#------------------------------------------------------------------------------
#$Date: 2019-06-28 07:20:03 +0300 (Fri, 28 Jun 2019) $
#$Revision: 216610 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021690.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_2021690
loop_
_publ_author_name
'Wang, Xia'
'Ling, Ning'
'Li, Hanbing'
'Xiao, Xiaohe'
'Zhang, Yawen'
_publ_section_title
;
Synthesis, crystal structure and biological properties of Cd and Zn
coordination polymers based on a flexible tripodal ligand
;
_journal_coeditor_code FN3312
_journal_issue 7
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619008714
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac '[Cd3 (S C N)6 (C18 H21 N9)4], 3.5H2 O'
_chemical_formula_moiety 'C78 H84 Cd3 N42 S8, 3.5(H2 O)'
_chemical_formula_sum 'C78 H91 Cd3 N42 O3.5 S6'
_chemical_formula_weight 2202.48
_chemical_name_systematic
'Poly[[hexathiocyanatotetrakis{\m~3~-2,4,6-trimethyl-1,3,5-tris[(triazol-1-yl)methyl]benzene}tricadmium(II)] 3.5-hydrate]'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha 90
_cell_angle_beta 90.4848(12)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 24.1578(3)
_cell_length_b 16.1342(3)
_cell_length_c 24.0155(4)
_cell_measurement_reflns_used 7118
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.8880
_cell_measurement_theta_min 3.6730
_cell_volume 9360.1(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Agilent Xcalibur Eos Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0352
_diffrn_reflns_av_unetI/netI 0.0434
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 19725
_diffrn_reflns_theta_full 67.077
_diffrn_reflns_theta_max 67.077
_diffrn_reflns_theta_min 3.659
_diffrn_source 'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 7.253
_exptl_absorpt_correction_T_max 0.515
_exptl_absorpt_correction_T_min 0.269
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.563
_exptl_crystal_description prism
_exptl_crystal_F_000 4484
_exptl_crystal_size_max 0.3384
_exptl_crystal_size_mid 0.1933
_exptl_crystal_size_min 0.1611
_refine_diff_density_max 0.590
_refine_diff_density_min -0.620
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 620
_refine_ls_number_reflns 8329
_refine_ls_number_restraints 8
_refine_ls_restrained_S_all 1.026
_refine_ls_R_factor_all 0.0491
_refine_ls_R_factor_gt 0.0397
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+7.2542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1050
_refine_ls_wR_factor_ref 0.1138
_reflns_number_gt 6979
_reflns_number_total 8329
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file fn3312sup1.cif
_cod_data_source_block polymer1
_cod_original_cell_volume 9360.1(2)
_cod_original_formula_sum 'C78 H91 Cd3 N42 O3.50 S6'
_cod_database_code 2021690
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 -2 31719.9 689.175 2
0 0 -3 969.248 170.677 2
0 0 -4 225812. 2649.59 2
0 0 -5 357.074 188.335 2
0 0 -6 433933. 4597.73 2
0 0 -7-107.352 170.152 2
0 0 -8 194953. 3656.07 2
0 0 -8 213382. 3404.92 11
0 0 -9 296.108 204.442 11
0 0 -9 1279.50 372.825 6
0 0 -10 21294.4 1261.32 11
0 0 -10 21427.2 1366.45 6
0 0 -10 21526.4 1287.87 3
0 0 -11-8.48823 155.939 3
0 0 -11 49.8430 196.369 11
0 0 -11-93.3083 252.894 6
0 0 -12 169818. 3945.07 11
0 0 -12 171935. 4282.82 6
0 0 -12 180488. 4140.65 3
0 0 -13 2.24249 237.906 11
0 0 -13-11.7204 211.968 6
0 0 -13 178.035 133.555 3
0 0 -14 9401.82 1041.91 11
0 0 -14 10933.7 1121.56 3
0 0 -14 11252.9 1229.74 6
0 0 -14 8977.41 876.526 9
0 0 -15-223.927 219.459 11
0 0 -15 113.193 168.154 3
0 0 -15-457.690 297.628 6
0 0 -16 139206. 4693.29 6
0 0 -16 135722. 4327.60 11
0 0 -16 136440. 4300.21 3
0 0 -17-134.963 190.186 11
0 0 -17-13.3476 113.546 6
0 0 -17 47.0236 101.315 3
0 0 -18 22044.9 2030.03 6
0 0 -19 101.711 140.267 18
0 0 -20 59701.9 1940.75 18
0 0 -21-54.9275 151.022 18
0 0 -22 3996.09 514.374 18
0 0 -23 108.000 149.801 18
0 0 -24 55396.7 1888.22 18
0 0 -25 257.483 247.635 18
0 0 -26 930.880 259.079 18
0 0 -27 194.357 177.511 18
0 0 -28 7991.05 593.676 18
0 0 -28 8637.03 620.470 20
0 -2 0 30330.5 1132.49 1
0 -2 1 548.768 164.938 1
0 -2 2 338727. 3014.38 1
0 -2 -2 338817. 2536.43 2
0 2 -3 19953.4 632.630 7
0 -2 3 21917.1 780.783 1
0 -2 -3 22521.6 737.501 2
0 -2 -3 21034.0 740.185 6
0 2 -4 8939.86 419.971 3
0 -2 -4 8135.66 497.295 9
0 -2 -4 7623.06 494.055 6
0 -2 4 8151.96 507.268 1
0 -2 -4 7718.76 492.387 2
0 -2 -5 204009. 2814.46 6
0 -2 -5 210611. 2679.73 9
0 -2 -5 203051. 2758.40 2
0 -2 -6 103289. 2202.56 6
0 -2 -6 100456. 2187.71 2
0 -2 -7 26758.4 1219.88 2
0 -2 -7 26464.7 1208.55 6
0 -2 -8 32540.2 1444.16 6
0 -2 -8 34606.7 1516.31 2
0 -2 -8 34049.8 1269.02 9
0 2 -8 32888.4 1404.53 10
0 2 -9 17219.1 943.030 3
0 -2 -9 15445.1 908.387 9
0 -2 -9 16118.5 1123.74 2
0 -2 -9 15769.8 1075.11 6
0 -2 -10 140772. 2888.49 9
0 -2 -10 136447. 3364.17 6
0 2 -10 153100. 3019.65 3
0 -2 -10 137027. 3496.29 2
0 2 -10 148169. 3393.47 11
0 -2 -11 8176.60 871.007 6
0 -2 -11 9641.68 998.420 2
0 2 -11 8413.60 862.179 11
0 -2 -11 8675.63 763.793 9
0 2 -11 10273.5 834.304 3
0 -2 -12 51728.7 1945.71 9
