#------------------------------------------------------------------------------
#$Date: 2022-07-27 03:08:08 +0100 (Wed, 27 Jul 2022) $
#$Revision: 276958 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244135.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_2244135
loop_
_publ_author_name
'Petrenko, Yuliia P.'
'Bibik, Yurii S.'
'Khomenko, Dmytro M.'
'Doroshchuk, Roman O.'
'Gural'skiy, Il`ya A.'
'Shova, Sergiu'
'Lampeka, Rostyslav D.'
'Raspertova, Ilona V.'
_publ_section_title
;
Synthesis and crystal structure of hydrated
\m-oxalato-bis{bis[3-methyl-5-(pyridin-2-yl)-1H-1,2,4-triazole]iron(II)}
bis(toluenesulfonate) 2.75-hydrate
;
_journal_coeditor_code VM2269
_journal_issue 8
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989022007460
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac
'[Fe2 (C2 O4) (C8 H8 N4)4] (C7 H7 O3 S1)2, 2.75H2 O'
_chemical_formula_moiety
'C34 H32 Fe2 N16 O4 2+, 2(C7 H7 O3 S -), 2.75(H2 O)'
_chemical_formula_sum 'C48 H51.5 Fe2 N16 O12.75 S2'
_chemical_formula_weight 1232.37
_chemical_name_systematic
'\m-Oxalato-\k^4^O^1^,O^2^:O^1'^,O^2'^-bis{bis[3-methyl-5-(pyridin-2-yl)-1H-1,2,4-triazole-\k^2^N^4^,N^5^]iron(II)} bis(toluenesulfonate) 2.75-hydrate'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha 96.736(4)
_cell_angle_beta 101.490(4)
_cell_angle_gamma 95.216(4)
_cell_formula_units_Z 2
_cell_length_a 9.9635(4)
_cell_length_b 14.4905(6)
_cell_length_c 20.1131(8)
_cell_measurement_reflns_used 5996
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.2330
_cell_measurement_theta_min 1.9810
_cell_volume 2806.5(2)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0309
_diffrn_reflns_av_unetI/netI 0.0578
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 20140
_diffrn_reflns_theta_full 25.027
_diffrn_reflns_theta_max 25.027
_diffrn_reflns_theta_min 1.645
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.667
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.92320
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour 'clear light brown'
_exptl_crystal_density_diffrn 1.458
_exptl_crystal_description block
_exptl_crystal_F_000 1275
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.594
_refine_diff_density_min -0.523
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.055
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 739
_refine_ls_number_reflns 9886
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.055
_refine_ls_R_factor_all 0.0867
_refine_ls_R_factor_gt 0.0582
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+1.2466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1173
_refine_ls_wR_factor_ref 0.1318
_reflns_number_gt 7117
_reflns_number_total 9886
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2269sup1.cif
_cod_data_source_block I
_cod_original_formula_sum 'C48 H51.50 Fe2 N16 O12.75 S2'
_cod_database_code 2244135
_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_estimated_absorpt_t_min 0.800
_shelx_estimated_absorpt_t_max 0.907
_shelx_hkl_file
;
0 0 -3-12.6403 63.2026 1
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0 0 3 37.6991 37.6895 4
0 0 -3-2.81469 44.4196 5
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0 0 3-7.49543 44.1623 5
0 0 4 39107.6 1070.17 4
0 0 -4 41099.7 1089.80 4
0 0 -4 42215.8 1190.23 1
0 0 -4 39249.3 982.417 6
0 0 4 39255.1 973.839 6
0 0 4 40466.4 957.683 5
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0 0 -6 14922.5 642.379 6
0 0 6 15364.9 645.764 6
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-11 -2 4 2746.17 740.155 5
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-11 -2 1 1778.42 675.399 5
-11 -2 0 1614.24 603.515 5
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-11 -2 -2 2110.95 712.202 5
-11 -2 -3 1410.44 652.817 5
-11 -2 -4 2201.28 688.395 5
-11 -2 -5 2566.78 726.094 5
-11 -2 -6 1725.85 687.715 5
11 3 -17 1600.25 598.891 7
11 3 -16 625.297 582.752 7
11 3 -15 542.415 411.027 7
11 3 -14 598.944 418.010 7
11 3 -13 1631.29 618.412 7
11 3 -12 492.047 346.692 7
11 3 -11 1671.42 632.244 7
-11 -3 10 347.158 265.582 5
11 3 -10 893.818 543.809 7
-11 -3 9 2825.33 705.296 5
11 3 -9 1847.18 642.717 7
-11 -3 8 2157.07 657.185 5
-11 -3 7 2325.61 647.527 5
-11 -3 6 907.568 466.919 5
-11 -3 5 7440.15 1103.77 5
-11 -3 4 2243.78 690.338 5
-11 -3 3 1886.78 650.784 5
-11 -3 2 1126.43 492.798 5
-11 -3 1 925.925 478.085 5
-11 -3 0 1824.22 659.822 5
-11 -3 -1 348.559 408.230 5
-11 -3 -2 802.391 461.354 5
-11 -3 -3-77.6555 366.627 5
-11 -3 -4 653.413 476.990 5
-11 -4 19 1132.67 529.438 6
-11 -4 18 499.639 334.401 6
11 4 -17 1169.16 626.410 7
-11 -4 16 50.8133 276.251 5
11 4 -16-9.59868 399.903 7
-11 -4 15 1156.68 535.046 5
11 4 -15-63.1749 290.023 7
-11 -4 14 119.072 279.721 5
11 4 -14 196.010 405.789 7
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-11 -4 12 365.963 337.255 5
-11 -4 11 267.888 223.841 5
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-11 -4 9 68.7915 293.768 5
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-11 -4 7-394.670 238.739 5
-11 -4 6 29.9583 325.588 5
-11 -4 5-487.363 370.427 5
-11 -4 4 1103.34 539.985 5
-11 -4 3 716.105 344.454 5
-11 -4 2 443.830 387.991 5
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-11 -4 -1 1206.29 580.137 5
-11 -4 -2 760.051 478.336 5
-11 -4 -3-179.796 258.704 5
-11 -5 18 523.939 373.155 6
-11 -5 16 73.2796 191.016 5
-11 -5 15 250.532 324.097 5
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-11 -5 12 1055.88 498.685 5
-11 -5 11 446.074 412.202 5
-11 -5 10 659.204 409.163 5
-11 -5 9 507.377 335.048 5
-11 -5 8 398.054 300.954 5
-11 -5 7 760.966 391.004 5
-11 -5 6 6.76439 336.519 5
-11 -5 5 6806.29 1132.69 5
-11 -5 4 1479.48 556.249 5
-11 -5 3 2413.80 762.455 5
-11 -5 2 2264.43 721.915 5
-11 -5 1 6169.15 1150.56 5
-11 -5 0 1091.41 600.747 5
-11 -5 -1 858.604 538.374 5
-11 -6 15 1548.34 532.620 5
-11 -6 14 863.545 460.319 5
-11 -6 13 627.829 350.803 5
-11 -6 12 460.649 342.704 5
-11 -6 11 875.578 501.354 5
-11 -6 10 825.620 438.491 5
-11 -6 9 454.494 340.159 5
-11 -6 8 84.3439 245.340 5
-11 -6 7 7954.52 1196.67 5
-11 -6 6 2239.85 712.118 5
-11 -6 5 4818.58 960.358 5
-11 -6 4 1543.50 623.097 5
-11 -6 3 8182.07 1266.35 5
-11 -6 2 621.921 465.543 5
-11 -6 1 2338.71 761.808 5
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-11 -7 14-229.547 366.670 5
-11 -7 13 646.620 401.645 5
-11 -7 12 441.015 347.219 5
-11 -7 11 1236.88 503.917 5
-11 -7 10 73.8344 300.724 5
-11 -7 9 157.376 300.032 5
-11 -7 8 590.467 389.791 5
-11 -7 7 100.125 321.335 5
-11 -7 6 949.962 443.706 5
-11 -7 5 86.9991 355.185 5
-11 -7 4 265.865 429.202 5
-11 -7 3 747.958 526.503 5
-11 -7 2 1970.20 693.633 5
-11 -8 13 406.966 359.853 5
-11 -8 12-136.168 248.754 5
-11 -8 11 657.910 460.746 5
-11 -8 10 451.626 473.237 5
-11 -8 9 492.824 306.797 5
-11 -8 8 378.250 385.625 5
-11 -8 7 1942.26 664.487 5
-11 -8 6 116.761 319.817 5
-11 -8 5 2114.13 708.038 5
-11 -9 12 608.968 364.955 5
-11 -9 11 592.825 449.010 5
-11 -9 10 132.274 322.405 5
-11 -9 9 2280.79 672.031 5
-11 -9 8-29.9953 246.069 5
12 -10 -9 180.296 340.608 3
12 -10 1-366.859 339.240 7
-12 10 -1 761.235 512.282 2
12 -10 2 459.798 443.031 7
12 -9 -10 269.431 349.002 3
12 -9 -9 566.855 382.377 3
12 -9 -8 298.682 492.604 3
12 -9 -2 433.605 555.741 7
12 -9 -1 375.595 399.314 7
12 -9 0 1395.00 691.551 7
-12 9 0 19.7640 327.021 2
12 -9 1 778.845 511.790 7
-12 9 -1 967.602 536.820 2
12 -9 2-176.443 227.647 7
-12 9 -2 267.188 258.386 2
12 -8 -10 433.704 488.346 3
12 -8 -9 592.734 516.523 3
12 -8 -8 753.362 455.399 3
12 -8 -7 605.285 454.981 3
12 -8 -6 300.040 343.928 3
12 -8 -4 268.868 375.960 7
12 -8 -3 109.312 278.054 7
