805.413 3
0 -1 12 10976.3 779.066 4
0 1 12 11376.0 829.976 2
0 1 12 11578.3 1167.41 1
0 1 12 10864.5 780.956 4
0 1 12 11519.7 787.886 9
0 -1 12 10842.0 1073.63 8
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0 -1 12 12346.9 813.261 10
0 -1 12 12143.0 796.711 9
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0 -1 12 11597.9 792.874 11
0 -1 12 11551.9 792.275 5
0 -1 12 10654.8 799.148 7
0 1 12 12021.3 800.828 5
0 1 12 10870.0 806.915 7
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0 -1 12 11050.9 807.259 6
0 1 13 1777.95 200.209 4
0 -1 13 2168.98 207.982 4
0 1 13 2608.15 495.036 1
0 1 13 2238.90 257.047 2
0 -1 13 2017.53 231.721 3
0 1 13 2351.36 224.068 10
0 -1 13 1834.03 210.058 11
0 -1 13 2083.47 224.802 10
0 -1 13 1656.46 200.122 9
0 1 13 2376.59 214.283 9
0 1 13 1845.91 210.000 11
0 -1 13 1569.91 392.327 8
0 1 13 2125.55 244.818 6
0 1 13 2067.85 234.869 7
0 1 13 1995.83 214.627 5
0 -1 13 1978.10 223.380 7
0 -1 13 2214.61 236.500 6
0 -1 13 2207.28 214.905 5
0 1 14-17.5131 78.4093 11
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0 -1 14-17.6847 72.5181 9
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0 -1 14 63.9985 80.3443 4
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0 -1 14-123.112 127.765 6
0 -1 14 118.876 88.6950 7
0 -1 14 16.6968 64.4063 5
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0 1 14 66.3268 77.4949 7
0 -1 15 143.454 85.1595 4
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0 1 15 150.602 118.458 2
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0 1 15 316.410 90.4395 10
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0 1 16 4043.34 332.008 4
0 -1 16 3881.85 330.269 4
0 -1 16 4152.44 334.117 9
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0 -1 16 4451.10 342.752 10
0 1 16 4150.63 327.387 9
0 -1 16 3567.59 322.615 11
0 1 16 4228.61 339.230 11
0 -1 16 3895.48 347.084 6
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0 1 16 3887.83 349.260 7
0 1 17 454.806 133.888 2
0 1 17 436.330 95.6813 4
0 -1 17 409.541 101.295 4
0 -1 17 352.557 86.4231 10
0 -1 17 511.485 92.5555 9
0 1 17 453.827 81.3080 10
0 1 17 684.843 98.9725 11
0 -1 17 468.437 82.7063 11
0 1 17 225.708 96.5055 6
0 -1 17 387.227 101.572 6
0 -1 18 20633.9 1354.53 6
0 1 18 20166.6 1359.40 6
0 1 18 20764.4 1352.13 4
0 -1 18 21407.8 1361.85 4
0 2 0 341328. 21382.6 48
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0 -2 1 116.072 27.4119 39
0 2 1 128.151 29.3448 42
0 2 1 133.297 32.3439 1
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0 2 2 7081.05 463.279 42
0 -2 2 6245.59 450.862 8
0 2 2 5846.98 427.397 33
0 2 3 5314.80 398.670 1
0 -2 3 5165.47 384.698 39
0 2 3 5274.96 394.638 42
0 2 3 4550.20 335.006 33
0 2 3 4447.73 330.439 32
0 -2 3 4827.80 382.216 8
0 2 4 275.758 107.316 1
0 -2 4 243.092 91.3914 39
0 2 4 144.133 95.3748 42
0 -2 4 65.8036 67.0903 8
0 2 4 251.263 42.9158 31
0 2 4 175.741 45.1194 32
0 -2 5 84.5384 81.7034 8
0 2 5 30.7350 95.7086 42
0 -2 5 56.8426 82.4038 39
0 2 5 64.1519 99.8812 1
0 2 5 36.6755 25.8360 32
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0 2 6 31937.2 2117.06 1
0 2 6 29713.0 2097.16 42
0 -2 7 4986.11 491.714 8
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0 2 7 3965.45 487.142 1
0 2 8 74245.8 4721.56 1
0 -2 8 71294.2 4470.78 35
0 2 8 68926.4 4462.54 35
0 2 8 72584.3 4702.21 42
0 -2 8 68847.9 4670.79 8
0 -2 9 1576.45 163.607 35
0 2 9 2085.50 361.051 42
0 -2 9 1233.08 283.500 8
0 2 9 1255.36 291.959 1
0 2 10 1014.16 280.496 42
0 -2 10 879.292 262.903 8
0 2 10 1216.69 293.735 1
0 -2 11 4808.08 618.644 8
0 -2 11 4880.52 409.461 6
0 2 11 5327.03 680.407 1
0 -2 11 4936.54 430.497 2
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0 2 11 5167.92 403.033 3
0 -2 11 4909.20 407.075 3
0 -2 11 5025.55 385.255 4
0 -2 12 2562.54 252.242 11
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0 2 12 3020.62 265.782 5
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0 -2 12 2462.65 238.114 4
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0 2 12 2553.88 468.473 1
0 -2 13 4731.89 386.896 11
0 2 13 4022.32 361.651 11
0 2 13 4879.85 371.511 9
0 -2 13 4662.38 376.536 9
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0 -2 13 4462.84 368.586 5
0 2 13 4456.93 396.322 7
0 -2 13 4313.78 374.527 7
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0 -2 13 4417.44 388.099 6
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0 -2 13 5304.13 375.368 4
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0 -2 13 4924.34 399.716 3
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0 2 14 11898.7 895.503 12
0 -2 14 13609.7 951.152 10
0 -2 14 14270.5 942.028 9
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0 2 14 13809.8 935.168 10
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0 2 14 14534.6 974.371 6
0 2 14 13335.4 938.861 5
0 -2 14 13457.1 939.294 7
0 2 14 13757.8 965.256 7
0 -2 14 12976.9 923.524 4
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0 -2 14 13308.8 951.860 3
0 2 14 14063.2 931.440 4
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0 2 15 395.689 88.7740 9
0 -2 15 354.031 102.450 10
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0 -2 16 8446.54 583.436 9
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0 2 16 7802.60 608.587 6
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0 -2 16 8259.17 578.579 4
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0 2 16 7310.26 603.058 2
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0 -2 17 778.848 100.007 11
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0 2 18 366.432 72.2523 4
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0 2 19 177.423 50.2377 6
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0 3 -1 1405.89 102.568 48
0 -3 1 1152.41 111.003 1
0 3 1 1396.31 113.755 1
0 3 1 1336.47 119.143 27
0 3 1 1345.10 111.999 42
0 -3 1 1357.05 114.140 42
0 -3 1 1213.90 107.916 8
0 3 1 1396.23 109.146 8
0 3 1 1550.80 110.639 39
0 -3 1 1349.23 109.996 39
0 3 2 26165.3 1737.61 33
0 3 2 26939.0 1753.68 1
0 -3 2 25589.2 1755.23 1
0 3 -2 27198.9 1716.11 48
0 3 2 29290.6 1747.16 8
0 -3 2 25948.3 1744.29 8
0 3 2 28869.6 1746.10 39
0 -3 2 26588.4 1746.62 39
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0 -3 3 4563.62 420.605 1
0 3 3 5636.66 432.163 1
0 3 3 5592.79 423.755 42
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0 -3 3 5438.68 418.634 39
0 -3 3 5305.60 413.340 8
0 3 3 5931.32 415.192 8
0 3 3 4865.31 381.632 33
0 3 4 12408.3 846.203 42
0 -3 4 11092.0 848.531 42
0 -3 4 12615.0 840.711 39
0 3 4 13217.2 834.931 39
0 -3 4 11826.2 854.477 1
0 3 4 13958.5 865.111 1
0 3 4 12505.7 784.711 33
0 3 -4 10624.5 733.863 33
0 3 4 11864.2 776.048 32
0 -3 4 11351.8 831.533 8
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0 3 5 3562.98 268.737 31
0 3 5 3776.82 290.480 32
0 3 5 3983.19 356.112 8
0 -3 5 3473.70 359.854 8
0 -3 5 4042.55 387.685 1
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0 3 5 3972.56 376.211 42
0 -3 5 3786.47 387.797 42
0 3 6 10511.6 795.861 32
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0 3 6 13444.1 955.848 1
0 -3 6 13702.3 973.418 1
