#------------------------------------------------------------------------------
#$Date: 2021-03-05 20:42:13 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262767 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022324.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_2022324
loop_
_publ_author_name
'Marczak, Maria'
'Biereg, Kinga'
'Zadykowicz, Beata'
'Sikorski, Artur'
_publ_section_title
;
Structural characterization and theoretical calculations of the
monohydrate of the 1:2 cocrystal salt formed from acriflavine and
3,5-dinitrobenzoic acid
;
_journal_coeditor_code EF3011
_journal_issue 2
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 116
_journal_page_last 122
_journal_paper_doi 10.1107/S2053229621000681
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac
'C14 H14 N3 +, C7 H3 N2 O6 -, C7 H4 N2 O6, H2 O'
_chemical_formula_moiety
'C14 H14 N3 +, C7 H3 N2 O6 -, C7 H4 N2 O6, H2 O'
_chemical_formula_sum 'C28 H23 N7 O13'
_chemical_formula_weight 665.53
_chemical_name_common
;
Acriflavinium 3,5-dinitrobenzoate--3,5-dinitrobenzoic acid--water (1/1/1)
;
_chemical_name_systematic
'3,6-Diamino-10-methylacridin-10-ium 3,5-dinitrobenzoate--3,5-dinitrobenzoic acid--water (1/1/1)'
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary difmap
_audit_creation_method SHELXL-2017/1
_cell_angle_alpha 90
_cell_angle_beta 97.362(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.45320(17)
_cell_length_b 8.26902(19)
_cell_length_c 23.1876(6)
_cell_measurement_reflns_used 18663
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 25.000
_cell_measurement_theta_min 3.462
_cell_volume 1417.29(6)
_computing_cell_refinement
;
CrysAlis RED (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis CCD (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis RED (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976)
;
_computing_publication_material
;
SHELXL2017 (Sheldrick, 2015) , PLATON (Spek, 2020)
and Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 295(2)
_diffrn_detector_area_resol_mean 10.4002
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra Ruby CCD'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0263
_diffrn_reflns_av_unetI/netI 0.0192
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 18663
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 25.000
_diffrn_reflns_theta_min 3.462
_exptl_absorpt_coefficient_mu 0.126
_exptl_absorpt_correction_T_max 0.999
_exptl_absorpt_correction_T_min 0.951
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Rigaku OD, 2015)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.560
_exptl_crystal_description plate
_exptl_crystal_F_000 688
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.241
_refine_diff_density_min -0.167
_refine_ls_abs_structure_details
;
Flack x determined using 2143 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.2(2)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 455
_refine_ls_number_reflns 4966
_refine_ls_number_restraints 8
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0353
_refine_ls_R_factor_gt 0.0344
_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^)+(0.0454P)^2^+0.5024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0894
_refine_ls_wR_factor_ref 0.0901
_reflns_number_gt 4841
_reflns_number_total 4966
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ef3011sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022324.cif.'