0 -2 -12 52507.1 2452.62 2
0 2 -12 54874.1 2049.17 3
0 2 -12 50211.7 2434.72 6
0 2 -12 49736.1 2201.26 11
0 -2 -12 51099.5 2299.57 6
0 2 -13 21337.6 1675.46 6
0 2 -13 18689.4 1422.07 11
0 -2 -13 19853.9 1274.46 9
0 -2 -13 18554.2 1465.12 6
0 2 -13 20126.9 1306.97 3
0 -2 -14 70036.7 2504.84 9
0 2 -14 68766.2 2854.41 11
0 -2 -14 67405.9 2926.31 6
0 -2 -14 71964.0 3226.00 3
0 2 -14 70655.5 3203.61 6
0 2 -15 5936.18 986.679 6
0 -2 -15 6183.33 944.789 6
0 -2 -15 7719.57 1090.53 3
0 2 -15 6652.61 947.546 11
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0 -2 -16 2240.75 619.853 6
0 2 -16 1663.88 525.286 6
0 -2 -16 2720.65 694.175 3
0 -2 -17 5658.26 1023.10 3
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0 -2 -17 9181.58 1252.63 6
0 2 -17 4922.34 957.827 6
0 -2 -18 56711.7 3239.04 3
0 -2 -18 58213.5 1833.11 18
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0 -2 -20 13368.6 920.096 18
0 -2 -21 2365.57 422.792 18
0 2 -21 2613.20 426.257 18
0 2 -22 63469.7 2071.67 18
0 -2 -22 66056.5 2098.18 18
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0 2 -23 6705.81 685.863 18
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0 -2 -25 3503.81 501.745 18
0 2 -25 4339.87 537.837 18
0 -2 -26 16830.3 976.835 18
0 2 -26 17127.8 989.778 18
0 -2 -27 6421.74 550.682 20
0 2 -27 6064.32 557.527 18
0 -2 -27 5710.06 541.790 18
0 -2 -28 1577.17 269.098 18
0 2 -28 1560.23 291.409 18
0 -2 -28 2057.97 281.133 20
0 -4 0 142407. 3383.22 1
0 -4 1 92427.7 2656.09 1
0 -4 -1 92823.9 1672.72 5
0 -4 2 149.270 235.255 1
0 -4 -2 36.4366 94.8546 5
0 -4 3 59942.4 1948.07 1
0 4 -3 58107.0 1305.14 7
0 -4 -3 60072.1 1515.43 2
0 4 -4 30914.0 973.791 7
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0 -4 5 35546.7 1456.96 1
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0 4 -6 3623.36 498.435 10
0 -4 6 3264.84 458.149 1
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0 -4 7 75659.0 2214.61 1
0 4 -7 77335.7 2326.99 10
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0 -4 -19 7938.17 713.635 18
0 -4 -20 23226.5 1238.54 18
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0 4 -23 9601.86 806.488 18
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0 -6 -3 1748.30 347.287 2
0 -6 3 1263.58 452.088 1
0 -6 -3 2017.48 325.903 5
0 -6 3 1782.64 424.596 4
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0 6 -9 35737.6 1970.09 10
0 -6 9 35662.8 1971.09 1
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0 -6 10 25474.6 1711.50 1
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0 6 -27 3833.96 395.160 18
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0 8 -8 24356.0 1810.02 10
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0 8 -9 8056.62 1069.26 10
0 8 -10 9374.55 1153.38 10
0 -8 -10 9228.31 1101.02 4
0 -8 10 10493.9 1355.29 1
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0 -8 -18 5418.21 607.665 21
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0 -10 -13 26196.3 1293.10 21
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0 -10 -20 9090.80 728.814 21
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0 -12 -13 1723.56 352.594 21
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0 0 0 0.00 0.00 0
TITL 201901WX3 in C2/c
REM C2/c (#15 in standard setting)
CELL 1.54184 24.157816 16.134194 24.015549 90.0000 90.4848 90.0000
ZERR 4.00 0.000291 0.000271 0.000367 0.0000 0.0012 0.0000
LATT 7
SYMM -x, y,-z+1/2
SFAC C H N O S Cd
UNIT 312.00 368.00 168.00 12.00 24.00 12.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 5692
_shelx_res_file
;
TITL 201901WX3 in C2/c #15
201901wx3.res
created by SHELXL-2018/1 at 20:12:12 on 31-May-2019
REM reset to C2/c #15
CELL 1.54184 24.157816 16.134194 24.015549 90 90.4848 90
ZERR 4 0.000291 0.000271 0.000367 0 0.0012 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cd N O S
UNIT 312 364 12 168 14 24
EQIV $1 1.5-X,0.5-Y,1-Z
EQIV $2 +X,1-Y,0.5+Z
DFIX 0.88 O2 H2b O2 H2a
DFIX 0.88 O1 H1a O1 H1b
DANG 2.65 H2b N2_$2
DANG 2.5 S3 H2a
DANG 2.5 H1b S1_$1
DANG 2.1 H1a N2
L.S. 30 0 0
PLAN 30
MPLA C1 C2 C3 C4 C5 C6
MPLA C14 C13 N4 N5 N6
MPLA C15 C16 N7 N8 N9
MPLA C18 C17 N10 N11 N12
MPLA C19 C20 C21 C22 C23 C24
MPLA C31 C32 N13 N14 N15
MPLA C33 C34 N16 N17 N18
MPLA C35 C36 N19 N20 N21
HTAB O1 N2
HTAB O1 S1_$1
HTAB O2 S3
HTAB O2 N2_$2
conf
fmap 2
acta
REM
REM
REM
WGHT 0.062600 7.254200
FVAR 1.02169
C1 1 0.414009 0.341831 0.521996 11.00000 0.02867 0.03175 =
0.02449 -0.00334 -0.00495 0.00312
C2 1 0.383736 0.279949 0.549507 11.00000 0.02477 0.04405 =
0.02631 -0.00018 -0.00357 0.00578
C3 1 0.399247 0.197583 0.543474 11.00000 0.02596 0.03943 =
0.03290 0.00556 -0.00616 -0.00568
C4 1 0.441362 0.174992 0.506498 11.00000 0.02489 0.03350 =
0.03683 -0.00316 -0.00901 0.00404
C5 1 0.471046 0.237462 0.479010 11.00000 0.02030 0.03922 =
0.02600 -0.00686 -0.00492 0.00123
C6 1 0.458918 0.321090 0.488114 11.00000 0.02646 0.03322 =
0.02638 -0.00219 -0.00577 -0.00208
C7 1 0.397121 0.431408 0.529939 11.00000 0.03565 0.03502 =
0.02864 -0.00232 -0.00488 0.00998
AFIX 23
H7A 2 0.415918 0.465611 0.502788 11.00000 -1.20000