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10 15 8 5382.11 425.851 35
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14 11 -3 1369.37 157.085 25
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14 11 4 649.550 107.916 25
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14 11 7 1548.72 169.552 35
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14 -11 8 1762.65 186.000 35
14 11 8 1893.48 176.760 35
14 11 8 2395.51 247.679 37
14 11 8 1879.71 183.011 47
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14 -11 9 180.926 63.5524 35
14 11 9 178.963 51.6796 35
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14 12 -9-34.2821 52.0085 25
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14 12 -8 3940.72 287.680 25
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14 12 -5 11925.8 780.931 25
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14 -12 6 3121.76 289.656 29
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14 12 6 3666.27 281.575 47
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14 12 10 202.287 42.2404 12
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19 6 2 99.9030 34.2955 29
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0 0 0 0.00 0.00 0
TITL ErTMPA_LT_auto in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 1.54184 15.396651 30.674081 16.061152 90.0000 90.1721 90.0000
ZERR 1.00 0.000099 0.000204 0.000095 0.0000 0.0006 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N O S Er
UNIT 264.00 400.00 20.00 70.24 12.00 4.00
REM CrysAlisPro recorded range (K): Min=219.9; max=220.0; aver:220.0
TEMP -53
SIZE 0.04 0.24 0.44
TREF
HKLF 4
END
;
_shelx_hkl_checksum 90547
_shelx_res_file
;
TITL ErTMPA_LT_auto in P2(1)/n
shelx.res
created by SHELXL-2018/3 at 11:54:17 on 21-May-2024
CELL 1.54184 15.3967 30.6741 16.0612 90.000 90.172 90.000
ZERR 4.00 0.0001 0.0002 0.0001 0.000 0.001 0.000
LATT 1
SYMM 1/2 - X, 1/2 + Y, 1/2 - Z
SFAC C H N O S ER
UNIT 264 424 20 70 12 4
MERG 2
DFIX 0.9 0.001 H13A O13 H13B O13 H18E O18 H18F O18
DFIX 1.4 0.002 H13A H13B H18E H18F
eqiv $15 1-x, 1-y, -z
DFIX 1.9 0.05 H18E O10_$15
shel 50 0.83
eqiv $11 1/2+x, 3/2-y, -1/2+z
htab N1 O8_$11
eqiv $12 1/2+x, 3/2-y, 1/2+z
htab N2 O11_$12
eqiv $13 -1/2+x, 3/2-y, 1/2+z
htab N3 O2_$13
eqiv $14 -1/2+x, 3/2-y, -1/2+z
htab N4 O5_$14
htab O13 O17
eqiv $16 1-x, 1-y, -z
htab O13 O18_$16
htab O18 O10_$16
htab O18 O16_$16
FMAP 2
PLAN 20
ACTA
LIST 4
L.S. 50
WGHT 0.050100 7.800300
FVAR 1.16319 0.63157 0.52412
C1 1 0.739248 0.729306 -0.057856 11.00000 0.01880 0.03244 =
0.02106 0.00112 0.00093 0.00228
C2 1 0.690874 0.770924 -0.086354 11.00000 0.02135 0.03391 =
0.02079 0.00272 -0.00029 0.00133
C3 1 0.681878 0.828046 -0.189704 11.00000 0.02556 0.03828 =
0.02922 0.01261 0.00753 0.00649
C4 1 0.699218 0.868143 -0.154346 11.00000 0.03544 0.04546 =
0.03719 0.01236 0.00491 0.00118
C5 1 0.659299 0.904791 -0.189052 11.00000 0.04261 0.03864 =
0.05365 0.01241 0.00842 0.00097
AFIX 43
H5 2 0.668586 0.931946 -0.164860 11.00000 -1.20000
AFIX 0
C6 1 0.606324 0.901730 -0.258460 11.00000 0.03397 0.04858 =
0.05809 0.02496 0.00339 0.00537
C7 1 0.592778 0.861023 -0.293402 11.00000 0.03115 0.05620 =
0.04331 0.01964 -0.00288 0.00193
AFIX 43
H7 2 0.558664 0.858746 -0.341086 11.00000 -1.20000
AFIX 0
C8 1 0.628509 0.823658 -0.259446 11.00000 0.02789 0.04909 =
0.03333 0.01029 0.00518 0.00404
C9 1 0.761888 0.871996 -0.082504 11.00000 0.06318 0.05375 =
0.05185 0.00443 -0.01194 -0.00199
AFIX 33
H9A 2 0.766214 0.901963 -0.065765 11.00000 -1.50000
H9B 2 0.741376 0.854818 -0.036632 11.00000 -1.50000
H9C 2 0.818007 0.861660 -0.099338 11.00000 -1.50000
AFIX 0
C10 1 0.563809 0.941830 -0.296062 11.00000 0.05734 0.05861 =
0.09901 0.03645 -0.01125 0.00962
AFIX 33
H10A 2 0.529658 0.933442 -0.343534 11.00000 -1.50000
H10B 2 0.527016 0.955328 -0.255375 11.00000 -1.50000
H10C 2 0.607861 0.962082 -0.313059 11.00000 -1.50000
AFIX 0
C11 1 0.609808 0.779302 -0.295945 11.00000 0.05204 0.05536 =
0.04688 0.00289 -0.00836 0.00108
AFIX 33
H11A 2 0.640014 0.757436 -0.264391 11.00000 -1.50000
H11B 2 0.548487 0.773754 -0.293935 11.00000 -1.50000
H11C 2 0.629026 0.778496 -0.352730 11.00000 -1.50000
AFIX 0
C12 1 0.696490 0.738435 0.232469 11.00000 0.02434 0.03372 =
0.02370 0.00559 -0.00271 -0.00141
C13 1 0.731538 0.776938 0.180578 11.00000 0.02231 0.03348 =
0.02045 0.00071 -0.00226 -0.00269
C14 1 0.836457 0.836062 0.175682 11.00000 0.03064 0.03776 =
0.03132 0.00262 -0.00772 -0.01034
C15 1 0.887083 0.832226 0.104524 11.00000 0.03004 0.04304 =
0.03497 0.00101 -0.00455 -0.00659
C16 1 0.920646 0.870325 0.069856 11.00000 0.03464 0.06062 =
0.03837 0.00945 -0.00063 -0.01402
AFIX 43
H16 2 0.953853 0.868276 0.021742 11.00000 -1.20000
AFIX 0
C17 1 0.906570 0.910774 0.104006 11.00000 0.05247 0.05041 =
0.06143 0.01475 -0.00357 -0.01719
C18 1 0.860532 0.912809 0.178263 11.00000 0.08193 0.03995 =
0.07366 -0.00682 0.00695 -0.01390
AFIX 43
H18 2 0.854067 0.939598 0.204642 11.00000 -1.20000
AFIX 0
C19 1 0.823934 0.875964 0.214140 11.00000 0.06349 0.04679 =
0.04742 -0.00370 0.00831 -0.00936
C20 1 0.771371 0.878816 0.293655 11.00000 0.12553 0.06567 =
0.06743 -0.01686 0.03483 -0.01409
AFIX 33
H20A 2 0.769026 0.908586 0.311951 11.00000 -1.50000
H20B 2 0.713524 0.868404 0.283388 11.00000 -1.50000
H20C 2 0.798289 0.861265 0.335960 11.00000 -1.50000
AFIX 0
C21 1 0.942172 0.951739 0.063067 11.00000 0.09397 0.06081 =
0.10643 0.02809 0.00873 -0.03021
AFIX 33
H21A 2 0.926082 0.976781 0.095384 11.00000 -1.50000
H21B 2 1.004326 0.949887 0.060074 11.00000 -1.50000
H21C 2 0.918578 0.954401 0.007907 11.00000 -1.50000
AFIX 0
C22 1 0.905559 0.789247 0.064670 11.00000 0.05426 0.05977 =
0.06908 -0.00795 0.01959 -0.00721
AFIX 33
H22A 2 0.941438 0.793582 0.016595 11.00000 -1.50000
H22B 2 0.935196 0.770732 0.103679 11.00000 -1.50000
H22C 2 0.851923 0.775797 0.048114 11.00000 -1.50000
AFIX 0
C23 1 0.411388 0.737681 0.187040 11.00000 0.02460 0.03653 =
0.02794 -0.00577 0.00497 -0.00747
C24 1 0.461687 0.779223 0.213357 11.00000 0.02081 0.03424 =
0.02045 -0.00335 0.00100 -0.00196
C25 1 0.463754 0.840777 0.308764 11.00000 0.02361 0.03362 =
0.02887 -0.00900 0.00822 -0.00326
C26 1 0.447174 0.879653 0.266674 11.00000 0.03436 0.04375 =
0.03169 -0.00133 0.00636 0.00042
C27 1 0.480629 0.917885 0.301000 11.00000 0.05025 0.03186 =
0.04795 -0.00107 0.00606 -0.00066
AFIX 43
H27 2 0.470071 0.944194 0.274028 11.00000 -1.20000
AFIX 0
C28 1 0.529169 0.918110 0.374039 11.00000 0.04372 0.03847 =
0.05275 -0.01391 0.00516 -0.00784
C29 1 0.544163 0.878593 0.413621 11.00000 0.03724 0.04753 =
0.03754 -0.00906 -0.00485 -0.00504
AFIX 43
H29 2 0.576438 0.878280 0.462654 11.00000 -1.20000
AFIX 0
C30 1 0.512379 0.839416 0.382185 11.00000 0.02707 0.03716 =
0.03382 -0.00413 0.00356 -0.00050
C31 1 0.395745 0.880196 0.186545 11.00000 0.05297 0.06431 =
0.03832 0.00388 -0.00577 0.00294
AFIX 33
H31A 2 0.390927 0.909621 0.166700 11.00000 -1.50000
H31B 2 0.424812 0.862720 0.145614 11.00000 -1.50000
H31C 2 0.338779 0.868592 0.196349 11.00000 -1.50000
AFIX 0
C32 1 0.566061 0.959857 0.409394 11.00000 0.08899 0.04776 =
0.08939 -0.02022 -0.00613 -0.02137
AFIX 33