12 -8 -2 196.117 431.274 7
12 -8 -1 813.279 543.308 7
-12 8 1 1001.15 486.634 2
12 -8 0 652.740 470.875 7
-12 8 0 738.550 452.359 2
12 -8 1 856.638 481.733 7
-12 8 -1 979.600 464.099 2
12 -8 2 140.034 350.148 7
-12 8 -2 234.291 316.803 2
12 -8 3 735.641 430.657 7
-12 8 -3 705.873 497.579 2
12 -7 -11 799.334 566.224 3
12 -7 -10 96.6935 287.229 3
12 -7 -9 220.759 397.714 3
12 -7 -8 795.908 470.133 3
12 -7 -7 982.810 520.527 3
12 -7 -6 92.1984 379.009 7
12 -7 -5 1418.42 602.404 7
12 -7 -4 591.402 422.800 7
12 -7 -3-345.666 386.944 7
12 -7 -2 110.906 404.301 7
12 -7 -1-360.883 360.366 7
-12 7 1 635.146 423.049 2
12 -7 0 57.5633 214.734 7
-12 7 0 80.7930 274.960 2
12 -7 1 717.446 487.711 7
-12 7 -1 260.836 340.029 2
12 -7 2 40.0674 314.686 7
-12 7 -2 197.844 366.390 2
12 -7 3 270.810 263.444 7
-12 7 -3 93.9006 262.023 2
12 -7 4 335.638 391.500 7
12 -6 -11 2708.75 828.130 3
12 -6 -10 1406.44 683.447 3
12 -6 -9 3164.07 860.733 3
12 -6 -8 810.158 541.996 3
12 -6 -8 189.083 446.219 7
12 -6 -7 2371.72 702.251 7
12 -6 -6 753.088 452.446 7
12 -6 -5 2303.45 768.201 7
12 -6 -4 821.764 540.386 7
12 -6 -3 934.133 526.351 7
12 -6 -2-48.2780 308.736 7
-12 6 2 711.945 442.822 2
12 -6 -1 211.769 326.585 7
-12 6 1 501.876 304.820 2
12 -6 0-312.954 314.881 7
-12 6 0 164.334 315.828 2
12 -6 1 569.317 457.922 7
12 -6 2 549.744 360.210 7
12 -6 3 619.867 388.969 7
12 -6 4 875.609 511.178 7
12 -5 -12 1779.39 749.311 3
12 -5 -11 1271.89 585.193 3
12 -5 -10 848.956 437.905 3
12 -5 -9 2718.45 760.494 3
12 -5 -9 3639.93 962.759 7
12 -5 -8 427.836 549.049 7
12 -5 -7 1536.45 650.390 7
12 -5 -6 600.519 392.576 7
12 -5 -5 2372.72 665.598 7
12 -5 -4 797.947 549.154 7
12 -5 -3 1746.05 649.778 7
12 -5 -2 668.481 432.677 7
12 -5 -1 1931.62 705.131 7
12 -5 0 195.275 287.982 7
12 -5 1-458.239 313.237 7
12 -5 2-140.907 241.212 7
12 -5 3 467.441 399.088 7
12 -5 4 611.462 430.557 7
12 -5 5 289.352 413.943 7
12 -4 -12 112.220 339.905 3
12 -4 -11 258.639 426.041 3
12 -4 -10 701.205 511.306 7
12 -4 -9 1233.57 637.700 7
12 -4 -8 507.748 521.044 7
12 -4 -7 178.351 358.953 7
12 -4 -6 67.6517 278.685 7
12 -4 -5 1342.69 601.905 7
12 -4 -4 760.188 530.084 7
12 -4 -3 219.846 249.680 7
12 -4 -2-44.8831 358.211 7
12 -4 -1 817.594 462.090 7
12 -4 0 726.328 409.286 7
12 -4 1-64.1346 300.629 7
12 -4 2 293.083 339.747 7
-12 4 -3 399.007 389.445 5
12 -4 3 257.448 417.056 7
12 -4 4 426.131 371.951 7
12 -3 -12 652.114 448.455 3
12 -3 -11 562.164 429.941 7
12 -3 -10 1977.58 805.637 7
12 -3 -9 388.331 393.545 7
12 -3 -8-304.550 302.085 7
12 -3 -7 558.122 381.329 7
12 -3 -6 389.474 520.784 7
12 -3 -5 1387.75 608.583 7
12 -3 -4 5.32408 330.117 7
12 -3 -3 3897.96 893.090 7
12 -3 -2 731.793 452.101 7
12 -3 -1 6333.91 1133.89 7
12 -3 0 270.717 257.851 7
12 -3 1 1263.84 492.743 7
-12 3 -2 459.577 461.951 5
12 -3 2-370.876 315.888 7
-12 3 -3 1733.97 665.646 5
12 -2 -11 1032.03 521.124 7
12 -2 -10 42.6249 368.955 7
12 -2 -9 920.808 545.514 7
12 -2 -8 627.459 505.631 7
12 -2 -7 1144.87 620.406 7
12 -2 -6 821.546 570.425 7
12 -2 -5 1121.76 604.597 7
12 -2 -4-394.350 474.385 7
12 -2 -3 1488.52 661.163 7
12 -2 -2 323.316 346.574 7
12 -2 -1 1802.70 717.010 7
-12 2 0 1646.88 636.202 5
12 -2 0 1752.27 605.599 7
-12 2 -1 922.499 526.180 5
12 -2 1 1140.36 520.558 7
-12 2 -2-67.5071 419.448 5
-12 2 -3 646.817 494.860 5
12 -1 -11 314.987 367.232 7
12 -1 -10 659.412 499.276 7
12 -1 -9-100.528 257.847 7
12 -1 -8 1177.30 605.282 7
12 -1 -7 77.1874 320.796 7
12 -1 -6 203.811 427.777 7
12 -1 -5 362.564 381.735 7
12 -1 -4 239.713 423.179 7
12 -1 -3 806.060 487.624 7
12 -1 -2 933.915 534.407 7
-12 1 1 900.904 511.712 5
12 -1 -1-307.953 365.287 7
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-12 1 -1 91.3871 231.110 5
-12 1 -2 735.395 537.994 5
12 0 -11 1043.14 549.535 7
12 0 -10 685.765 496.862 7
12 0 -9 252.795 343.617 7
12 0 -8 877.634 544.461 7
12 0 -7 704.668 531.429 7
12 0 -6 76.7641 285.012 7
12 0 -5 851.564 374.796 7
-12 0 4 1953.16 640.399 5
12 0 -4 2062.45 722.604 7
-12 0 3 1914.00 673.861 5
12 0 -3 1396.01 597.345 7
-12 0 2 645.746 420.572 5
-12 0 1 1181.58 548.463 5
-12 0 0 979.733 551.703 5
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12 1 -11 798.621 499.884 7
12 1 -10 3854.66 964.536 7
12 1 -9 2037.73 764.626 7
12 1 -8 2064.79 683.454 7
12 1 -7 1520.08 699.545 7
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12 1 -6 6782.73 1229.19 7
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12 1 -5 1604.99 612.126 7
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12 2 -10 417.636 500.607 7
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12 2 -9 1238.28 616.425 7
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12 2 -8 1860.31 729.042 7
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-12 -4 7 916.895 454.427 5
-12 -4 6 776.872 547.426 5
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-12 -5 15 388.066 308.733 5
-12 -5 14 883.182 467.759 5
-12 -5 13 284.907 336.618 5
-12 -5 12 477.611 427.790 5
-12 -5 11 104.356 239.704 5
-12 -5 10 2846.10 777.169 5
-12 -5 9 1403.67 553.181 5
-12 -5 8 823.328 459.924 5
-13 6 0 884.946 517.376 2
0 0 0 0.00 0.00 0
TITL shI_4382_RoLa in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 9.963455 14.490463 20.113038 96.7350 101.4893 95.2157
ZERR 4.00 0.000435 0.000632 0.000834 0.0035 0.0036 0.0036
LATT 1
SFAC C H N O Fe
UNIT 100.00 100.00 24.00 16.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 52248
_shelx_res_file
;
TITL shi_4382_rola_a.res in P-1
shi_4382_rola.res
created by SHELXL-2018/3 at 10:04:22 on 29-May-2022
REM Old TITL shI_4382_RoLa in P-1
REM SHELXT solution in P-1: R1 0.272, Rweak 0.038, Alpha 0.165
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C48 N11 O17 Fe3
CELL 0.71073 9.96351 14.490481 20.113068 96.7357 101.4904 95.2165
ZERR 2 0.00044 0.000639 0.000842 0.0035 0.0036 0.0036
LATT 1
SFAC C H Fe N O S
UNIT 96 103 4 32 25.5 4
EQIV $1 -X,1-Y,1-Z
EQIV $2 -X,-Y,-Z
EQIV $3 1-X,2-Y,1-Z
EQIV $4 1-X,1-Y,-Z
EQIV $5 -X,1-Y,-Z
EQIV $6 1-X,1-Y,1-Z
L.S. 12 0 0
PLAN 6
SIZE 0.15 0.2 0.35
CONF
HTAB N3 O10_$1
HTAB N7 S1_$2
HTAB N7 O6_$2
HTAB N7 O7_$2
HTAB N11 O9_$3
HTAB N15 S1_$4
HTAB N15 O5_$4
HTAB C3 O1W
HTAB C4 O2W_$5
HTAB C10 O10_$1
HTAB C11 O5W
HTAB C20 O1W_$5
HTAB C27 O5W_$6
HTAB C28 O4W_$6
HTAB C36 O2
HTAB O1W O2W_$5
HTAB O1W O2W
HTAB O2W O4
HTAB O2W O5
HTAB O4W O1
HTAB O4W O3
HTAB O4W O10
HTAB O3W O3
HTAB O3W S2
HTAB O3W O10
htab
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
SHEL 99 0.84
OMIT 3 -2 7
OMIT -1 -1 4
OMIT 1 1 9
OMIT 0 4 10
OMIT -3 -2 1
OMIT 0 0 8
REM
REM
REM
WGHT 0.044700 1.246600
FVAR 3.90165
FE1 3 0.066269 0.333841 0.246629 11.00000 0.03808 0.03913 =
0.04256 0.00405 0.00626 -0.00450
FE2 3 0.460593 0.637027 0.257052 11.00000 0.04001 0.04130 =
0.04383 0.00179 0.00791 -0.00725
O1 5 0.163583 0.462831 0.311076 11.00000 0.04931 0.04814 =
0.04530 -0.00365 0.02132 -0.00742
O2 5 0.203497 0.389994 0.189288 11.00000 0.05512 0.04404 =
0.04268 -0.00716 0.01630 -0.00991
O3 5 0.325505 0.580576 0.315337 11.00000 0.05805 0.04495 =
0.04299 -0.01214 0.01691 -0.01347
O4 5 0.365417 0.508050 0.193784 11.00000 0.05128 0.04950 =
0.04453 -0.00445 0.02219 -0.01144
N1 4 -0.114989 0.387444 0.188604 11.00000 0.05217 0.03665 =
0.04139 0.00436 0.00422 0.00268
N2 4 -0.085496 0.317201 0.308134 11.00000 0.04306 0.04982 =
0.04163 0.01128 0.00656 -0.00041
N3 4 -0.236364 0.294841 0.369951 11.00000 0.05185 0.07027 =
0.04486 0.01034 0.01519 -0.00144
AFIX 43
H3 2 -0.271736 0.279820 0.403417 11.00000 -1.20000
AFIX 0
N4 4 -0.307107 0.327446 0.314819 11.00000 0.04969 0.06001 =
0.05256 0.00899 0.01207 0.00410
N5 4 0.212719 0.252080 0.303959 11.00000 0.03455 0.05319 =
