#------------------------------------------------------------------------------
#$Date: 2025-01-04 03:37:25 +0100 (Sat, 04 Jan 2025) $
#$Revision: 297060 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023343.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_2023343
loop_
_publ_author_name
'Tsymbal, Liudmyla V.'
'Andriichuk, Irina L.'
'Bahrin, Lucian G.'
'Lampeka, Yaroslaw D.'
_publ_section_title
;
Syntheses and structures of two coordination polymers formed by
Ni(cyclam)2+ cations and sulfate anions
;
_journal_coeditor_code HB8118
_journal_issue 2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024012337
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '[Ni (S O4) (C10 H24 N4)]2, C46 H38 O8, 18H2 O'
_chemical_formula_moiety 'C20 H48 N8 Ni2 O8 S2, C46 H38 O8'
_chemical_formula_sum 'C66 H86 N8 Ni2 O16 S2'
_chemical_formula_weight 1428.96
_chemical_name_systematic
;catena-Poly[[[(1,4,8,11-tetraazacyclotetradecane-\k^4^N^1^,N^4^,N^8^,N^11^)nickel(II)]-\m~2~-sulfato-\k^2^O^3^:O^4^]
hemi[4,4',4'',4'''-(2,2',4,4',6,6'-hexamethyl-[1,1'-biphenyl]-3,3',5,5'-tetrayl)tetrabenzoic acid] nonahydrate]
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 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 90
_cell_angle_beta 94.777(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.1299(5)
_cell_length_b 18.5163(11)
_cell_length_c 35.621(2)
_cell_measurement_reflns_used 2340
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.1120
_cell_measurement_theta_min 2.0080
_cell_volume 7972.7(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type '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 0.0859
_diffrn_reflns_av_unetI/netI 0.1724
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 44
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 20054
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.372
_diffrn_reflns_theta_min 2.043
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.587
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.92008
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_density_diffrn 1.190
_exptl_crystal_description plate
_exptl_crystal_F_000 3016
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.247
_refine_diff_density_min -0.353
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.985
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 432
_refine_ls_number_reflns 8085
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.985
_refine_ls_R_factor_all 0.1881
_refine_ls_R_factor_gt 0.0769
_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^)+(0.0206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0960
_refine_ls_wR_factor_ref 0.1228
_reflns_number_gt 3223
_reflns_number_total 8085
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8118.cif
_cod_data_source_block II
_cod_original_cell_volume 7972.7(8)
_cod_database_code 2023343
_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 0.944
_shelx_estimated_absorpt_t_max 0.994
_shelx_hkl_file
;
0 0 4 27952.4 260.431 3
0 0 -4 28096.1 260.613 3
0 0 6 8186.08 172.289 3
0 0 -6 8424.13 173.897 3
0 0 -8 1126.26 80.2336 1
0 0 8 889.926 66.4179 3
0 0 -8 856.507 65.4417 3
0 0 -10 8867.18 245.701 1
0 0 10 8595.10 226.196 3
0 0 -10 8359.65 226.809 3
0 0 -12 11282.2 302.027 1
0 0 -12 11267.2 287.455 3
0 0 12 10902.3 284.442 3
0 0 -14 6763.02 253.363 1
0 0 14 6594.82 239.828 3
0 0 -14 7103.08 245.143 3
0 0 -16 8602.57 301.951 1
0 0 16 7920.78 281.651 3
0 0 -16 8312.75 287.073 3
0 0 18 3352.68 193.421 3
0 0 20 5371.65 261.339 3
0 0 22 4711.84 254.984 3
0 0 24 3159.16 224.443 3
0 0 26 2643.01 213.361 3
0 0 28 1516.48 174.328 3
0 0 30 973.238 147.715 3
0 0 32 553.865 111.822 3
0 0 34-1.16585 27.0130 3
0 0 36 274.750 93.9033 3
0 0 38 363.434 108.014 3
0 0 40 141.888 69.8396 3
0 0 42 136.623 68.7885 3
0 0 44 140.477 86.2821 3
0 -1 -3 320.506 26.6205 3
0 1 -3 372.048 27.4808 3
0 1 3 378.757 29.6297 3
0 1 -5 559.850 41.7102 3
0 -1 5 511.131 40.4340 3
0 -1 -5 509.987 41.7026 3
0 1 5 549.612 43.7864 3
0 1 -7 228.837 38.6605 1
0 -1 -7 190.602 32.9615 1
0 -1 7 148.594 30.5375 3
0 1 -7 166.512 26.8744 3
0 -1 -7 223.614 33.7586 3
0 1 7 157.731 28.3506 3
0 -1 -9-3.01084 19.2881 1
0 1 -9-7.86563 17.3485 1
0 1 -9-15.9157 17.7661 3
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0 -1 -9-18.7629 19.8662 3
0 1 9 23.8942 24.8473 3
0 1 -11 334.815 52.8644 1
0 -1 -11 315.504 50.6157 1
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0 -1 -11 307.801 46.2530 3
0 -1 -13-19.0925 19.4900 1
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0 1 -13 19.3675 26.9994 3
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0 1 13 15.4966 15.3373 3
0 -1 -13 9.92814 19.3906 3
0 1 -15 103.298 33.5612 1
0 -1 -15 117.922 40.2280 1
0 1 15 93.4742 33.8918 3
0 1 -15 49.3632 25.7757 3
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0 -1 -15 67.8573 26.4611 3
0 1 -17 113.260 39.3665 1
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0 1 -17 162.662 46.6433 3
0 -1 -17 122.803 41.8902 3
0 -1 19 99.2644 41.8616 3
0 1 19 175.955 51.0716 3
0 1 21 13.3900 23.9476 3
0 -1 21 51.2645 40.7849 3
0 1 23 81.1281 49.3762 3
0 -1 23 66.3546 41.7696 3
0 -1 25 27.0954 24.3792 3
0 1 25 85.0128 40.1781 3
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0 -1 29-37.5876 47.1078 3
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0 -1 31 63.1588 47.1172 3
0 1 31 13.6096 43.2969 3
0 -1 33-38.8040 57.8480 3
0 1 33-28.1848 26.5337 3
0 -1 35-14.4354 33.2601 3
0 1 35 52.8506 61.0695 3
0 -1 37 65.4504 60.5509 3
0 1 37-43.5021 34.0366 3
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0 1 41-39.3223 52.8177 3
0 -1 41 23.0380 42.4800 3
0 1 43 47.4499 59.0899 3
0 -1 43-5.81811 39.9104 3
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0 -2 -6 4350.92 138.228 3
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0 -2 8 51.2898 18.6669 3
0 2 -8 67.2816 23.7853 3
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0 -2 -8 38.6215 19.1049 3
0 -2 -10 5662.77 193.705 1
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0 -2 -12 5103.48 198.772 3
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0 2 -14 7326.43 253.783 3
0 -2 -14 7631.05 260.348 3
0 -2 -16 4912.74 230.497 1
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0 -2 -16 4462.28 215.230 3
0 2 -16 4806.10 220.302 3
0 -2 16 4569.09 213.876 3
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0 2 18 3873.37 212.711 3
0 -2 18 3909.27 206.784 3
0 2 20 2132.59 169.047 3
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0 2 26 1779.24 178.612 3
0 -2 26 1861.43 178.810 3
0 -2 28 1214.42 155.392 3
0 2 28 1345.51 162.521 3
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0 -2 32 20.3281 35.5500 3
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0 -2 36 319.037 103.100 3
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0 -2 40 228.622 79.4113 3
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0 3 -1 3509.92 107.874 5
0 -3 1 3405.78 108.538 5
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0 3 -5 37.9598 13.8458 1