H32A 2 0.549561 0.983903 0.374514 11.00000 -1.50000
H32B 2 0.543815 0.964346 0.464506 11.00000 -1.50000
H32C 2 0.628246 0.957845 0.411627 11.00000 -1.50000
AFIX 0
C33 1 0.530087 0.796732 0.425081 11.00000 0.05122 0.04853 =
0.05044 0.00277 -0.01006 0.00201
AFIX 33
H33A 2 0.503085 0.773509 0.394417 11.00000 -1.50000
H33B 2 0.591625 0.791865 0.427748 11.00000 -1.50000
H33C 2 0.506852 0.797578 0.480457 11.00000 -1.50000
AFIX 0
C34 1 0.445519 0.727476 -0.083878 11.00000 0.02675 0.03742 =
0.02364 -0.00420 -0.00579 0.00492
C35 1 0.421041 0.771398 -0.043784 11.00000 0.02110 0.03530 =
0.02186 -0.00035 -0.00102 0.00405
C36 1 0.320223 0.832128 -0.043935 11.00000 0.02970 0.03892 =
0.02290 -0.00332 -0.00802 0.01000
C37 1 0.365782 0.870368 -0.058127 11.00000 0.03611 0.04412 =
0.03379 -0.00165 -0.00630 0.00575
C38 1 0.331434 0.908928 -0.027126 11.00000 0.05553 0.03798 =
0.05187 -0.00471 -0.01361 0.00377
AFIX 43
H38 2 0.361258 0.934873 -0.035994 11.00000 -1.20000
AFIX 0
C39 1 0.254103 0.909889 0.016593 11.00000 0.05460 0.05008 =
0.05249 -0.01398 -0.01026 0.02210
C40 1 0.210662 0.871149 0.029501 11.00000 0.04410 0.06660 =
0.03872 -0.00729 0.00552 0.02097
AFIX 43
H40 2 0.158474 0.871532 0.058495 11.00000 -1.20000
AFIX 0
C41 1 0.242377 0.831658 0.000599 11.00000 0.03586 0.04864 =
0.02953 0.00017 -0.00125 0.01015
C42 1 0.449561 0.870445 -0.105685 11.00000 0.04491 0.06090 =
0.06689 0.00039 0.00848 -0.00425
AFIX 33
H42A 2 0.471436 0.899694 -0.109174 11.00000 -1.50000
H42B 2 0.491217 0.852366 -0.077533 11.00000 -1.50000
H42C 2 0.439609 0.859325 -0.160765 11.00000 -1.50000
AFIX 0
C43 1 0.217319 0.952563 0.048754 11.00000 0.10697 0.07149 =
0.10260 -0.03557 -0.00583 0.04084
AFIX 33
H43A 2 0.255717 0.976014 0.034308 11.00000 -1.50000
H43B 2 0.161324 0.957573 0.024104 11.00000 -1.50000
H43C 2 0.211646 0.951099 0.108195 11.00000 -1.50000
AFIX 0
C44 1 0.195183 0.789590 0.017753 11.00000 0.05224 0.06555 =
0.06336 0.00587 0.01412 -0.00192
AFIX 33
H44A 2 0.226434 0.765794 -0.006850 11.00000 -1.50000
H44B 2 0.191195 0.785190 0.076795 11.00000 -1.50000
H44C 2 0.137852 0.790982 -0.005757 11.00000 -1.50000
AFIX 0
C51 1 0.369832 0.525520 0.289668 11.00000 0.07016 0.05790 =
0.05283 -0.00827 -0.00623 -0.00870
AFIX 33
H51A 2 0.346285 0.543315 0.333282 11.00000 -1.50000
H51B 2 0.400994 0.501475 0.313662 11.00000 -1.50000
H51C 2 0.408622 0.542638 0.256297 11.00000 -1.50000
AFIX 0
C52 1 0.296285 0.508295 0.235408 11.00000 0.05253 0.04804 =
0.04724 -0.00733 0.00264 -0.00348
AFIX 23
H52A 2 0.256664 0.491588 0.269743 11.00000 -1.20000
H52B 2 0.264291 0.532748 0.212383 11.00000 -1.20000
AFIX 0
C53 1 0.328051 0.479845 0.164946 11.00000 0.04180 0.04281 =
0.05957 -0.01444 0.00268 0.00132
AFIX 23
H53A 2 0.363912 0.456592 0.187265 11.00000 -1.20000
H53B 2 0.363474 0.497094 0.127510 11.00000 -1.20000
AFIX 0
C55 1 0.252331 0.460331 0.116994 11.00000 0.03794 0.04016 =
0.05548 -0.01425 0.00087 0.01006
AFIX 23
H55A 2 0.222142 0.483607 0.088030 11.00000 -1.20000
H55B 2 0.211998 0.447632 0.156428 11.00000 -1.20000
AFIX 0
C57 1 0.433480 0.505603 -0.123914 11.00000 0.08377 0.09322 =
0.11864 0.00630 0.02300 -0.01382
AFIX 33
H57A 2 0.461065 0.511839 -0.176098 11.00000 -1.50000
H57B 2 0.434448 0.531194 -0.089517 11.00000 -1.50000
H57C 2 0.464003 0.482421 -0.096325 11.00000 -1.50000
AFIX 0
C58 1 0.343739 0.492469 -0.138803 11.00000 0.09838 0.05896 =
0.07889 0.01738 0.00351 0.00550
AFIX 23
H58A 2 0.343425 0.467060 -0.174755 11.00000 -1.20000
H58B 2 0.313895 0.515793 -0.167953 11.00000 -1.20000
AFIX 0
C59 1 0.294933 0.482008 -0.061257 11.00000 0.07439 0.03633 =
0.07374 0.00712 -0.00111 -0.00165
AFIX 23
H59A 2 0.235574 0.474516 -0.075734 11.00000 -1.20000
H59B 2 0.293325 0.507651 -0.025952 11.00000 -1.20000
AFIX 0
C60 1 0.335443 0.444475 -0.013048 11.00000 0.04474 0.03548 =
0.05055 -0.00236 0.00575 -0.00274
AFIX 23
H60A 2 0.350361 0.421475 -0.051906 11.00000 -1.20000
H60B 2 0.388916 0.454569 0.012567 11.00000 -1.20000
AFIX 0
C61 1 0.132680 0.329954 -0.161137 11.00000 0.04600 0.06240 =
0.06645 -0.01826 -0.00477 -0.00101
AFIX 33
H61A 2 0.079863 0.314383 -0.172458 11.00000 -1.50000
H61B 2 0.144520 0.349659 -0.206131 11.00000 -1.50000
H61C 2 0.179760 0.309629 -0.155621 11.00000 -1.50000
AFIX 0
C62 1 0.123137 0.355272 -0.081698 11.00000 0.03610 0.06326 =
0.06315 -0.01352 -0.00723 -0.00149
AFIX 23
H62A 2 0.110157 0.335350 -0.036515 11.00000 -1.20000
H62B 2 0.074883 0.375418 -0.087072 11.00000 -1.20000
AFIX 0
C63 1 0.205324 0.380586 -0.060938 11.00000 0.03751 0.03627 =
0.04118 0.00359 -0.00409 0.00323
AFIX 23
H63A 2 0.253054 0.360365 -0.052896 11.00000 -1.20000
H63B 2 0.219852 0.399564 -0.107156 11.00000 -1.20000
AFIX 0
C64 1 0.193677 0.407596 0.016883 11.00000 0.02859 0.04479 =
0.05147 -0.00625 -0.00478 0.00686
AFIX 23
H64A 2 0.165194 0.389814 0.058616 11.00000 -1.20000
H64B 2 0.155401 0.431819 0.004089 11.00000 -1.20000
AFIX 0
C65 1 0.429007 0.355886 0.253851 11.00000 0.06443 0.11679 =
0.04787 -0.00311 -0.01854 0.00533
AFIX 33
H65A 2 0.463793 0.332890 0.277013 11.00000 -1.50000
H65B 2 0.462132 0.371429 0.212921 11.00000 -1.50000
H65C 2 0.411936 0.375547 0.297332 11.00000 -1.50000
AFIX 0
C67 1 0.348930 0.336657 0.213351 11.00000 0.05663 0.06146 =
0.04519 0.00354 -0.00822 0.00650
AFIX 23
H67A 2 0.316802 0.320390 0.254897 11.00000 -1.20000
H67B 2 0.366945 0.316277 0.170575 11.00000 -1.20000
AFIX 0
C68 1 0.288658 0.370437 0.174297 11.00000 0.03634 0.04710 =
0.04703 0.00007 0.00316 -0.00094
AFIX 23
H68A 2 0.233111 0.357071 0.161477 11.00000 -1.20000
H68B 2 0.278696 0.393944 0.213521 11.00000 -1.20000
AFIX 0
C69 1 0.328265 0.388559 0.095502 11.00000 0.02741 0.03521 =
0.04294 -0.00494 0.00024 0.00512
AFIX 23
H69A 2 0.334109 0.364958 0.055713 11.00000 -1.20000
H69B 2 0.386236 0.398989 0.108412 11.00000 -1.20000
AFIX 0
C48 1 0.332612 0.622360 0.149719 11.00000 0.06551 0.05223 =
0.05489 0.00103 -0.00339 -0.00770
AFIX 33
H48A 2 0.304909 0.639948 0.191341 11.00000 -1.50000
H48B 2 0.347715 0.594577 0.173163 11.00000 -1.50000
H48C 2 0.384237 0.636753 0.130686 11.00000 -1.50000
AFIX 0
C47 1 0.263886 0.668946 0.027823 11.00000 0.07539 0.06147 =
0.06684 0.00454 0.00211 0.01682
AFIX 33
H47A 2 0.234557 0.687653 0.066541 11.00000 -1.50000
H47B 2 0.323299 0.678015 0.022623 11.00000 -1.50000
H47C 2 0.235786 0.670678 -0.025513 11.00000 -1.50000
AFIX 0
C49 1 0.530584 0.660643 0.335874 11.00000 0.08008 0.10733 =
0.06630 0.01257 0.02683 -0.01512
AFIX 33
H49A 2 0.546663 0.663853 0.393344 11.00000 -1.50000
H49B 2 0.558620 0.682830 0.303478 11.00000 -1.50000
H49C 2 0.468740 0.663449 0.330299 11.00000 -1.50000
AFIX 0
C50 1 0.675954 0.618868 0.298441 11.00000 0.08455 0.06233 =
0.06104 0.00072 -0.01982 -0.00732
AFIX 33
H50A 2 0.697161 0.621180 0.354536 11.00000 -1.50000
H50B 2 0.705218 0.595408 0.270626 11.00000 -1.50000
H50C 2 0.686800 0.645669 0.269413 11.00000 -1.50000
AFIX 0
N1 3 0.720788 0.789670 -0.154359 11.00000 0.02683 0.04102 =
0.02869 0.01278 0.00759 0.00992
AFIX 43
H1 2 0.765322 0.778493 -0.178499 11.00000 -1.20000
AFIX 0
N2 3 0.799170 0.798184 0.213060 11.00000 0.03234 0.04163 =
0.02690 0.00720 -0.00973 -0.01080
AFIX 43
H2 2 0.821429 0.788628 0.258717 11.00000 -1.20000
AFIX 0