0.04604 0.00387 0.00181 -0.00069
N6 4 0.015518 0.195638 0.188139 11.00000 0.04621 0.03919 =
0.04056 0.00326 -0.00133 -0.00012
N7 4 -0.033031 0.058336 0.130028 11.00000 0.12932 0.04367 =
0.07115 -0.01376 -0.04526 0.01546
AFIX 43
H7 2 -0.071277 0.014005 0.097691 11.00000 -1.20000
AFIX 0
N8 4 0.063206 0.047043 0.185570 11.00000 0.11534 0.04678 =
0.06983 -0.00394 -0.03126 0.01952
N9 4 0.308124 0.715874 0.199425 11.00000 0.03933 0.05801 =
0.04882 0.00235 0.00141 -0.00118
N10 4 0.510623 0.777228 0.312629 11.00000 0.04248 0.04012 =
0.04306 0.00179 0.00562 -0.00293
N11 4 0.572177 0.918738 0.363338 11.00000 0.07282 0.04591 =
0.04861 -0.00929 -0.00154 -0.00226
AFIX 43
H11 2 0.615093 0.965062 0.392887 11.00000 -1.20000
AFIX 0
N12 4 0.473555 0.927083 0.307998 11.00000 0.07342 0.04880 =
0.05654 -0.00174 0.00027 0.00929
N13 4 0.648850 0.589215 0.313644 11.00000 0.05496 0.03990 =
0.04031 0.00656 0.01016 -0.00283
N14 4 0.606987 0.654571 0.192190 11.00000 0.04201 0.04621 =
0.04357 0.00762 0.00772 -0.00272
N15 4 0.751845 0.681009 0.128107 11.00000 0.05345 0.06833 =
0.04267 0.01303 0.01446 -0.00127
AFIX 43
H15 2 0.783958 0.695836 0.093650 11.00000 -1.20000
AFIX 0
N16 4 0.828917 0.653839 0.184265 11.00000 0.05001 0.05739 =
0.05196 0.00844 0.01428 0.00075
C1 1 0.252678 0.506298 0.287698 11.00000 0.03812 0.03753 =
0.03905 0.00003 0.01053 0.00071
C2 1 0.275796 0.464117 0.217195 11.00000 0.03664 0.03639 =
0.03731 -0.00021 0.00735 0.00229
C3 1 -0.123381 0.420353 0.128069 11.00000 0.07376 0.05264 =
0.04898 0.01326 0.00983 -0.00022
AFIX 43
H3A 2 -0.043788 0.429579 0.110984 11.00000 -1.20000
AFIX 0
C4 1 -0.246213 0.440743 0.090724 11.00000 0.09194 0.04803 =
0.05263 0.01430 -0.00645 0.00771
AFIX 43
H4 2 -0.249256 0.462694 0.048877 11.00000 -1.20000
AFIX 0
C5 1 -0.362653 0.428489 0.115589 11.00000 0.07207 0.05929 =
0.06949 0.01199 -0.01240 0.01407
AFIX 43
H5 2 -0.446072 0.441986 0.090806 11.00000 -1.20000
AFIX 0
C6 1 -0.356833 0.395816 0.177993 11.00000 0.04762 0.05327 =
0.06589 0.00386 -0.00078 0.00933
AFIX 43
H6 2 -0.435366 0.387506 0.196046 11.00000 -1.20000
AFIX 0
C7 1 -0.231214 0.376010 0.212493 11.00000 0.04581 0.03447 =
0.04627 0.00263 0.00768 0.00499
C8 1 -0.211194 0.340514 0.278999 11.00000 0.04318 0.03556 =
0.04445 0.00137 0.00641 0.00067
C9 1 -0.105343 0.288666 0.366434 11.00000 0.04842 0.05666 =
0.04331 0.00866 0.00667 -0.00320
C10 1 -0.002301 0.254773 0.419247 11.00000 0.06651 0.11875 =
0.06209 0.03846 0.01230 0.00807
AFIX 137
H10A 2 0.024759 0.197175 0.400311 11.00000 -1.50000
H10B 2 -0.042144 0.244484 0.457843 11.00000 -1.50000
H10C 2 0.077127 0.300738 0.433744 11.00000 -1.50000
AFIX 0
C11 1 0.308392 0.282972 0.361427 11.00000 0.04390 0.06249 =
0.05747 -0.00014 -0.00354 0.00065
AFIX 43
H11A 2 0.326791 0.347058 0.375872 11.00000 -1.20000
AFIX 0
C12 1 0.379887 0.223874 0.399578 11.00000 0.04597 0.08571 =
0.05579 0.00067 -0.00802 0.00813
AFIX 43
H12 2 0.446270 0.247802 0.438745 11.00000 -1.20000
AFIX 0
C13 1 0.352783 0.129463 0.379564 11.00000 0.06564 0.08812 =
0.05663 0.01418 -0.00022 0.02863
AFIX 43
H13 2 0.398179 0.088386 0.405802 11.00000 -1.20000
AFIX 0
C14 1 0.256972 0.095648 0.319780 11.00000 0.06995 0.05738 =
0.05522 0.00058 -0.00045 0.02066
AFIX 43
H14 2 0.237582 0.031753 0.304686 11.00000 -1.20000
AFIX 0
C15 1 0.191168 0.159357 0.283282 11.00000 0.04304 0.04939 =
0.04485 0.00598 0.00515 0.00762
C16 1 0.089266 0.131690 0.218946 11.00000 0.05163 0.04040 =
0.05040 0.00426 0.00146 0.00358
C17 1 -0.060650 0.145723 0.131779 11.00000 0.07511 0.04422 =
0.05257 0.00179 -0.01173 0.00051
C18 1 -0.162250 0.177926 0.077486 11.00000 0.09861 0.06059 =
0.06598 -0.00519 -0.03230 0.00959
AFIX 137
H18A 2 -0.235851 0.200596 0.096682 11.00000 -1.50000
H18B 2 -0.198935 0.126680 0.041786 11.00000 -1.50000
H18C 2 -0.117722 0.227346 0.058849 11.00000 -1.50000
AFIX 0
C19 1 0.208235 0.683612 0.144348 11.00000 0.04541 0.07397 =
0.06240 -0.00410 -0.00194 -0.00257
AFIX 43
H19 2 0.188657 0.619209 0.131749 11.00000 -1.20000
AFIX 0
C20 1 0.133220 0.740606 0.105509 11.00000 0.04893 0.10597 =
0.05987 -0.00107 -0.01137 0.01474
AFIX 43
H20 2 0.063650 0.715303 0.067988 11.00000 -1.20000
AFIX 0
C21 1 0.162679 0.834794 0.123002 11.00000 0.07974 0.09812 =
0.06139 0.00926 -0.00172 0.04067
AFIX 43
H21 2 0.114664 0.874722 0.096693 11.00000 -1.20000
AFIX 0
C22 1 0.263953 0.871185 0.179867 11.00000 0.07611 0.07212 =
0.05880 0.00370 -0.00026 0.02940
AFIX 43
H22 2 0.284770 0.935471 0.192785 11.00000 -1.20000
AFIX 0
C23 1 0.333386 0.809191 0.216971 11.00000 0.04748 0.05557 =
0.04583 0.00348 0.00827 0.00717
C24 1 0.439580 0.840135 0.278944 11.00000 0.05070 0.04724 =
0.04395 0.00037 0.00568 0.00433
C25 1 0.594358 0.830113 0.366292 11.00000 0.05062 0.04435 =
0.04733 0.00056 0.00793 -0.00076
C26 1 0.694984 0.800437 0.421848 11.00000 0.07529 0.06185 =
0.05201 -0.00207 -0.01081 0.00169
AFIX 137
H26A 2 0.650605 0.751460 0.440960 11.00000 -1.50000
H26B 2 0.729815 0.852738 0.456919 11.00000 -1.50000
H26C 2 0.769906 0.777834 0.403759 11.00000 -1.50000
AFIX 0
C27 1 0.664506 0.556463 0.373940 11.00000 0.07511 0.05306 =
0.05182 0.01406 0.01675 0.00361
AFIX 43
H27 2 0.586820 0.544259 0.392017 11.00000 -1.20000
AFIX 0
C28 1 0.789813 0.540106 0.410229 11.00000 0.09455 0.05908 =
0.04730 0.01563 -0.00023 0.01004
AFIX 43
H28 2 0.796418 0.518366 0.452334 11.00000 -1.20000
AFIX 0
C29 1 0.904750 0.555967 0.384093 11.00000 0.06796 0.06849 =
0.06742 0.01508 -0.00652 0.01246
AFIX 43
H29 2 0.990504 0.545042 0.407988 11.00000 -1.20000
AFIX 0
C30 1 0.891565 0.588586 0.321427 11.00000 0.05096 0.06244 =
0.06199 0.00946 0.00568 0.00500
AFIX 43
H30 2 0.968095 0.599935 0.302321 11.00000 -1.20000
AFIX 0
C31 1 0.762556 0.603861 0.288003 11.00000 0.04815 0.03445 =
0.04381 0.00045 0.00516 -0.00224
C32 1 0.736639 0.638248 0.221155 11.00000 0.04327 0.03781 =
0.04509 0.00186 0.00808 -0.00104
C33 1 0.620532 0.682032 0.132590 11.00000 0.05211 0.05726 =
0.04383 0.00885 0.00973 -0.00184
C34 1 0.511013 0.707715 0.078951 11.00000 0.05812 0.12032 =
0.05293 0.02905 0.00526 -0.00027
AFIX 137
H34A 2 0.486349 0.768028 0.093915 11.00000 -1.50000
H34B 2 0.431515 0.661919 0.070729 11.00000 -1.50000
H34C 2 0.544165 0.709851 0.037429 11.00000 -1.50000
AFIX 0
S1 6 0.198151 0.151584 -0.010026 11.00000 0.05717 0.05860 =
0.06181 0.01592 -0.00824 -0.00953
O5 5 0.192114 0.250517 -0.009423 11.00000 0.08948 0.06285 =
0.04417 0.00632 0.00110 0.01772
O6 5 0.245651 0.112294 -0.069924 11.00000 0.16526 0.10085 =
0.05004 -0.02083 -0.01115 0.03381
O7 5 0.073191 0.100380 -0.004769 11.00000 0.06111 0.18310 =
0.16421 0.11545 -0.03576 -0.04583
C35 1 0.323374 0.137794 0.062072 11.00000 0.04365 0.04322 =
0.05267 0.00409 0.01005 0.00096
C36 1 0.341351 0.195768 0.123192 11.00000 0.04866 0.04706 =
0.05930 -0.00207 0.00217 0.01096
AFIX 43
H36 2 0.287580 0.244558 0.126915 11.00000 -1.20000
AFIX 0
C37 1 0.439295 0.181610 0.179134 11.00000 0.05811 0.05643 =
0.04877 -0.00061 0.00373 -0.00009
AFIX 43
H37 2 0.450062 0.221047 0.220260 11.00000 -1.20000
AFIX 0
C38 1 0.520674 0.110866 0.175291 11.00000 0.05686 0.04765 =
0.06779 0.01580 -0.00404 -0.00008
C39 1 0.500838 0.052756 0.114560 11.00000 0.08094 0.06529 =
0.10202 0.00426 0.00146 0.03814
AFIX 43
H39 2 0.554298 0.003751 0.111059 11.00000 -1.20000
AFIX 0
C40 1 0.402645 0.065597 0.058246 11.00000 0.08140 0.06900 =
0.06820 -0.01713 0.00580 0.02324
AFIX 43
H40 2 0.390360 0.024997 0.017557 11.00000 -1.20000
AFIX 0
C41 1 0.631584 0.097202 0.235987 11.00000 0.08687 0.06627 =
0.10646 0.02872 -0.02195 0.00763
AFIX 137
H41A 2 0.718786 0.127442 0.231879 11.00000 -1.50000
H41B 2 0.637337 0.031548 0.236750 11.00000 -1.50000