H7B 2 0.357590 0.436721 0.523478 11.00000 -1.20000
AFIX 0
C8 1 0.493993 0.388979 0.462818 11.00000 0.04236 0.04127 =
0.05846 -0.00129 0.00924 -0.00884
AFIX 137
H8A 2 0.527930 0.365670 0.449415 11.00000 -1.50000
H8B 2 0.502128 0.430123 0.490580 11.00000 -1.50000
H8C 2 0.474146 0.414157 0.432429 11.00000 -1.50000
AFIX 0
C9 1 0.515726 0.214385 0.437809 11.00000 0.02768 0.04823 =
0.03677 -0.00742 -0.00297 0.00806
AFIX 23
H9A 2 0.504648 0.164176 0.418496 11.00000 -1.20000
H9B 2 0.518642 0.258144 0.410291 11.00000 -1.20000
AFIX 0
C10 1 0.453057 0.084250 0.496198 11.00000 0.05111 0.03371 =
0.07553 -0.00498 0.00209 0.00167
AFIX 137
H10A 2 0.480595 0.078988 0.467830 11.00000 -1.50000
H10B 2 0.419657 0.057079 0.484255 11.00000 -1.50000
H10C 2 0.466346 0.059062 0.529970 11.00000 -1.50000
AFIX 0
C11 1 0.372126 0.131892 0.579108 11.00000 0.03206 0.04967 =
0.04005 0.01208 -0.00917 -0.00878
AFIX 23
H11A 2 0.334768 0.149055 0.588080 11.00000 -1.20000
H11B 2 0.369863 0.080344 0.558427 11.00000 -1.20000
AFIX 0
C12 1 0.335266 0.303867 0.585699 11.00000 0.03657 0.06138 =
0.04504 0.00542 0.01430 0.01268
AFIX 137
H12A 2 0.344168 0.292563 0.623986 11.00000 -1.50000
H12B 2 0.303269 0.272310 0.574816 11.00000 -1.50000
H12C 2 0.327630 0.361892 0.581242 11.00000 -1.50000
AFIX 0
C13 1 0.407877 0.536684 0.656563 11.00000 0.05974 0.04833 =
0.04095 -0.01504 -0.01079 0.02164
AFIX 43
H13 2 0.398809 0.579412 0.680825 11.00000 -1.20000
AFIX 0
C14 1 0.444032 0.429046 0.624877 11.00000 0.04266 0.03789 =
0.03824 -0.00656 -0.00977 0.01577
AFIX 43
H14 2 0.464997 0.381186 0.620465 11.00000 -1.20000
AFIX 0
C15 1 0.440620 0.145993 0.707390 11.00000 0.04674 0.06769 =
0.04284 -0.00211 -0.00467 0.01227
AFIX 43
H15 2 0.451358 0.173551 0.739733 11.00000 -1.20000
AFIX 0
C16 1 0.432735 0.053200 0.646603 11.00000 0.05058 0.04907 =
0.04802 0.00613 -0.00632 0.00667
AFIX 43
H16 2 0.435531 0.004111 0.626524 11.00000 -1.20000
AFIX 0
C17 1 0.633321 0.144571 0.510317 11.00000 0.03060 0.05959 =
0.09826 0.02593 -0.00609 0.00488
AFIX 43
H17 2 0.652739 0.107476 0.532776 11.00000 -1.20000
AFIX 0
C18 1 0.615605 0.246959 0.462050 11.00000 0.03264 0.04604 =
0.04303 0.01076 0.00265 0.00069
AFIX 43
H18 2 0.618139 0.297563 0.443706 11.00000 -1.20000
AFIX 0
C19 1 0.704925 0.696006 0.648006 11.00000 0.03404 0.03608 =
0.02649 -0.00132 0.00478 -0.00782
C20 1 0.741853 0.669234 0.689743 11.00000 0.03873 0.02943 =
0.02883 -0.00024 0.00724 -0.00138
C21 1 0.770250 0.728639 0.721468 11.00000 0.02668 0.03604 =
0.02273 0.00110 -0.00032 0.00496
C22 1 0.762640 0.813137 0.711780 11.00000 0.02897 0.03424 =
0.02724 -0.00533 0.00165 0.00047
C23 1 0.727794 0.838591 0.667612 11.00000 0.02239 0.03279 =
0.03324 0.00175 0.00600 0.00056
C24 1 0.699142 0.779569 0.635548 11.00000 0.02610 0.04080 =
0.02754 0.00362 0.00221 -0.00109
C25 1 0.667468 0.633374 0.619294 11.00000 0.04169 0.04314 =
0.03141 -0.00280 0.00299 -0.00969
AFIX 23
H25A 2 0.657790 0.653112 0.582323 11.00000 -1.20000
H25B 2 0.686887 0.581093 0.615436 11.00000 -1.20000
AFIX 0
C26 1 0.750410 0.577929 0.699571 11.00000 0.07640 0.03156 =
0.05221 -0.00011 -0.00947 -0.00035
AFIX 137
H26A 2 0.722404 0.557659 0.724209 11.00000 -1.50000
H26B 2 0.786269 0.569013 0.716032 11.00000 -1.50000
H26C 2 0.748013 0.548910 0.664736 11.00000 -1.50000
AFIX 0
C27 1 0.809275 0.700566 0.768282 11.00000 0.03067 0.04690 =
0.03034 -0.00066 0.00139 0.00702
AFIX 23
H27A 2 0.825268 0.647434 0.758496 11.00000 -1.20000
H27B 2 0.839256 0.740221 0.772025 11.00000 -1.20000
AFIX 0
C28 1 0.791883 0.876570 0.747656 11.00000 0.07575 0.04124 =
0.05348 -0.00537 -0.02405 -0.00574
AFIX 137
H28A 2 0.816139 0.909194 0.725009 11.00000 -1.50000
H28B 2 0.813091 0.848815 0.776035 11.00000 -1.50000
H28C 2 0.765018 0.912044 0.764740 11.00000 -1.50000
AFIX 0
C29 1 0.721153 0.928963 0.653046 11.00000 0.02592 0.03481 =
0.04890 0.00846 0.00715 -0.00016
AFIX 23
H29A 2 0.747537 0.961391 0.674541 11.00000 -1.20000
H29B 2 0.729240 0.936864 0.613909 11.00000 -1.20000
AFIX 0
C30 1 0.662786 0.807999 0.587746 11.00000 0.05101 0.05349 =
0.04316 0.01570 -0.01426 -0.00963
AFIX 137
H30A 2 0.624659 0.798613 0.596767 11.00000 -1.50000
H30B 2 0.671955 0.777399 0.554805 11.00000 -1.50000
H30C 2 0.668643 0.866048 0.581293 11.00000 -1.50000
AFIX 0
C31 1 0.600167 0.554443 0.679885 11.00000 0.04435 0.04411 =
0.05051 0.00818 -0.00061 -0.00799
AFIX 43
H31 2 0.619004 0.504205 0.681259 11.00000 -1.20000
AFIX 0
C32 1 0.542116 0.648682 0.690036 11.00000 0.04584 0.05924 =
0.04400 0.00728 0.00733 0.00351
AFIX 43
H32 2 0.510396 0.676546 0.701222 11.00000 -1.20000
AFIX 0
C33 1 0.788618 0.734618 0.868402 11.00000 0.03716 0.04813 =
0.03531 -0.00332 -0.00206 -0.00963
AFIX 43
H33 2 0.813576 0.778073 0.872747 11.00000 -1.20000
AFIX 0
C34 1 0.728696 0.644366 0.882438 11.00000 0.03688 0.04455 =
0.03532 -0.00023 0.00377 -0.00472
AFIX 43
H34 2 0.702493 0.611988 0.900429 11.00000 -1.20000
AFIX 0
C35 1 0.626672 0.929422 0.698403 11.00000 0.04142 0.04519 =
0.04572 0.01829 0.01432 0.00865
AFIX 43
H35 2 0.631524 0.883893 0.721686 11.00000 -1.20000
AFIX 0