0 -3 -5 27.6575 16.2699 1
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0 3 5 17.0393 15.3874 3
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0 -3 -9 74.2985 26.5663 3
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15 -5 4 8.73139 37.1130 4
15 -5 6 48.8224 56.3195 4
15 -5 8 77.9962 69.5054 4
15 -5 10 32.8577 59.5842 4
15 -5 12-91.6668 71.6356 4
15 -6 -9-3.94793 41.6040 4
15 -6 -7-13.8823 54.3027 4
-15 -6 5 67.8650 75.3654 2
15 -6 -5 12.3273 33.7695 4
15 -6 -3 16.6290 31.3076 4
15 -6 -1 41.3809 61.0983 4
15 -6 1 11.6438 40.1002 4
15 -6 3-27.8713 39.1653 4
15 -6 5-32.7068 46.7591 4
15 -6 7-17.6756 35.4828 4
15 -6 9-28.1122 57.3138 4
15 -6 11-29.5577 41.0269 4
15 -7 4-21.3849 30.4602 4
15 -7 6 11.4682 38.4096 4
15 -7 8-24.1199 65.4202 4
15 -7 10 46.9815 37.7159 4
15 -7 12 96.2213 83.3551 4
16 -2 -8 214.992 95.8345 4
16 -2 -6 236.569 96.2438 4
16 -2 -4 235.643 103.719 4
16 -3 -11 71.7787 60.9927 4
16 -3 -9 504.687 135.167 4
16 -3 -7 22.1787 56.7815 4
16 -3 -5-6.14160 42.9032 4
16 -3 -3 11.1170 70.0458 4
16 -3 -1-16.6586 53.9282 4
16 -4 -14 34.9863 47.5577 4
16 -4 -12 50.7685 57.3633 4
16 -4 -10 218.280 88.6114 4
16 -4 -8 59.6817 45.8448 4
16 -4 -6 42.0145 47.4417 4
16 -4 -4 240.747 94.8153 4
16 -4 -2 87.9918 62.2405 4
16 -4 0 35.7831 47.5941 4
16 -4 2 105.658 69.6768 4
16 -5 -9 65.4283 59.4100 4
16 -5 -7-21.2966 32.3041 4
16 -5 -5 66.4915 47.6401 4
16 -5 -3 112.142 75.1190 4
16 -5 -1 108.047 67.6385 4
16 -5 1-15.2584 38.3413 4
16 -5 3-39.3160 37.2078 4
0 0 0 0.00 0.00 0
TITL II in I2/a
REM I2/a (#15 in standard setting)
CELL 0.71073 12.129919 18.516345 35.620731 90.0000 94.7773 90.0000
ZERR 8.00 0.000492 0.001110 0.002209 0.0000 0.0040 0.0000
LATT 2
SYMM -x+1/2, y,-z
SFAC C H N O Ni
UNIT 320.00 320.00 16.00 128.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 25186
_shelx_res_file
;
TITL II_a.res in I2/a
II.res
created by SHELXL-2018/3 at 10:53:05 on 22-Jul-2023
REM Old TITL II in I2/a #15
REM SHELXT solution in I2/a: R1 0.367, Rweak 0.106, Alpha 0.156
REM 0.494 for 112 systematic absences, Orientation as input
REM Formula found by SHELXT: C51 N21 O20 Ni4
CELL 0.71073 12.129919 18.516345 35.620731 90 94.7773 90
ZERR 4 0.000492 0.00111 0.002209 0 0.004 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H N Ni O S
UNIT 264 344 32 8 64 8
EQIV $1 1.5-X,1.5-Y,1.5-Z
EQIV $2 0.5-X,1.5-Y,1.5-Z
EQIV $3 +X,0.5-Y,-0.5+Z
L.S. 11
PLAN 17
SIZE 0.01 0.04 0.1
CONF
HTAB N3 S1_$1
HTAB N3 O1_$1
HTAB N1 S1
HTAB N1 O4
HTAB N1 O6
HTAB N2 S1_$2
HTAB N2 O4_$2
HTAB N4 S1_$1
HTAB N4 O3_$1
HTAB O5 S1
HTAB O5 O4
HTAB O7 S1_$3
HTAB O7 O3_$3
HTAB C6 O2
HTAB C3 O1
HTAB C8 O2
htab
BOND
list 4
ABIN
MORE -1
BOND $H
fmap 2
acta
SHEL 999 0.8
OMIT -1 1 2
OMIT 1 1 0
OMIT -1 1 4
OMIT 1 1 4
OMIT -1 2 1
OMIT 2 0 4
OMIT -8 16 4
OMIT -1 2 3
REM
REM
REM
WGHT 0.020600
FVAR 0.30111
NI1 4 0.250000 0.750000 0.750000 10.50000 0.02824 0.10316 =
0.03810 0.02128 0.00810 0.01536
NI2 4 0.750000 0.750000 0.750000 10.50000 0.02685 0.11555 =
0.04741 0.03030 0.01135 0.01600
S1 6 0.500535 0.678555 0.756490 11.00000 0.02722 0.11309 =
0.05622 0.03015 0.01550 0.01676
O3 5 0.519351 0.676649 0.797681 11.00000 0.04740 0.14019 =
0.04927 0.04446 0.01384 0.02858
O2 5 0.606952 0.686176 0.739567 11.00000 0.02166 0.11673 =
0.05455 0.01755 0.01501 0.01416
N3 3 0.845974 0.657762 0.747457 11.00000 0.03023 0.12172 =
0.06611 0.02305 0.01035 0.01357
AFIX 13
H3 2 0.923074 0.673461 0.747240 11.00000 -1.20000
AFIX 0
O1 5 0.428551 0.740676 0.745708 11.00000 0.03130 0.10404 =
0.05526 0.02589 0.00819 0.02236
O4 5 0.446740 0.609947 0.742835 11.00000 0.04026 0.10469 =
0.11048 0.00893 0.02793 0.00547
N1 3 0.224404 0.674322 0.707761 11.00000 0.03174 0.11711 =
0.04624 -0.00061 0.01037 0.02231
AFIX 13
H1 2 0.296188 0.651709 0.704761 11.00000 -1.20000
AFIX 0
N2 3 0.249284 0.675779 0.793234 11.00000 0.02987 0.13244 =
0.05687 0.04194 0.01523 0.02495
AFIX 13
H2 2 0.322725 0.653431 0.796249 11.00000 -1.20000
AFIX 0
N4 3 0.745456 0.769816 0.692939 11.00000 0.03688 0.13944 =
0.05083 0.02872 0.01365 0.00968
AFIX 13
H4 2 0.815571 0.792987 0.688167 11.00000 -1.20000
AFIX 0
C30 1 0.631121 0.102814 0.439718 11.00000 0.06787 0.03310 =
0.06615 0.00390 0.02041 0.00399
O6 5 0.395791 0.609200 0.647539 11.00000 0.06466 0.14272 =
0.10779 -0.00813 0.01097 0.05338
C11 1 0.478489 0.574016 0.650954 11.00000 0.04738 0.08392 =
0.09188 -0.00890 0.01507 0.01180
O8 5 0.387863 -0.047751 0.347676 11.00000 0.05114 0.13332 =
0.11645 -0.04351 0.02497 -0.01981
C18 1 0.692238 0.451999 0.525859 11.00000 0.04083 0.04430 =
0.08510 -0.00692 0.01031 0.00929
C15 1 0.638732 0.489065 0.557001 11.00000 0.04453 0.04798 =
0.08177 0.00373 0.01092 -0.00226
O5 5 0.527348 0.555958 0.683646 11.00000 0.07454 0.16713 =
0.08439 -0.00472 0.01031 0.05693
AFIX 147
H5 2 0.494848 0.574604 0.700454 11.00000 -1.50000
AFIX 0
C35 1 0.691993 0.074914 0.412162 11.00000 0.05554 0.05886 =
0.07942 0.00032 0.01478 -0.01016
AFIX 43
H35 2 0.767412 0.084687 0.413391 11.00000 -1.20000
AFIX 0
O7 5 0.550085 -0.043783 0.324478 11.00000 0.10330 0.16340 =
0.17183 -0.11517 0.09638 -0.07619
AFIX 147
H7 2 0.544646 -0.087006 0.319664 11.00000 -1.50000
AFIX 0
C24 1 0.750000 0.256505 0.500000 10.50000 0.06940 0.03196 =
0.08626 0.00000 0.02624 0.00000
C10 1 0.835763 0.620063 0.783688 11.00000 0.04706 0.14410 =
0.10513 0.04791 0.00836 0.02140
AFIX 23
H10A 2 0.894279 0.584556 0.787911 11.00000 -1.20000
H10B 2 0.765234 0.595217 0.783070 11.00000 -1.20000
AFIX 0
C12 1 0.536871 0.545782 0.618751 11.00000 0.04159 0.06793 =
0.08087 0.00389 0.00943 0.01184
C33 1 0.533852 0.020178 0.379787 11.00000 0.04856 0.05203 =
0.06674 -0.00258 0.02129 -0.00126
C32 1 0.470646 0.048535 0.406933 11.00000 0.04266 0.07227 =
0.08725 -0.01925 0.01804 -0.00384
AFIX 43
H32 2 0.394832 0.040027 0.405222 11.00000 -1.20000
AFIX 0
C29 1 0.750000 0.023963 0.500000 10.50000 0.11556 0.04422 =
0.08067 0.00000 -0.01009 0.00000
PART -1
AFIX 3
H29A 2 0.682200 0.006673 0.508860 10.50000 -1.50000
H29B 2 0.811420 0.006673 0.516270 10.50000 -1.50000
H29C 2 0.756370 0.006673 0.474860 10.50000 -1.50000
AFIX 0
PART 0
C25 1 0.686707 0.219803 0.471846 11.00000 0.07170 0.03715 =
0.08152 0.00984 0.01173 0.00213
C31 1 0.517770 0.088721 0.436125 11.00000 0.06236 0.07283 =
0.08635 -0.01479 0.03229 0.00343
AFIX 43
H31 2 0.473456 0.107060 0.453963 11.00000 -1.20000
AFIX 0
C21 1 0.688739 0.375405 0.524882 11.00000 0.05512 0.04164 =
0.08560 0.00423 0.02409 -0.00609
C2 1 0.179240 0.576137 0.752070 11.00000 0.04243 0.10533 =
0.16102 0.02508 0.01891 0.00517
AFIX 23
H2A 2 0.134603 0.532745 0.752629 11.00000 -1.20000
H2B 2 0.255789 0.561034 0.751981 11.00000 -1.20000
AFIX 0
C14 1 0.540807 0.526773 0.551783 11.00000 0.05213 0.09653 =
0.07916 -0.02027 0.00294 0.01987
AFIX 43
H14 2 0.507398 0.533655 0.527591 11.00000 -1.20000
AFIX 0
C19 1 0.750000 0.489675 0.500000 10.50000 0.04125 0.04133 =
0.09525 0.00000 0.01328 0.00000
C7 1 0.826889 0.652588 0.677806 11.00000 0.07127 0.15579 =
0.07668 -0.00446 0.02693 -0.00696
AFIX 23
H7A 2 0.827753 0.618110 0.657331 11.00000 -1.20000