H41C 2 0.608687 0.123984 0.277673 11.00000 -1.50000
AFIX 0
S2 6 0.302954 0.860784 0.497506 11.00000 0.04742 0.06114 =
0.04414 0.00660 0.00094 -0.00792
O8 5 0.431665 0.882733 0.477841 11.00000 0.04454 0.16137 =
0.08570 0.05315 0.00246 -0.01949
O9 5 0.280170 0.923260 0.554556 11.00000 0.09769 0.07391 =
0.05620 -0.02119 -0.00951 0.00140
O10 5 0.283691 0.764421 0.510056 11.00000 0.08072 0.05994 =
0.04349 0.01040 0.00718 0.00760
C42 1 0.170120 0.870736 0.426818 11.00000 0.04345 0.04183 =
0.04878 0.00604 0.01018 -0.00216
C43 1 0.082793 0.938320 0.430507 11.00000 0.06289 0.06360 =
0.06055 -0.00927 0.01100 0.00707
AFIX 43
H43 2 0.092198 0.979305 0.470797 11.00000 -1.20000
AFIX 0
C44 1 -0.019574 0.945359 0.373976 11.00000 0.06121 0.05650 =
0.09140 0.00496 0.00727 0.02041
AFIX 43
H44 2 -0.078646 0.991101 0.376928 11.00000 -1.20000
AFIX 0
C45 1 -0.035294 0.885664 0.313426 11.00000 0.05341 0.05148 =
0.06163 0.01320 0.00150 -0.00132
C46 1 0.054925 0.819952 0.310521 11.00000 0.05843 0.05898 =
0.04534 -0.00397 0.00487 0.00535
AFIX 43
H46 2 0.047203 0.779862 0.269950 11.00000 -1.20000
AFIX 0
C47 1 0.156494 0.811938 0.366150 11.00000 0.05153 0.05189 =
0.05091 -0.00159 0.00346 0.01159
AFIX 43
H47 2 0.216238 0.766700 0.362861 11.00000 -1.20000
AFIX 0
C48 1 -0.148479 0.893527 0.252650 11.00000 0.07366 0.08204 =
0.08848 0.02294 -0.01152 0.01216
AFIX 137
H48A 2 -0.121972 0.869788 0.211156 11.00000 -1.50000
H48B 2 -0.163294 0.957970 0.251877 11.00000 -1.50000
H48C 2 -0.232041 0.857815 0.256327 11.00000 -1.50000
AFIX 0
PART -1
O1W 5 -0.018391 0.459606 -0.013080 10.25000 0.15919
AFIX 3
H1WA 2 -0.026571 0.516586 -0.000700 10.25000 -1.50000
H1WB 2 0.065089 0.453836 0.003990 10.25000 -1.50000
AFIX 0
PART 0
O2W 5 0.269266 0.441659 0.046058 11.00000 0.25224 0.08628 =
0.05060 0.01352 0.01231 0.02391
AFIX 3
H2WA 2 0.302346 0.458579 0.088428 11.00000 -1.50000
H2WB 2 0.249386 0.382599 0.033148 11.00000 -1.50000
AFIX 0
PART 1
O4W 5 0.266056 0.575975 0.457351 10.75000 0.20113 0.09592 =
0.05050 0.00449 0.03371 0.04603
AFIX 3
H4WA 2 0.264626 0.557925 0.414491 10.75000 -1.50000
H4WB 2 0.272806 0.635525 0.470971 10.75000 -1.50000
AFIX 0
PART -1
O5W 5 0.460616 0.444930 0.482473 10.50000 0.13647
AFIX 3
H5WA 2 0.536786 0.439800 0.510473 10.50000 -1.50000
H5WB 2 0.458166 0.499590 0.469693 10.50000 -1.50000
AFIX 0
PART 2
O3W 5 0.394266 0.620997 0.457261 10.25000 0.09386
AFIX 3
H3WA 2 0.376336 0.611397 0.413001 10.25000 -1.50000
H3WB 2 0.362126 0.671997 0.469671 10.25000 -1.50000
AFIX 0
HKLF 4
REM shi_4382_rola_a.res in P-1
REM wR2 = 0.1318, GooF = S = 1.055, Restrained GooF = 1.055 for all data
REM R1 = 0.0582 for 7117 Fo > 4sig(Fo) and 0.0867 for all 9886 data
REM 739 parameters refined using 0 restraints
END
WGHT 0.0447 1.2467
REM Instructions for potential hydrogen bonds
HTAB N3 O10_$1
HTAB N7 S1_$2
HTAB N7 O6_$2
HTAB N7 O7_$2
HTAB N11 O9_$3
HTAB N15 S1_$4
HTAB N15 O5_$4
HTAB C3 O1W
HTAB C4 O2W_$5
HTAB C10 O10_$1
HTAB C11 O5W
HTAB C20 O1W_$5
HTAB C27 O5W_$6
HTAB C28 O4W_$6
HTAB C36 O2
HTAB O1W O2W_$5
HTAB O1W O2W
HTAB O2W O4
HTAB O2W O5
HTAB O4W O1
HTAB O4W O3
HTAB O4W O10
HTAB O3W O3
HTAB O3W S2
HTAB O3W O10
REM Highest difference peak 0.594, deepest hole -0.523, 1-sigma level 0.051
Q1 1 0.0788 0.0840 -0.0197 11.00000 0.05 0.59
Q2 1 0.0607 0.1667 0.0252 11.00000 0.05 0.54
Q3 1 0.3926 0.9389 0.5180 11.00000 0.05 0.33
Q4 1 0.1335 0.3994 0.0408 11.00000 0.05 0.32
Q5 1 0.4403 0.6480 0.4439 11.00000 0.05 0.32
Q6 1 0.2338 0.8853 0.5212 11.00000 0.05 0.32
;
_shelx_res_checksum 21218
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Fe Fe1 0.06627(5) 0.33384(3) 0.24663(2) 0.04095(15) Uani d 1 . .
Fe Fe2 0.46059(5) 0.63703(3) 0.25705(2) 0.04295(15) Uani d 1 . .
O O1 0.1636(2) 0.46283(16) 0.31108(11) 0.0477(6) Uani d 1 . .
O O2 0.2035(3) 0.38999(16) 0.18929(11) 0.0485(6) Uani d 1 . .
O O3 0.3255(3) 0.58058(16) 0.31534(11) 0.0505(6) Uani d 1 . .
O O4 0.3654(3) 0.50805(16) 0.19378(11) 0.0487(6) Uani d 1 . .
N N1 -0.1150(3) 0.38744(19) 0.18860(13) 0.0445(7) Uani d 1 . .
N N2 -0.0855(3) 0.3172(2) 0.30813(13) 0.0451(7) Uani d 1 . .
N N3 -0.2364(3) 0.2948(2) 0.36995(14) 0.0553(8) Uani d 1 . .
H H3 -0.271736 0.279820 0.403417 0.066 Uiso calc 1 . .
N N4 -0.3071(3) 0.3274(2) 0.31482(15) 0.0540(8) Uani d 1 . .
N N5 0.2127(3) 0.2521(2) 0.30396(13) 0.0462(7) Uani d 1 . .
N N6 0.0155(3) 0.19564(19) 0.18814(13) 0.0440(7) Uani d 1 . .
N N7 -0.0330(4) 0.0583(2) 0.13003(17) 0.0922(14) Uani d 1 . .
H H7 -0.071277 0.014005 0.097691 0.111 Uiso calc 1 . .
N N8 0.0632(4) 0.0470(2) 0.18557(17) 0.0848(13) Uani d 1 . .
N N9 0.3081(3) 0.7159(2) 0.19942(14) 0.0507(8) Uani d 1 . .
N N10 0.5106(3) 0.77723(19) 0.31263(13) 0.0432(7) Uani d 1 . .
N N11 0.5722(3) 0.9187(2) 0.36334(15) 0.0597(9) Uani d 1 . .
H H11 0.615093 0.965062 0.392887 0.072 Uiso calc 1 . .
N N12 0.4736(4) 0.9271(2) 0.30800(16) 0.0621(9) Uani d 1 . .
N N13 0.6489(3) 0.58921(19) 0.31364(13) 0.0455(7) Uani d 1 . .
N N14 0.6070(3) 0.65457(19) 0.19219(13) 0.0445(7) Uani d 1 . .
N N15 0.7518(3) 0.6810(2) 0.12811(14) 0.0543(8) Uani d 1 . .
H H15 0.783958 0.695836 0.093650 0.065 Uiso calc 1 . .
N N16 0.8289(3) 0.6538(2) 0.18426(14) 0.0529(8) Uani d 1 . .
C C1 0.2527(4) 0.5063(2) 0.28770(16) 0.0386(8) Uani d 1 . .
C C2 0.2758(3) 0.4641(2) 0.21719(16) 0.0374(8) Uani d 1 . .
C C3 -0.1234(4) 0.4204(3) 0.12807(18) 0.0589(11) Uani d 1 . .
H H3A -0.043788 0.429579 0.110984 0.071 Uiso calc 1 . .
C C4 -0.2462(5) 0.4407(3) 0.0907(2) 0.0667(12) Uani d 1 . .
H H4 -0.249256 0.462694 0.048877 0.080 Uiso calc 1 . .
C C5 -0.3627(5) 0.4285(3) 0.1156(2) 0.0702(13) Uani d 1 . .
H H5 -0.446072 0.441986 0.090806 0.084 Uiso calc 1 . .
C C6 -0.3568(4) 0.3958(3) 0.17799(19) 0.0575(10) Uani d 1 . .
H H6 -0.435366 0.387506 0.196046 0.069 Uiso calc 1 . .
C C7 -0.2312(4) 0.3760(2) 0.21249(16) 0.0427(8) Uani d 1 . .
C C8 -0.2112(4) 0.3405(2) 0.27900(16) 0.0421(8) Uani d 1 . .
C C9 -0.1053(4) 0.2887(3) 0.36643(17) 0.0503(9) Uani d 1 . .
C C10 -0.0023(4) 0.2548(4) 0.4192(2) 0.0807(14) Uani d 1 . .
H H10A 0.024759 0.197175 0.400311 0.121 Uiso calc 1 . .
H H10B -0.042144 0.244484 0.457843 0.121 Uiso calc 1 . .
H H10C 0.077127 0.300738 0.433744 0.121 Uiso calc 1 . .
C C11 0.3084(4) 0.2830(3) 0.36143(18) 0.0577(10) Uani d 1 . .
H H11A 0.326791 0.347058 0.375872 0.069 Uiso calc 1 . .
C C12 0.3799(4) 0.2239(3) 0.3996(2) 0.0659(12) Uani d 1 . .
H H12 0.446270 0.247802 0.438745 0.079 Uiso calc 1 . .
C C13 0.3528(4) 0.1295(3) 0.3796(2) 0.0704(13) Uani d 1 . .
H H13 0.398179 0.088386 0.405802 0.084 Uiso calc 1 . .
C C14 0.2570(4) 0.0956(3) 0.31978(18) 0.0625(11) Uani d 1 . .
H H14 0.237582 0.031753 0.304686 0.075 Uiso calc 1 . .
C C15 0.1912(4) 0.1594(3) 0.28328(17) 0.0463(9) Uani d 1 . .
C C16 0.0893(4) 0.1317(3) 0.21895(17) 0.0491(9) Uani d 1 . .
C C17 -0.0606(4) 0.1457(3) 0.13178(19) 0.0617(11) Uani d 1 . .
C C18 -0.1622(5) 0.1779(3) 0.0775(2) 0.0832(15) Uani d 1 . .
H H18A -0.235851 0.200596 0.096682 0.125 Uiso calc 1 . .
H H18B -0.198935 0.126680 0.041786 0.125 Uiso calc 1 . .
H H18C -0.117722 0.227346 0.058849 0.125 Uiso calc 1 . .
C C19 0.2082(4) 0.6836(3) 0.14435(19) 0.0642(11) Uani d 1 . .
H H19 0.188657 0.619209 0.131749 0.077 Uiso calc 1 . .
C C20 0.1332(4) 0.7406(4) 0.1055(2) 0.0755(14) Uani d 1 . .
H H20 0.063650 0.715303 0.067988 0.091 Uiso calc 1 . .
C C21 0.1627(5) 0.8348(4) 0.1230(2) 0.0803(15) Uani d 1 . .
H H21 0.114664 0.874722 0.096693 0.096 Uiso calc 1 . .
C C22 0.2640(5) 0.8712(3) 0.17987(19) 0.0702(13) Uani d 1 . .
H H22 0.284770 0.935471 0.192785 0.084 Uiso calc 1 . .
C C23 0.3334(4) 0.8092(3) 0.21697(17) 0.0501(9) Uani d 1 . .
C C24 0.4396(4) 0.8401(3) 0.27894(17) 0.0485(9) Uani d 1 . .