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2022324
_cod_database_fobs_code 2022324
_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
;
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0 0 -4 294387. 3564.74 7
0 0 -5 30431.3 494.128 7
0 0 5 30738.1 480.438 3
0 0 -6 130280. 1620.39 7
0 0 6 116854. 1583.77 3
0 0 7 22831.2 425.333 3
0 0 -7 23458.5 444.950 7
0 0 -8 7297.19 231.285 7
0 0 8 7242.51 217.544 3
0 0 -9 15047.3 368.212 7
0 0 9 14510.9 344.911 3
0 0 -10 3130.52 155.395 3
0 0 10 2880.02 148.621 3
0 0 -10 2785.05 158.986 7
0 0 -11 80449.6 1200.54 3
0 0 -11 77565.1 1224.54 7
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0 0 12 4099.41 197.833 3
0 0 -12 3633.99 204.537 7
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0 0 13 4164.25 203.961 3
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0 0 -14 1842.05 154.546 7
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0 0 -15 1206.61 122.324 3
0 0 -15 1011.84 121.659 7
0 0 -16 2460.61 186.192 7
0 0 16 2815.53 202.438 7
0 0 16 2687.76 183.626 3
0 0 -16 2600.79 174.847 5
0 0 -16 2971.61 191.798 3
0 0 -17 1819.80 165.932 7
0 0 -17 1808.56 153.678 5
0 0 -17 1990.65 168.026 3
0 0 17 1637.88 149.861 3
0 0 18 6113.42 297.310 3
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0 0 -18 5934.75 309.126 7
0 0 19 9681.10 392.939 3
0 0 -19 9772.62 415.997 7
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0 0 -23 42554.5 1039.32 7
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0 0 -24 908.131 170.699 7
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0 0 -27 187.585 102.330 7
0 0 27 176.143 90.8912 6
0 0 28 1192.66 184.282 3
0 0 28 1132.03 178.194 6
0 0 -28 1261.11 192.247 7
0 0 -29 160.782 111.929 7
0 0 29 27.7672 80.2331 3
0 0 29 130.833 101.759 6
0 0 30 126.805 94.1778 6
0 1 -3 18666.2 308.760 7
0 1 3 17598.6 296.709 5
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0 -1 -3 18528.5 301.816 7
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0 1 4 174367. 2165.16 5
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0 -1 5 289198. 3497.65 6
0 1 5 289812. 3513.58 5
0 1 5 295105. 3447.16 2
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0 1 6 31384.4 428.491 2
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0 -1 6 29644.6 521.871 3
0 1 7 4175.19 146.998 5
0 -1 -7 4107.03 158.414 7
0 1 7 4001.92 97.8138 2
0 -1 7 4385.56 165.537 3
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0 -1 7 4393.08 151.724 6
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9 2 -2 620.835 134.076 6
9 -2 -2 426.948 122.253 6
-9 2 1 128.277 109.381 2
-9 -2 1 252.456 111.788 2
9 2 -1 132.901 108.461 4
9 -2 -1-10.9705 92.7152 4
9 2 -1 122.340 93.6244 6
9 -2 -1 145.981 116.571 6
-9 2 0 320.350 121.986 2
-9 -2 0 336.700 115.550 2
9 2 0 128.269 98.2131 4