N3 3 0.427829 0.801142 0.276963 11.00000 0.02731 0.03854 =
0.02967 -0.01082 0.00927 -0.00880
AFIX 43
H3 2 0.381876 0.790916 0.300179 11.00000 -1.20000
AFIX 0
N4 3 0.352223 0.791669 -0.075754 11.00000 0.03010 0.04069 =
0.02882 -0.00816 -0.01079 0.01078
AFIX 43
H4 2 0.325830 0.779936 -0.117361 11.00000 -1.20000
AFIX 0
N5 3 0.277603 0.425631 0.053969 11.00000 0.03074 0.03382 =
0.04251 -0.00546 0.00002 0.00473
O1 4 0.703719 0.711026 0.003335 11.00000 0.02278 0.03440 =
0.02511 0.00716 0.00524 0.00599
O2 4 0.805386 0.717991 -0.095251 11.00000 0.02955 0.04671 =
0.03277 0.00939 0.00999 0.01175
O3 4 0.627859 0.784130 -0.046311 11.00000 0.02555 0.03580 =
0.02150 0.00432 0.00396 0.00798
O5 4 0.723790 0.732938 0.303700 11.00000 0.03912 0.05837 =
0.02791 0.01308 -0.01462 -0.01586
O4 4 0.641030 0.715934 0.193966 11.00000 0.02958 0.03432 =
0.02305 0.00643 -0.00690 -0.00718
O6 4 0.697168 0.785818 0.113295 11.00000 0.02210 0.03709 =
0.02219 0.00458 -0.00314 -0.00570
O8 4 0.341408 0.729919 0.221115 11.00000 0.04208 0.06397 =
0.05268 -0.02912 0.02818 -0.02574
O7 4 0.448388 0.716240 0.131329 11.00000 0.02448 0.03440 =
0.02985 -0.00903 0.00788 -0.00528
O9 4 0.528129 0.789767 0.176214 11.00000 0.02186 0.03465 =
0.02379 -0.00530 0.00370 -0.00442
O11 4 0.401239 0.712927 -0.140678 11.00000 0.05403 0.05872 =
0.05378 -0.02771 -0.03253 0.02337
O10 4 0.510093 0.709357 -0.050093 11.00000 0.03101 0.03639 =
0.02346 -0.00722 -0.00798 0.00882
O12 4 0.463767 0.785380 0.015759 11.00000 0.02260 0.03560 =
0.02372 -0.00565 -0.00522 0.00621
O13 4 0.574949 0.659201 0.076314 11.00000 0.02907 0.03566 =
0.03049 -0.00223 -0.00020 0.00025
O16 4 0.306646 0.587119 0.001865 11.00000 0.06837 0.05949 =
0.07647 -0.02567 0.01462 -0.01023
O17 4 0.536753 0.605462 0.210658 11.00000 0.09174 0.07292 =
0.06063 0.02090 -0.03563 -0.03370
S2 5 0.260233 0.614575 0.064337 11.00000 0.04401 0.05533 =
0.05824 -0.01089 0.01059 -0.01032
S3 5 0.563372 0.608484 0.299815 11.00000 0.08452 0.07442 =
0.05195 0.02636 -0.01765 -0.03729
ER1 6 0.578665 0.738904 0.068377 11.00000 0.01724 0.02918 =
0.01621 -0.00017 0.00011 0.00079
O18 4 0.530612 0.382949 0.045835 11.00000 0.05012 0.05454 =
0.06653 -0.00911 0.00437 -0.00223
O15 4 0.563875 1.005553 -0.119986 31.00000 0.13046
PART 1
S1 5 0.652398 0.944346 0.068378 21.00000 0.13750
C45 1 0.614302 0.885710 0.081475 21.00000 0.11684
AFIX 33
H45A 2 0.652036 0.870851 0.119778 21.00000 -1.50000
H45B 2 0.556087 0.885520 0.102710 21.00000 -1.50000
H45C 2 0.615574 0.871192 0.028543 21.00000 -1.50000
AFIX 0
C46 1 0.649772 0.967366 0.156951 21.00000 0.10398
AFIX 33
H46A 2 0.694871 0.955606 0.191708 21.00000 -1.50000
H46B 2 0.658501 0.998156 0.150279 21.00000 -1.50000
H46C 2 0.594356 0.962247 0.182385 21.00000 -1.50000
AFIX 0
O14 4 0.585765 0.959609 0.008458 21.00000 0.19827
PART 2
S1B 5 0.584053 0.939711 0.068040 -21.00000 0.14016
C46B 1 0.655495 0.962560 -0.002765 -21.00000 0.09044
AFIX 33
H46D 2 0.692259 0.940200 -0.025178 -21.00000 -1.50000
H46E 2 0.623282 0.976032 -0.047095 -21.00000 -1.50000
H46F 2 0.690529 0.984106 0.024747 -21.00000 -1.50000
AFIX 0
O14A 4 0.532731 0.975458 0.097466 -21.00000 0.31062
C45A 1 0.622333 0.893067 0.103517 -21.00000 0.07635
AFIX 33
H45D 2 0.654922 0.878828 0.060516 -21.00000 -1.50000
H45E 2 0.659443 0.898473 0.150532 -21.00000 -1.50000
H45F 2 0.574927 0.874735 0.120163 -21.00000 -1.50000
AFIX 0
PART 0
H13B 2 0.564667 0.647340 0.126578 11.00000 -1.50000
H13A 2 0.533787 0.646596 0.044522 11.00000 -1.50000
H18E 2 0.536318 0.355350 0.064085 11.00000 -1.50000
H18F 2 0.584932 0.389289 0.029195 11.00000 -1.50000
HKLF 4
REM ErTMPA_LT_auto in P2(1)/n
REM wR2 = 0.1005, GooF = S = 1.042, Restrained GooF = 1.043 for all data
REM R1 = 0.0372 for 12290 Fo > 4sig(Fo) and 0.0424 for all 13894 data
REM 843 parameters refined using 7 restraints
END
WGHT 0.0504 7.8234
REM Highest difference peak 1.320, deepest hole -1.038, 1-sigma level 0.071
Q1 1 0.6241 0.9318 0.0394 11.00000 0.05 1.32
Q2 1 0.3282 0.6177 0.0389 11.00000 0.05 1.20
Q3 1 0.5789 0.7834 0.0688 11.00000 0.05 0.93
Q4 1 0.5348 0.9489 0.0203 11.00000 0.05 0.78
Q5 1 0.6315 0.9574 0.1118 11.00000 0.05 0.66
Q6 1 0.6169 0.6243 0.2847 11.00000 0.05 0.66
Q7 1 0.3953 0.5257 -0.1833 11.00000 0.05 0.52
Q8 1 0.5787 0.6903 0.0668 11.00000 0.05 0.49
Q9 1 0.5740 0.7617 -0.2567 11.00000 0.05 0.49
Q10 1 0.7835 0.8812 0.1781 11.00000 0.05 0.48
Q11 1 0.8181 0.9151 0.1379 11.00000 0.05 0.48
Q12 1 0.5637 0.8012 0.4781 11.00000 0.05 0.45
Q13 1 0.6115 0.9735 0.0216 11.00000 0.05 0.43
Q14 1 0.5780 0.9677 -0.2604 11.00000 0.05 0.41
Q15 1 0.5653 0.7774 0.3881 11.00000 0.05 0.41
Q16 1 0.2475 0.5763 0.0365 11.00000 0.05 0.41
Q17 1 0.7179 0.8846 0.2473 11.00000 0.05 0.40
Q18 1 0.6660 0.7615 -0.3138 11.00000 0.05 0.39
Q19 1 0.1787 0.7744 -0.0392 11.00000 0.05 0.39
Q20 1 0.4654 0.7806 0.4394 11.00000 0.05 0.37
;
_shelx_res_checksum 12619
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.73925(16) 0.72931(8) -0.05786(15) 0.0241(5) Uani d 1 . .
C C2 0.69087(16) 0.77092(9) -0.08635(15) 0.0254(5) Uani d 1 . .
C C3 0.68188(17) 0.82805(9) -0.18970(17) 0.0310(6) Uani d 1 . .
C C4 0.6992(2) 0.86814(10) -0.15435(19) 0.0394(7) Uani d 1 . .
C C5 0.6593(2) 0.90479(11) -0.1891(2) 0.0449(7) Uani d 1 . .
H H5 0.668586 0.931946 -0.164860 0.054 Uiso calc 1 . .
C C6 0.6063(2) 0.90173(11) -0.2585(2) 0.0469(8) Uani d 1 . .
C C7 0.5928(2) 0.86102(11) -0.2934(2) 0.0436(7) Uani d 1 . .
H H7 0.558664 0.858746 -0.341086 0.052 Uiso calc 1 . .
C C8 0.62851(18) 0.82366(10) -0.25945(18) 0.0368(6) Uani d 1 . .
C C9 0.7619(3) 0.87200(13) -0.0825(2) 0.0563(9) Uani d 1 . .
H H9A 0.766214 0.901963 -0.065765 0.084 Uiso calc 1 . .
H H9B 0.741376 0.854818 -0.036632 0.084 Uiso calc 1 . .
H H9C 0.818007 0.861660 -0.099338 0.084 Uiso calc 1 . .
C C10 0.5638(3) 0.94183(14) -0.2961(3) 0.0717(12) Uani d 1 . .
H H10A 0.529658 0.933442 -0.343534 0.108 Uiso calc 1 . .
H H10B 0.527016 0.955328 -0.255375 0.108 Uiso calc 1 . .
H H10C 0.607861 0.962082 -0.313059 0.108 Uiso calc 1 . .
C C11 0.6098(2) 0.77930(12) -0.2959(2) 0.0514(8) Uani d 1 . .
H H11A 0.640014 0.757436 -0.264391 0.077 Uiso calc 1 . .
H H11B 0.548487 0.773754 -0.293935 0.077 Uiso calc 1 . .
H H11C 0.629026 0.778496 -0.352730 0.077 Uiso calc 1 . .
C C12 0.69649(17) 0.73844(8) 0.23247(16) 0.0273(5) Uani d 1 . .
C C13 0.73154(16) 0.77694(9) 0.18058(15) 0.0254(5) Uani d 1 . .
C C14 0.83646(18) 0.83606(9) 0.17568(17) 0.0333(6) Uani d 1 . .
C C15 0.88708(19) 0.83223(10) 0.10452(18) 0.0360(6) Uani d 1 . .
C C16 0.9206(2) 0.87032(12) 0.0699(2) 0.0445(7) Uani d 1 . .
H H16 0.953853 0.868276 0.021742 0.053 Uiso calc 1 . .
C C17 0.9066(2) 0.91077(12) 0.1040(2) 0.0548(9) Uani d 1 . .
C C18 0.8605(3) 0.91281(12) 0.1783(3) 0.0652(11) Uani d 1 . .
H H18 0.854067 0.939598 0.204642 0.078 Uiso calc 1 . .
C C19 0.8239(3) 0.87596(12) 0.2141(2) 0.0526(8) Uani d 1 . .
C C20 0.7714(4) 0.87882(16) 0.2937(3) 0.0861(16) Uani d 1 . .
H H20A 0.769026 0.908586 0.311951 0.129 Uiso calc 1 . .
H H20B 0.713524 0.868404 0.283388 0.129 Uiso calc 1 . .
H H20C 0.798289 0.861265 0.335960 0.129 Uiso calc 1 . .
C C21 0.9422(4) 0.95174(15) 0.0631(4) 0.0871(15) Uani d 1 . .