H7B 2 0.896294 0.678843 0.679027 11.00000 -1.20000
AFIX 0
C1 1 0.147033 0.615637 0.715043 11.00000 0.04252 0.12138 =
0.11068 -0.02238 0.01144 -0.00292
AFIX 23
H1A 2 0.145034 0.581271 0.694445 11.00000 -1.20000
H1B 2 0.073304 0.635565 0.715824 11.00000 -1.20000
AFIX 0
C34 1 0.646333 0.033243 0.382897 11.00000 0.05356 0.05704 =
0.08196 0.00652 0.03005 -0.00565
AFIX 43
H34 2 0.690847 0.014029 0.365352 11.00000 -1.20000
AFIX 0
C26 1 0.614374 0.260220 0.441649 11.00000 0.10494 0.05305 =
0.12069 0.00460 0.00026 0.00920
AFIX 3
H26A 2 0.628524 0.311130 0.443719 11.00000 -1.50000
H26B 2 0.537924 0.251010 0.444999 11.00000 -1.50000
H26C 2 0.630924 0.243690 0.417199 11.00000 -1.50000
AFIX 0
C28 1 0.750000 0.106288 0.500000 10.50000 0.08287 0.01010 =
0.06828 0.00000 0.01334 0.00000
C36 1 0.481602 -0.026786 0.349313 11.00000 0.06604 0.07738 =
0.07360 -0.02169 0.02911 -0.01375
C6 1 0.821391 0.611295 0.714154 11.00000 0.04009 0.13448 =
0.10672 0.01140 0.01753 0.01053
AFIX 23
H6A 2 0.748034 0.590791 0.714947 11.00000 -1.20000
H6B 2 0.874045 0.571789 0.714897 11.00000 -1.20000
AFIX 0
C27 1 0.688898 0.144038 0.471614 11.00000 0.05523 0.04530 =
0.07420 -0.00069 0.00846 -0.00041
C23 1 0.750000 0.338063 0.500000 10.50000 0.04959 0.02832 =
0.09947 0.00000 0.01367 0.00000
C4 1 0.235202 0.719107 0.827760 11.00000 0.05945 0.16754 =
0.05385 0.04073 0.02654 0.04562
AFIX 23
H4A 2 0.257107 0.690753 0.850039 11.00000 -1.20000
H4B 2 0.158213 0.732707 0.828578 11.00000 -1.20000
AFIX 0
C13 1 0.492195 0.554341 0.582344 11.00000 0.04901 0.08075 =
0.10022 0.00440 0.00755 0.02722
AFIX 43
H13 2 0.426278 0.579840 0.578109 11.00000 -1.20000
AFIX 0
C17 1 0.636852 0.510523 0.623739 11.00000 0.05842 0.12090 =
0.08178 -0.00537 0.00440 0.04049
AFIX 43
H17 2 0.671219 0.504953 0.647893 11.00000 -1.20000
AFIX 0
C16 1 0.686691 0.483337 0.593305 11.00000 0.05471 0.13942 =
0.10301 -0.01510 0.01566 0.04618
AFIX 43
H16 2 0.754840 0.460414 0.597436 11.00000 -1.20000
AFIX 0
C5 1 0.193973 0.714430 0.673079 11.00000 0.06415 0.15942 =
0.04326 0.00163 0.00813 0.03874
AFIX 23
H5A 2 0.116564 0.728053 0.672049 11.00000 -1.20000
H5B 2 0.204755 0.684329 0.651400 11.00000 -1.20000
AFIX 0
C3 1 0.167195 0.617315 0.787633 11.00000 0.05036 0.12944 =
0.12281 0.05732 0.03190 0.01536
AFIX 23
H3A 2 0.093417 0.637773 0.786818 11.00000 -1.20000
H3B 2 0.175758 0.584418 0.808869 11.00000 -1.20000
AFIX 0
C9 1 0.655975 0.824470 0.684794 11.00000 0.05344 0.17766 =
0.06739 0.06414 0.00212 0.01805
AFIX 23
H9A 2 0.584152 0.801136 0.683389 11.00000 -1.20000
H9B 2 0.664611 0.847849 0.660847 11.00000 -1.20000
AFIX 0
C22 1 0.614999 0.334640 0.550381 11.00000 0.10296 0.06351 =
0.12888 0.01684 0.05126 -0.00756
AFIX 3
H22A 2 0.652519 0.330370 0.575101 11.00000 -1.50000
H22B 2 0.598969 0.287350 0.540311 11.00000 -1.50000
H22C 2 0.547179 0.360810 0.551891 11.00000 -1.50000
AFIX 0
C8 1 0.733007 0.705872 0.668388 11.00000 0.05660 0.18055 =
0.06153 0.02132 0.01275 -0.00040
AFIX 23
H8A 2 0.733069 0.720682 0.642270 11.00000 -1.20000
H8B 2 0.662777 0.682610 0.671625 11.00000 -1.20000
AFIX 0
C20 1 0.750000 0.571027 0.500000 10.50000 0.11098 0.01901 =
0.13515 0.00000 0.05548 0.00000
PART -1
AFIX 3
H20A 2 0.675440 0.588307 0.500220 10.50000 -1.50000
H20B 2 0.781320 0.588307 0.477810 10.50000 -1.50000
H20C 2 0.793240 0.588307 0.521970 10.50000 -1.50000
AFIX 0
HKLF 4
REM II_a.res in I2/a
REM wR2 = 0.1228, GooF = S = 0.985, Restrained GooF = 0.985 for all data
REM R1 = 0.0769 for 3223 Fo > 4sig(Fo) and 0.1881 for all 8085 data
REM 432 parameters refined using 0 restraints
END
WGHT 0.0418 0.0000
REM Instructions for potential hydrogen bonds
HTAB N3 S1_$1
HTAB N3 O1_$1
HTAB N1 S1
HTAB N1 O4
HTAB N1 O6
HTAB N2 S1
HTAB N2 O3
HTAB N2 O4
HTAB N4 S1_$1
HTAB N4 O3_$1
HTAB O5 S1
HTAB O5 O4
HTAB O7 S1_$3
HTAB O7 O3_$3
HTAB C2 O4
HTAB C6 O2
HTAB C3 O1_$2
HTAB C8 O2
REM Highest difference peak 0.247, deepest hole -0.353, 1-sigma level 0.056
Q1 1 0.4121 0.1677 0.5717 11.00000 0.05 0.25
Q2 1 0.4731 -0.0509 0.2926 11.00000 0.05 0.24
Q3 1 0.8136 0.7466 0.7318 11.00000 0.05 0.23
Q4 1 0.8810 0.6608 0.6502 11.00000 0.05 0.23
Q5 1 0.5738 -0.0503 0.3314 11.00000 0.05 0.23
Q6 1 0.5191 0.7197 0.6730 11.00000 0.05 0.22
Q7 1 0.7932 0.5153 0.8003 11.00000 0.05 0.21
Q8 1 0.6050 0.5822 0.6061 11.00000 0.05 0.21
Q9 1 0.1038 0.7099 0.6804 11.00000 0.05 0.21
Q10 1 0.9218 0.5897 0.6711 11.00000 0.05 0.20
Q11 1 0.5804 0.2497 0.4849 11.00000 0.05 0.20
Q12 1 0.6238 0.2692 0.5760 11.00000 0.05 0.20
Q13 1 0.2492 0.5729 0.7344 11.00000 0.05 0.20
Q14 1 0.5783 0.7150 0.7586 11.00000 0.05 0.20
Q15 1 0.1425 0.5305 0.8039 11.00000 0.05 0.20
Q16 1 0.7198 0.6173 0.7057 11.00000 0.05 0.19
Q17 1 0.6658 0.5825 0.7818 11.00000 0.05 0.19
;
_shelx_res_checksum 66252
_shelx_fab_file
;
0 0 -44 -0.7849 0.0708
0 0 -42 -10.6769 -0.0249
0 0 -40 -14.8597 -0.0460
0 0 -38 -16.0918 -0.0101
0 0 -36 -8.8531 0.0035
0 0 -34 -1.8277 -0.0154
0 0 -32 -5.7477 -0.0381
0 0 -30 -4.1321 0.0043
0 0 -28 9.5548 0.0389
0 0 -26 10.0158 -0.0174
0 0 -24 -4.3980 -0.0203
0 0 -22 -6.3697 0.0309
0 0 -20 3.5531 -0.0098
0 0 -18 7.4664 -0.0108
0 0 -16 5.8617 0.0281
0 0 -14 2.6264 -0.0670
0 0 -12 1.9982 0.0004
0 0 -10 -2.2999 0.1926
0 0 -8 -49.8959 -0.1563
0 0 -6 -112.2480 -0.4292
0 0 -4 -32.3738 0.4677
0 1 -43 15.8745 0.0286
0 1 -41 9.5625 -0.0456
0 1 -39 -2.0874 0.0112
0 1 -37 -0.2584 0.0327
0 1 -35 9.3676 -0.0327
0 1 -33 9.4196 -0.0057
0 1 -31 1.1787 0.0604
0 1 -29 -3.3000 0.0040
0 1 -27 -2.6830 -0.0503
0 1 -25 -2.2802 0.0020
0 1 -23 -2.1039 0.0245
0 1 -21 -0.4219 -0.0132
0 1 -19 0.1923 -0.0161
0 1 -17 -1.8199 -0.0041
0 1 -15 -2.8106 -0.0007
0 1 -13 -0.5543 0.0171
0 1 -11 4.7785 0.0117
0 1 -9 17.6216 -0.0102
0 1 -7 33.2333 -0.0085
0 1 -5 19.6869 -0.0443
0 1 -3 -44.1207 -0.1005
0 2 -44 1.6960 -0.2040
0 2 -42 12.5508 -0.0265
0 2 -40 3.0961 0.0994
0 2 -38 -6.8423 0.0205
0 2 -36 -6.9571 -0.0382
0 2 -34 -4.0633 0.0101
0 2 -32 -0.9941 0.0377
0 2 -30 0.9693 -0.0154
0 2 -28 0.4803 -0.0459
0 2 -26 2.7280 0.0054
0 2 -24 6.8132 0.0314
0 2 -22 3.7589 0.0016
0 2 -20 -3.8340 0.0095
0 2 -18 -6.1514 0.0161
0 2 -16 -2.6870 -0.0060
0 2 -14 0.7961 0.0292
0 2 -12 -3.1429 0.0084
0 2 -10 -7.5448 -0.0983
0 2 -8 18.5137 0.0219
0 2 -6 61.7568 0.1924
0 2 -4 29.7623 -0.1185
0 2 -2 -98.9905 -0.4345
0 2 0 -178.0362 -0.0333
0 3 -43 -10.9218 0.0521
0 3 -41 -3.3789 0.0318
0 3 -39 5.3903 -0.0406
0 3 -37 3.9084 -0.0226
0 3 -35 -0.6155 0.0432
0 3 -33 0.3425 0.0018
0 3 -31 2.4243 -0.0561
0 3 -29 0.8682 0.0012
0 3 -27 -1.6459 0.0368
0 3 -25 -2.1714 -0.0172
0 3 -23 -2.2329 -0.0192
0 3 -21 -3.2743 0.0123
0 3 -19 -1.7692 -0.0121
0 3 -17 3.3703 -0.0126
0 3 -15 4.7635 0.0083
0 3 -13 1.2526 -0.0177
0 3 -11 -1.6176 0.0015
0 3 -9 -17.3540 0.0380
0 3 -7 -52.9488 -0.0394
0 3 -5 -51.3544 -0.0517
0 3 -3 44.4255 0.1014
0 3 -1 161.5882 0.1005
0 4 -42 -11.8324 -0.0120
0 4 -40 -3.6211 -0.0625
0 4 -38 7.8367 0.0277
0 4 -36 1.7773 0.0383
0 4 -34 -8.3477 -0.0237
0 4 -32 -4.9989 -0.0036
0 4 -30 1.5593 0.0380
0 4 -28 -0.0663 0.0177
0 4 -26 -2.6516 -0.0082