C C25 0.5944(4) 0.8301(3) 0.36629(17) 0.0487(9) Uani d 1 . .
C C26 0.6950(4) 0.8004(3) 0.42185(18) 0.0677(12) Uani d 1 . .
H H26A 0.650605 0.751460 0.440960 0.102 Uiso calc 1 . .
H H26B 0.729815 0.852738 0.456919 0.102 Uiso calc 1 . .
H H26C 0.769906 0.777834 0.403759 0.102 Uiso calc 1 . .
C C27 0.6645(4) 0.5565(3) 0.37394(18) 0.0592(11) Uani d 1 . .
H H27 0.586820 0.544259 0.392017 0.071 Uiso calc 1 . .
C C28 0.7898(5) 0.5401(3) 0.4102(2) 0.0684(12) Uani d 1 . .
H H28 0.796418 0.518366 0.452334 0.082 Uiso calc 1 . .
C C29 0.9047(5) 0.5560(3) 0.3841(2) 0.0702(12) Uani d 1 . .
H H29 0.990504 0.545042 0.407988 0.084 Uiso calc 1 . .
C C30 0.8916(4) 0.5886(3) 0.32143(19) 0.0594(11) Uani d 1 . .
H H30 0.968095 0.599935 0.302321 0.071 Uiso calc 1 . .
C C31 0.7626(4) 0.6039(2) 0.28800(16) 0.0436(8) Uani d 1 . .
C C32 0.7366(4) 0.6382(2) 0.22115(16) 0.0429(8) Uani d 1 . .
C C33 0.6205(4) 0.6820(3) 0.13259(17) 0.0515(10) Uani d 1 . .
C C34 0.5110(4) 0.7077(3) 0.07895(18) 0.0773(14) Uani d 1 . .
H H34A 0.486349 0.768028 0.093915 0.116 Uiso calc 1 . .
H H34B 0.431515 0.661919 0.070729 0.116 Uiso calc 1 . .
H H34C 0.544165 0.709851 0.037429 0.116 Uiso calc 1 . .
S S1 0.19815(11) 0.15158(8) -0.01003(5) 0.0625(3) Uani d 1 . .
O O5 0.1921(3) 0.25052(19) -0.00942(11) 0.0669(8) Uani d 1 . .
O O6 0.2457(4) 0.1123(2) -0.06992(14) 0.1116(13) Uani d 1 . .
O O7 0.0732(4) 0.1004(3) -0.0048(2) 0.1409(18) Uani d 1 . .
C C35 0.3234(4) 0.1378(3) 0.06207(17) 0.0470(9) Uani d 1 . .
C C36 0.3414(4) 0.1958(3) 0.12319(18) 0.0534(10) Uani d 1 . .
H H36 0.287580 0.244558 0.126915 0.064 Uiso calc 1 . .
C C37 0.4393(4) 0.1816(3) 0.17913(18) 0.0566(10) Uani d 1 . .
H H37 0.450062 0.221047 0.220260 0.068 Uiso calc 1 . .
C C38 0.5207(4) 0.1109(3) 0.1753(2) 0.0596(11) Uani d 1 . .
C C39 0.5008(5) 0.0528(3) 0.1146(2) 0.0840(15) Uani d 1 . .
H H39 0.554298 0.003751 0.111059 0.101 Uiso calc 1 . .
C C40 0.4026(5) 0.0656(3) 0.0582(2) 0.0755(13) Uani d 1 . .
H H40 0.390360 0.024997 0.017557 0.091 Uiso calc 1 . .
C C41 0.6316(5) 0.0972(3) 0.2360(2) 0.0912(16) Uani d 1 . .
H H41A 0.718786 0.127442 0.231879 0.137 Uiso calc 1 . .
H H41B 0.637337 0.031548 0.236750 0.137 Uiso calc 1 . .
H H41C 0.608687 0.123984 0.277673 0.137 Uiso calc 1 . .
S S2 0.30295(10) 0.86078(7) 0.49751(4) 0.0531(3) Uani d 1 . .
O O8 0.4317(3) 0.8827(3) 0.47784(15) 0.0979(12) Uani d 1 . .
O O9 0.2802(3) 0.9233(2) 0.55456(13) 0.0826(9) Uani d 1 . .
O O10 0.2837(3) 0.76442(18) 0.51006(11) 0.0620(7) Uani d 1 . .
C C42 0.1701(4) 0.8707(2) 0.42682(17) 0.0451(9) Uani d 1 . .
C C43 0.0828(4) 0.9383(3) 0.4305(2) 0.0641(11) Uani d 1 . .
H H43 0.092198 0.979305 0.470797 0.077 Uiso calc 1 . .
C C44 -0.0196(4) 0.9454(3) 0.3740(2) 0.0705(12) Uani d 1 . .
H H44 -0.078646 0.991101 0.376928 0.085 Uiso calc 1 . .
C C45 -0.0353(4) 0.8857(3) 0.3134(2) 0.0570(10) Uani d 1 . .
C C46 0.0549(4) 0.8200(3) 0.31052(18) 0.0561(10) Uani d 1 . .
H H46 0.047203 0.779862 0.269950 0.067 Uiso calc 1 . .
C C47 0.1565(4) 0.8119(3) 0.36615(17) 0.0529(10) Uani d 1 . .
H H47 0.216238 0.766700 0.362861 0.063 Uiso calc 1 . .
C C48 -0.1485(5) 0.8935(3) 0.2527(2) 0.0843(15) Uani d 1 . .
H H48A -0.121972 0.869788 0.211156 0.126 Uiso calc 1 . .
H H48B -0.163294 0.957970 0.251877 0.126 Uiso calc 1 . .
H H48C -0.232041 0.857815 0.256327 0.126 Uiso calc 1 . .
O O1W -0.018(2) 0.4596(12) -0.0131(10) 0.159(7) Uiso d 0.25 A -1
H H1WA -0.026571 0.516586 -0.000700 0.239 Uiso d 0.25 A -1
H H1WB 0.065089 0.453836 0.003990 0.239 Uiso d 0.25 A -1
O O2W 0.2693(5) 0.4417(2) 0.04606(14) 0.1319(16) Uani d 1 . .
H H2WA 0.302346 0.458579 0.088428 0.198 Uiso d 1 . .
H H2WB 0.249386 0.382599 0.033148 0.198 Uiso d 1 . .
O O4W 0.2661(6) 0.5760(3) 0.45735(18) 0.1135(19) Uani d 0.75 B 1
H H4WA 0.264626 0.557925 0.414491 0.170 Uiso d 0.75 B 1
H H4WB 0.272806 0.635525 0.470971 0.170 Uiso d 0.75 B 1
O O5W 0.4606(9) 0.4449(5) 0.4825(4) 0.136(3) Uiso d 0.5 C -1
H H5WA 0.536786 0.439800 0.510473 0.205 Uiso d 0.5 C -1
H H5WB 0.458166 0.499590 0.469693 0.205 Uiso d 0.5 C -1
O O3W 0.3943(15) 0.6210(10) 0.4573(6) 0.094(4) Uiso d 0.25 D 2
H H3WA 0.376336 0.611397 0.413001 0.141 Uiso d 0.25 D 2
H H3WB 0.362126 0.671997 0.469671 0.141 Uiso d 0.25 D 2
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
Fe1 0.0381(3) 0.0391(3) 0.0426(3) -0.0045(2) 0.0063(2) 0.0040(2)
Fe2 0.0400(3) 0.0413(3) 0.0438(3) -0.0073(2) 0.0079(2) 0.0018(2)
O1 0.0493(16) 0.0481(15) 0.0453(13) -0.0074(12) 0.0213(12) -0.0037(11)
O2 0.0551(17) 0.0440(15) 0.0427(13) -0.0099(13) 0.0163(12) -0.0072(11)
O3 0.0580(17) 0.0450(15) 0.0430(13) -0.0135(13) 0.0169(12) -0.0121(12)
O4 0.0513(16) 0.0495(15) 0.0445(13) -0.0114(13) 0.0222(12) -0.0044(12)
N1 0.052(2) 0.0367(17) 0.0414(16) 0.0027(15) 0.0042(14) 0.0044(13)
N2 0.0431(19) 0.0498(19) 0.0416(15) -0.0004(15) 0.0066(13) 0.0113(14)
N3 0.052(2) 0.070(2) 0.0449(17) -0.0014(18) 0.0152(15) 0.0103(16)
N4 0.050(2) 0.060(2) 0.0526(18) 0.0041(17) 0.0121(16) 0.0090(16)
N5 0.0345(18) 0.053(2) 0.0460(16) -0.0007(15) 0.0018(13) 0.0039(15)
N6 0.0462(19) 0.0392(17) 0.0406(15) -0.0001(14) -0.0013(13) 0.0033(14)
N7 0.129(4) 0.044(2) 0.071(2) 0.015(2) -0.045(2) -0.0138(18)
N8 0.115(3) 0.047(2) 0.070(2) 0.020(2) -0.031(2) -0.0039(18)
N9 0.0393(19) 0.058(2) 0.0488(17) -0.0012(16) 0.0014(14) 0.0024(16)
N10 0.0425(18) 0.0401(17) 0.0431(16) -0.0029(14) 0.0056(14) 0.0018(14)
N11 0.073(3) 0.046(2) 0.0486(18) -0.0023(18) -0.0015(17) -0.0093(15)
N12 0.073(3) 0.049(2) 0.0565(19) 0.0093(19) 0.0003(18) -0.0017(17)
N13 0.055(2) 0.0399(17) 0.0403(16) -0.0028(15) 0.0102(14) 0.0066(14)
N14 0.0420(19) 0.0462(18) 0.0436(16) -0.0027(15) 0.0077(14) 0.0076(14)
N15 0.053(2) 0.068(2) 0.0427(17) -0.0013(18) 0.0145(15) 0.0130(16)
N16 0.050(2) 0.057(2) 0.0520(18) 0.0007(16) 0.0143(16) 0.0084(16)
C1 0.038(2) 0.038(2) 0.0391(18) 0.0007(17) 0.0105(16) 0.0000(16)
C2 0.037(2) 0.036(2) 0.0373(18) 0.0023(17) 0.0074(15) -0.0002(16)
C3 0.074(3) 0.053(3) 0.049(2) 0.000(2) 0.010(2) 0.013(2)
C4 0.092(4) 0.048(3) 0.053(2) 0.008(3) -0.006(2) 0.014(2)
C5 0.072(3) 0.059(3) 0.069(3) 0.014(3) -0.012(2) 0.012(2)
C6 0.048(3) 0.053(3) 0.066(2) 0.009(2) -0.001(2) 0.004(2)
C7 0.046(2) 0.034(2) 0.0463(19) 0.0050(17) 0.0077(17) 0.0026(16)
C8 0.043(2) 0.036(2) 0.0445(19) 0.0007(17) 0.0064(17) 0.0014(16)
C9 0.048(3) 0.057(2) 0.043(2) -0.003(2) 0.0067(18) 0.0087(18)
C10 0.067(3) 0.119(4) 0.062(3) 0.008(3) 0.012(2) 0.038(3)
C11 0.044(2) 0.062(3) 0.057(2) 0.001(2) -0.0035(19) 0.000(2)