C36 1 0.593954 1.031483 0.656464 11.00000 0.04028 0.04532 =
0.06456 0.02205 0.00709 0.01500
AFIX 43
H36 2 0.569331 1.072516 0.645019 11.00000 -1.20000
AFIX 0
C37 1 0.554578 0.317908 0.673513 11.00000 0.03842 0.04856 =
0.05712 0.00836 0.00561 0.01244
C38 1 0.762275 0.045666 0.483035 11.00000 0.03214 0.06252 =
0.04391 -0.00634 0.00108 0.01414
C39 1 0.576745 0.819230 0.807166 11.00000 0.06213 0.05106 =
0.04071 0.01488 -0.00247 -0.00773
CD1 3 0.500000 0.465138 0.750000 10.50000 0.03400 0.04008 =
0.02684 0.00000 -0.00257 0.00000
CD2 3 0.750000 0.250000 0.500000 10.50000 0.02667 0.03993 =
0.02817 0.00500 0.00127 0.00210
CD3 3 0.500000 0.963134 0.750000 10.50000 0.02751 0.03947 =
0.03127 0.00000 0.00140 0.00000
N1 4 0.554067 0.365259 0.708909 11.00000 0.06637 0.06561 =
0.05554 -0.00941 0.00031 0.01620
N2 4 0.775779 0.113835 0.477330 11.00000 0.06839 0.04354 =
0.07727 0.00002 0.00684 0.00681
N3 4 0.541463 0.866341 0.805722 11.00000 0.05886 0.06901 =
0.06647 0.02950 0.00613 0.01713
N4 4 0.442995 0.475132 0.670556 11.00000 0.04289 0.04423 =
0.03315 -0.00648 -0.01248 0.00893
N5 4 0.387447 0.531344 0.605676 11.00000 0.06352 0.04591 =
0.04313 -0.00853 -0.00687 0.02630
N6 4 0.410744 0.461303 0.586405 11.00000 0.03534 0.02859 =
0.03309 -0.00500 -0.00231 0.01071
N7 4 0.403845 0.118502 0.630847 11.00000 0.03468 0.04333 =
0.03891 0.00866 -0.00141 -0.00315
N8 4 0.408089 0.179446 0.669525 11.00000 0.05247 0.05774 =
0.04662 -0.00332 -0.00752 0.01419
N9 4 0.457248 0.067650 0.695258 11.00000 0.04279 0.05827 =
0.03778 0.00808 -0.00689 0.01089
N10 4 0.570499 0.201049 0.463497 11.00000 0.02560 0.03984 =
0.04241 0.00084 0.00285 0.00474
N11 4 0.580896 0.133672 0.496654 11.00000 0.04171 0.05400 =
0.11136 0.02378 -0.00746 0.00472
N12 4 0.656290 0.212339 0.489657 11.00000 0.02712 0.05077 =
0.04622 0.01034 -0.00214 -0.00150
N13 4 0.553281 0.569929 0.705529 11.00000 0.03980 0.05558 =
0.03873 0.00807 0.00145 -0.00718
N14 4 0.579603 0.683009 0.657861 11.00000 0.05314 0.04933 =
0.05113 0.00922 0.00500 -0.00144
N15 4 0.616691 0.620705 0.651819 11.00000 0.04202 0.03984 =
0.03374 -0.00093 0.00243 -0.01120
N16 4 0.780900 0.692913 0.821887 11.00000 0.02608 0.04010 =
0.03016 0.00231 -0.00419 0.00297
N17 4 0.741998 0.633176 0.829656 11.00000 0.04393 0.04176 =
0.03288 -0.00068 -0.00215 -0.00622
N18 4 0.756161 0.706432 0.908020 11.00000 0.03763 0.04628 =
0.02919 -0.00696 -0.00210 -0.00511
N19 4 0.664752 0.958847 0.664361 11.00000 0.03218 0.02869 =
0.04014 0.00896 0.00511 0.00505
N20 4 0.644123 1.025302 0.636674 11.00000 0.04273 0.04332 =
0.06992 0.02373 0.01085 0.01122
N21 4 0.580763 0.973824 0.694675 11.00000 0.03618 0.04525 =
0.04543 0.01115 0.00937 0.00892
S1 6 0.555699 0.251710 0.621967 11.00000 0.08006 0.05537 =
0.08367 -0.01601 0.01437 0.00530
S2 6 0.743976 -0.049941 0.492421 11.00000 0.05218 0.05993 =
0.07287 0.00403 -0.00321 -0.00897
S3 6 0.627915 0.753106 0.808794 11.00000 0.08274 0.06133 =
0.08371 0.01300 -0.00606 0.02031
O1 5 0.887430 0.073235 0.426834 11.00000 0.16442 0.09959 =
0.16326 0.03101 0.09840 0.01986
H1A 2 0.858198 0.090104 0.447150 11.00000 -1.50000
H1B 2 0.904547 0.115414 0.410302 11.00000 -1.50000
O2 5 0.677168 0.923114 0.871611 10.75000 0.23689 0.14057 =
0.17573 0.04460 -0.11176 -0.06421
H2A 2 0.666086 0.883022 0.848545 10.75000 -1.50000
H2B 2 0.696485 0.924611 0.903186 10.75000 -1.50000
HKLF 4
REM 201901WX3 in C2/c #15
REM R1 = 0.0397 for 6979 Fo > 4sig(Fo) and 0.0491 for all 8329 data
REM 620 parameters refined using 8 restraints
END
WGHT 0.0626 7.2463
REM Highest difference peak 0.590, deepest hole -0.620, 1-sigma level 0.086
Q1 1 0.7498 0.3163 0.5019 11.00000 0.05 0.59
Q2 1 0.5843 0.1192 0.4506 11.00000 0.05 0.53
Q3 1 0.4739 0.9643 0.7781 11.00000 0.05 0.52
Q4 1 0.6450 0.8022 0.8250 11.00000 0.05 0.51
Q5 1 0.7223 0.2532 0.4722 11.00000 0.05 0.51
Q6 1 0.7109 0.2825 0.4995 11.00000 0.05 0.50
Q7 1 0.7822 0.2546 0.4754 11.00000 0.05 0.50
Q8 1 0.7904 0.2796 0.4965 11.00000 0.05 0.49
Q9 1 0.4626 0.4461 0.7576 11.00000 0.05 0.47
Q10 1 0.5000 1.0256 0.7500 10.50000 0.05 0.46
Q11 1 0.5209 0.4734 0.7812 11.00000 0.05 0.46
Q12 1 0.4540 0.9477 0.7525 11.00000 0.05 0.44
Q13 1 0.4517 0.4633 0.7553 11.00000 0.05 0.44
Q14 1 0.8492 0.0853 0.3937 11.00000 0.05 0.43
Q15 1 0.5283 0.9637 0.7794 11.00000 0.05 0.41
Q16 1 0.5000 0.5248 0.7500 10.50000 0.05 0.39
Q17 1 0.5368 0.4907 0.7561 11.00000 0.05 0.39
Q18 1 0.8024 0.0971 0.4588 11.00000 0.05 0.37
Q19 1 0.7509 0.8286 0.6834 11.00000 0.05 0.36
Q20 1 0.5728 0.8832 0.8053 11.00000 0.05 0.35
Q21 1 0.5991 0.7173 0.8256 11.00000 0.05 0.34
Q22 1 0.4983 0.0630 0.7095 11.00000 0.05 0.34
Q23 1 0.6396 0.1152 0.4688 11.00000 0.05 0.34
Q24 1 0.6619 0.8627 0.8498 11.00000 0.05 0.33
Q25 1 0.4976 0.8596 0.7884 11.00000 0.05 0.33
Q26 1 0.4445 0.3261 0.5074 11.00000 0.05 0.32
Q27 1 0.4921 0.2248 0.4624 11.00000 0.05 0.31
Q28 1 0.4715 0.2174 0.5062 11.00000 0.05 0.31
Q29 1 0.4995 0.3728 0.7155 11.00000 0.05 0.31
Q30 1 0.7847 0.7165 0.7446 11.00000 0.05 0.30
;
_shelx_res_checksum 7156
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C1 0.41401(14) 0.3418(2) 0.52200(14) 0.0283(7) Uani d 1