0 4 -24 -1.6307 -0.0130
0 4 -22 -0.7907 -0.0050
0 4 -20 1.2435 0.0132
0 4 -18 4.1123 0.0046
0 4 -16 1.6648 -0.0060
0 4 -14 -1.5467 0.0220
0 4 -12 5.5231 0.0079
0 4 -10 17.9961 -0.0364
0 4 -8 21.1882 0.0275
0 4 -6 10.8584 0.0876
0 4 -4 -8.6307 -0.0398
0 4 -2 -29.8298 -0.1419
0 4 0 -39.6053 -0.0041
0 5 -43 -6.4820 -0.0447
0 5 -41 -9.6057 -0.0005
0 5 -39 -2.7052 0.0223
0 5 -37 12.0254 -0.0125
0 5 -35 19.5768 -0.0369
0 5 -33 8.2133 -0.0168
0 5 -31 -8.2836 0.0013
0 5 -29 -7.1625 -0.0106
0 5 -27 6.4389 -0.0069
0 5 -25 9.8582 0.0129
0 5 -23 2.7578 0.0004
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12 4 18 3.4747 -0.0262
12 4 20 0.2070 -0.0408
12 4 22 -5.2356 0.0013
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12 5 -5 -1.9083 0.0063
12 5 -3 -2.3512 -0.0133
12 5 -1 -0.7723 0.0023
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12 5 3 4.1922 0.0019
12 5 5 4.5813 -0.0064
12 5 7 2.5537 0.0140
12 5 9 -0.3704 -0.0122
12 5 11 -1.1469 -0.0325
12 5 13 0.2617 0.0163
12 5 15 1.3449 0.0254
12 5 17 -0.1884 -0.0121
12 5 19 -2.8927 0.0109
12 5 21 0.2246 0.0167
12 6 -26 4.7165 -0.0064
12 6 -24 -0.8170 0.0374
12 6 -22 -3.8345 0.0112
12 6 -20 1.0674 0.0290
12 6 -18 4.2991 0.0234
12 6 -16 0.3373 -0.0003
12 6 -14 0.6168 0.0378
12 6 -12 5.9257 0.0314
12 6 -10 2.9213 -0.0316
12 6 -8 -2.8629 -0.0029
12 6 -6 1.4387 0.0562
12 6 -4 5.5967 0.0225
12 6 -2 1.4772 -0.0126
12 6 0 0.4126 0.0126
12 6 2 1.6810 0.0116
12 6 4 -4.2480 -0.0277
12 6 6 -7.3977 -0.0236
12 6 8 -1.1445 0.0293
12 6 10 1.1633 0.0451
12 6 12 -1.9156 0.0093
12 6 14 -0.7251 0.0052
12 6 16 -1.0329 0.0186
12 6 18 -4.9863 -0.0078
12 6 20 -0.5910 0.0051
12 7 -25 10.6413 -0.0187
12 7 -23 4.2125 -0.1096
12 7 -21 3.5419 -0.0376
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12 7 -17 1.5046 0.0046
12 7 -15 3.5847 -0.0149
12 7 -13 2.4673 0.0063
12 7 -11 -0.4559 -0.0068
12 7 -9 2.3665 -0.0178
12 7 -7 3.8720 -0.0038
12 7 -5 -0.0976 -0.0014
12 7 -3 -1.5356 0.0042
12 7 -1 -1.8425 0.0041
12 7 1 -3.6771 -0.0163
12 7 3 -0.1628 0.0029
12 7 5 4.0621 0.0259
12 7 7 0.7642 -0.0263
12 7 9 -1.3755 -0.0377
12 7 11 -0.0670 0.0397
12 7 13 -4.1440 0.0335
12 7 15 -6.1322 -0.0250
12 7 17 -0.2675 0.0233
12 7 19 -0.7577 0.0543
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12 8 -22 1.2598 0.0159
12 8 -20 -4.7933 -0.0105
12 8 -18 -5.7730 0.0002
12 8 -16 -1.7648 0.0063
12 8 -14 -5.4904 -0.0207
12 8 -12 -11.1216 0.0100
12 8 -10 -3.3114 0.0151
12 8 -8 7.4950 -0.0382
12 8 -6 3.8388 -0.0062
12 8 -4 -4.4448 0.0400
12 8 -2 -4.5642 -0.0147
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12 8 2 -2.9355 0.0183
12 8 4 2.1452 0.0095
12 8 6 2.6111 -0.0052
12 8 8 -4.8738 0.0035
12 8 10 -4.3655 -0.0161
12 8 12 5.4615 0.0010
12 8 14 7.6713 0.0198
12 8 16 1.2203 -0.0396
12 8 18 -3.3288 -0.0297
12 9 -23 -5.8766 -0.0156
12 9 -21 -15.7156 -0.0668
12 9 -19 -8.4859 -0.0290
12 9 -17 5.0764 0.0251
12 9 -15 6.2325 0.0096
12 9 -13 2.2524 -0.0195
12 9 -11 -0.1972 0.0031
12 9 -9 -5.6949 0.0306
12 9 -7 -7.2162 0.0085
12 9 -5 -1.6077 -0.0205
12 9 -3 0.0634 -0.0122
12 9 -1 -0.9386 0.0037
12 9 1 0.7999 0.0029
12 9 3 -2.4408 -0.0098
12 9 5 -6.4477 -0.0249
12 9 7 1.0012 -0.0118
12 9 9 9.5812 0.0048
12 9 11 8.4424 -0.0329
12 9 13 5.0778 -0.0439
12 9 15 -0.5406 0.0254
12 9 17 -8.7870 0.0222
12 10 -22 1.1132 -0.0219
12 10 -20 5.1700 0.0558
12 10 -18 5.5468 0.0307
12 10 -16 3.0945 0.0083
12 10 -14 1.6159 -0.0039
12 10 -12 1.9856 -0.0360
12 10 -10 1.2608 0.0076
12 10 -8 -3.1078 0.0469
12 10 -6 -6.3639 -0.0254
12 10 -4 -2.7154 -0.0378
12 10 -2 2.6499 0.0419
12 10 0 2.8036 0.0186
12 10 2 1.9805 -0.0295
12 10 4 5.8209 0.0291
12 10 6 12.0830 0.0378
12 10 8 15.4741 -0.0060
12 10 10 10.9291 0.0429
12 10 12 -0.0017 0.0447
12 10 14 -4.9732 -0.0450
12 10 16 1.0739 -0.0044
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12 11 -17 -9.1007 0.0072
12 11 -15 -18.9397 -0.0114
12 11 -13 -11.4662 -0.0344
12 11 -11 9.5650 0.0016
12 11 -9 24.7345 0.0113
12 11 -7 18.0767 -0.0061
12 11 -5 1.2505 -0.0014
12 11 -3 -4.8438 -0.0134
12 11 -1 -1.4175 -0.0134
12 11 1 -2.5170 0.0187
12 11 3 -10.1763 -0.0033
12 11 5 -15.3580 -0.0283
12 11 7 -13.6169 0.0109
12 11 9 -10.4444 -0.0164
12 11 11 -10.8205 -0.0806
12 11 13 -9.9176 -0.0112
12 12 -16 3.0377 0.0418
12 12 -14 -5.3471 -0.0137
12 12 -12 -4.2559 -0.0198
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12 12 -8 4.3315 0.0206
12 12 -6 1.7268 0.0267
12 12 -4 3.8838 0.0085
12 12 -2 9.4803 -0.0099
12 12 0 13.0701 0.0034
12 12 2 8.3096 0.0127
12 12 4 -2.5987 -0.0087
12 12 6 -4.8198 -0.0155
12 12 8 4.1086 0.0107
12 12 10 8.7394 0.0289
12 13 -13 11.5133 0.0022
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12 13 -7 -13.2447 0.0088
12 13 -3 -5.9325 -0.0035
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12 14 -2 -7.4349 -0.0181
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13 1 -12 -2.6664 0.0314
13 1 -10 -9.1976 -0.0074
13 1 -8 -5.7202 -0.0035
13 1 -6 1.9513 0.0290
13 1 -4 3.7732 -0.0322
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13 1 4 0.8126 -0.0505
13 1 6 4.0763 0.0381
13 1 8 0.0780 0.0305
13 1 10 0.3931 -0.0561
13 1 12 5.5228 -0.0197
13 1 14 3.6870 0.0018
13 1 16 -1.2591 -0.0328
13 1 18 -1.3240 0.0575
13 2 -25 1.1372 0.0525
13 2 -23 -1.7233 0.0771
13 2 -21 -3.3136 0.0318
13 2 -19 -0.7058 0.0136
13 2 -17 0.1927 0.0675
13 2 -15 -1.6135 0.0465
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13 2 -9 -4.1533 0.0215
13 2 -7 -1.0736 -0.0084
13 2 -5 3.6472 -0.0192
13 2 -3 3.1319 0.0111
13 2 -1 -1.4226 0.0055
13 2 1 -2.8316 -0.0043
13 2 3 1.3304 0.0067
13 2 5 3.9127 -0.0039
13 2 7 -1.2289 -0.0016
13 2 9 -4.2179 0.0428
13 2 11 4.7994 0.0678
13 2 13 11.8999 0.0461
13 2 15 5.6476 -0.0006
13 2 17 2.3621 -0.0367
13 2 19 8.7496 -0.0079
13 3 -24 1.5755 0.1019
13 3 -22 -5.0513 0.0896
13 3 -20 -7.9517 -0.1256
13 3 -18 -1.8962 -0.0471
13 3 -16 4.8657 0.1272
13 3 -14 7.5708 0.0339
13 3 -12 7.3783 -0.0600
13 3 -10 2.3742 0.0273
13 3 -8 -3.1059 0.0370
13 3 -6 0.7356 -0.0157
13 3 -4 8.0840 0.0378
13 3 -2 6.3890 0.0336
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13 3 4 0.3199 0.0609
13 3 6 -5.4165 0.0001
13 3 8 -4.9946 -0.0122
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13 3 14 -2.4528 -0.0459
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13 4 -7 -0.9752 0.0393
13 4 -5 -9.4777 -0.0052
13 4 -3 -6.7723 -0.0089
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13 4 3 2.9150 -0.0270
13 4 5 -4.1988 0.0004
13 4 7 -4.3684 -0.0023
13 4 9 -0.4556 0.0027
13 4 11 0.3449 0.0608
13 4 13 -1.8697 0.0423
13 4 15 -4.3144 -0.0368
13 4 17 -10.3283 0.0051
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13 5 -20 6.4016 0.0767
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13 5 -14 -6.9389 0.0325
13 5 -12 0.0691 0.0401
13 5 -10 6.5454 -0.0530
13 5 -8 9.4633 -0.0281
13 5 -6 3.7176 0.0324
13 5 -4 -7.6490 0.0013
13 5 -2 -9.2692 -0.0255
13 5 0 -1.3871 0.0105
13 5 2 0.4426 0.0190
13 5 4 -1.1851 -0.0112
13 5 6 3.5416 -0.0122
13 5 8 5.3510 -0.0113
13 5 10 0.3164 -0.0319
13 5 12 0.0272 -0.0136
13 5 14 -0.7440 -0.0007