H H21A 0.926082 0.976781 0.095384 0.131 Uiso calc 1 . .
H H21B 1.004326 0.949887 0.060074 0.131 Uiso calc 1 . .
H H21C 0.918578 0.954401 0.007907 0.131 Uiso calc 1 . .
C C22 0.9056(3) 0.78925(13) 0.0647(3) 0.0610(10) Uani d 1 . .
H H22A 0.941438 0.793582 0.016595 0.091 Uiso calc 1 . .
H H22B 0.935196 0.770732 0.103679 0.091 Uiso calc 1 . .
H H22C 0.851923 0.775797 0.048114 0.091 Uiso calc 1 . .
C C23 0.41139(18) 0.73768(9) 0.18704(17) 0.0297(6) Uani d 1 . .
C C24 0.46169(16) 0.77922(9) 0.21336(15) 0.0252(5) Uani d 1 . .
C C25 0.46375(17) 0.84078(9) 0.30876(16) 0.0287(5) Uani d 1 . .
C C26 0.44717(19) 0.87965(10) 0.26667(18) 0.0366(6) Uani d 1 . .
C C27 0.4806(2) 0.91789(10) 0.3010(2) 0.0433(7) Uani d 1 . .
H H27 0.470071 0.944194 0.274028 0.052 Uiso calc 1 . .
C C28 0.5292(2) 0.91811(10) 0.3740(2) 0.0450(7) Uani d 1 . .
C C29 0.5442(2) 0.87859(11) 0.41362(19) 0.0408(7) Uani d 1 . .
H H29 0.576438 0.878280 0.462654 0.049 Uiso calc 1 . .
C C30 0.51238(18) 0.83942(9) 0.38219(17) 0.0327(6) Uani d 1 . .
C C31 0.3957(2) 0.88020(13) 0.1865(2) 0.0519(8) Uani d 1 . .
H H31A 0.390927 0.909621 0.166700 0.078 Uiso calc 1 . .
H H31B 0.424812 0.862720 0.145614 0.078 Uiso calc 1 . .
H H31C 0.338779 0.868592 0.196349 0.078 Uiso calc 1 . .
C C32 0.5661(3) 0.95986(13) 0.4094(3) 0.0754(13) Uani d 1 . .
H H32A 0.549561 0.983903 0.374514 0.113 Uiso calc 1 . .
H H32B 0.543815 0.964346 0.464506 0.113 Uiso calc 1 . .
H H32C 0.628246 0.957845 0.411627 0.113 Uiso calc 1 . .
C C33 0.5301(2) 0.79673(11) 0.4251(2) 0.0501(8) Uani d 1 . .
H H33A 0.503085 0.773509 0.394417 0.075 Uiso calc 1 . .
H H33B 0.591625 0.791865 0.427748 0.075 Uiso calc 1 . .
H H33C 0.506852 0.797578 0.480457 0.075 Uiso calc 1 . .
C C34 0.44552(17) 0.72748(9) -0.08388(16) 0.0293(5) Uani d 1 . .
C C35 0.42104(16) 0.77140(9) -0.04378(16) 0.0261(5) Uani d 1 . .
C C36 0.32022(18) 0.83213(9) -0.04394(16) 0.0305(6) Uani d 1 . .
C C37 0.3658(2) 0.87037(10) -0.05813(18) 0.0380(6) Uani d 1 . .
C C38 0.3314(2) 0.90893(11) -0.0271(2) 0.0485(8) Uani d 1 . .
H H38 0.361258 0.934873 -0.035994 0.058 Uiso calc 1 . .
C C39 0.2541(2) 0.90989(12) 0.0166(2) 0.0524(9) Uani d 1 . .
C C40 0.2107(2) 0.87115(13) 0.0295(2) 0.0498(8) Uani d 1 . .
H H40 0.158474 0.871532 0.058495 0.060 Uiso calc 1 . .
C C41 0.2424(2) 0.83166(11) 0.00060(18) 0.0380(6) Uani d 1 . .
C C42 0.4496(2) 0.87045(13) -0.1057(3) 0.0575(9) Uani d 1 . .
H H42A 0.471436 0.899694 -0.109174 0.086 Uiso calc 1 . .
H H42B 0.491217 0.852366 -0.077533 0.086 Uiso calc 1 . .
H H42C 0.439609 0.859325 -0.160765 0.086 Uiso calc 1 . .
C C43 0.2173(4) 0.95256(17) 0.0488(4) 0.0937(17) Uani d 1 . .
H H43A 0.255717 0.976014 0.034308 0.141 Uiso calc 1 . .
H H43B 0.161324 0.957573 0.024104 0.141 Uiso calc 1 . .
H H43C 0.211646 0.951099 0.108195 0.141 Uiso calc 1 . .
C C44 0.1952(3) 0.78959(14) 0.0178(3) 0.0604(10) Uani d 1 . .
H H44A 0.226434 0.765794 -0.006850 0.091 Uiso calc 1 . .
H H44B 0.191195 0.785190 0.076795 0.091 Uiso calc 1 . .
H H44C 0.137852 0.790982 -0.005757 0.091 Uiso calc 1 . .
C C51 0.3698(3) 0.52552(13) 0.2897(2) 0.0603(10) Uani d 1 . .
H H51A 0.346285 0.543315 0.333282 0.090 Uiso calc 1 . .
H H51B 0.400994 0.501475 0.313662 0.090 Uiso calc 1 . .
H H51C 0.408622 0.542638 0.256297 0.090 Uiso calc 1 . .
C C52 0.2963(2) 0.50830(12) 0.2354(2) 0.0493(8) Uani d 1 . .
H H52A 0.256664 0.491588 0.269743 0.059 Uiso calc 1 . .
H H52B 0.264291 0.532748 0.212383 0.059 Uiso calc 1 . .
C C53 0.3281(2) 0.47984(11) 0.1649(2) 0.0481(8) Uani d 1 . .
H H53A 0.363912 0.456592 0.187265 0.058 Uiso calc 1 . .
H H53B 0.363474 0.497094 0.127510 0.058 Uiso calc 1 . .
C C55 0.2523(2) 0.46033(11) 0.1170(2) 0.0445(7) Uani d 1 . .
H H55A 0.222142 0.483607 0.088030 0.053 Uiso calc 1 . .
H H55B 0.211998 0.447632 0.156428 0.053 Uiso calc 1 . .
C C57 0.4335(4) 0.5056(2) -0.1239(4) 0.0985(17) Uani d 1 . .
H H57A 0.461065 0.511839 -0.176098 0.148 Uiso calc 1 . .
H H57B 0.434448 0.531194 -0.089517 0.148 Uiso calc 1 . .
H H57C 0.464003 0.482421 -0.096325 0.148 Uiso calc 1 . .
C C58 0.3437(4) 0.49247(16) -0.1388(3) 0.0787(13) Uani d 1 . .
H H58A 0.343425 0.467060 -0.174755 0.094 Uiso calc 1 . .
H H58B 0.313895 0.515793 -0.167953 0.094 Uiso calc 1 . .
C C59 0.2949(3) 0.48201(12) -0.0613(3) 0.0615(10) Uani d 1 . .
H H59A 0.235574 0.474516 -0.075734 0.074 Uiso calc 1 . .
H H59B 0.293325 0.507651 -0.025952 0.074 Uiso calc 1 . .
C C60 0.3354(2) 0.44448(10) -0.0130(2) 0.0436(7) Uani d 1 . .
H H60A 0.350361 0.421475 -0.051906 0.052 Uiso calc 1 . .
H H60B 0.388916 0.454569 0.012567 0.052 Uiso calc 1 . .
C C61 0.1327(2) 0.32995(13) -0.1611(3) 0.0583(9) Uani d 1 . .
H H61A 0.079863 0.314383 -0.172458 0.087 Uiso calc 1 . .
H H61B 0.144520 0.349659 -0.206131 0.087 Uiso calc 1 . .
H H61C 0.179760 0.309629 -0.155621 0.087 Uiso calc 1 . .
C C62 0.1231(2) 0.35527(13) -0.0817(2) 0.0542(9) Uani d 1 . .
H H62A 0.110157 0.335350 -0.036515 0.065 Uiso calc 1 . .
H H62B 0.074883 0.375418 -0.087072 0.065 Uiso calc 1 . .
C C63 0.2053(2) 0.38059(10) -0.06094(19) 0.0383(6) Uani d 1 . .
H H63A 0.253054 0.360365 -0.052896 0.046 Uiso calc 1 . .
H H63B 0.219852 0.399564 -0.107156 0.046 Uiso calc 1 . .
C C64 0.19368(19) 0.40760(11) 0.0169(2) 0.0416(7) Uani d 1 . .
H H64A 0.165194 0.389814 0.058616 0.050 Uiso calc 1 . .
H H64B 0.155401 0.431819 0.004089 0.050 Uiso calc 1 . .
C C65 0.4290(3) 0.35589(18) 0.2539(3) 0.0764(13) Uani d 1 . .
H H65A 0.463793 0.332890 0.277013 0.115 Uiso calc 1 . .
H H65B 0.462132 0.371429 0.212921 0.115 Uiso calc 1 . .
H H65C 0.411936 0.375547 0.297332 0.115 Uiso calc 1 . .
C C67 0.3489(3) 0.33666(13) 0.2134(2) 0.0544(9) Uani d 1 . .
H H67A 0.316802 0.320390 0.254897 0.065 Uiso calc 1 . .
H H67B 0.366945 0.316277 0.170575 0.065 Uiso calc 1 . .
C C68 0.2887(2) 0.37044(11) 0.1743(2) 0.0435(7) Uani d 1 . .
H H68A 0.233111 0.357071 0.161477 0.052 Uiso calc 1 . .
H H68B 0.278696 0.393944 0.213521 0.052 Uiso calc 1 . .
C C69 0.32827(18) 0.38856(9) 0.09550(19) 0.0352(6) Uani d 1 . .
H H69A 0.334109 0.364958 0.055713 0.042 Uiso calc 1 . .
H H69B 0.386236 0.398989 0.108412 0.042 Uiso calc 1 . .
C C48 0.3326(3) 0.62236(13) 0.1497(2) 0.0575(9) Uani d 1 . .
H H48A 0.304909 0.639948 0.191341 0.086 Uiso calc 1 . .
H H48B 0.347715 0.594577 0.173163 0.086 Uiso calc 1 . .