C C2 0.38374(14) 0.2799(2) 0.54951(15) 0.0317(8) Uani d 1
C C3 0.39925(14) 0.1976(2) 0.54347(15) 0.0328(8) Uani d 1
C C4 0.44136(14) 0.1750(2) 0.50650(15) 0.0318(7) Uani d 1
C C5 0.47105(13) 0.2375(2) 0.47901(14) 0.0285(7) Uani d 1
C C6 0.45892(13) 0.3211(2) 0.48811(14) 0.0287(7) Uani d 1
C C7 0.39712(15) 0.4314(2) 0.52994(15) 0.0331(8) Uani d 1
H H7A 0.415918 0.465611 0.502788 0.040 Uiso calc 1
H H7B 0.357590 0.436721 0.523478 0.040 Uiso calc 1
C C8 0.49399(17) 0.3890(3) 0.46282(19) 0.0473(10) Uani d 1
H H8A 0.527930 0.365670 0.449415 0.071 Uiso calc 1
H H8B 0.502128 0.430123 0.490580 0.071 Uiso calc 1
H H8C 0.474146 0.414157 0.432429 0.071 Uiso calc 1
C C9 0.51573(15) 0.2144(3) 0.43781(17) 0.0376(8) Uani d 1
H H9A 0.504648 0.164176 0.418496 0.045 Uiso calc 1
H H9B 0.518642 0.258144 0.410291 0.045 Uiso calc 1
C C10 0.45306(19) 0.0843(3) 0.4962(2) 0.0534(11) Uani d 1
H H10A 0.480595 0.078988 0.467830 0.080 Uiso calc 1
H H10B 0.419657 0.057079 0.484255 0.080 Uiso calc 1
H H10C 0.466346 0.059062 0.529970 0.080 Uiso calc 1
C C11 0.37213(15) 0.1319(3) 0.57911(16) 0.0406(9) Uani d 1
H H11A 0.334768 0.149055 0.588080 0.049 Uiso calc 1
H H11B 0.369863 0.080344 0.558427 0.049 Uiso calc 1
C C12 0.33527(17) 0.3039(3) 0.58570(18) 0.0476(10) Uani d 1
H H12A 0.344168 0.292563 0.623986 0.071 Uiso calc 1
H H12B 0.303269 0.272310 0.574816 0.071 Uiso calc 1
H H12C 0.327630 0.361892 0.581242 0.071 Uiso calc 1
C C13 0.4079(2) 0.5367(3) 0.65656(18) 0.0497(11) Uani d 1
H H13 0.398809 0.579412 0.680825 0.060 Uiso calc 1
C C14 0.44403(16) 0.4290(3) 0.62488(16) 0.0397(9) Uani d 1
H H14 0.464997 0.381186 0.620465 0.048 Uiso calc 1
C C15 0.44062(18) 0.1460(3) 0.70739(19) 0.0525(11) Uani d 1
H H15 0.451358 0.173551 0.739733 0.063 Uiso calc 1
C C16 0.43274(18) 0.0532(3) 0.64660(19) 0.0493(10) Uani d 1
H H16 0.435531 0.004111 0.626524 0.059 Uiso calc 1
C C17 0.63332(17) 0.1446(3) 0.5103(3) 0.0629(14) Uani d 1
H H17 0.652739 0.107476 0.532776 0.075 Uiso calc 1
C C18 0.61560(16) 0.2470(3) 0.46205(17) 0.0406(9) Uani d 1
H H18 0.618139 0.297563 0.443706 0.049 Uiso calc 1
C C19 0.70493(15) 0.6960(2) 0.64801(15) 0.0322(8) Uani d 1
C C20 0.74185(15) 0.6692(2) 0.68974(15) 0.0323(7) Uani d 1
C C21 0.77025(14) 0.7286(2) 0.72147(14) 0.0285(7) Uani d 1
C C22 0.76264(14) 0.8131(2) 0.71178(14) 0.0301(7) Uani d 1
C C23 0.72779(13) 0.8386(2) 0.66761(15) 0.0294(7) Uani d 1
C C24 0.69914(14) 0.7796(2) 0.63555(15) 0.0315(7) Uani d 1
C C25 0.66747(16) 0.6334(3) 0.61929(16) 0.0387(8) Uani d 1
H H25A 0.657790 0.653112 0.582323 0.046 Uiso calc 1
H H25B 0.686887 0.581093 0.615436 0.046 Uiso calc 1
C C26 0.7504(2) 0.5779(3) 0.6996(2) 0.0534(11) Uani d 1
H H26A 0.722404 0.557659 0.724209 0.080 Uiso calc 1
H H26B 0.786269 0.569013 0.716032 0.080 Uiso calc 1
H H26C 0.748013 0.548910 0.664736 0.080 Uiso calc 1
C C27 0.80928(15) 0.7006(3) 0.76828(15) 0.0360(8) Uani d 1
H H27A 0.825268 0.647434 0.758496 0.043 Uiso calc 1
H H27B 0.839256 0.740221 0.772025 0.043 Uiso calc 1
C C28 0.7919(2) 0.8766(3) 0.7477(2) 0.0570(12) Uani d 1
H H28A 0.816139 0.909194 0.725009 0.085 Uiso calc 1
H H28B 0.813091 0.848815 0.776035 0.085 Uiso calc 1
H H28C 0.765018 0.912044 0.764740 0.085 Uiso calc 1
C C29 0.72115(14) 0.9290(2) 0.65305(17) 0.0365(8) Uani d 1
H H29A 0.747537 0.961391 0.674541 0.044 Uiso calc 1
H H29B 0.729240 0.936864 0.613909 0.044 Uiso calc 1
C C30 0.66279(19) 0.8080(3) 0.58775(19) 0.0493(11) Uani d 1
H H30A 0.624659 0.798613 0.596767 0.074 Uiso calc 1
H H30B 0.671955 0.777399 0.554805 0.074 Uiso calc 1
H H30C 0.668643 0.866048 0.581293 0.074 Uiso calc 1
C C31 0.60017(18) 0.5544(3) 0.67988(19) 0.0463(10) Uani d 1
H H31 0.619004 0.504205 0.681259 0.056 Uiso calc 1
C C32 0.54212(18) 0.6487(3) 0.69004(18) 0.0497(10) Uani d 1
H H32 0.510396 0.676546 0.701222 0.060 Uiso calc 1
C C33 0.78862(16) 0.7346(3) 0.86840(17) 0.0402(9) Uani d 1
H H33 0.813576 0.778073 0.872747 0.048 Uiso calc 1
C C34 0.72870(16) 0.6444(3) 0.88244(16) 0.0389(8) Uani d 1
H H34 0.702493 0.611988 0.900429 0.047 Uiso calc 1
C C35 0.62667(17) 0.9294(3) 0.69840(18) 0.0440(10) Uani d 1
H H35 0.631524 0.883893 0.721686 0.053 Uiso calc 1
C C36 0.59395(18) 1.0315(3) 0.6565(2) 0.0500(11) Uani d 1
H H36 0.569331 1.072516 0.645019 0.060 Uiso calc 1
C C37 0.55458(17) 0.3179(3) 0.6735(2) 0.0480(10) Uani d 1
C C38 0.76228(16) 0.0457(3) 0.48304(18) 0.0462(11) Uani d 1
C C39 0.5767(2) 0.8192(3) 0.80717(18) 0.0513(11) Uani d 1
Cd Cd1 0.500000 0.46514(2) 0.750000 0.03365(11) Uani d 1
Cd Cd2 0.750000 0.250000 0.500000 0.03159(10) Uani d 1
Cd Cd3 0.500000 0.96313(2) 0.750000 0.03274(10) Uani d 1
N N1 0.55407(18) 0.3653(3) 0.70891(18) 0.0625(11) Uani d 1
N N2 0.77578(19) 0.1138(3) 0.4773(2) 0.0630(11) Uani d 1
N N3 0.54146(18) 0.8663(3) 0.80572(19) 0.0647(12) Uani d 1
N N4 0.44300(14) 0.4751(2) 0.67056(14) 0.0402(8) Uani d 1
N N5 0.38745(16) 0.5313(2) 0.60568(15) 0.0509(10) Uani d 1
N N6 0.41074(12) 0.46130(18) 0.58640(13) 0.0324(7) Uani d 1
N N7 0.40385(13) 0.1185(2) 0.63085(14) 0.0390(7) Uani d 1