C12 0.046(3) 0.086(3) 0.056(2) 0.008(2) -0.0080(19) 0.001(2)
C13 0.066(3) 0.088(4) 0.057(2) 0.029(3) 0.000(2) 0.014(3)
C14 0.070(3) 0.057(3) 0.055(2) 0.021(2) 0.000(2) 0.001(2)
C15 0.043(2) 0.049(2) 0.0449(19) 0.0076(19) 0.0052(17) 0.0060(18)
C16 0.052(2) 0.040(2) 0.050(2) 0.0036(19) 0.0015(18) 0.0043(18)
C17 0.075(3) 0.044(2) 0.053(2) 0.001(2) -0.012(2) 0.0018(19)
C18 0.099(4) 0.061(3) 0.066(3) 0.010(3) -0.032(2) -0.005(2)
C19 0.045(3) 0.074(3) 0.062(2) -0.003(2) -0.002(2) -0.004(2)
C20 0.049(3) 0.106(4) 0.060(3) 0.015(3) -0.011(2) -0.001(3)
C21 0.080(4) 0.098(4) 0.061(3) 0.041(3) -0.002(2) 0.009(3)
C22 0.076(3) 0.072(3) 0.059(2) 0.029(3) 0.000(2) 0.004(2)
C23 0.047(2) 0.056(3) 0.046(2) 0.007(2) 0.0083(17) 0.0035(19)
C24 0.051(2) 0.047(2) 0.044(2) 0.004(2) 0.0057(17) 0.0004(18)
C25 0.051(2) 0.044(2) 0.047(2) -0.0008(19) 0.0079(18) 0.0006(18)
C26 0.075(3) 0.062(3) 0.052(2) 0.002(2) -0.011(2) -0.002(2)
C27 0.075(3) 0.053(3) 0.052(2) 0.004(2) 0.017(2) 0.014(2)
C28 0.095(4) 0.059(3) 0.047(2) 0.010(3) 0.000(2) 0.016(2)
C29 0.068(3) 0.068(3) 0.067(3) 0.012(3) -0.007(2) 0.015(2)
C30 0.051(3) 0.062(3) 0.062(2) 0.005(2) 0.006(2) 0.009(2)
C31 0.048(2) 0.034(2) 0.0438(19) -0.0022(17) 0.0052(17) 0.0004(16)
C32 0.043(2) 0.038(2) 0.0451(19) -0.0010(17) 0.0081(17) 0.0019(16)
C33 0.052(3) 0.057(2) 0.044(2) -0.002(2) 0.0097(18) 0.0089(19)
C34 0.058(3) 0.120(4) 0.053(2) 0.000(3) 0.005(2) 0.029(3)
S1 0.0572(7) 0.0586(7) 0.0618(6) -0.0095(5) -0.0082(5) 0.0159(6)
O5 0.089(2) 0.0629(19) 0.0442(14) 0.0177(16) 0.0011(14) 0.0063(13)
O6 0.165(4) 0.101(3) 0.0500(17) 0.034(3) -0.011(2) -0.0208(17)
O7 0.061(2) 0.183(4) 0.164(3) -0.046(2) -0.036(2) 0.115(3)
C35 0.044(2) 0.043(2) 0.053(2) 0.0010(18) 0.0101(17) 0.0041(18)
C36 0.049(2) 0.047(2) 0.059(2) 0.0110(19) 0.0022(19) -0.0021(19)
C37 0.058(3) 0.056(3) 0.049(2) 0.000(2) 0.0037(19) -0.0006(19)
C38 0.057(3) 0.048(2) 0.068(3) 0.000(2) -0.004(2) 0.016(2)
C39 0.081(4) 0.065(3) 0.102(4) 0.038(3) 0.001(3) 0.004(3)
C40 0.081(4) 0.069(3) 0.068(3) 0.023(3) 0.006(2) -0.017(2)
C41 0.087(4) 0.066(3) 0.106(4) 0.008(3) -0.022(3) 0.029(3)
S2 0.0474(6) 0.0611(7) 0.0441(5) -0.0079(5) 0.0009(4) 0.0066(5)
O8 0.0445(19) 0.161(3) 0.086(2) -0.019(2) 0.0025(16) 0.053(2)
O9 0.098(3) 0.074(2) 0.0562(16) 0.0014(18) -0.0095(16) -0.0212(15)
O10 0.081(2) 0.0599(18) 0.0435(14) 0.0076(15) 0.0072(13) 0.0104(13)
C42 0.043(2) 0.042(2) 0.049(2) -0.0022(18) 0.0102(17) 0.0060(17)
C43 0.063(3) 0.064(3) 0.061(2) 0.007(2) 0.011(2) -0.009(2)
C44 0.061(3) 0.057(3) 0.091(3) 0.020(2) 0.007(3) 0.005(3)
C45 0.053(3) 0.051(2) 0.062(2) -0.001(2) 0.002(2) 0.013(2)
C46 0.058(3) 0.059(3) 0.045(2) 0.005(2) 0.0049(19) -0.0040(19)
C47 0.052(3) 0.052(2) 0.051(2) 0.012(2) 0.0035(18) -0.0016(19)
C48 0.074(3) 0.082(4) 0.088(3) 0.012(3) -0.012(3) 0.023(3)
O2W 0.252(5) 0.086(3) 0.0506(18) 0.024(3) 0.012(2) 0.0135(18)
O4W 0.201(6) 0.096(4) 0.051(2) 0.046(4) 0.034(3) 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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 '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
O1 Fe1 N1 . . 98.95(10) ?
O1 Fe1 N5 . . 91.45(10) ?
O2 Fe1 O1 . . 76.88(8) ?
O2 Fe1 N1 . . 94.10(10) ?
O2 Fe1 N2 . . 163.77(10) ?
O2 Fe1 N5 . . 96.26(10) ?
O2 Fe1 N6 . . 97.91(10) ?
N2 Fe1 O1 . . 91.45(10) ?
N2 Fe1 N1 . . 76.39(10) ?
N2 Fe1 N5 . . 95.26(10) ?
N2 Fe1 N6 . . 95.76(11) ?
N5 Fe1 N1 . . 166.75(11) ?
N6 Fe1 O1 . . 167.01(10) ?
N6 Fe1 N1 . . 93.25(10) ?
N6 Fe1 N5 . . 77.17(10) ?
O3 Fe2 O4 . . 77.01(8) ?
O3 Fe2 N9 . . 95.46(10) ?
O3 Fe2 N10 . . 99.08(9) ?
O3 Fe2 N13 . . 96.09(10) ?
O3 Fe2 N14 . . 164.19(10) ?
O4 Fe2 N9 . . 90.81(10) ?
O4 Fe2 N10 . . 166.87(10) ?
O4 Fe2 N13 . . 100.13(10) ?
O4 Fe2 N14 . . 90.65(9) ?
N10 Fe2 N9 . . 76.99(11) ?
N10 Fe2 N13 . . 92.72(10) ?
N13 Fe2 N9 . . 165.61(11) ?
N14 Fe2 N9 . . 94.55(10) ?
N14 Fe2 N10 . . 95.07(10) ?
N14 Fe2 N13 . . 76.15(10) ?
C1 O1 Fe1 . . 113.9(2) ?
C2 O2 Fe1 . . 115.3(2) ?
C1 O3 Fe2 . . 115.4(2) ?
C2 O4 Fe2 . . 114.1(2) ?
C3 N1 Fe1 . . 126.0(3) ?
C7 N1 Fe1 . . 115.9(2) ?
C7 N1 C3 . . 117.7(3) ?
C8 N2 Fe1 . . 113.6(2) ?
C9 N2 Fe1 . . 142.8(2) ?
C9 N2 C8 . . 103.6(3) ?
N4 N3 H3 . . 124.0 ?
C9 N3 H3 . . 124.0 ?
C9 N3 N4 . . 112.1(3) ?
C8 N4 N3 . . 101.7(3) ?
C11 N5 Fe1 . . 127.1(3) ?
C15 N5 Fe1 . . 115.0(2) ?
C15 N5 C11 . . 117.3(3) ?
C16 N6 Fe1 . . 111.9(2) ?
C17 N6 Fe1 . . 144.8(2) ?
C17 N6 C16 . . 103.3(3) ?
N8 N7 H7 . . 124.2 ?
C17 N7 H7 . . 124.2 ?
C17 N7 N8 . . 111.6(3) ?
C16 N8 N7 . . 101.8(3) ?
C19 N9 Fe2 . . 128.0(3) ?
C19 N9 C23 . . 117.1(3) ?
C23 N9 Fe2 . . 114.2(2) ?
C24 N10 Fe2 . . 111.8(2) ?
C25 N10 Fe2 . . 144.1(2) ?
C25 N10 C24 . . 103.8(3) ?
N12 N11 H11 . . 124.2 ?
C25 N11 H11 . . 124.2 ?
C25 N11 N12 . . 111.6(3) ?
C24 N12 N11 . . 102.2(3) ?
C27 N13 Fe2 . . 126.7(3) ?
C27 N13 C31 . . 117.1(3) ?
C31 N13 Fe2 . . 115.8(2) ?
C32 N14 Fe2 . . 113.6(2) ?
C33 N14 Fe2 . . 142.5(3) ?
C33 N14 C32 . . 103.7(3) ?
N16 N15 H15 . . 124.0 ?
C33 N15 H15 . . 124.0 ?
C33 N15 N16 . . 112.0(3) ?
C32 N16 N15 . . 101.7(3) ?
O1 C1 O3 . . 126.5(3) ?
O1 C1 C2 . . 116.8(3) ?
O3 C1 C2 . . 116.6(3) ?
O2 C2 O4 . . 126.3(3) ?
O2 C2 C1 . . 117.0(3) ?
O4 C2 C1 . . 116.7(3) ?
N1 C3 H3A . . 119.0 ?
N1 C3 C4 . . 122.1(4) ?
C4 C3 H3A . . 119.0 ?
C3 C4 H4 . . 120.3 ?
C5 C4 C3 . . 119.4(4) ?
C5 C4 H4 . . 120.3 ?
C4 C5 H5 . . 120.1 ?
C4 C5 C6 . . 119.8(4) ?
C6 C5 H5 . . 120.1 ?
C5 C6 H6 . . 121.0 ?
C7 C6 C5 . . 118.0(4) ?
C7 C6 H6 . . 121.0 ?
N1 C7 C6 . . 123.1(3) ?
N1 C7 C8 . . 113.6(3) ?
C6 C7 C8 . . 123.4(3) ?
N2 C8 C7 . . 120.0(3) ?
N4 C8 N2 . . 114.5(3) ?
N4 C8 C7 . . 125.5(3) ?
N2 C9 C10 . . 127.2(3) ?
N3 C9 N2 . . 108.2(3) ?
N3 C9 C10 . . 124.5(3) ?
C9 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
C9 C10 H10C . . 109.5 ?
H10A C10 H10B . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
N5 C11 H11A . . 118.7 ?
N5 C11 C12 . . 122.7(4) ?
C12 C11 H11A . . 118.7 ?
C11 C12 H12 . . 120.3 ?
C13 C12 C11 . . 119.4(4) ?
C13 C12 H12 . . 120.3 ?
C12 C13 H13 . . 120.4 ?
C12 C13 C14 . . 119.2(4) ?
C14 C13 H13 . . 120.4 ?
C13 C14 H14 . . 120.9 ?
C15 C14 C13 . . 118.1(4) ?
C15 C14 H14 . . 120.9 ?
N5 C15 C14 . . 123.2(3) ?
N5 C15 C16 . . 114.0(3) ?
C14 C15 C16 . . 122.8(3) ?
N6 C16 C15 . . 121.1(3) ?
N8 C16 N6 . . 114.5(3) ?
N8 C16 C15 . . 124.4(3) ?
N6 C17 C18 . . 128.1(4) ?
N7 C17 N6 . . 108.8(3) ?
N7 C17 C18 . . 123.1(4) ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18B . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
N9 C19 H19 . . 118.3 ?