H H48C 0.384237 0.636753 0.130686 0.086 Uiso calc 1 . .
C C47 0.2639(3) 0.66895(14) 0.0278(3) 0.0679(11) Uani d 1 . .
H H47A 0.234557 0.687653 0.066541 0.102 Uiso calc 1 . .
H H47B 0.323299 0.678015 0.022623 0.102 Uiso calc 1 . .
H H47C 0.235786 0.670678 -0.025513 0.102 Uiso calc 1 . .
C C49 0.5306(3) 0.66064(18) 0.3359(3) 0.0845(15) Uani d 1 . .
H H49A 0.546663 0.663853 0.393344 0.127 Uiso calc 1 . .
H H49B 0.558620 0.682830 0.303478 0.127 Uiso calc 1 . .
H H49C 0.468740 0.663449 0.330299 0.127 Uiso calc 1 . .
C C50 0.6760(3) 0.61887(14) 0.2984(3) 0.0693(11) Uani d 1 . .
H H50A 0.697161 0.621180 0.354536 0.104 Uiso calc 1 . .
H H50B 0.705218 0.595408 0.270626 0.104 Uiso calc 1 . .
H H50C 0.686800 0.645669 0.269413 0.104 Uiso calc 1 . .
N N1 0.72079(15) 0.78967(8) -0.15436(14) 0.0322(5) Uani d 1 . .
H H1 0.765322 0.778493 -0.178499 0.039 Uiso calc 1 . .
N N2 0.79917(15) 0.79818(8) 0.21306(14) 0.0336(5) Uani d 1 . .
H H2 0.821429 0.788628 0.258717 0.040 Uiso calc 1 . .
N N3 0.42783(15) 0.80114(8) 0.27696(14) 0.0318(5) Uani d 1 . .
H H3 0.381876 0.790916 0.300179 0.038 Uiso calc 1 . .
N N4 0.35222(15) 0.79167(8) -0.07575(14) 0.0332(5) Uani d 1 . .
H H4 0.325830 0.779936 -0.117361 0.040 Uiso calc 1 . .
N N5 0.27760(15) 0.42563(8) 0.05397(16) 0.0357(5) Uani d 1 . .
O O1 0.70372(11) 0.71103(6) 0.00333(11) 0.0274(4) Uani d 1 . .
O O2 0.80539(12) 0.71799(7) -0.09525(12) 0.0363(4) Uani d 1 . .
O O3 0.62786(11) 0.78413(6) -0.04631(10) 0.0276(4) Uani d 1 . .
O O5 0.72379(14) 0.73294(7) 0.30370(12) 0.0418(5) Uani d 1 . .
O O4 0.64103(12) 0.71593(6) 0.19397(11) 0.0290(4) Uani d 1 . .
O O6 0.69717(11) 0.78582(6) 0.11330(10) 0.0271(4) Uani d 1 . .
O O8 0.34141(15) 0.72992(8) 0.22112(15) 0.0529(7) Uani d 1 . .
O O7 0.44839(11) 0.71624(6) 0.13133(11) 0.0296(4) Uani d 1 . .
O O9 0.52813(11) 0.78977(6) 0.17621(10) 0.0268(4) Uani d 1 . .
O O11 0.40124(16) 0.71293(8) -0.14068(15) 0.0556(7) Uani d 1 . .
O O10 0.51009(12) 0.70936(6) -0.05009(11) 0.0303(4) Uani d 1 . .
O O12 0.46377(11) 0.78538(6) 0.01576(10) 0.0273(4) Uani d 1 . .
O O13 0.57495(12) 0.65920(6) 0.07631(11) 0.0317(4) Uani d 1 . .
O O16 0.30665(19) 0.58712(9) 0.00186(19) 0.0681(8) Uani d 1 . .
O O17 0.5368(2) 0.60546(10) 0.21066(18) 0.0752(9) Uani d 1 . .
S S2 0.26023(6) 0.61457(3) 0.06434(6) 0.0525(2) Uani d 1 . .
S S3 0.56337(8) 0.60848(4) 0.29982(6) 0.0703(3) Uani d 1 . .
Er Er1 0.57866(2) 0.73890(2) 0.06838(2) 0.02088(6) Uani d 1 . .
O O18 0.53061(17) 0.38295(9) 0.04584(17) 0.0571(6) Uani d 1 . .
O O15 0.5639(7) 1.0056(3) -0.1200(6) 0.130(5) Uiso d 0.524(14) . .
S S1 0.6524(3) 0.94435(13) 0.0684(3) 0.1375(16) Uiso d 0.632(7) A 1
C C45 0.6143(10) 0.8857(5) 0.0815(9) 0.117(5) Uiso d 0.632(7) A 1
H H45A 0.652036 0.870851 0.119778 0.175 Uiso calc 0.632(7) A 1
H H45B 0.556087 0.885520 0.102710 0.175 Uiso calc 0.632(7) A 1
H H45C 0.615574 0.871192 0.028543 0.175 Uiso calc 0.632(7) A 1
C C46 0.6498(7) 0.9674(3) 0.1570(6) 0.104(3) Uiso d 0.632(7) A 1
H H46A 0.694871 0.955606 0.191708 0.156 Uiso calc 0.632(7) A 1
H H46B 0.658501 0.998156 0.150279 0.156 Uiso calc 0.632(7) A 1
H H46C 0.594356 0.962247 0.182385 0.156 Uiso calc 0.632(7) A 1
O O14 0.5858(10) 0.9596(5) 0.0085(9) 0.198(5) Uiso d 0.632(7) A 1
S S1B 0.5841(6) 0.9397(3) 0.0680(4) 0.140(3) Uiso d 0.368(7) A 2
C C46B 0.6555(11) 0.9626(5) -0.0028(10) 0.090(4) Uiso d 0.368(7) A 2
H H46D 0.692259 0.940200 -0.025178 0.136 Uiso calc 0.368(7) A 2
H H46E 0.623282 0.976032 -0.047095 0.136 Uiso calc 0.368(7) A 2
H H46F 0.690529 0.984106 0.024747 0.136 Uiso calc 0.368(7) A 2
O O14A 0.533(3) 0.9755(12) 0.097(2) 0.311(17) Uiso d 0.368(7) A 2
C C45A 0.6223(12) 0.8931(6) 0.1035(12) 0.076(5) Uiso d 0.368(7) A 2
H H45D 0.654922 0.878828 0.060516 0.115 Uiso calc 0.368(7) A 2
H H45E 0.659443 0.898473 0.150532 0.115 Uiso calc 0.368(7) A 2
H H45F 0.574927 0.874735 0.120163 0.115 Uiso calc 0.368(7) A 2
H H13B 0.565(3) 0.6473(13) 0.1266(10) 0.115 Uiso d 1 . .
H H13A 0.5338(19) 0.6466(13) 0.0445(17) 0.115 Uiso d 1 . .
H H18E 0.536(2) 0.3554(5) 0.064(3) 0.115 Uiso d 1 . .
H H18F 0.5849(10) 0.3893(13) 0.029(3) 0.115 Uiso d 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
C1 0.0188(12) 0.0324(13) 0.0211(12) 0.0023(10) 0.0009(9) 0.0011(10)
C2 0.0214(12) 0.0339(13) 0.0208(12) 0.0013(10) -0.0003(9) 0.0027(10)
C3 0.0256(13) 0.0383(15) 0.0292(13) 0.0065(11) 0.0075(10) 0.0126(11)
C4 0.0354(15) 0.0455(17) 0.0372(15) 0.0012(13) 0.0049(12) 0.0124(13)
C5 0.0426(17) 0.0386(16) 0.0536(19) 0.0010(13) 0.0084(15) 0.0124(14)
C6 0.0340(16) 0.0486(19) 0.058(2) 0.0054(14) 0.0034(14) 0.0250(16)
C7 0.0312(15) 0.0562(19) 0.0433(17) 0.0019(13) -0.0029(13) 0.0196(15)
C8 0.0279(14) 0.0491(17) 0.0333(14) 0.0040(12) 0.0052(11) 0.0103(13)
C9 0.063(2) 0.054(2) 0.052(2) -0.0020(17) -0.0119(17) 0.0044(17)
C10 0.057(2) 0.059(2) 0.099(3) 0.0096(19) -0.011(2) 0.036(2)
C11 0.052(2) 0.055(2) 0.0469(19) 0.0011(16) -0.0084(15) 0.0029(16)
C12 0.0243(13) 0.0337(14) 0.0237(13) -0.0014(10) -0.0027(10) 0.0056(10)
C13 0.0223(12) 0.0335(13) 0.0204(12) -0.0027(10) -0.0023(9) 0.0007(10)
C14 0.0306(14) 0.0378(15) 0.0313(14) -0.0103(11) -0.0077(11) 0.0026(11)
C15 0.0300(14) 0.0430(16) 0.0350(15) -0.0066(12) -0.0046(11) 0.0010(12)
C16 0.0346(16) 0.061(2) 0.0384(16) -0.0140(14) -0.0006(13) 0.0095(15)
C17 0.052(2) 0.050(2) 0.061(2) -0.0172(16) -0.0036(17) 0.0147(17)
C18 0.082(3) 0.0400(19) 0.074(3) -0.0139(19) 0.007(2) -0.0068(18)
C19 0.063(2) 0.0468(19) 0.0474(19) -0.0094(16) 0.0083(16) -0.0037(15)
C20 0.126(5) 0.066(3) 0.067(3) -0.014(3) 0.035(3) -0.017(2)
C21 0.094(4) 0.061(3) 0.106(4) -0.030(3) 0.009(3) 0.028(3)
C22 0.054(2) 0.060(2) 0.069(2) -0.0072(18) 0.0196(19) -0.0079(19)
C23 0.0246(13) 0.0365(15) 0.0279(13) -0.0075(10) 0.0050(11) -0.0058(11)
C24 0.0208(12) 0.0342(13) 0.0205(11) -0.0020(10) 0.0010(9) -0.0033(10)
C25 0.0236(12) 0.0336(14) 0.0289(13) -0.0033(10) 0.0082(10) -0.0090(11)