N N8 0.40809(16) 0.1794(3) 0.66952(16) 0.0523(9) Uani d 1
N N9 0.45725(14) 0.0677(3) 0.69526(15) 0.0463(8) Uani d 1
N N10 0.57050(12) 0.2010(2) 0.46350(14) 0.0359(7) Uani d 1
N N11 0.58090(16) 0.1337(3) 0.4967(2) 0.0691(13) Uani d 1
N N12 0.65629(13) 0.2123(2) 0.48966(15) 0.0414(8) Uani d 1
N N13 0.55328(14) 0.5699(2) 0.70553(14) 0.0447(8) Uani d 1
N N14 0.57960(16) 0.6830(3) 0.65786(16) 0.0512(9) Uani d 1
N N15 0.61669(13) 0.6207(2) 0.65182(13) 0.0385(7) Uani d 1
N N16 0.78090(12) 0.6929(2) 0.82189(13) 0.0321(6) Uani d 1
N N17 0.74200(14) 0.6332(2) 0.82966(13) 0.0395(7) Uani d 1
N N18 0.75616(13) 0.7064(2) 0.90802(13) 0.0377(7) Uani d 1
N N19 0.66475(12) 0.95885(19) 0.66436(13) 0.0336(7) Uani d 1
N N20 0.64412(15) 1.0253(2) 0.63667(18) 0.0519(10) Uani d 1
N N21 0.58076(13) 0.9738(2) 0.69467(15) 0.0422(8) Uani d 1
S S1 0.55570(7) 0.25171(9) 0.62197(7) 0.0730(4) Uani d 1
S S2 0.74398(5) -0.04994(9) 0.49242(6) 0.0617(3) Uani d 1
S S3 0.62792(7) 0.75311(10) 0.80879(7) 0.0760(4) Uani d 1
O O1 0.8874(3) 0.0732(4) 0.4268(3) 0.142(3) Uani d 1
H H1A 0.858(2) 0.090(7) 0.447(4) 0.213 Uiso d 1
H H1B 0.905(4) 0.115(4) 0.410(4) 0.213 Uiso d 1
O O2 0.6772(6) 0.9231(7) 0.8716(5) 0.185(5) Uani d 0.75
H H2A 0.666(8) 0.883(7) 0.849(5) 0.278 Uiso d 0.75
H H2B 0.696(6) 0.925(10) 0.903(4) 0.278 Uiso d 0.75
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0287(16) 0.0317(18) 0.0245(15) 0.0031(14) -0.0050(13) -0.0033(14)
C2 0.0248(16) 0.044(2) 0.0263(17) 0.0058(14) -0.0036(14) -0.0002(15)
C3 0.0260(16) 0.039(2) 0.0329(18) -0.0057(14) -0.0062(14) 0.0056(16)
C4 0.0249(15) 0.0335(19) 0.0368(18) 0.0040(14) -0.0090(14) -0.0032(15)
C5 0.0203(15) 0.0392(19) 0.0260(16) 0.0012(13) -0.0049(13) -0.0069(14)
C6 0.0265(15) 0.0332(18) 0.0264(16) -0.0021(14) -0.0058(13) -0.0022(14)
C7 0.0356(18) 0.0350(19) 0.0286(17) 0.0100(15) -0.0049(14) -0.0023(15)
C8 0.042(2) 0.041(2) 0.058(3) -0.0088(18) 0.0092(19) -0.001(2)
C9 0.0277(17) 0.048(2) 0.037(2) 0.0081(15) -0.0030(15) -0.0074(17)
C10 0.051(2) 0.034(2) 0.076(3) 0.0017(18) 0.002(2) -0.005(2)
C11 0.0321(18) 0.050(2) 0.040(2) -0.0088(17) -0.0092(16) 0.0121(18)
C12 0.037(2) 0.061(3) 0.045(2) 0.0127(19) 0.0143(18) 0.005(2)
C13 0.060(3) 0.048(3) 0.041(2) 0.022(2) -0.011(2) -0.0150(19)
C14 0.043(2) 0.038(2) 0.038(2) 0.0158(17) -0.0098(16) -0.0066(17)
C15 0.047(2) 0.068(3) 0.043(2) 0.012(2) -0.0047(19) -0.002(2)
C16 0.051(2) 0.049(2) 0.048(2) 0.007(2) -0.006(2) 0.006(2)
C17 0.031(2) 0.060(3) 0.098(4) 0.005(2) -0.006(2) 0.026(3)
C18 0.0326(19) 0.046(2) 0.043(2) 0.0007(17) 0.0027(16) 0.0108(18)
C19 0.0340(18) 0.0361(19) 0.0265(17) -0.0078(15) 0.0048(14) -0.0013(15)
C20 0.0387(18) 0.0294(18) 0.0288(17) -0.0014(15) 0.0072(14) -0.0002(14)
C21 0.0267(16) 0.0360(18) 0.0227(16) 0.0050(14) -0.0003(13) 0.0011(14)
C22 0.0290(16) 0.0342(18) 0.0272(16) 0.0005(14) 0.0016(13) -0.0053(15)
C23 0.0224(15) 0.0328(18) 0.0332(17) 0.0006(13) 0.0060(13) 0.0017(14)
C24 0.0261(16) 0.041(2) 0.0275(17) -0.0011(14) 0.0022(14) 0.0036(15)
C25 0.042(2) 0.043(2) 0.0314(18) -0.0097(17) 0.0030(16) -0.0028(16)
C26 0.076(3) 0.032(2) 0.052(3) 0.000(2) -0.009(2) -0.0001(19)
C27 0.0307(17) 0.047(2) 0.0303(18) 0.0070(16) 0.0014(15) -0.0007(16)
C28 0.076(3) 0.041(2) 0.053(3) -0.006(2) -0.024(2) -0.005(2)
C29 0.0259(16) 0.0348(19) 0.049(2) -0.0002(15) 0.0071(15) 0.0085(17)
C30 0.051(2) 0.053(3) 0.043(2) -0.010(2) -0.0143(19) 0.016(2)
C31 0.044(2) 0.044(2) 0.051(2) -0.0080(18) -0.0006(19) 0.0082(19)
C32 0.046(2) 0.059(3) 0.044(2) 0.004(2) 0.0073(19) 0.007(2)
C33 0.0372(19) 0.048(2) 0.035(2) -0.0096(17) -0.0021(16) -0.0033(17)
C34 0.0369(19) 0.045(2) 0.0353(19) -0.0047(17) 0.0038(16) -0.0002(17)
C35 0.041(2) 0.045(2) 0.046(2) 0.0086(18) 0.0143(18) 0.0183(19)
C36 0.040(2) 0.045(2) 0.065(3) 0.0150(18) 0.007(2) 0.022(2)
C37 0.038(2) 0.049(2) 0.057(3) 0.0124(19) 0.0056(19) 0.008(2)
C38 0.0321(19) 0.063(3) 0.044(2) 0.0141(19) 0.0011(17) -0.006(2)
C39 0.062(3) 0.051(3) 0.041(2) -0.008(2) -0.002(2) 0.015(2)
Cd1 0.03400(19) 0.0401(2) 0.02684(18) 0.000 -0.00257(14) 0.000
Cd2 0.02667(17) 0.0399(2) 0.02817(18) 0.00210(14) 0.00127(13) 0.00500(15)
Cd3 0.02751(18) 0.0395(2) 0.03127(18) 0.000 0.00140(13) 0.000
N1 0.066(3) 0.066(3) 0.056(2) 0.016(2) 0.000(2) -0.009(2)
N2 0.068(3) 0.044(2) 0.077(3) 0.007(2) 0.007(2) 0.000(2)
N3 0.059(2) 0.069(3) 0.066(3) 0.017(2) 0.006(2) 0.030(2)
N4 0.0429(17) 0.0442(19) 0.0331(16) 0.0089(15) -0.0125(14) -0.0065(15)
N5 0.064(2) 0.046(2) 0.0431(19) 0.0263(18) -0.0069(17) -0.0085(16)
N6 0.0353(15) 0.0286(15) 0.0331(16) 0.0107(12) -0.0023(13) -0.0050(12)
N7 0.0347(15) 0.0433(19) 0.0389(17) -0.0032(14) -0.0014(14) 0.0087(15)
N8 0.052(2) 0.058(2) 0.047(2) 0.0142(18) -0.0075(17) -0.0033(18)
N9 0.0428(18) 0.058(2) 0.0378(18) 0.0109(17) -0.0069(15) 0.0081(17)
N10 0.0256(15) 0.0398(17) 0.0424(18) 0.0047(13) 0.0029(13) 0.0008(14)
N11 0.042(2) 0.054(2) 0.111(4) 0.0047(19) -0.007(2) 0.024(3)
N12 0.0271(15) 0.051(2) 0.0462(19) -0.0015(14) -0.0021(14) 0.0103(16)
N13 0.0398(18) 0.056(2) 0.0387(18) -0.0072(16) 0.0014(14) 0.0081(16)
N14 0.053(2) 0.049(2) 0.051(2) -0.0014(17) 0.0050(17) 0.0092(18)