N9 C19 C20 . . 123.4(4) ?
C20 C19 H19 . . 118.3 ?
C19 C20 H20 . . 120.7 ?
C21 C20 C19 . . 118.6(4) ?
C21 C20 H20 . . 120.7 ?
C20 C21 H21 . . 120.0 ?
C20 C21 C22 . . 119.9(4) ?
C22 C21 H21 . . 120.0 ?
C21 C22 H22 . . 121.0 ?
C21 C22 C23 . . 118.0(4) ?
C23 C22 H22 . . 121.0 ?
N9 C23 C22 . . 122.9(4) ?
N9 C23 C24 . . 114.7(3) ?
C22 C23 C24 . . 122.4(4) ?
N10 C24 C23 . . 120.9(3) ?
N12 C24 N10 . . 114.2(3) ?
N12 C24 C23 . . 124.9(3) ?
N10 C25 C26 . . 128.6(3) ?
N11 C25 N10 . . 108.2(3) ?
N11 C25 C26 . . 123.2(3) ?
C25 C26 H26A . . 109.5 ?
C25 C26 H26B . . 109.5 ?
C25 C26 H26C . . 109.5 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
N13 C27 H27 . . 118.5 ?
N13 C27 C28 . . 123.0(4) ?
C28 C27 H27 . . 118.5 ?
C27 C28 H28 . . 120.3 ?
C29 C28 C27 . . 119.5(4) ?
C29 C28 H28 . . 120.3 ?
C28 C29 H29 . . 120.6 ?
C28 C29 C30 . . 118.9(4) ?
C30 C29 H29 . . 120.6 ?
C29 C30 H30 . . 120.8 ?
C31 C30 C29 . . 118.5(4) ?
C31 C30 H30 . . 120.8 ?
N13 C31 C30 . . 123.1(3) ?
N13 C31 C32 . . 113.9(3) ?
C30 C31 C32 . . 123.1(3) ?
N14 C32 C31 . . 119.8(3) ?
N16 C32 N14 . . 114.6(3) ?
N16 C32 C31 . . 125.6(3) ?
N14 C33 C34 . . 127.4(4) ?
N15 C33 N14 . . 108.0(3) ?
N15 C33 C34 . . 124.6(3) ?
C33 C34 H34A . . 109.5 ?
C33 C34 H34B . . 109.5 ?
C33 C34 H34C . . 109.5 ?
H34A C34 H34B . . 109.5 ?
H34A C34 H34C . . 109.5 ?
H34B C34 H34C . . 109.5 ?
O5 S1 O6 . . 110.60(19) ?
O5 S1 C35 . . 106.93(17) ?
O6 S1 C35 . . 106.78(19) ?
O7 S1 O5 . . 114.3(2) ?
O7 S1 O6 . . 110.8(3) ?
O7 S1 C35 . . 106.96(18) ?
C36 C35 S1 . . 121.8(3) ?
C40 C35 S1 . . 119.4(3) ?
C40 C35 C36 . . 118.8(3) ?
C35 C36 H36 . . 120.0 ?
C35 C36 C37 . . 120.1(3) ?
C37 C36 H36 . . 120.0 ?
C36 C37 H37 . . 119.3 ?
C38 C37 C36 . . 121.4(4) ?
C38 C37 H37 . . 119.3 ?
C37 C38 C39 . . 118.1(4) ?
C37 C38 C41 . . 121.5(4) ?
C39 C38 C41 . . 120.4(4) ?
C38 C39 H39 . . 119.4 ?
C38 C39 C40 . . 121.2(4) ?
C40 C39 H39 . . 119.4 ?
C35 C40 C39 . . 120.4(4) ?
C35 C40 H40 . . 119.8 ?
C39 C40 H40 . . 119.8 ?
C38 C41 H41A . . 109.5 ?
C38 C41 H41B . . 109.5 ?
C38 C41 H41C . . 109.5 ?
H41A C41 H41B . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
O8 S2 O9 . . 114.8(2) ?
O8 S2 O10 . . 111.9(2) ?
O8 S2 C42 . . 107.17(16) ?
O9 S2 O10 . . 110.33(16) ?
O9 S2 C42 . . 106.35(17) ?
O10 S2 C42 . . 105.76(17) ?
C43 C42 S2 . . 121.0(3) ?
C43 C42 C47 . . 119.2(3) ?
C47 C42 S2 . . 119.7(3) ?
C42 C43 H43 . . 120.1 ?
C42 C43 C44 . . 119.9(4) ?
C44 C43 H43 . . 120.1 ?
C43 C44 H44 . . 119.4 ?
C45 C44 C43 . . 121.2(4) ?
C45 C44 H44 . . 119.4 ?
C44 C45 C48 . . 120.5(4) ?
C46 C45 C44 . . 117.9(4) ?
C46 C45 C48 . . 121.6(4) ?
C45 C46 H46 . . 119.2 ?
C45 C46 C47 . . 121.6(4) ?
C47 C46 H46 . . 119.2 ?
C42 C47 H47 . . 119.9 ?
C46 C47 C42 . . 120.3(3) ?
C46 C47 H47 . . 119.9 ?
C45 C48 H48A . . 109.5 ?
C45 C48 H48B . . 109.5 ?
C45 C48 H48C . . 109.5 ?
H48A C48 H48B . . 109.5 ?
H48A C48 H48C . . 109.5 ?
H48B C48 H48C . . 109.5 ?
H1WA O1W H1WB . . 104.5 ?
H2WA O2W H2WB . . 116.3 ?
H4WA O4W H4WB . . 117.9 ?
H5WA O5W H5WB . . 112.9 ?
H3WA O3W H3WB . . 107.7 ?
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
Fe1 O1 . 2.171(2) yes
Fe1 O2 . 2.123(2) yes
Fe1 N1 . 2.203(3) yes
Fe1 N2 . 2.150(3) yes
Fe1 N5 . 2.197(3) yes
Fe1 N6 . 2.162(3) yes
Fe2 O3 . 2.123(2) yes
Fe2 O4 . 2.157(2) yes
Fe2 N9 . 2.209(3) yes
Fe2 N10 . 2.165(3) yes
Fe2 N13 . 2.206(3) yes
Fe2 N14 . 2.159(3) yes
O1 C1 . 1.241(4) ?
O2 C2 . 1.243(4) ?
O3 C1 . 1.245(4) ?
O4 C2 . 1.249(4) ?
N1 C3 . 1.349(4) ?
N1 C7 . 1.343(4) ?
N2 C8 . 1.363(4) ?
N2 C9 . 1.333(4) ?
N3 H3 . 0.8600 ?
N3 N4 . 1.350(4) ?
N3 C9 . 1.332(4) ?
N4 C8 . 1.320(4) ?
N5 C11 . 1.344(4) ?
N5 C15 . 1.344(4) ?
N6 C16 . 1.364(4) ?
N6 C17 . 1.323(4) ?
N7 H7 . 0.8600 ?
N7 N8 . 1.356(4) ?
N7 C17 . 1.318(5) ?
N8 C16 . 1.305(4) ?
N9 C19 . 1.338(4) ?
N9 C23 . 1.344(4) ?
N10 C24 . 1.365(4) ?
N10 C25 . 1.334(4) ?
N11 H11 . 0.8600 ?
N11 N12 . 1.355(4) ?
N11 C25 . 1.329(4) ?
N12 C24 . 1.309(4) ?
N13 C27 . 1.339(4) ?
N13 C31 . 1.345(4) ?
N14 C32 . 1.361(4) ?
N14 C33 . 1.334(4) ?
N15 H15 . 0.8600 ?
N15 N16 . 1.354(4) ?
N15 C33 . 1.331(4) ?
N16 C32 . 1.312(4) ?
C1 C2 . 1.546(4) ?
C3 H3A . 0.9300 ?
C3 C4 . 1.379(5) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.357(6) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.385(5) ?
C6 H6 . 0.9300 ?
C6 C7 . 1.377(5) ?
C7 C8 . 1.472(4) ?
C9 C10 . 1.484(5) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C10 H10C . 0.9600 ?
C11 H11A . 0.9300 ?
C11 C12 . 1.370(5) ?
C12 H12 . 0.9300 ?
C12 C13 . 1.366(6) ?
C13 H13 . 0.9300 ?
C13 C14 . 1.384(5) ?
C14 H14 . 0.9300 ?
C14 C15 . 1.378(5) ?
C15 C16 . 1.465(5) ?
C17 C18 . 1.483(5) ?
C18 H18A . 0.9600 ?
C18 H18B . 0.9600 ?
C18 H18C . 0.9600 ?
C19 H19 . 0.9300 ?
C19 C20 . 1.372(5) ?
C20 H20 . 0.9300 ?
C20 C21 . 1.359(6) ?
C21 H21 . 0.9300 ?
C21 C22 . 1.381(6) ?
C22 H22 . 0.9300 ?
C22 C23 . 1.381(5) ?
C23 C24 . 1.460(5) ?
C25 C26 . 1.478(5) ?
C26 H26A . 0.9600 ?
C26 H26B . 0.9600 ?
C26 H26C . 0.9600 ?
C27 H27 . 0.9300 ?
C27 C28 . 1.371(5) ?
C28 H28 . 0.9300 ?
C28 C29 . 1.364(6) ?
C29 H29 . 0.9300 ?
C29 C30 . 1.384(5) ?
C30 H30 . 0.9300 ?
C30 C31 . 1.377(5) ?
C31 C32 . 1.471(4) ?
C33 C34 . 1.481(5) ?
C34 H34A . 0.9600 ?
C34 H34B . 0.9600 ?
C34 H34C . 0.9600 ?
S1 O5 . 1.439(3) ?
S1 O6 . 1.454(3) ?
S1 O7 . 1.419(3) ?
S1 C35 . 1.758(4) ?
C35 C36 . 1.375(5) ?
C35 C40 . 1.371(5) ?
C36 H36 . 0.9300 ?
C36 C37 . 1.383(5) ?
C37 H37 . 0.9300 ?
C37 C38 . 1.368(5) ?
C38 C39 . 1.368(6) ?
C38 C41 . 1.520(5) ?
C39 H39 . 0.9300 ?
C39 C40 . 1.384(5) ?
C40 H40 . 0.9300 ?
C41 H41A . 0.9600 ?
C41 H41B . 0.9600 ?
C41 H41C . 0.9600 ?
S2 O8 . 1.435(3) ?
S2 O9 . 1.444(3) ?
S2 O10 . 1.450(3) ?
S2 C42 . 1.768(4) ?
C42 C43 . 1.373(5) ?
C42 C47 . 1.379(5) ?
C43 H43 . 0.9300 ?
C43 C44 . 1.388(5) ?
C44 H44 . 0.9300 ?
C44 C45 . 1.381(5) ?
C45 C46 . 1.372(5) ?
C45 C48 . 1.512(5) ?
C46 H46 . 0.9300 ?
C46 C47 . 1.375(5) ?
C47 H47 . 0.9300 ?
C48 H48A . 0.9600 ?
C48 H48B . 0.9600 ?
C48 H48C . 0.9600 ?
O1W H1WA . 0.8500 ?
O1W H1WB . 0.8499 ?
O2W H2WA . 0.8482 ?
O2W H2WB . 0.8577 ?
O4W H4WA . 0.8679 ?
O4W H4WB . 0.8665 ?
O5W H5WA . 0.8651 ?
O5W H5WB . 0.8618 ?
O3W H3WA . 0.8642 ?
O3W H3WB . 0.8617 ?