9 -2 0 336.533 121.865 4
9 2 0 563.335 122.212 6
9 -2 0 614.186 153.834 6
-9 2 -1 263.362 113.426 2
-9 -2 -1 344.232 127.202 2
9 2 1 143.434 106.994 4
9 -2 1 144.885 89.0224 4
9 2 1 397.953 123.418 6
9 -2 1 93.6614 103.117 6
-9 -2 -2 678.688 158.443 2
9 -2 2 318.511 120.822 4
9 2 2 386.998 118.910 6
9 -2 2 375.760 128.139 6
9 -2 3 726.881 164.160 4
9 2 3 787.748 149.091 6
9 -2 3 795.829 169.170 6
9 2 4 7205.62 406.892 6
9 -2 4 6410.27 420.109 6
9 -2 4 6871.86 429.463 4
9 -2 5 428.064 155.305 4
9 2 5 492.319 137.666 6
9 -2 6 683.216 161.336 4
9 2 6 875.032 166.760 6
9 2 7 4702.86 347.769 6
9 -2 7 4615.61 357.060 4
9 2 8 424.297 139.007 6
9 2 9 2200.47 260.491 6
-9 3 16 273.080 111.605 2
-9 3 15 1196.06 187.152 2
-9 3 15 1122.78 184.785 3
-9 3 14 294.128 117.109 2
9 -3 -14 292.280 130.372 4
-9 3 14 249.354 139.737 3
-9 3 13 1973.08 233.528 2
9 -3 -13 1685.52 223.302 4
-9 3 13 1778.58 217.516 3
-9 3 12 881.485 166.072 2
9 -3 -12 818.366 178.463 4
9 -3 -12 815.984 167.273 7
-9 3 12 914.823 158.949 3
-9 3 11 380.311 113.541 2
9 -3 -11 686.748 168.183 4
9 -3 -11 656.929 157.361 7
-9 3 11 635.682 146.979 3
-9 3 10 899.456 164.206 2
-9 -3 10 1169.44 183.193 2
9 -3 -10 931.103 164.467 4
9 -3 -10 1169.34 198.979 7
-9 3 10 1100.38 182.413 3
-9 3 9 116.571 90.6155 2
-9 -3 9 322.587 127.461 2
9 -3 -9 168.775 114.954 4
9 -3 -9 221.171 111.962 7
-9 3 9 283.702 104.081 3
-9 -3 8 1297.03 204.308 2
9 -3 -8 998.173 182.179 4
-9 3 8 1250.88 177.300 3
9 -3 -8 1060.02 182.290 7
-9 3 8 902.417 173.989 2
9 -3 -7 6149.35 393.870 4
-9 3 7 6223.05 421.286 2
-9 -3 7 6909.10 442.016 2
9 -3 -7 6716.22 415.330 7
9 -3 -6 1900.82 234.917 4
-9 -3 6 1490.57 210.213 2
9 -3 -6 1957.68 244.641 7
-9 3 6 1478.16 213.317 2
9 -3 -5 1053.54 182.318 4
9 -3 -5 1212.88 193.417 7
-9 3 5 1087.80 183.128 2
9 -3 -4 1505.52 203.777 4
9 -3 -4 1604.91 215.589 7
-9 3 4 1135.94 188.267 2
9 -3 -3 384.025 103.078 4
9 -3 -2 151.261 101.503 4
9 -3 -1 3260.89 279.329 4
9 -3 -1 3243.64 302.013 6
9 -3 0 1673.19 216.116 4
9 -3 0 1957.83 245.265 6
9 -3 1 87.6789 87.7957 4
9 -3 1 171.929 105.854 6
9 -3 2 814.257 175.186 4
9 -3 3 1086.38 181.037 4
9 3 3 1078.88 164.837 6
9 -3 4 315.747 117.823 4
9 3 4 463.032 135.554 6
9 3 5 2957.55 263.592 6
9 -3 5 2780.11 278.437 4
9 -3 6 1483.92 215.953 4
9 3 6 1676.29 216.213 6
9 -3 7 1348.23 205.600 4
9 3 7 947.376 171.891 6
9 3 8 4934.93 347.680 6
9 -4 -13 107.482 109.991 4
-9 4 13 227.089 123.347 3
9 -4 -12 1616.01 214.897 4
-9 4 12 1798.26 233.742 3
9 -4 -11 1716.73 221.598 4
-9 4 11 1623.03 219.022 3
9 -4 -10 1292.15 193.454 4
9 -4 -9 1654.69 205.352 4
9 -4 -8 341.573 129.809 4
9 -4 -7 2265.97 244.338 4
9 -4 -6 948.065 162.664 4
9 -4 -5 2062.42 228.250 4
9 -4 -5 2401.09 274.399 7
9 -4 -4 4968.51 341.962 4
9 -4 -3 32.0205 99.1604 4
9 -4 -2 422.390 117.647 4