C26 0.0344(15) 0.0437(16) 0.0317(14) 0.0004(12) 0.0064(12) -0.0013(12)
C27 0.0503(18) 0.0319(15) 0.0480(18) -0.0007(13) 0.0061(14) -0.0011(13)
C28 0.0437(17) 0.0385(16) 0.0527(19) -0.0078(13) 0.0052(14) -0.0139(14)
C29 0.0372(16) 0.0475(18) 0.0375(16) -0.0050(13) -0.0049(12) -0.0091(13)
C30 0.0271(13) 0.0372(15) 0.0338(14) -0.0005(11) 0.0036(11) -0.0041(12)
C31 0.053(2) 0.064(2) 0.0383(17) 0.0029(17) -0.0058(15) 0.0039(16)
C32 0.089(3) 0.048(2) 0.089(3) -0.021(2) -0.006(3) -0.020(2)
C33 0.051(2) 0.0485(19) 0.0504(19) 0.0020(15) -0.0101(16) 0.0028(15)
C34 0.0267(13) 0.0374(14) 0.0236(12) 0.0049(11) -0.0058(10) -0.0042(11)
C35 0.0211(12) 0.0353(13) 0.0219(12) 0.0041(10) -0.0010(9) -0.0003(10)
C36 0.0297(13) 0.0389(15) 0.0229(12) 0.0100(11) -0.0080(10) -0.0033(11)
C37 0.0361(16) 0.0441(16) 0.0338(15) 0.0058(13) -0.0063(12) -0.0017(12)
C38 0.056(2) 0.0380(16) 0.0519(19) 0.0038(15) -0.0136(16) -0.0047(15)
C39 0.055(2) 0.050(2) 0.052(2) 0.0221(16) -0.0103(16) -0.0140(16)
C40 0.0441(18) 0.067(2) 0.0387(17) 0.0210(16) 0.0055(14) -0.0073(16)
C41 0.0359(15) 0.0486(17) 0.0295(14) 0.0101(13) -0.0013(11) 0.0002(12)
C42 0.045(2) 0.061(2) 0.067(2) -0.0043(17) 0.0085(17) 0.0004(19)
C43 0.107(4) 0.071(3) 0.103(4) 0.041(3) -0.006(3) -0.036(3)
C44 0.052(2) 0.066(2) 0.063(2) -0.0019(18) 0.0141(18) 0.0059(19)
C51 0.070(3) 0.058(2) 0.053(2) -0.0087(19) -0.0062(18) -0.0083(17)
C52 0.053(2) 0.0480(18) 0.0472(18) -0.0035(15) 0.0026(15) -0.0073(15)
C53 0.0418(18) 0.0428(17) 0.060(2) 0.0013(14) 0.0027(15) -0.0144(15)
C55 0.0379(16) 0.0402(16) 0.0555(19) 0.0101(13) 0.0009(14) -0.0143(15)
C57 0.084(4) 0.093(4) 0.119(5) -0.014(3) 0.023(3) 0.006(3)
C58 0.098(4) 0.059(2) 0.079(3) 0.005(2) 0.004(3) 0.017(2)
C59 0.074(3) 0.0363(18) 0.074(3) -0.0017(17) -0.001(2) 0.0071(17)
C60 0.0447(18) 0.0355(15) 0.0505(18) -0.0027(13) 0.0057(14) -0.0024(14)
C61 0.046(2) 0.062(2) 0.066(2) -0.0010(17) -0.0048(17) -0.0183(19)
C62 0.0361(17) 0.063(2) 0.063(2) -0.0015(16) -0.0072(15) -0.0135(18)
C63 0.0375(16) 0.0363(15) 0.0412(16) 0.0032(12) -0.0041(12) 0.0036(13)
C64 0.0286(15) 0.0448(17) 0.0515(18) 0.0069(12) -0.0048(13) -0.0063(14)
C65 0.064(3) 0.117(4) 0.048(2) 0.005(3) -0.0185(19) -0.003(2)
C67 0.057(2) 0.061(2) 0.0452(19) 0.0065(17) -0.0082(16) 0.0035(16)
C68 0.0363(16) 0.0471(18) 0.0470(18) -0.0009(13) 0.0032(13) 0.0001(14)
C69 0.0274(14) 0.0352(15) 0.0429(16) 0.0051(11) 0.0002(12) -0.0049(12)
C48 0.066(2) 0.052(2) 0.055(2) -0.0077(18) -0.0034(18) 0.0010(17)
C47 0.075(3) 0.061(2) 0.067(3) 0.017(2) 0.002(2) 0.005(2)
C49 0.080(3) 0.107(4) 0.066(3) -0.015(3) 0.027(2) 0.013(3)
C50 0.085(3) 0.062(2) 0.061(2) -0.007(2) -0.020(2) 0.001(2)
N1 0.0268(11) 0.0410(13) 0.0287(11) 0.0099(10) 0.0076(9) 0.0128(10)
N2 0.0323(12) 0.0416(13) 0.0269(11) -0.0108(10) -0.0097(9) 0.0072(10)
N3 0.0273(11) 0.0385(13) 0.0297(11) -0.0088(9) 0.0093(9) -0.0108(10)
N4 0.0301(12) 0.0407(13) 0.0288(11) 0.0108(10) -0.0108(9) -0.0082(10)
N5 0.0307(12) 0.0338(12) 0.0425(13) 0.0047(10) 0.0000(10) -0.0055(10)
O1 0.0228(9) 0.0344(9) 0.0251(9) 0.0060(7) 0.0052(7) 0.0072(7)
O2 0.0296(10) 0.0467(11) 0.0328(10) 0.0118(9) 0.0100(8) 0.0094(9)
O3 0.0256(9) 0.0358(10) 0.0215(8) 0.0080(7) 0.0040(7) 0.0043(7)
O5 0.0391(12) 0.0584(13) 0.0279(10) -0.0159(10) -0.0146(9) 0.0131(9)
O4 0.0296(9) 0.0343(10) 0.0230(8) -0.0072(8) -0.0069(7) 0.0064(7)
O6 0.0221(8) 0.0371(10) 0.0222(8) -0.0057(7) -0.0031(7) 0.0046(7)
O8 0.0421(13) 0.0640(15) 0.0527(14) -0.0257(11) 0.0282(11) -0.0291(11)
O7 0.0245(9) 0.0344(10) 0.0299(9) -0.0053(7) 0.0079(7) -0.0090(8)
O9 0.0219(9) 0.0346(9) 0.0238(8) -0.0044(7) 0.0037(7) -0.0053(7)
O11 0.0540(14) 0.0587(14) 0.0538(14) 0.0234(12) -0.0325(12) -0.0277(12)
O10 0.0310(10) 0.0364(10) 0.0235(9) 0.0088(8) -0.0080(7) -0.0072(7)
O12 0.0226(9) 0.0356(10) 0.0237(9) 0.0062(7) -0.0052(7) -0.0056(7)
O13 0.0291(10) 0.0357(10) 0.0305(9) 0.0002(7) -0.0002(8) -0.0022(8)
O16 0.0684(18) 0.0595(16) 0.0765(18) -0.0102(14) 0.0146(14) -0.0257(14)
O17 0.092(2) 0.0729(18) 0.0606(17) -0.0337(16) -0.0356(16) 0.0209(14)
S2 0.0440(4) 0.0553(5) 0.0582(5) -0.0103(4) 0.0106(4) -0.0109(4)
S3 0.0845(7) 0.0744(7) 0.0520(5) -0.0373(6) -0.0177(5) 0.0264(5)
Er1 0.01724(9) 0.02918(9) 0.01621(9) 0.00079(5) 0.00011(5) -0.00017(5)
O18 0.0501(14) 0.0545(14) 0.0665(16) -0.0022(11) 0.0044(12) -0.0091(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 '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
_geom_angle_publ_flag
O2 C1 O1 . . 128.1(2) ?
O2 C1 C2 . . 119.1(2) ?
O1 C1 C2 . . 112.9(2) ?
O3 C2 N1 . . 124.4(2) ?
O3 C2 C1 . . 119.7(2) ?
N1 C2 C1 . . 115.8(2) ?
C4 C3 C8 . . 122.0(3) ?
C4 C3 N1 . . 119.2(3) ?
C8 C3 N1 . . 118.8(3) ?
C3 C4 C5 . . 117.9(3) ?
C3 C4 C9 . . 120.5(3) ?
C5 C4 C9 . . 121.5(3) ?
C6 C5 C4 . . 121.7(3) ?
C5 C6 C7 . . 118.4(3) ?
C5 C6 C10 . . 121.2(4) ?
C7 C6 C10 . . 120.4(3) ?
C8 C7 C6 . . 121.9(3) ?
C7 C8 C3 . . 118.0(3) ?
C7 C8 C11 . . 121.3(3) ?
C3 C8 C11 . . 120.7(3) ?
O5 C12 O4 . . 127.7(2) ?
O5 C12 C13 . . 119.2(2) ?
O4 C12 C13 . . 113.1(2) ?
O6 C13 N2 . . 124.6(2) ?
O6 C13 C12 . . 119.5(2) ?
N2 C13 C12 . . 115.9(2) ?
C19 C14 C15 . . 121.4(3) ?
C19 C14 N2 . . 118.3(3) ?
C15 C14 N2 . . 120.2(3) ?
C14 C15 C16 . . 117.8(3) ?
C14 C15 C22 . . 122.4(3) ?
C16 C15 C22 . . 119.8(3) ?
C17 C16 C15 . . 122.6(3) ?
C16 C17 C18 . . 117.7(3) ?
C16 C17 C21 . . 121.1(4) ?
C18 C17 C21 . . 121.3(4) ?
C19 C18 C17 . . 121.9(4) ?
C14 C19 C18 . . 118.5(3) ?
C14 C19 C20 . . 120.1(3) ?
C18 C19 C20 . . 121.4(4) ?
O8 C23 O7 . . 128.1(2) ?
O8 C23 C24 . . 118.3(2) ?
O7 C23 C24 . . 113.6(2) ?
O9 C24 N3 . . 124.6(2) ?
O9 C24 C23 . . 120.0(2) ?
N3 C24 C23 . . 115.4(2) ?
C26 C25 C30 . . 122.2(3) ?
C26 C25 N3 . . 119.0(3) ?
C30 C25 N3 . . 118.9(3) ?
C25 C26 C27 . . 117.5(3) ?
C25 C26 C31 . . 121.2(3) ?
C27 C26 C31 . . 121.4(3) ?
C28 C27 C26 . . 122.4(3) ?
C29 C28 C27 . . 118.1(3) ?
C29 C28 C32 . . 120.4(3) ?