13 5 16 -11.2752 -0.0510
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13 6 -19 -1.2935 0.0370
13 6 -17 4.0588 0.0048
13 6 -15 4.4215 -0.0380
13 6 -13 1.3991 -0.0093
13 6 -11 0.5012 0.0450
13 6 -9 -1.1188 0.0233
13 6 -7 -1.1460 -0.0322
13 6 -5 3.6329 -0.0131
13 6 -3 1.9714 0.0246
13 6 -1 -7.8329 -0.0087
13 6 1 -9.0034 -0.0274
13 6 3 -2.1061 0.0128
13 6 5 -0.7749 0.0043
13 6 7 0.4326 -0.0358
13 6 9 5.4019 -0.0200
13 6 11 1.0814 -0.0126
13 6 13 -7.9290 -0.0143
13 6 15 -2.7896 0.0531
13 7 -20 -5.8875 0.0032
13 7 -18 -2.1530 0.1160
13 7 -16 0.1595 -0.0121
13 7 -14 -5.8532 -0.0836
13 7 -12 -5.7937 0.0133
13 7 -10 2.5575 0.0456
13 7 -8 1.5892 -0.0084
13 7 -6 -5.6950 -0.0256
13 7 -4 -2.7067 -0.0212
13 7 -2 2.3736 -0.0077
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13 8 -17 -2.0604 0.0442
13 8 -15 -4.3406 0.0303
13 8 -13 5.4891 0.0361
13 8 -11 7.6610 0.0199
13 8 -9 -2.0543 -0.0152
13 8 -7 -8.2815 -0.0016
13 8 -5 -8.1335 0.0117
13 8 -3 -2.2967 -0.0190
13 8 -1 6.4706 -0.0035
13 8 1 3.5418 0.0428
13 8 3 -6.0143 0.0185
13 8 5 -0.5610 0.0025
13 8 7 8.3027 0.0382
13 8 9 1.4163 -0.0120
13 8 11 -2.1499 -0.0835
13 8 13 7.7754 -0.0130
13 9 -18 5.7337 -0.0012
13 9 -16 -2.3762 0.0827
13 9 -14 -4.4549 -0.0287
13 9 -12 -0.8052 -0.0802
13 9 -10 0.6079 0.0350
13 9 -8 -0.5345 0.0461
13 9 -6 0.3511 -0.0406
13 9 -4 3.2504 -0.0108
13 9 -2 6.0829 0.0312
13 9 0 6.7984 -0.0101
13 9 2 2.4941 -0.0010
13 9 4 -3.6429 0.0135
13 9 6 -3.3071 -0.0427
13 9 8 1.7468 -0.0160
13 9 10 0.9016 0.0656
13 10 -15 -1.7232 0.0109
13 10 -13 -1.5924 0.0250
13 10 -11 1.6987 0.0085
13 10 -9 8.4005 -0.0143
13 10 -7 8.9492 -0.0024
13 10 -5 5.0710 0.0049
13 10 -3 2.4477 -0.0012
13 10 -1 -0.1432 0.0091
13 10 1 -1.3040 0.0020
13 10 3 -0.8919 -0.0092
13 10 5 -5.0076 0.0242
13 10 7 -10.7662 0.0243
13 10 9 -9.1015 -0.0299
13 11 -10 1.0818 -0.0235
13 11 -8 -2.2151 -0.0362
13 11 -6 2.8393 0.0422
13 11 -4 5.2504 0.0264
13 11 -2 4.3281 -0.0263
13 11 0 4.1753 -0.0042
13 11 2 2.6488 0.0190
13 11 4 0.6100 0.0006
14 0 -20 -1.1832 0.0662
14 0 -18 -14.6764 0.0329
14 0 -16 -12.8040 -0.0338
14 0 -14 -8.2694 0.0264
14 0 -12 -11.8277 0.0426
14 0 -10 -10.2447 0.0043
14 0 -8 -0.3555 0.0223
14 0 -6 5.8265 0.0270
14 0 -4 6.0488 -0.0027
14 0 -2 3.7413 0.0027
14 0 0 -0.3675 0.0108
14 0 2 -3.4964 0.0138
14 0 4 -6.2786 0.0306
14 0 6 -9.4290 -0.0004
14 0 8 -5.8629 -0.0258
14 0 10 0.7680 0.0401
14 0 12 -3.8554 0.0462
14 1 -19 -0.4110 -0.0142
14 1 -17 5.5533 0.0143
14 1 -15 8.2546 -0.0591
14 1 -13 4.4525 -0.1055
14 1 -11 -1.6986 0.0037
14 1 -9 -3.7935 0.0454
14 1 -7 -1.6945 -0.0281
14 1 -5 0.8693 -0.0120
14 1 -3 1.5471 0.0400
14 1 -1 0.7431 -0.0085
14 1 1 1.4442 -0.0442
14 1 3 4.0454 0.0057
14 1 5 4.3490 0.0327
14 1 7 3.0974 -0.0045
14 1 9 5.5729 -0.0421
14 1 11 8.1679 -0.0481
14 1 13 4.9735 -0.0488
14 2 -20 2.2947 -0.1707
14 2 -18 6.6876 0.0248
14 2 -16 3.9107 0.0577
14 2 -14 6.6605 -0.0252
14 2 -12 12.6198 0.0657
14 2 -10 6.5950 0.0674
14 2 -8 -4.0169 -0.0452
14 2 -6 -4.2939 0.0146
14 2 -4 -0.6474 0.0583
14 2 -2 -0.0542 -0.0448
14 2 0 2.1938 -0.0027
14 2 2 3.4277 0.0799
14 2 4 0.0263 -0.0391
14 2 6 -1.5774 -0.0565
14 2 8 -1.7431 0.0869
14 2 10 -4.8471 0.0235
14 2 12 -3.3629 -0.0569
14 3 -19 -0.7696 -0.0112
14 3 -17 -8.2717 -0.0040
14 3 -15 -10.1103 0.0288
14 3 -13 -4.7039 0.0096
14 3 -11 4.2852 -0.0174
14 3 -9 6.2996 -0.0021
14 3 -7 -1.8870 -0.0002
14 3 -5 -8.4200 -0.0097
14 3 -3 -4.5188 0.0032
14 3 -1 1.6348 -0.0049
14 3 1 -0.6896 -0.0192
14 3 3 -7.0981 0.0062
14 3 5 -6.1068 0.0065
14 3 7 0.4813 -0.0252
14 3 9 0.8683 -0.0020
14 3 11 -4.7795 0.0189
14 4 -18 -1.2382 -0.0414
14 4 -16 -0.0564 -0.0359
14 4 -14 -2.5661 0.0052
14 4 -12 -4.6361 -0.0647
14 4 -10 1.4999 -0.0429
14 4 -8 6.1455 0.0211
14 4 -6 0.6574 -0.0333
14 4 -4 -2.1777 -0.0471
14 4 -2 2.6280 0.0288
14 4 0 1.1855 -0.0001
14 4 2 -3.7714 -0.0519
14 4 4 1.8260 0.0332
14 4 6 8.0729 0.0617
14 4 8 3.4201 -0.0379
14 4 10 0.9815 -0.0206
14 5 -17 2.6504 0.0110
14 5 -15 3.6802 0.0119
14 5 -13 7.3892 0.0353
14 5 -11 2.9612 -0.0133
14 5 -9 -5.7848 -0.0626
14 5 -7 -1.4778 -0.0034
14 5 -5 6.1594 0.0328
14 5 -3 -0.8403 -0.0257
14 5 -1 -8.4648 -0.0195
14 5 1 -2.1753 0.0442
14 5 3 4.4453 0.0070
14 5 5 3.0802 -0.0463
14 5 7 1.4167 -0.0028
14 5 9 -0.6971 0.0023
14 6 -14 -4.6459 0.0415
14 6 -12 0.4643 0.0414
14 6 -10 3.8415 0.0016
14 6 -8 0.3194 0.0091
14 6 -6 -0.3854 0.0200
14 6 -4 1.1388 0.0051
14 6 -2 -3.0335 0.0109
14 6 0 -4.5808 0.0196
14 6 2 1.8872 0.0140
14 6 4 2.7949 -0.0053
14 6 6 -3.2822 -0.0336
14 6 8 -2.2254 0.0131
14 7 -13 -6.2331 -0.0124
14 7 -11 -9.1690 -0.0540
14 7 -9 -4.1756 -0.0209
14 7 -7 -3.0861 0.0223
14 7 -5 -4.7790 0.0015
14 7 -3 4.0993 -0.0077
14 7 -1 10.2004 0.0191
14 7 1 1.9714 0.0026
14 7 3 -1.1344 -0.0118
14 7 5 3.1563 0.0245
14 7 7 -3.9695 -0.0017
14 8 -10 -0.4484 0.0157
14 8 -8 3.8304 -0.0121
14 8 -6 5.7246 0.0116
14 8 -4 2.2202 0.0247
14 8 -2 2.6667 -0.0289
14 8 0 6.4991 -0.0025
14 8 2 2.8987 0.0600
15 1 -8 -7.4359 -0.0765
15 1 -6 0.4047 -0.0206
15 1 -4 -1.4869 0.0193
15 1 -2 -8.8630 0.0136
15 1 0 -6.5353 0.0216
15 1 2 4.4528 -0.0280
15 2 -7 -4.8181 0.0294
15 2 -5 -4.4108 -0.0128
15 2 -3 1.7615 -0.0285
15 2 -1 3.3216 0.0004
15 2 1 -2.7741 0.0150
15 3 -6 1.4223 -0.0126
15 3 -4 -2.2297 -0.0087
15 3 -2 1.8986 0.0257
0 0 0 0.0 0.0
;
_shelx_fab_checksum 29400
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
Ni Ni1 0.250000 0.750000 0.750000 0.0562(3) Uani d 1 . .
Ni Ni2 0.750000 0.750000 0.750000 0.0628(3) Uani d 1 . .
S S1 0.50054(10) 0.67856(9) 0.75649(4) 0.0648(5) Uani d 1 . .
O O3 0.5194(2) 0.6766(2) 0.79768(10) 0.0784(12) Uani d 1 . .
O O2 0.60695(19) 0.68618(17) 0.73957(8) 0.0637(10) Uani d 1 . .
N N3 0.8460(3) 0.6578(3) 0.74746(15) 0.0723(14) Uani d 1 . .
H H3 0.923074 0.673461 0.747240 0.087 Uiso calc 1 . .
O O1 0.4286(2) 0.74068(18) 0.74571(9) 0.0633(10) Uani d 1 . .
O O4 0.4467(2) 0.6099(2) 0.74284(10) 0.0839(13) Uani d 1 . .
N N1 0.2244(3) 0.6743(3) 0.70776(12) 0.0646(13) Uani d 1 . .
H H1 0.296188 0.651709 0.704761 0.078 Uiso calc 1 . .
N N2 0.2493(3) 0.6758(3) 0.79323(12) 0.0724(15) Uani d 1 . .
H H2 0.322725 0.653431 0.796249 0.087 Uiso calc 1 . .
N N4 0.7455(3) 0.7698(3) 0.69294(12) 0.0752(15) Uani d 1 . .
H H4 0.815571 0.792987 0.688167 0.090 Uiso calc 1 . .
C C30 0.6311(4) 0.1028(2) 0.43972(16) 0.0549(15) Uani d 1 . .
O O6 0.3958(3) 0.6092(2) 0.64754(11) 0.1048(15) Uani d 1 . .
C C11 0.4785(4) 0.5740(3) 0.6510(2) 0.0739(19) Uani d 1 . .
O O8 0.3879(3) -0.0478(2) 0.34768(11) 0.0993(15) Uani d 1 . .
C C18 0.6922(3) 0.4520(2) 0.52586(16) 0.0565(15) Uani d 1 . .
C C15 0.6387(4) 0.4891(3) 0.55700(18) 0.0578(16) Uani d 1 . .
O O5 0.5273(3) 0.5560(3) 0.68365(12) 0.1085(17) Uani d 1 . .
H H5 0.494848 0.574604 0.700454 0.163 Uiso calc 1 . .
C C35 0.6920(4) 0.0749(3) 0.41216(17) 0.0641(17) Uani d 1 . .
H H35 0.767412 0.084687 0.413391 0.077 Uiso calc 1 . .
O O7 0.5501(4) -0.0438(2) 0.32448(15) 0.141(2) Uani d 1 . .
H H7 0.544646 -0.087006 0.319664 0.212 Uiso calc 1 . .
C C24 0.750000 0.2565(4) 0.500000 0.061(2) Uani d 1 . .