9 -4 -1 482.124 121.482 4
9 -4 0 1379.85 186.545 4
9 -4 1 600.587 130.757 4
9 -4 2 951.703 170.839 4
9 -4 3 795.174 163.762 4
9 -4 4 4084.16 320.912 4
9 -4 5 258.655 116.504 4
9 -4 6 200.413 122.380 4
10 0 -2 303.576 133.806 6
10 0 -1 55.5322 100.924 6
10 0 0 596.240 171.625 6
10 0 1 12016.5 568.571 6
10 -1 -8 885.941 176.251 7
10 -1 -7 1571.33 207.231 7
10 -1 -6 984.028 171.157 7
10 1 -2 2279.70 237.883 6
10 1 -1 1251.46 187.715 6
10 1 0 111.186 111.069 6
10 1 1 1846.12 226.043 6
10 1 2 1357.21 195.293 6
10 -2 -8 1116.10 180.485 7
10 -2 -7 1502.48 210.877 7
10 -2 -6 809.889 156.581 7
10 -2 -5 1134.67 193.953 7
10 -2 -4 1861.20 230.098 7
10 -2 -3 401.708 124.772 7
10 -2 -2 160.616 124.642 7
0 0 0 0.00 0.00 0
TITL ACF in P2(1)
REM P2(1) (#11 in standard setting)
CELL 0.71073 7.453196 8.269018 23.187633 90.0000 97.3620 90.0000
ZERR 2.00 0.000167 0.000194 0.000628 0.0000 0.0022 0.0000
LATT 1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 56 46 14 26
TREF
HKLF 4
END
;
_shelx_hkl_checksum 45166
_shelx_res_file
;
TITL ACF in P2(1)
acf.res
created by SHELXL-2017/1 at 09:41:26 on 19-Mar-2020
REM P2(1) (#11 in standard setting)
CELL 0.71073 7.453196 8.269018 23.187633 90.0000 97.3620 90.0000
ZERR 2.00 0.000167 0.000194 0.000628 0.0000 0.0022 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 56 46 14 26
L.S. 20
BOND$h
conf
omit -2 50
acta 50
FMAP 2
PLAN 20
dfix o1w h1w 0.85
dfix o1w h2w 0.85
dfix n15 h15a 0.86
dfix n15 h15b 0.86
dfix n17 h17a 0.86
dfix n17 h17b 0.86
dfix O25b h25b 0.98 0.01
omit -6 0 17
omit -2 0 13
WGHT 0.045400 0.502400
FVAR 6.71823
O1W 4 -0.253496 0.035289 0.347538 11.00000 0.03840 0.07370 =
0.05078 -0.00281 -0.00342 0.00813
H2W 2 -0.357011 0.045730 0.326766 11.00000 -1.50000
H1W 2 -0.174539 -0.015731 0.326496 11.00000 -1.50000
C1 1 -0.005634 0.459191 0.218295 11.00000 0.03854 0.04699 =
0.03923 -0.01264 -0.01270 0.01283
AFIX 43
H1A 2 -0.094647 0.469846 0.186540 11.00000 -1.20000
AFIX 0
C2 1 -0.040026 0.365399 0.263115 11.00000 0.03071 0.04925 =
0.05284 -0.01783 -0.00238 0.00523
AFIX 43
H2A 2 -0.149889 0.311245 0.261609 11.00000 -1.20000
AFIX 0
C3 1 0.093408 0.349382 0.313154 11.00000 0.03982 0.03983 =
0.04128 -0.00937 0.00042 0.01166
C4 1 0.259033 0.427325 0.313074 11.00000 0.02824 0.03989 =
0.04064 -0.01321 -0.00511 0.00827
AFIX 43
H4A 2 0.346847 0.415927 0.345125 11.00000 -1.20000
AFIX 0
C5 1 0.667782 0.765320 0.219741 11.00000 0.03525 0.03927 =
0.02688 -0.00971 -0.00867 0.00976
AFIX 43
H5A 2 0.756458 0.750124 0.251324 11.00000 -1.20000
AFIX 0
C6 1 0.706030 0.861850 0.173624 11.00000 0.04901 0.03959 =
0.02530 -0.00484 0.00124 0.01391
C7 1 0.568566 0.882854 0.124755 11.00000 0.04794 0.04368 =
0.02833 -0.00236 -0.00047 0.01391
AFIX 43
H7A 2 0.591623 0.946237 0.093398 11.00000 -1.20000
AFIX 0