C27 C28 C32 . . 121.5(3) ?
C28 C29 C30 . . 122.0(3) ?
C29 C30 C25 . . 117.9(3) ?
C29 C30 C33 . . 121.5(3) ?
C25 C30 C33 . . 120.6(3) ?
O11 C34 O10 . . 126.7(3) ?
O11 C34 C35 . . 119.7(2) ?
O10 C34 C35 . . 113.5(2) ?
O12 C35 N4 . . 123.9(2) ?
O12 C35 C34 . . 119.8(2) ?
N4 C35 C34 . . 116.3(2) ?
C37 C36 C41 . . 121.9(3) ?
C37 C36 N4 . . 120.0(3) ?
C41 C36 N4 . . 118.1(3) ?
C36 C37 C38 . . 117.9(3) ?
C36 C37 C42 . . 121.4(3) ?
C38 C37 C42 . . 120.7(3) ?
C39 C38 C37 . . 121.9(3) ?
C40 C39 C38 . . 118.4(3) ?
C40 C39 C43 . . 120.7(4) ?
C38 C39 C43 . . 120.9(4) ?
C39 C40 C41 . . 122.1(3) ?
C40 C41 C36 . . 117.8(3) ?
C40 C41 C44 . . 121.1(3) ?
C36 C41 C44 . . 121.1(3) ?
C53 C52 C51 . . 112.8(3) ?
C52 C53 C55 . . 111.0(3) ?
C53 C55 N5 . . 114.6(3) ?
C57 C58 C59 . . 113.7(5) ?
C58 C59 C60 . . 112.4(4) ?
N5 C60 C59 . . 114.2(3) ?
C61 C62 C63 . . 111.5(3) ?
C64 C63 C62 . . 111.1(3) ?
C63 C64 N5 . . 114.8(2) ?
C65 C67 C68 . . 114.0(4) ?
C69 C68 C67 . . 110.3(3) ?
C68 C69 N5 . . 115.6(2) ?
C2 N1 C3 . . 122.6(2) ?
C13 N2 C14 . . 123.2(2) ?
C24 N3 C25 . . 123.5(2) ?
C35 N4 C36 . . 122.9(2) ?
C60 N5 C55 . . 111.0(2) ?
C60 N5 C64 . . 111.1(2) ?
C55 N5 C64 . . 107.2(2) ?
C60 N5 C69 . . 107.1(2) ?
C55 N5 C69 . . 111.2(2) ?
C64 N5 C69 . . 109.3(2) ?
C1 O1 Er1 . . 122.88(15) ?
C2 O3 Er1 . . 117.08(16) ?
C12 O4 Er1 . . 122.30(16) ?
C13 O6 Er1 . . 116.69(16) ?
C23 O7 Er1 . . 122.90(16) ?
C24 O9 Er1 . . 116.13(16) ?
C34 O10 Er1 . . 121.96(16) ?
C35 O12 Er1 . . 116.89(16) ?
O16 S2 C47 . . 107.0(2) ?
O16 S2 C48 . . 107.06(19) ?
C47 S2 C48 . . 96.2(2) ?
O17 S3 C50 . . 105.5(2) ?
O17 S3 C49 . . 107.0(2) ?
C50 S3 C49 . . 97.0(2) ?
O4 Er1 O1 . . 86.51(6) ?
O4 Er1 O7 . . 83.62(6) ?
O1 Er1 O7 . . 141.49(7) ?
O4 Er1 O10 . . 139.69(7) ?
O1 Er1 O10 . . 82.35(6) ?
O7 Er1 O10 . . 81.54(6) ?
O4 Er1 O12 . . 140.84(6) ?
O1 Er1 O12 . . 131.03(6) ?
O7 Er1 O12 . . 72.62(6) ?
O10 Er1 O12 . . 67.63(6) ?
O4 Er1 O3 . . 134.24(6) ?
O1 Er1 O3 . . 67.27(6) ?
O7 Er1 O3 . . 139.68(6) ?
O10 Er1 O3 . . 75.35(7) ?
O12 Er1 O3 . . 68.18(6) ?
O4 Er1 O6 . . 67.47(6) ?
O1 Er1 O6 . . 74.49(6) ?
O7 Er1 O6 . . 133.39(6) ?
O10 Er1 O6 . . 143.30(6) ?
O12 Er1 O6 . . 107.56(6) ?
O3 Er1 O6 . . 69.61(6) ?
O4 Er1 O13 . . 70.37(6) ?
O1 Er1 O13 . . 71.32(6) ?
O7 Er1 O13 . . 70.29(6) ?
O10 Er1 O13 . . 69.35(6) ?
O12 Er1 O13 . . 126.06(6) ?
O3 Er1 O13 . . 128.10(6) ?
O6 Er1 O13 . . 126.37(6) ?
O4 Er1 O9 . . 73.37(6) ?
O1 Er1 O9 . . 143.51(6) ?
O7 Er1 O9 . . 67.23(6) ?
O10 Er1 O9 . . 132.17(6) ?
O12 Er1 O9 . . 68.90(6) ?
O3 Er1 O9 . . 105.77(6) ?
O6 Er1 O9 . . 69.77(6) ?
O13 Er1 O9 . . 126.10(6) ?
O14 S1 C46 . . 115.0(7) ?
O14 S1 C45 . . 99.1(8) ?
C46 S1 C45 . . 108.2(6) ?
O14A S1B C45A . . 138.4(17) ?
O14A S1B C46B . . 105.0(17) ?
C45A S1B C46B . . 110.5(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O2 . 1.234(3) ?
C1 O1 . 1.258(3) ?
C1 C2 . 1.547(3) ?
C2 O3 . 1.234(3) ?
C2 N1 . 1.319(3) ?
C3 C4 . 1.380(4) ?
C3 C8 . 1.394(4) ?
C3 N1 . 1.437(3) ?
C4 C5 . 1.396(4) ?
C4 C9 . 1.507(5) ?
C5 C6 . 1.383(5) ?
C6 C7 . 1.384(5) ?
C6 C10 . 1.518(5) ?
C7 C8 . 1.383(4) ?
C8 C11 . 1.509(5) ?
C12 O5 . 1.229(3) ?
C12 O4 . 1.259(3) ?
C12 C13 . 1.544(4) ?
C13 O6 . 1.232(3) ?
C13 N2 . 1.333(3) ?
C14 C19 . 1.385(5) ?
C14 C15 . 1.390(4) ?
C14 N2 . 1.429(4) ?
C15 C16 . 1.394(4) ?
C15 C22 . 1.493(5) ?
C16 C17 . 1.374(5) ?
C17 C18 . 1.391(6) ?
C17 C21 . 1.521(5) ?
C18 C19 . 1.389(5) ?
C19 C20 . 1.517(5) ?
C23 O8 . 1.233(3) ?
C23 O7 . 1.249(3) ?
C23 C24 . 1.549(4) ?
C24 O9 . 1.229(3) ?
C24 N3 . 1.331(3) ?
C25 C26 . 1.394(4) ?
C25 C30 . 1.396(4) ?
C25 N3 . 1.429(3) ?
C26 C27 . 1.394(4) ?
C26 C31 . 1.509(4) ?
C27 C28 . 1.389(5) ?
C28 C29 . 1.388(5) ?
C28 C32 . 1.511(5) ?
C29 C30 . 1.392(4) ?
C30 C33 . 1.504(4) ?
C34 O11 . 1.222(3) ?
C34 O10 . 1.260(3) ?
C34 C35 . 1.541(4) ?
C35 O12 . 1.236(3) ?
C35 N4 . 1.330(3) ?
C36 C37 . 1.386(4) ?
C36 C41 . 1.398(4) ?
C36 N4 . 1.430(4) ?
C37 C38 . 1.389(5) ?
C37 C42 . 1.501(5) ?
C38 C39 . 1.384(5) ?
C39 C40 . 1.380(6) ?
C39 C43 . 1.517(5) ?
C40 C41 . 1.387(5) ?
C41 C44 . 1.507(5) ?
C51 C52 . 1.522(5) ?
C52 C53 . 1.512(5) ?
C53 C55 . 1.518(5) ?
C55 N5 . 1.520(4) ?
C57 C58 . 1.458(8) ?
C58 C59 . 1.491(6) ?
C59 C60 . 1.520(5) ?
C60 N5 . 1.514(4) ?
C61 C62 . 1.501(5) ?
C62 C63 . 1.521(4) ?
C63 C64 . 1.511(4) ?
C64 N5 . 1.525(4) ?
C65 C67 . 1.512(6) ?
C67 C68 . 1.525(5) ?
C68 C69 . 1.512(4) ?
C69 N5 . 1.531(4) ?
C48 S2 . 1.781(4) ?
C47 S2 . 1.769(4) ?
C49 S3 . 1.775(6) ?
C50 S3 . 1.763(5) ?
O1 Er1 . 2.3541(17) ?
O3 Er1 . 2.4289(17) ?
O4 Er1 . 2.3400(17) ?
O6 Er1 . 2.4316(17) ?
O7 Er1 . 2.3540(17) ?
O9 Er1 . 2.4592(17) ?
O10 Er1 . 2.3547(17) ?
O12 Er1 . 2.4222(17) ?
O13 Er1 . 2.449(2) ?
O16 S2 . 1.494(3) ?
O17 S3 . 1.491(3) ?
O15 O14A 3_675 1.64(4) ?
S1 O14 . 1.481(15) ?
S1 C46 . 1.589(10) ?
S1 C45 . 1.904(15) ?
S1B O14A . 1.43(4) ?
S1B C45A . 1.648(19) ?
S1B C46B . 1.73(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 O8 4_675 0.86 2.01 2.799(3) 151.5 yes
N2 H2 O11 4_676 0.86 2.03 2.843(3) 157.9 yes
N3 H3 O2 4_576 0.86 2.07 2.852(3) 150.4 yes
N4 H4 O5 4_575 0.86 2.05 2.865(3) 156.7 yes
O13 H13B O17 . 0.9000(10) 1.914(13) 2.780(3) 161(4) yes
O13 H13A O18 3_665 0.9000(10) 1.975(10) 2.854(3) 165(3) yes
O18 H18E O10 3_665 0.9001(10) 2.12(2) 2.901(3) 144(4) yes
O18 H18F O16 3_665 0.9000(11) 1.888(8) 2.778(4) 170(4) yes
_cod_database_fobs_code 2312547