N15 0.0420(17) 0.0398(18) 0.0337(16) -0.0112(14) 0.0024(14) -0.0009(14)
N16 0.0261(14) 0.0401(17) 0.0302(15) 0.0030(12) -0.0042(12) 0.0023(13)
N17 0.0439(17) 0.0418(18) 0.0329(16) -0.0062(15) -0.0021(14) -0.0007(14)
N18 0.0376(16) 0.0463(19) 0.0292(15) -0.0051(14) -0.0021(13) -0.0070(14)
N19 0.0322(15) 0.0287(15) 0.0401(17) 0.0051(12) 0.0051(13) 0.0090(13)
N20 0.0427(19) 0.043(2) 0.070(3) 0.0112(16) 0.0108(18) 0.0237(19)
N21 0.0362(17) 0.045(2) 0.0454(19) 0.0089(15) 0.0094(14) 0.0111(16)
S1 0.0801(9) 0.0554(8) 0.0837(10) 0.0053(7) 0.0144(8) -0.0160(7)
S2 0.0522(6) 0.0599(7) 0.0729(8) -0.0090(5) -0.0032(6) 0.0040(6)
S3 0.0827(9) 0.0613(8) 0.0837(10) 0.0203(7) -0.0061(8) 0.0130(7)
O1 0.164(6) 0.100(4) 0.163(6) 0.020(4) 0.098(5) 0.031(4)
O2 0.237(12) 0.141(9) 0.176(10) -0.064(9) -0.112(9) 0.045(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 -5 -11 0.0842
15 -1 6 0.1250
14 -1 7 0.1315
6 6 -11 0.0691
-9 4 11 0.0952
-6 -9 4 0.0702
-2 -7 -12 0.0960
0 -1 -16 0.0921
-2 10 1 0.0329
-14 0 -7 0.1885
-15 3 1 0.1546
-3 5 14 0.1125
-11 1 11 0.0689
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
C2 C1 C7 . . 118.5(3)
C6 C1 C2 . . 120.8(3)
C6 C1 C7 . . 120.8(3)
C1 C2 C12 . . 119.8(4)
C3 C2 C1 . . 119.3(3)
C3 C2 C12 . . 121.0(4)
C2 C3 C4 . . 120.8(3)
C2 C3 C11 . . 119.5(3)
C4 C3 C11 . . 119.7(4)
C3 C4 C5 . . 119.1(3)
C3 C4 C10 . . 119.5(4)
C5 C4 C10 . . 121.4(3)
C4 C5 C9 . . 120.0(3)
C6 C5 C4 . . 120.7(3)
C6 C5 C9 . . 119.3(3)
C1 C6 C8 . . 119.9(3)
C5 C6 C1 . . 119.0(3)
C5 C6 C8 . . 121.1(3)
N6 C7 C1 . . 111.7(3)
N10 C9 C5 . . 113.9(3)
N7 C11 C3 . . 110.8(3)
N5 C13 N4 . . 114.4(4)
N4 C14 N6 . . 109.9(3)
N8 C15 N9 . . 114.2(4)
N7 C16 N9 . . 110.1(4)
N11 C17 N12 . . 114.9(4)
N12 C18 N10 . . 111.4(4)
C20 C19 C25 . . 119.5(3)
C24 C19 C20 . . 121.0(3)
C24 C19 C25 . . 119.4(3)
C19 C20 C26 . . 119.9(4)
C21 C20 C19 . . 118.9(3)
C21 C20 C26 . . 121.2(4)
C20 C21 C27 . . 119.6(3)
C22 C21 C20 . . 121.0(3)
C22 C21 C27 . . 119.4(3)
C21 C22 C23 . . 119.2(3)
C21 C22 C28 . . 120.5(3)
C23 C22 C28 . . 120.4(4)
C22 C23 C29 . . 121.2(3)
C24 C23 C22 . . 120.2(3)
C24 C23 C29 . . 118.5(3)
C19 C24 C23 . . 119.5(3)
C19 C24 C30 . . 121.0(4)
C23 C24 C30 . . 119.5(4)
N15 C25 C19 . . 110.3(3)
N16 C27 C21 . . 112.3(3)
N19 C29 C23 . . 111.8(3)
N13 C31 N15 . . 110.4(4)
N14 C32 N13 . . 114.9(4)
N16 C33 N18 . . 110.8(4)
N17 C34 N18 . . 114.6(4)
N21 C35 N19 . . 110.5(3)
N20 C36 N21 . . 114.8(4)
N1 C37 S1 . . 178.8(5)
N2 C38 S2 . . 178.7(5)
N3 C39 S3 . . 179.0(5)
N1 Cd1 N1 . 2_656 91.1(2)
N1 Cd1 N4 2_656 2_656 91.76(14)
N1 Cd1 N4 . . 91.76(14)
N1 Cd1 N4 . 2_656 93.75(14)
N1 Cd1 N4 2_656 . 93.75(14)
N1 Cd1 N13 . . 89.65(16)
N1 Cd1 N13 2_656 2_656 89.65(16)
N1 Cd1 N13 . 2_656 178.01(14)
N1 Cd1 N13 2_656 . 178.01(14)
N4 Cd1 N4 2_656 . 172.13(17)
N4 Cd1 N13 . 2_656 90.01(12)
N4 Cd1 N13 2_656 2_656 84.40(12)
N4 Cd1 N13 2_656 . 90.01(12)
N4 Cd1 N13 . . 84.40(12)
N13 Cd1 N13 . 2_656 89.62(19)
N2 Cd2 N2 . 7_656 180.0
N2 Cd2 N12 . 7_656 90.53(14)
N2 Cd2 N12 7_656 7_656 89.47(14)
N2 Cd2 N12 7_656 . 90.53(14)
N2 Cd2 N12 . . 89.47(14)
N12 Cd2 N12 . 7_656 180.0
N18 Cd2 N2 4_646 . 87.51(14)
N18 Cd2 N2 6_565 7_656 87.51(14)
N18 Cd2 N2 4_646 7_656 92.49(14)
N18 Cd2 N2 6_565 . 92.49(14)
N18 Cd2 N12 6_565 7_656 87.31(12)
N18 Cd2 N12 6_565 . 92.69(12)
N18 Cd2 N12 4_646 . 87.31(12)
N18 Cd2 N12 4_646 7_656 92.69(12)
N18 Cd2 N18 6_565 4_646 180.0
N3 Cd3 N3 2_656 . 93.7(3)
N3 Cd3 N9 2_656 1_565 88.54(17)
N3 Cd3 N9 . 1_565 177.60(16)
N3 Cd3 N9 . 2_666 88.54(17)
N3 Cd3 N9 2_656 2_666 177.60(16)
N3 Cd3 N21 2_656 2_656 91.10(13)
N3 Cd3 N21 . . 91.10(13)
N3 Cd3 N21 . 2_656 94.60(14)
N3 Cd3 N21 2_656 . 94.60(14)
N9 Cd3 N9 2_666 1_565 89.27(19)
N9 Cd3 N21 2_666 2_656 89.66(12)
N9 Cd3 N21 1_565 2_656 84.41(13)
N9 Cd3 N21 2_666 . 84.41(13)
N9 Cd3 N21 1_565 . 89.67(12)
N21 Cd3 N21 2_656 . 171.67(18)
C37 N1 Cd1 . . 142.8(4)
C38 N2 Cd2 . . 141.9(4)
C39 N3 Cd3 . . 142.8(4)
C13 N4 Cd1 . . 128.1(3)
C14 N4 C13 . . 102.9(3)
C14 N4 Cd1 . . 128.2(3)
C13 N5 N6 . . 102.7(3)
C14 N6 C7 . . 129.9(3)
C14 N6 N5 . . 110.0(3)
N5 N6 C7 . . 120.0(3)
C16 N7 C11 . . 129.1(4)
C16 N7 N8 . . 110.3(4)
N8 N7 C11 . . 120.5(3)
C15 N8 N7 . . 102.6(4)
C15 N9 Cd3 . 1_545 132.2(3)
C16 N9 C15 . . 102.8(4)
C16 N9 Cd3 . 1_545 123.6(3)
C18 N10 C9 . . 130.4(4)
C18 N10 N11 . . 108.3(3)
N11 N10 C9 . . 121.3(3)
C17 N11 N10 . . 102.1(4)
C17 N12 Cd2 . . 125.4(3)
C18 N12 C17 . . 103.1(3)
C18 N12 Cd2 . . 131.4(3)
C31 N13 C32 . . 102.7(4)
C31 N13 Cd1 . . 123.0(3)
C32 N13 Cd1 . . 133.1(3)
C32 N14 N15 . . 102.1(4)
C31 N15 C25 . . 129.5(4)
C31 N15 N14 . . 110.0(3)
N14 N15 C25 . . 120.5(3)
C33 N16 C27 . . 129.6(3)
C33 N16 N17 . . 109.8(3)
N17 N16 C27 . . 120.5(3)
C34 N17 N16 . . 102.0(3)
C33 N18 C34 . . 102.8(3)
C33 N18 Cd2 . 4_656 128.7(3)
C34 N18 Cd2 . 4_656 128.6(3)
C35 N19 C29 . . 130.2(3)
C35 N19 N20 . . 109.4(3)
N20 N19 C29 . . 120.4(3)
C36 N20 N19 . . 102.7(3)
C35 N21 C36 . . 102.5(3)
C35 N21 Cd3 . . 127.9(3)
C36 N21 Cd3 . . 129.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.406(5)
C1 C6 . 1.402(5)
C1 C7 . 1.514(5)
C2 C3 . 1.389(5)
C2 C12 . 1.514(5)
C3 C4 . 1.404(5)