C C10 0.8358(4) 0.6201(4) 0.7837(2) 0.099(2) Uani d 1 . .
H H10A 0.894279 0.584556 0.787911 0.118 Uiso calc 1 . .
H H10B 0.765234 0.595217 0.783070 0.118 Uiso calc 1 . .
C C12 0.5369(4) 0.5458(3) 0.61875(18) 0.0632(17) Uani d 1 . .
C C33 0.5339(4) 0.0202(2) 0.37979(15) 0.0549(15) Uani d 1 . .
C C32 0.4706(4) 0.0485(3) 0.40693(17) 0.0667(17) Uani d 1 . .
H H32 0.394832 0.040027 0.405222 0.080 Uiso calc 1 . .
C C29 0.750000 0.0240(3) 0.500000 0.081(3) Uani d 1 . .
H H29A 0.682200 0.006673 0.508860 0.122 Uiso d 0.5 A -1
H H29B 0.811420 0.006673 0.516270 0.122 Uiso d 0.5 A -1
H H29C 0.756370 0.006673 0.474860 0.122 Uiso d 0.5 A -1
C C25 0.6867(4) 0.2198(3) 0.47185(17) 0.0632(16) Uani d 1 . .
C C31 0.5178(4) 0.0887(3) 0.43612(17) 0.0724(18) Uani d 1 . .
H H31 0.473456 0.107060 0.453963 0.087 Uiso calc 1 . .
C C21 0.6887(4) 0.3754(2) 0.52488(16) 0.0598(16) Uani d 1 . .
C C2 0.1792(4) 0.5761(3) 0.7521(2) 0.102(3) Uani d 1 . .
H H2A 0.134603 0.532745 0.752629 0.123 Uiso calc 1 . .
H H2B 0.255789 0.561034 0.751981 0.123 Uiso calc 1 . .
C C14 0.5408(4) 0.5268(3) 0.55178(17) 0.0761(18) Uani d 1 . .
H H14 0.507398 0.533655 0.527591 0.091 Uiso calc 1 . .
C C19 0.750000 0.4897(4) 0.500000 0.059(2) Uani d 1 . .
C C7 0.8269(4) 0.6526(4) 0.67781(18) 0.100(2) Uani d 1 . .
H H7A 0.827753 0.618110 0.657331 0.120 Uiso calc 1 . .
H H7B 0.896294 0.678843 0.679027 0.120 Uiso calc 1 . .
C C1 0.1470(4) 0.6156(3) 0.71504(19) 0.091(2) Uani d 1 . .
H H1A 0.145034 0.581271 0.694445 0.109 Uiso calc 1 . .
H H1B 0.073304 0.635565 0.715824 0.109 Uiso calc 1 . .
C C34 0.6463(4) 0.0332(3) 0.38290(16) 0.0628(16) Uani d 1 . .
H H34 0.690847 0.014029 0.365352 0.075 Uiso calc 1 . .
C C26 0.6144(4) 0.2602(3) 0.44165(17) 0.093(2) Uani d 1 . .
H H26A 0.628524 0.311130 0.443719 0.140 Uiso d 1 . .
H H26B 0.537924 0.251010 0.444999 0.140 Uiso d 1 . .
H H26C 0.630924 0.243690 0.417199 0.140 Uiso d 1 . .
C C28 0.750000 0.1063(3) 0.500000 0.053(2) Uani d 1 . .
C C36 0.4816(5) -0.0268(3) 0.34931(17) 0.0710(18) Uani d 1 . .
C C6 0.8214(4) 0.6113(3) 0.7142(2) 0.093(2) Uani d 1 . .
H H6A 0.748034 0.590791 0.714947 0.112 Uiso calc 1 . .
H H6B 0.874045 0.571789 0.714897 0.112 Uiso calc 1 . .
C C27 0.6889(4) 0.1440(3) 0.47161(16) 0.0581(15) Uani d 1 . .
C C23 0.750000 0.3381(3) 0.500000 0.059(2) Uani d 1 . .
C C4 0.2352(4) 0.7191(4) 0.82776(17) 0.092(2) Uani d 1 . .
H H4A 0.257107 0.690753 0.850039 0.111 Uiso calc 1 . .
H H4B 0.158213 0.732707 0.828578 0.111 Uiso calc 1 . .
C C13 0.4922(4) 0.5543(3) 0.5823(2) 0.077(2) Uani d 1 . .
H H13 0.426278 0.579840 0.578109 0.092 Uiso calc 1 . .
C C17 0.6369(4) 0.5105(3) 0.62374(17) 0.087(2) Uani d 1 . .
H H17 0.671219 0.504953 0.647893 0.105 Uiso calc 1 . .
C C16 0.6867(4) 0.4833(3) 0.5933(2) 0.099(2) Uani d 1 . .
H H16 0.754840 0.460414 0.597436 0.118 Uiso calc 1 . .
C C5 0.1940(4) 0.7144(4) 0.67308(16) 0.089(2) Uani d 1 . .
H H5A 0.116564 0.728053 0.672049 0.106 Uiso calc 1 . .
H H5B 0.204755 0.684329 0.651400 0.106 Uiso calc 1 . .
C C3 0.1672(4) 0.6173(4) 0.7876(2) 0.099(2) Uani d 1 . .
H H3A 0.093417 0.637773 0.786818 0.119 Uiso calc 1 . .
H H3B 0.175758 0.584418 0.808869 0.119 Uiso calc 1 . .
C C9 0.6560(4) 0.8245(4) 0.68479(18) 0.100(2) Uani d 1 . .
H H9A 0.584152 0.801136 0.683389 0.120 Uiso calc 1 . .
H H9B 0.664611 0.847849 0.660847 0.120 Uiso calc 1 . .
C C22 0.6150(4) 0.3346(3) 0.55038(16) 0.096(2) Uani d 1 . .
H H22A 0.652519 0.330370 0.575101 0.144 Uiso d 1 . .
H H22B 0.598969 0.287350 0.540311 0.144 Uiso d 1 . .
H H22C 0.547179 0.360810 0.551891 0.144 Uiso d 1 . .
C C8 0.7330(4) 0.7059(4) 0.66839(17) 0.099(2) Uani d 1 . .
H H8A 0.733069 0.720682 0.642270 0.119 Uiso calc 1 . .
H H8B 0.662777 0.682610 0.671625 0.119 Uiso calc 1 . .
C C20 0.750000 0.5710(3) 0.500000 0.086(3) Uani d 1 . .
H H20A 0.675440 0.588307 0.500220 0.129 Uiso d 0.5 B -1
H H20B 0.781320 0.588307 0.477810 0.129 Uiso d 0.5 B -1
H H20C 0.793240 0.588307 0.521970 0.129 Uiso d 0.5 B -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
Ni1 0.0282(5) 0.1032(8) 0.0381(6) 0.0154(5) 0.0081(4) 0.0213(6)
Ni2 0.0268(5) 0.1156(8) 0.0474(7) 0.0160(5) 0.0113(4) 0.0303(7)
S1 0.0272(6) 0.1131(13) 0.0562(11) 0.0168(8) 0.0155(6) 0.0301(11)
O3 0.047(2) 0.140(3) 0.049(3) 0.029(2) 0.0138(17) 0.044(3)
O2 0.0217(16) 0.117(3) 0.055(3) 0.0142(16) 0.0150(15) 0.018(2)
N3 0.030(2) 0.122(4) 0.066(4) 0.014(2) 0.010(2) 0.023(4)
O1 0.0313(16) 0.104(3) 0.055(2) 0.0224(17) 0.0082(15) 0.026(2)
O4 0.040(2) 0.105(3) 0.110(4) 0.005(2) 0.028(2) 0.009(3)
N1 0.032(2) 0.117(4) 0.046(3) 0.022(2) 0.010(2) -0.001(3)
N2 0.030(2) 0.132(4) 0.057(4) 0.025(3) 0.015(2) 0.042(3)
N4 0.037(2) 0.139(5) 0.051(4) 0.010(3) 0.014(2) 0.029(3)
C30 0.068(4) 0.033(3) 0.066(5) 0.004(3) 0.020(3) 0.004(3)
O6 0.065(3) 0.143(4) 0.108(4) 0.053(2) 0.011(2) -0.008(3)
C11 0.047(4) 0.084(5) 0.092(6) 0.012(3) 0.015(4) -0.009(4)
O8 0.051(2) 0.133(3) 0.116(4) -0.020(2) 0.025(2) -0.044(3)
C18 0.041(3) 0.044(3) 0.085(5) 0.009(2) 0.010(3) -0.007(3)
C15 0.045(3) 0.048(3) 0.082(5) -0.002(3) 0.011(3) 0.004(4)
O5 0.075(3) 0.167(4) 0.084(4) 0.057(3) 0.010(3) -0.005(4)
C35 0.056(3) 0.059(4) 0.079(5) -0.010(3) 0.015(3) 0.000(4)
O7 0.103(3) 0.163(4) 0.172(5) -0.076(3) 0.096(3) -0.115(4)
C24 0.069(5) 0.032(5) 0.086(8) 0.000 0.026(5) 0.000
C10 0.047(4) 0.144(7) 0.105(7) 0.021(4) 0.008(4) 0.048(6)
C12 0.042(3) 0.068(4) 0.081(5) 0.012(3) 0.009(3) 0.004(4)
C33 0.049(3) 0.052(3) 0.067(5) -0.001(2) 0.021(3) -0.003(3)
C32 0.043(3) 0.072(4) 0.087(5) -0.004(3) 0.018(3) -0.019(4)
C29 0.116(6) 0.044(5) 0.081(7) 0.000 -0.010(5) 0.000
C25 0.072(4) 0.037(4) 0.082(5) 0.002(3) 0.012(3) 0.010(3)
C31 0.062(4) 0.073(4) 0.086(5) 0.003(3) 0.032(3) -0.015(4)
C21 0.055(3) 0.042(3) 0.086(5) -0.006(3) 0.024(3) 0.004(3)
C2 0.042(4) 0.105(6) 0.161(9) 0.005(3) 0.019(4) 0.025(6)
C14 0.052(3) 0.097(4) 0.079(5) 0.020(3) 0.003(3) -0.020(4)
C19 0.041(4) 0.041(5) 0.095(7) 0.000 0.013(4) 0.000
C7 0.071(4) 0.156(6) 0.077(6) -0.007(4) 0.027(4) -0.004(5)
C1 0.043(3) 0.121(6) 0.111(7) -0.003(4) 0.011(4) -0.022(5)
C34 0.054(3) 0.057(4) 0.082(5) -0.006(3) 0.030(3) 0.007(3)
C26 0.105(5) 0.053(4) 0.121(6) 0.009(3) 0.000(4) 0.005(4)
C28 0.083(5) 0.010(4) 0.068(7) 0.000 0.013(4) 0.000
C36 0.066(4) 0.077(4) 0.074(5) -0.014(3) 0.029(4) -0.022(4)
C6 0.040(3) 0.134(6) 0.107(7) 0.011(3) 0.018(4) 0.011(6)
C27 0.055(3) 0.045(4) 0.074(5) 0.000(3) 0.008(3) -0.001(3)
C23 0.050(4) 0.028(5) 0.099(8) 0.000 0.014(4) 0.000
C4 0.059(4) 0.168(7) 0.054(5) 0.046(4) 0.027(3) 0.041(5)
C13 0.049(4) 0.081(4) 0.100(6) 0.027(3) 0.008(4) 0.004(4)
C17 0.058(3) 0.121(5) 0.082(5) 0.040(3) 0.004(3) -0.005(4)
C16 0.055(4) 0.139(6) 0.103(6) 0.046(4) 0.016(4) -0.015(5)
C5 0.064(4) 0.159(7) 0.043(4) 0.039(4) 0.008(3) 0.002(5)
C3 0.050(4) 0.129(6) 0.123(7) 0.015(4) 0.032(4) 0.057(5)
C9 0.053(4) 0.178(7) 0.067(5) 0.018(4) 0.002(3) 0.064(5)
C22 0.103(5) 0.064(4) 0.129(6) -0.008(3) 0.051(4) 0.017(4)
C8 0.057(4) 0.181(7) 0.062(5) 0.000(4) 0.013(3) 0.021(5)
C20 0.111(6) 0.019(4) 0.135(9) 0.000 0.055(5) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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 Ni1 O1 . 7_566 180.0 ?