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
N3 H3 O10 2_566 0.86 1.95 2.766(4) 159 yes
N7 H7 O6 2_555 0.86 2.34 3.064(5) 142 yes
N7 H7 O7 2_555 0.86 2.34 3.141(6) 154 yes
N11 H11 O9 2_676 0.86 1.92 2.769(4) 170 yes
N15 H15 O5 2_665 0.86 1.99 2.825(4) 163 yes
C4 H4 O2W 2_565 0.93 2.48 3.383(5) 165 yes
C11 H11A O5W 1_555 0.93 2.49 3.206(8) 134 yes
C28 H28 O4W 2_666 0.93 2.54 3.421(6) 159 yes
O2W H2WA O4 1_555 0.85 2.10 2.949(4) 174 yes
O2W H2WB O5 1_555 0.86 1.99 2.838(4) 172 yes
O4W H4WA O1 1_555 0.87 2.34 3.123(5) 150 yes
O4W H4WA O3 1_555 0.87 2.25 3.037(4) 151 yes
O4W H4WB O10 1_555 0.87 1.92 2.788(5) 174 yes
O5W H5WA O4W 2_666 0.86 1.98 2.810(11) 159 yes
O5W H5WB O4W 1_555 0.86 2.28 2.850(10) 123 yes
C13 H13 O8 2_666 0.93 2.57 3.256(5) 131 yes
C21 H21 O7 2_565 0.93 2.44 3.280(6) 150 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Fe1 O1 C1 O3 . . . . -178.1(3) ?
Fe1 O1 C1 C2 . . . . 1.9(4) ?
Fe1 O2 C2 O4 . . . . 178.1(3) ?
Fe1 O2 C2 C1 . . . . -2.0(4) ?
Fe1 N1 C3 C4 . . . . 171.0(3) ?
Fe1 N1 C7 C6 . . . . -172.4(3) ?
Fe1 N1 C7 C8 . . . . 7.7(4) ?
Fe1 N2 C8 N4 . . . . 177.6(2) ?
Fe1 N2 C8 C7 . . . . -1.8(4) ?
Fe1 N2 C9 N3 . . . . -176.9(3) ?
Fe1 N2 C9 C10 . . . . 2.6(7) ?
Fe1 N5 C11 C12 . . . . 169.2(3) ?
Fe1 N5 C15 C14 . . . . -168.8(3) ?
Fe1 N5 C15 C16 . . . . 10.1(4) ?
Fe1 N6 C16 N8 . . . . -179.6(3) ?
Fe1 N6 C16 C15 . . . . -1.2(4) ?
Fe1 N6 C17 N7 . . . . 179.3(3) ?
Fe1 N6 C17 C18 . . . . -0.8(8) ?
Fe2 O3 C1 O1 . . . . -177.3(3) ?
Fe2 O3 C1 C2 . . . . 2.7(4) ?
Fe2 O4 C2 O2 . . . . 177.4(3) ?
Fe2 O4 C2 C1 . . . . -2.5(3) ?
Fe2 N9 C19 C20 . . . . -168.9(3) ?
Fe2 N9 C23 C22 . . . . 169.3(3) ?
Fe2 N9 C23 C24 . . . . -11.2(4) ?
Fe2 N10 C24 N12 . . . . -175.3(3) ?
Fe2 N10 C24 C23 . . . . 6.1(4) ?
Fe2 N10 C25 N11 . . . . 172.5(3) ?
Fe2 N10 C25 C26 . . . . -8.4(7) ?
Fe2 N13 C27 C28 . . . . -170.8(3) ?
Fe2 N13 C31 C30 . . . . 172.0(3) ?
Fe2 N13 C31 C32 . . . . -7.7(4) ?
Fe2 N14 C32 N16 . . . . -176.2(2) ?
Fe2 N14 C32 C31 . . . . 5.1(4) ?
Fe2 N14 C33 N15 . . . . 174.8(3) ?
Fe2 N14 C33 C34 . . . . -6.4(7) ?
O1 C1 C2 O2 . . . . 0.0(4) ?
O1 C1 C2 O4 . . . . 179.9(3) ?
O3 C1 C2 O2 . . . . 180.0(3) ?
O3 C1 C2 O4 . . . . -0.1(4) ?
N1 C3 C4 C5 . . . . 0.7(6) ?
N1 C7 C8 N2 . . . . -4.0(5) ?
N1 C7 C8 N4 . . . . 176.7(3) ?
N3 N4 C8 N2 . . . . 0.6(4) ?
N3 N4 C8 C7 . . . . 179.9(3) ?
N4 N3 C9 N2 . . . . -0.1(4) ?
N4 N3 C9 C10 . . . . -179.7(4) ?
N5 C11 C12 C13 . . . . -0.9(6) ?
N5 C15 C16 N6 . . . . -6.1(5) ?
N5 C15 C16 N8 . . . . 172.2(4) ?
N7 N8 C16 N6 . . . . 0.1(5) ?
N7 N8 C16 C15 . . . . -178.2(4) ?
N8 N7 C17 N6 . . . . 0.0(6) ?
N8 N7 C17 C18 . . . . -179.9(4) ?
N9 C19 C20 C21 . . . . 1.0(7) ?
N9 C23 C24 N10 . . . . 3.5(5) ?
N9 C23 C24 N12 . . . . -174.8(4) ?
N11 N12 C24 N10 . . . . 0.1(4) ?
N11 N12 C24 C23 . . . . 178.6(3) ?
N12 N11 C25 N10 . . . . 0.1(4) ?
N12 N11 C25 C26 . . . . -179.1(3) ?
N13 C27 C28 C29 . . . . -1.1(6) ?
N13 C31 C32 N14 . . . . 1.8(5) ?
N13 C31 C32 N16 . . . . -176.8(3) ?
N15 N16 C32 N14 . . . . -0.5(4) ?
N15 N16 C32 C31 . . . . 178.1(3) ?
N16 N15 C33 N14 . . . . -0.5(4) ?
N16 N15 C33 C34 . . . . -179.3(4) ?
C3 N1 C7 C6 . . . . 0.3(5) ?
C3 N1 C7 C8 . . . . -179.6(3) ?
C3 C4 C5 C6 . . . . 0.0(6) ?
C4 C5 C6 C7 . . . . -0.6(6) ?
C5 C6 C7 N1 . . . . 0.4(6) ?
C5 C6 C7 C8 . . . . -179.7(3) ?
C6 C7 C8 N2 . . . . 176.1(3) ?
C6 C7 C8 N4 . . . . -3.2(6) ?
C7 N1 C3 C4 . . . . -0.9(5) ?
C8 N2 C9 N3 . . . . 0.4(4) ?
C8 N2 C9 C10 . . . . -180.0(4) ?
C9 N2 C8 N4 . . . . -0.7(4) ?
C9 N2 C8 C7 . . . . 179.9(3) ?
C9 N3 N4 C8 . . . . -0.3(4) ?
C11 N5 C15 C14 . . . . 3.3(5) ?
C11 N5 C15 C16 . . . . -177.8(3) ?
C11 C12 C13 C14 . . . . 2.2(6) ?
C12 C13 C14 C15 . . . . -0.9(6) ?
C13 C14 C15 N5 . . . . -2.0(6) ?
C13 C14 C15 C16 . . . . 179.2(4) ?
C14 C15 C16 N6 . . . . 172.9(3) ?
C14 C15 C16 N8 . . . . -8.9(6) ?
C15 N5 C11 C12 . . . . -1.9(5) ?
C16 N6 C17 N7 . . . . 0.1(5) ?
C16 N6 C17 C18 . . . . -180.0(4) ?
C17 N6 C16 N8 . . . . -0.1(5) ?
C17 N6 C16 C15 . . . . 178.3(4) ?
C17 N7 N8 C16 . . . . -0.1(5) ?
C19 N9 C23 C22 . . . . -1.8(5) ?
C19 N9 C23 C24 . . . . 177.7(3) ?
C19 C20 C21 C22 . . . . -1.6(7) ?
C20 C21 C22 C23 . . . . 0.6(7) ?
C21 C22 C23 N9 . . . . 1.1(6) ?
C21 C22 C23 C24 . . . . -178.3(4) ?
C22 C23 C24 N10 . . . . -177.0(3) ?
C22 C23 C24 N12 . . . . 4.6(6) ?
C23 N9 C19 C20 . . . . 0.7(6) ?
C24 N10 C25 N11 . . . . 0.0(4) ?
C24 N10 C25 C26 . . . . 179.1(4) ?
C25 N10 C24 N12 . . . . -0.1(4) ?
C25 N10 C24 C23 . . . . -178.6(3) ?
C25 N11 N12 C24 . . . . -0.1(4) ?
C27 N13 C31 C30 . . . . -1.4(5) ?
C27 N13 C31 C32 . . . . 179.0(3) ?
C27 C28 C29 C30 . . . . 0.2(7) ?
C28 C29 C30 C31 . . . . 0.1(6) ?
C29 C30 C31 N13 . . . . 0.5(6) ?
C29 C30 C31 C32 . . . . -179.9(3) ?
C30 C31 C32 N14 . . . . -177.9(3) ?
C30 C31 C32 N16 . . . . 3.5(6) ?
C31 N13 C27 C28 . . . . 1.7(5) ?
C32 N14 C33 N15 . . . . 0.1(4) ?
C32 N14 C33 C34 . . . . 178.9(4) ?
C33 N14 C32 N16 . . . . 0.3(4) ?
C33 N14 C32 C31 . . . . -178.4(3) ?
C33 N15 N16 C32 . . . . 0.6(4) ?
S1 C35 C36 C37 . . . . 178.8(3) ?
S1 C35 C40 C39 . . . . -179.3(4) ?
O5 S1 C35 C36 . . . . 36.1(4) ?
O5 S1 C35 C40 . . . . -146.0(3) ?
O6 S1 C35 C36 . . . . 154.5(3) ?
O6 S1 C35 C40 . . . . -27.6(4) ?
O7 S1 C35 C36 . . . . -86.8(4) ?
O7 S1 C35 C40 . . . . 91.1(4) ?
C35 C36 C37 C38 . . . . 0.4(6) ?
C36 C35 C40 C39 . . . . -1.3(7) ?
C36 C37 C38 C39 . . . . -1.3(6) ?
C36 C37 C38 C41 . . . . 177.9(4) ?
C37 C38 C39 C40 . . . . 0.8(7) ?
C38 C39 C40 C35 . . . . 0.5(8) ?
C40 C35 C36 C37 . . . . 0.9(6) ?
C41 C38 C39 C40 . . . . -178.4(4) ?
S2 C42 C43 C44 . . . . 179.2(3) ?
S2 C42 C47 C46 . . . . -179.0(3) ?
O8 S2 C42 C43 . . . . -114.5(4) ?
O8 S2 C42 C47 . . . . 63.3(4) ?
O9 S2 C42 C43 . . . . 8.7(4) ?
O9 S2 C42 C47 . . . . -173.5(3) ?
O10 S2 C42 C43 . . . . 126.1(3) ?
O10 S2 C42 C47 . . . . -56.2(3) ?
C42 C43 C44 C45 . . . . -0.3(7) ?
C43 C42 C47 C46 . . . . -1.2(6) ?
C43 C44 C45 C46 . . . . -1.0(7) ?
C43 C44 C45 C48 . . . . 179.2(4) ?
C44 C45 C46 C47 . . . . 1.2(6) ?
C45 C46 C47 C42 . . . . -0.1(6) ?
C47 C42 C43 C44 . . . . 1.4(6) ?
C48 C45 C46 C47 . . . . -179.0(4) ?
_cod_database_fobs_code 2244135