C3 C11 . 1.515(5)
C4 C5 . 1.405(5)
C4 C10 . 1.512(5)
C5 C6 . 1.398(5)
C5 C9 . 1.517(5)
C6 C8 . 1.515(5)
C7 N6 . 1.474(4)
C9 N10 . 1.471(5)
C11 N7 . 1.470(5)
C13 N4 . 1.347(5)
C13 N5 . 1.317(5)
C14 N4 . 1.326(5)
C14 N6 . 1.326(5)
C15 N8 . 1.313(6)
C15 N9 . 1.359(6)
C16 N7 . 1.318(6)
C16 N9 . 1.326(6)
C17 N11 . 1.317(6)
C17 N12 . 1.324(6)
C18 N10 . 1.318(5)
C18 N12 . 1.306(5)
C19 C20 . 1.404(5)
C19 C24 . 1.388(5)
C19 C25 . 1.518(5)
C20 C21 . 1.400(5)
C20 C26 . 1.506(5)
C21 C22 . 1.395(5)
C21 C27 . 1.530(5)
C22 C23 . 1.410(5)
C22 C28 . 1.509(5)
C23 C24 . 1.403(5)
C23 C29 . 1.508(5)
C24 C30 . 1.511(5)
C25 N15 . 1.474(5)
C27 N16 . 1.469(5)
C29 N19 . 1.473(4)
C31 N13 . 1.318(6)
C31 N15 . 1.327(5)
C32 N13 . 1.351(6)
C32 N14 . 1.317(6)
C33 N16 . 1.316(5)
C33 N18 . 1.319(5)
C34 N17 . 1.323(5)
C34 N18 . 1.347(5)
C35 N19 . 1.324(5)
C35 N21 . 1.323(5)
C36 N20 . 1.309(6)
C36 N21 . 1.347(5)
C37 N1 . 1.143(6)
C37 S1 . 1.635(5)
C38 N2 . 1.156(6)
C38 S2 . 1.621(5)
C39 N3 . 1.142(6)
C39 S3 . 1.633(5)
Cd1 N1 2_656 2.302(4)
Cd1 N1 . 2.302(4)
Cd1 N4 . 2.349(3)
Cd1 N4 2_656 2.349(3)
Cd1 N13 . 2.383(4)
Cd1 N13 2_656 2.383(3)
Cd2 N2 7_656 2.349(4)
Cd2 N2 . 2.349(4)
Cd2 N12 7_656 2.355(3)
Cd2 N12 . 2.355(3)
Cd2 N18 4_646 2.324(3)
Cd2 N18 6_565 2.324(3)
Cd3 N3 2_656 2.283(4)
Cd3 N3 . 2.283(4)
Cd3 N9 2_666 2.370(4)
Cd3 N9 1_565 2.370(3)
Cd3 N21 2_656 2.376(3)
Cd3 N21 . 2.376(3)
N5 N6 . 1.346(4)
N7 N8 . 1.356(5)
N10 N11 . 1.369(5)
N14 N15 . 1.355(5)
N16 N17 . 1.360(5)
N19 N20 . 1.354(4)
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
O1 H1A N2 . 0.904(19) 2.16(3) 3.038(7) 164(9) yes
O1 H1B S1 7_656 0.891(19) 2.48(2) 3.356(6) 169(10) yes
O2 H2A S3 . 0.89(2) 2.48(3) 3.344(10) 164(12) yes
O2 H2B N2 6_566 0.89(2) 2.68(4) 3.518(11) 158(10) 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_4
_geom_torsion
C1 C2 C3 C4 . -5.8(5)
C1 C2 C3 C11 . 171.5(3)
C1 C7 N6 C14 . 15.4(6)
C1 C7 N6 N5 . -164.0(3)
C2 C1 C6 C5 . 4.2(5)
C2 C1 C6 C8 . -174.8(3)
C2 C1 C7 N6 . 71.2(4)
C2 C3 C4 C5 . 5.4(5)
C2 C3 C4 C10 . -173.4(4)
C2 C3 C11 N7 . -91.2(4)
C3 C4 C5 C6 . -0.1(5)
C3 C4 C5 C9 . -178.5(3)
C3 C11 N7 C16 . -111.6(5)
C3 C11 N7 N8 . 65.7(5)
C4 C3 C11 N7 . 86.1(4)
C4 C5 C6 C1 . -4.6(5)
C4 C5 C6 C8 . 174.4(3)
C4 C5 C9 N10 . -86.9(4)
C5 C9 N10 C18 . -107.5(5)
C5 C9 N10 N11 . 70.0(5)
C6 C1 C2 C3 . 0.9(5)
C6 C1 C2 C12 . -179.8(3)
C6 C1 C7 N6 . -108.6(4)
C6 C5 C9 N10 . 94.8(4)
C7 C1 C2 C3 . -178.9(3)
C7 C1 C2 C12 . 0.4(5)
C7 C1 C6 C5 . -176.0(3)
C7 C1 C6 C8 . 5.0(5)
C9 C5 C6 C1 . 173.8(3)
C9 C5 C6 C8 . -7.3(5)
C9 N10 N11 C17 . 179.5(4)
C10 C4 C5 C6 . 178.6(4)
C10 C4 C5 C9 . 0.3(5)
C11 C3 C4 C5 . -171.9(3)
C11 C3 C4 C10 . 9.3(5)
C11 N7 N8 C15 . -177.5(4)
C12 C2 C3 C4 . 174.9(3)
C12 C2 C3 C11 . -7.8(5)
C13 N5 N6 C7 . 178.4(4)
C13 N5 N6 C14 . -1.1(5)
C16 N7 N8 C15 . 0.3(5)
C18 N10 N11 C17 . -2.5(6)
C19 C20 C21 C22 . -0.6(5)
C19 C20 C21 C27 . 178.1(3)
C19 C25 N15 C31 . -111.5(5)
C19 C25 N15 N14 . 66.2(5)
C20 C19 C24 C23 . -4.3(5)
C20 C19 C24 C30 . 175.2(4)
C20 C19 C25 N15 . 85.4(4)
C20 C21 C22 C23 . -3.0(5)
C20 C21 C22 C28 . 177.7(4)
C20 C21 C27 N16 . -90.1(4)
C21 C22 C23 C24 . 3.0(5)
C21 C22 C23 C29 . -175.9(3)
C21 C27 N16 C33 . -116.0(4)
C21 C27 N16 N17 . 67.5(4)
C22 C21 C27 N16 . 88.6(4)
C22 C23 C24 C19 . 0.7(5)
C22 C23 C24 C30 . -178.9(3)
C22 C23 C29 N19 . -113.1(4)
C23 C29 N19 C35 . 22.4(6)
C23 C29 N19 N20 . -155.7(4)
C24 C19 C20 C21 . 4.3(5)
C24 C19 C20 C26 . -175.5(4)
C24 C19 C25 N15 . -89.7(4)
C24 C23 C29 N19 . 67.9(4)
C25 C19 C20 C21 . -170.8(3)
C25 C19 C20 C26 . 9.4(5)
C25 C19 C24 C23 . 170.7(3)
C25 C19 C24 C30 . -9.7(5)
C26 C20 C21 C22 . 179.3(4)
C26 C20 C21 C27 . -2.0(5)
C27 C21 C22 C23 . 178.3(3)
C27 C21 C22 C28 . -1.0(5)
C27 N16 N17 C34 . 177.3(3)
C28 C22 C23 C24 . -177.8(4)
C28 C22 C23 C29 . 3.3(5)
C29 C23 C24 C19 . 179.6(3)
C29 C23 C24 C30 . 0.0(5)
C29 N19 N20 C36 . 178.5(4)
C32 N14 N15 C25 . -178.3(3)
C32 N14 N15 C31 . -0.2(5)
C33 N16 N17 C34 . 0.2(4)
C35 N19 N20 C36 . 0.1(5)
N4 C13 N5 N6 . 0.7(6)
N4 C14 N6 C7 . -178.2(4)
N4 C14 N6 N5 . 1.2(5)
N5 C13 N4 C14 . 0.0(6)
N5 C13 N4 Cd1 . 170.4(3)
N6 C14 N4 C13 . -0.8(5)
N6 C14 N4 Cd1 . -171.1(3)
N7 C16 N9 C15 . 0.3(5)
N7 C16 N9 Cd3 1_545 168.1(3)
N8 C15 N9 C16 . -0.1(6)
N8 C15 N9 Cd3 1_545 -166.4(3)
N9 C15 N8 N7 . -0.1(5)
N9 C16 N7 C11 . 177.1(4)
N9 C16 N7 N8 . -0.4(5)
N10 C18 N12 C17 . -2.7(5)
N10 C18 N12 Cd2 . 174.4(3)
N11 C17 N12 C18 . 1.1(7)
N11 C17 N12 Cd2 . -176.3(4)
N12 C17 N11 N10 . 0.9(7)
N12 C18 N10 C9 . -178.8(4)
N12 C18 N10 N11 . 3.4(5)
N13 C31 N15 C25 . 177.0(4)
N13 C31 N15 N14 . -0.8(5)
N13 C32 N14 N15 . 1.1(5)
N14 C32 N13 C31 . -1.6(5)
N14 C32 N13 Cd1 . -169.1(3)
N15 C31 N13 C32 . 1.4(5)
N15 C31 N13 Cd1 . 170.5(3)
N16 C33 N18 C34 . 0.6(5)
N16 C33 N18 Cd2 4_656 178.7(3)
N17 C34 N18 C33 . -0.4(5)
N17 C34 N18 Cd2 4_656 -178.6(3)
N18 C33 N16 C27 . -177.3(3)
N18 C33 N16 N17 . -0.5(5)
N18 C34 N17 N16 . 0.1(5)
N19 C35 N21 C36 . -0.1(5)
N19 C35 N21 Cd3 . -173.6(3)
N20 C36 N21 C35 . 0.2(6)
N20 C36 N21 Cd3 . 173.5(3)
N21 C35 N19 C29 . -178.2(4)
N21 C35 N19 N20 . 0.0(5)
N21 C36 N20 N19 . -0.2(6)
_cod_database_fobs_code 2021690