N1 Ni1 O1 7_566 . 90.85(13) ?
N1 Ni1 O1 . 7_566 90.85(13) ?
N1 Ni1 O1 . . 89.15(13) ?
N1 Ni1 O1 7_566 7_566 89.15(13) ?
N1 Ni1 N1 . 7_566 180.0 ?
N1 Ni1 N2 7_566 7_566 94.72(19) ?
N1 Ni1 N2 7_566 . 85.28(19) ?
N1 Ni1 N2 . 7_566 85.28(19) ?
N1 Ni1 N2 . . 94.72(19) ?
N2 Ni1 O1 . 7_566 86.26(12) ?
N2 Ni1 O1 . . 93.74(12) ?
N2 Ni1 O1 7_566 7_566 93.74(12) ?
N2 Ni1 O1 7_566 . 86.26(12) ?
N2 Ni1 N2 . 7_566 180.0 ?
O2 Ni2 O2 7_666 . 180.0 ?
N3 Ni2 O2 7_666 7_666 89.28(14) ?
N3 Ni2 O2 . . 89.28(14) ?
N3 Ni2 O2 7_666 . 90.72(14) ?
N3 Ni2 O2 . 7_666 90.72(14) ?
N3 Ni2 N3 7_666 . 180.0 ?
N4 Ni2 O2 . 7_666 91.61(15) ?
N4 Ni2 O2 7_666 . 91.61(15) ?
N4 Ni2 O2 7_666 7_666 88.39(15) ?
N4 Ni2 O2 . . 88.39(15) ?
N4 Ni2 N3 . 7_666 85.84(19) ?
N4 Ni2 N3 7_666 7_666 94.16(19) ?
N4 Ni2 N3 7_666 . 85.84(19) ?
N4 Ni2 N3 . . 94.16(19) ?
N4 Ni2 N4 7_666 . 180.00(4) ?
O3 S1 O2 . . 110.02(18) ?
O3 S1 O1 . . 108.6(2) ?
O3 S1 O4 . . 109.5(2) ?
O2 S1 O4 . . 108.8(2) ?
O1 S1 O2 . . 109.74(19) ?
O1 S1 O4 . . 110.2(2) ?
S1 O2 Ni2 . . 135.8(2) ?
Ni2 N3 H3 . . 107.2 ?
C10 N3 Ni2 . . 105.2(3) ?
C10 N3 H3 . . 107.2 ?
C6 N3 Ni2 . . 116.0(3) ?
C6 N3 H3 . . 107.2 ?
C6 N3 C10 . . 113.6(5) ?
S1 O1 Ni1 . . 127.61(19) ?
Ni1 N1 H1 . . 106.8 ?
C1 N1 Ni1 . . 115.6(3) ?
C1 N1 H1 . . 106.8 ?
C5 N1 Ni1 . . 106.5(4) ?
C5 N1 H1 . . 106.8 ?
C5 N1 C1 . . 113.8(5) ?
Ni1 N2 H2 . . 107.6 ?
C4 N2 Ni1 . . 105.4(4) ?
C4 N2 H2 . . 107.6 ?
C3 N2 Ni1 . . 115.7(3) ?
C3 N2 H2 . . 107.6 ?
C3 N2 C4 . . 112.6(4) ?
Ni2 N4 H4 . . 107.3 ?
C9 N4 Ni2 . . 105.7(3) ?
C9 N4 H4 . . 107.3 ?
C8 N4 Ni2 . . 115.8(4) ?
C8 N4 H4 . . 107.3 ?
C8 N4 C9 . . 113.1(5) ?
C35 C30 C31 . . 116.6(5) ?
C35 C30 C27 . . 119.2(5) ?
C31 C30 C27 . . 124.2(5) ?
O6 C11 O5 . . 123.1(6) ?
O6 C11 C12 . . 124.2(6) ?
O5 C11 C12 . . 112.8(5) ?
C21 C18 C15 . . 117.5(5) ?
C19 C18 C15 . . 122.3(4) ?
C19 C18 C21 . . 120.1(5) ?
C14 C15 C18 . . 123.7(6) ?
C16 C15 C18 . . 119.0(5) ?
C16 C15 C14 . . 117.3(5) ?
C11 O5 H5 . . 109.5 ?
C30 C35 H35 . . 118.5 ?
C30 C35 C34 . . 123.0(5) ?
C34 C35 H35 . . 118.5 ?
C36 O7 H7 . . 109.5 ?
C25 C24 C25 . 2_656 121.4(7) ?
C25 C24 C23 2_656 . 119.3(4) ?
C25 C24 C23 . . 119.3(4) ?
N3 C10 H10A . . 110.0 ?
N3 C10 H10B . . 110.0 ?
N3 C10 C9 . 7_666 108.7(5) ?
H10A C10 H10B . . 108.3 ?
C9 C10 H10A 7_666 . 110.0 ?
C9 C10 H10B 7_666 . 110.0 ?
C13 C12 C11 . . 120.7(5) ?
C13 C12 C17 . . 116.8(5) ?
C17 C12 C11 . . 122.5(6) ?
C32 C33 C36 . . 120.2(5) ?
C34 C33 C32 . . 118.5(5) ?
C34 C33 C36 . . 121.2(5) ?
C33 C32 H32 . . 119.4 ?
C31 C32 C33 . . 121.1(5) ?
C31 C32 H32 . . 119.4 ?
H29A C29 H29B . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
C28 C29 H29A . . 109.5 ?
C28 C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5 ?
C24 C25 C26 . . 121.3(5) ?
C24 C25 C27 . . 118.9(6) ?
C27 C25 C26 . . 119.7(5) ?
C30 C31 H31 . . 119.4 ?
C32 C31 C30 . . 121.3(5) ?
C32 C31 H31 . . 119.4 ?
C18 C21 C22 . . 119.8(4) ?
C23 C21 C18 . . 119.8(5) ?
C23 C21 C22 . . 120.3(4) ?
H2A C2 H2B . . 107.3 ?
C1 C2 H2A . . 108.1 ?
C1 C2 H2B . . 108.1 ?
C3 C2 H2A . . 108.1 ?
C3 C2 H2B . . 108.1 ?
C3 C2 C1 . . 116.8(6) ?
C15 C14 H14 . . 119.9 ?
C15 C14 C13 . . 120.1(6) ?
C13 C14 H14 . . 119.9 ?
C18 C19 C18 . 2_656 119.8(6) ?
C18 C19 C20 2_656 . 120.1(3) ?
C18 C19 C20 . . 120.1(3) ?
H7A C7 H7B . . 107.5 ?
C6 C7 H7A . . 108.4 ?
C6 C7 H7B . . 108.4 ?
C6 C7 C8 . . 115.6(5) ?
C8 C7 H7A . . 108.4 ?
C8 C7 H7B . . 108.4 ?
N1 C1 C2 . . 112.6(5) ?
N1 C1 H1A . . 109.1 ?
N1 C1 H1B . . 109.1 ?
C2 C1 H1A . . 109.1 ?
C2 C1 H1B . . 109.1 ?
H1A C1 H1B . . 107.8 ?
C35 C34 C33 . . 119.5(5) ?
C35 C34 H34 . . 120.3 ?
C33 C34 H34 . . 120.3 ?
C25 C26 H26A . . 109.8 ?
C25 C26 H26B . . 109.3 ?
C25 C26 H26C . . 109.4 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C27 C28 C29 2_656 . 120.2(3) ?
C27 C28 C29 . . 120.2(3) ?
C27 C28 C27 2_656 . 119.7(7) ?
O8 C36 O7 . . 123.0(6) ?
O8 C36 C33 . . 124.7(5) ?
O7 C36 C33 . . 112.3(5) ?
N3 C6 C7 . . 111.9(6) ?
N3 C6 H6A . . 109.2 ?
N3 C6 H6B . . 109.2 ?
C7 C6 H6A . . 109.2 ?
C7 C6 H6B . . 109.2 ?
H6A C6 H6B . . 107.9 ?
C25 C27 C30 . . 120.5(5) ?
C28 C27 C30 . . 118.9(5) ?
C28 C27 C25 . . 120.5(6) ?
C21 C23 C24 . . 119.9(3) ?
C21 C23 C24 2_656 . 119.9(3) ?
C21 C23 C21 . 2_656 120.2(6) ?
N2 C4 H4A . . 110.0 ?
N2 C4 H4B . . 110.0 ?
N2 C4 C5 . 7_566 108.6(4) ?
H4A C4 H4B . . 108.3 ?
C5 C4 H4A 7_566 . 110.0 ?
C5 C4 H4B 7_566 . 110.0 ?
C12 C13 C14 . . 122.8(5) ?
C12 C13 H13 . . 118.6 ?
C14 C13 H13 . . 118.6 ?
C12 C17 H17 . . 119.6 ?
C12 C17 C16 . . 120.7(6) ?
C16 C17 H17 . . 119.6 ?
C15 C16 C17 . . 122.1(5) ?
C15 C16 H16 . . 119.0 ?
C17 C16 H16 . . 119.0 ?
N1 C5 C4 . 7_566 109.2(5) ?
N1 C5 H5A . . 109.8 ?
N1 C5 H5B . . 109.8 ?
C4 C5 H5A 7_566 . 109.8 ?
C4 C5 H5B 7_566 . 109.8 ?
H5A C5 H5B . . 108.3 ?
N2 C3 C2 . . 112.1(5) ?
N2 C3 H3A . . 109.2 ?
N2 C3 H3B . . 109.2 ?
C2 C3 H3A . . 109.2 ?
C2 C3 H3B . . 109.2 ?
H3A C3 H3B . . 107.9 ?
N4 C9 C10 . 7_666 108.2(5) ?
N4 C9 H9A . . 110.1 ?
N4 C9 H9B . . 110.1 ?
C10 C9 H9A 7_666 . 110.1 ?
C10 C9 H9B 7_666 . 110.1 ?
H9A C9 H9B . . 108.4 ?
C21 C22 H22A . . 109.3 ?
C21 C22 H22B . . 109.8 ?
C21 C22 H22C . . 109.3 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
N4 C8 C7 . . 110.6(5) ?
N4 C8 H8A . . 109.5 ?
N4 C8 H8B . . 109.5 ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 108.1 ?
C19 C20 H20A . . 109.5 ?
C19 C20 H20B . . 109.5 ?
C19 C20 H20C . . 109.5 ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
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
Ni1 O1 . 2.191(2) ?
Ni1 O1 7_566 2.191(2) ?
Ni1 N1 . 2.061(4) ?
Ni1 N1 7_566 2.061(4) ?
Ni1 N2 . 2.065(4) ?
Ni1 N2 7_566 2.065(4) ?
Ni2 O2 . 2.107(3) ?
Ni2 O2 7_666 2.107(3) ?
Ni2 N3 7_666 2.073(4) ?
Ni2 N3 . 2.073(4) ?
Ni2 N4 . 2.062(4) ?
Ni2 N4 7_666 2.062(4) ?
S1 O3 . 1.466(3) ?
S1 O2 . 1.476(3) ?
S1 O1 . 1.476(3) ?
S1 O4 . 1.491(4) ?
N3 H3 . 0.9800 ?
N3 C10 . 1.481(6) ?
N3 C6 . 1.476(6) ?
N1 H1 . 0.9800 ?
N1 C1 . 1.473(6) ?
N1 C5 . 1.462(6) ?
N2 H2 . 0.9800 ?
N2 C4 . 1.490(6) ?
N2 C3 . 1.473(6) ?
N4 H4 . 0.9800 ?
N4 C9 . 1.495(6) ?
N4 C8 . 1.472(6) ?
C30 C35 . 1.377(6) ?
C30 C31 . 1.395(6) ?
C30 C27 . 1.494(7) ?
O6 C11 . 1.194(5) ?
C11 O5 . 1.305(6) ?
C11 C12 . 1.492(7) ?
O8 C36 . 1.198(5) ?
C18 C15 . 1.498(6) ?
C18 C21 . 1.419(6) ?
C18 C19 . 1.391(5) ?
C15 C14 . 1.377(6) ?
C15 C16 . 1.377(7) ?
O5 H5 . 0.8200 ?
C35 H35 . 0.9300 ?
C35 C34 . 1.376(6) ?
O7 H7 . 0.8200 ?
O7 C36 . 1.302(5) ?
C24 C25 2_656 1.389(6) ?
C24 C25 . 1.389(6) ?
C24 C23 . 1.510(9) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C10 C9 7_666 1.519(7) ?
C12 C13 . 1.372(7) ?
C12 C17 . 1.376(6) ?
C33 C32 . 1.386(6) ?
C33 C34 . 1.381(5) ?
C33 C36 . 1.491(6) ?
C32 H32 . 0.9300 ?
C32 C31 . 1.365(6) ?
C29 H29A . 0.9600 ?
C29 H29B . 0.9600 ?
C29 H29C . 0.9602 ?
C29 C28 . 1.524(8) ?
C25 C26 . 1.526(6) ?
C25 C27 . 1.403(6) ?
C31 H31 . 0.9300 ?
C21 C23 . 1.388(5) ?
C21 C22 . 1.526(6) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 C1 . 1.530(7) ?
C2 C3 . 1.496(7) ?
C14 H14 . 0.9300 ?
C14 C13 . 1.378(7) ?
C19 C20 . 1.506(8) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C7 C6 . 1.510(7) ?
C7 C8 . 1.523(7) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C34 H34 . 0.9300 ?
C26 H26A . 0.9599 ?
C26 H26B . 0.9601 ?
C26 H26C . 0.9600 ?
C28 C27 2_656 1.391(5) ?
C28 C27 . 1.391(5) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C4 C5 7_566 1.503(7) ?
C13 H13 . 0.9300 ?
C17 H17 . 0.9300 ?
C17 C16 . 1.380(7) ?
C16 H16 . 0.9300 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C22 H22A . 0.9602 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9601 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9599 ?
C20 H20C . 0.9600 ?
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 O4 . 0.98 2.32 3.113(5) 138.0 yes
N2 H2 O3 . 0.98 2.42 3.267(4) 144.1 yes
N4 H4 O3 7_666 0.98 2.10 3.012(5) 154.1 yes
O5 H5 O4 . 0.82 1.79 2.597(5) 169.0 yes
O7 H7 O3 8_554 0.82 1.85 2.654(5) 166.4 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
Ni1 N1 C1 C2 . . . . -54.6(6) ?
Ni1 N1 C5 C4 . . . 7_566 40.7(4) ?
Ni1 N2 C4 C5 . . . 7_566 -41.7(5) ?
Ni1 N2 C3 C2 . . . . 56.4(6) ?
Ni2 N3 C10 C9 . . . 7_666 -42.8(5) ?
Ni2 N3 C6 C7 . . . . 55.0(5) ?
Ni2 N4 C9 C10 . . . 7_666 41.2(5) ?
Ni2 N4 C8 C7 . . . . -58.2(5) ?
O3 S1 O2 Ni2 . . . . -44.7(3) ?
O3 S1 O1 Ni1 . . . . -75.3(3) ?
O2 S1 O1 Ni1 . . . . 164.4(2) ?
O1 S1 O2 Ni2 . . . . 74.7(3) ?
O4 S1 O2 Ni2 . . . . -164.6(2) ?
O4 S1 O1 Ni1 . . . . 44.6(3) ?
C30 C35 C34 C33 . . . . 2.3(8) ?
O6 C11 C12 C13 . . . . -5.3(9) ?
O6 C11 C12 C17 . . . . 174.5(6) ?
C11 C12 C13 C14 . . . . -177.4(5) ?
C11 C12 C17 C16 . . . . 178.1(6) ?
C18 C15 C14 C13 . . . . 174.6(5) ?
C18 C15 C16 C17 . . . . -174.1(5) ?
C18 C21 C23 C24 . . . . 177.6(3) ?
C18 C21 C23 C21 . . . 2_656 -2.4(3) ?
C15 C18 C21 C23 . . . . -171.0(4) ?
C15 C18 C21 C22 . . . . 10.8(7) ?
C15 C18 C19 C18 . . . 2_656 173.3(5) ?
C15 C18 C19 C20 . . . . -6.7(5) ?
C15 C14 C13 C12 . . . . -0.3(9) ?
O5 C11 C12 C13 . . . . 174.5(6) ?
O5 C11 C12 C17 . . . . -5.7(8) ?
C35 C30 C31 C32 . . . . 0.8(8) ?
C35 C30 C27 C25 . . . . 101.0(6) ?
C35 C30 C27 C28 . . . . -75.5(6) ?
C24 C25 C27 C30 . . . . -173.8(4) ?
C24 C25 C27 C28 . . . . 2.6(7) ?
C10 N3 C6 C7 . . . . 177.0(4) ?
C12 C17 C16 C15 . . . . -1.0(10) ?
C33 C32 C31 C30 . . . . 0.1(9) ?
C32 C33 C34 C35 . . . . -1.3(7) ?
C32 C33 C36 O8 . . . . -6.3(9) ?
C32 C33 C36 O7 . . . . 174.6(5) ?
C29 C28 C27 C30 . . . . -4.9(5) ?
C29 C28 C27 C25 . . . . 178.7(3) ?
C25 C24 C25 C26 2_656 . . . 178.0(5) ?
C25 C24 C25 C27 2_656 . . . -1.3(3) ?
C25 C24 C23 C21 2_656 . . 2_656 102.8(3) ?
C25 C24 C23 C21 . . . . 102.8(3) ?
C25 C24 C23 C21 . . . 2_656 -77.2(3) ?
C25 C24 C23 C21 2_656 . . . -77.2(3) ?
C31 C30 C35 C34 . . . . -2.0(8) ?
C31 C30 C27 C25 . . . . -80.6(7) ?
C31 C30 C27 C28 . . . . 103.0(5) ?
C21 C18 C15 C14 . . . . -107.6(6) ?
C21 C18 C15 C16 . . . . 69.7(7) ?
C21 C18 C19 C18 . . . 2_656 -2.5(3) ?
C21 C18 C19 C20 . . . . 177.5(3) ?
C14 C15 C16 C17 . . . . 3.4(9) ?
C19 C18 C15 C14 . . . . 76.6(6) ?
C19 C18 C15 C16 . . . . -106.1(6) ?
C19 C18 C21 C23 . . . . 5.0(7) ?
C19 C18 C21 C22 . . . . -173.3(4) ?
C1 N1 C5 C4 . . . 7_566 169.2(4) ?
C1 C2 C3 N2 . . . . -70.0(6) ?
C34 C33 C32 C31 . . . . 0.2(8) ?
C34 C33 C36 O8 . . . . 170.1(5) ?
C34 C33 C36 O7 . . . . -9.0(8) ?
C26 C25 C27 C30 . . . . 6.9(8) ?
C26 C25 C27 C28 . . . . -176.8(4) ?
C36 C33 C32 C31 . . . . 176.7(5) ?
C36 C33 C34 C35 . . . . -177.8(5) ?
C6 N3 C10 C9 . . . 7_666 -170.7(4) ?
C6 C7 C8 N4 . . . . 73.2(7) ?
C27 C30 C35 C34 . . . . 176.6(5) ?
C27 C30 C31 C32 . . . . -177.7(5) ?
C27 C28 C27 C30 2_656 . . . 175.1(5) ?
C27 C28 C27 C25 2_656 . . . -1.3(3) ?
C23 C24 C25 C26 . . . . -2.0(5) ?
C23 C24 C25 C27 . . . . 178.7(3) ?
C4 N2 C3 C2 . . . . 177.7(5) ?
C13 C12 C17 C16 . . . . -2.1(9) ?
C17 C12 C13 C14 . . . . 2.8(9) ?
C16 C15 C14 C13 . . . . -2.8(8) ?
C5 N1 C1 C2 . . . . -178.3(5) ?
C3 N2 C4 C5 . . . 7_566 -168.6(4) ?
C3 C2 C1 N1 . . . . 69.3(6) ?
C9 N4 C8 C7 . . . . 179.5(4) ?
C22 C21 C23 C24 . . . . -4.2(5) ?
C22 C21 C23 C21 . . . 2_656 175.7(5) ?
C8 N4 C9 C10 . . . 7_666 169.0(5) ?
C8 C7 C6 N3 . . . . -71.6(7) ?