C8 1 0.406616 0.810855 0.124375 11.00000 0.05228 0.03965 =
0.02499 -0.00823 -0.00864 0.02082
AFIX 43
H8A 2 0.319427 0.825608 0.092351 11.00000 -1.20000
AFIX 0
C9 1 0.197741 0.638510 0.171884 11.00000 0.04489 0.04055 =
0.03243 -0.01357 -0.01329 0.01794
AFIX 43
H9A 2 0.108400 0.654003 0.140510 11.00000 -1.20000
AFIX 0
N10 3 0.461053 0.595954 0.265567 11.00000 0.02994 0.03473 =
0.03470 -0.00953 -0.00877 0.00264
C11 1 0.160350 0.542335 0.217444 11.00000 0.02977 0.03908 =
0.04190 -0.01866 -0.00749 0.00919
C12 1 0.296585 0.520677 0.266990 11.00000 0.03575 0.02860 =
0.03262 -0.01315 -0.00478 0.01160
C13 1 0.363690 0.712593 0.171354 11.00000 0.03403 0.03577 =
0.03411 -0.01437 -0.01075 0.00790
C14 1 0.501235 0.691473 0.219758 11.00000 0.04383 0.02780 =
0.02441 -0.00931 -0.00553 0.01232
N15 3 0.055823 0.263653 0.359709 11.00000 0.03692 0.06112 =
0.04870 -0.00348 -0.00372 -0.00133
H15B 2 0.134093 0.240322 0.388553 11.00000 -1.20000
H15A 2 -0.043052 0.204050 0.358119 11.00000 -1.20000
C16 1 0.596907 0.577821 0.316778 11.00000 0.03833 0.06940 =
0.03360 0.00780 -0.01005 -0.00404
AFIX 127
H16A 2 0.547681 0.513918 0.345548 10.50000 -1.50000
H16B 2 0.629892 0.682553 0.332578 10.50000 -1.50000
H16C 2 0.702102 0.525118 0.305738 10.50000 -1.50000
H16D 2 0.705436 0.633808 0.310361 10.50000 -1.50000
H16E 2 0.623225 0.465173 0.323331 10.50000 -1.50000
H16F 2 0.551015 0.622608 0.350171 10.50000 -1.50000
AFIX 0
N17 3 0.866852 0.933584 0.173491 11.00000 0.03922 0.06522 =
0.03388 0.00307 -0.00173 0.00126
H17A 2 0.943281 0.935375 0.205198 11.00000 -1.20000
H17B 2 0.876408 0.984820 0.136751 11.00000 -1.20000
C18A 1 1.208680 0.805010 0.384221 11.00000 0.02646 0.02114 =
0.02508 -0.00504 0.00378 0.00268
C18B 1 1.374618 1.253784 0.146634 11.00000 0.02284 0.02400 =
0.03176 -0.00560 0.00723 0.00124
C19A 1 1.369032 0.820639 0.421964 11.00000 0.02391 0.01838 =
0.03581 -0.00583 0.00704 0.00100
AFIX 43
H19A 2 1.468498 0.873246 0.410208 11.00000 -1.20000
AFIX 0
C19B 1 1.207116 1.239291 0.113303 11.00000 0.02592 0.02769 =
0.04349 -0.00897 0.00402 -0.00072
AFIX 43
H19B 2 1.116807 1.176785 0.126405 11.00000 -1.20000
AFIX 0
C20A 1 1.376996 0.756200 0.477285 11.00000 0.02382 0.02058 =
0.03217 -0.00430 -0.00383 0.00319
C20B 1 1.175819 1.317196 0.061277 11.00000 0.02895 0.03130 =
0.04066 -0.01252 -0.00588 0.00134
C21A 1 1.233998 0.678623 0.497539 11.00000 0.02797 0.01978 =
0.02879 0.00209 -0.00055 0.00178
AFIX 43
H21A 2 1.241106 0.639468 0.535361 11.00000 -1.20000
AFIX 0
C21B 1 1.306373 1.411004 0.039192 11.00000 0.04460 0.03072 =
0.02547 -0.00709 -0.00491 0.00874
AFIX 43
H21B 2 1.282852 1.463916 0.003634 11.00000 -1.20000
AFIX 0
C22A 1 1.079582 0.662563 0.458282 11.00000 0.02589 0.02298 =
0.02789 -0.00082 0.00122 -0.00273
C22B 1 1.472285 1.421219 0.072854 11.00000 0.03368 0.02048 =
0.03130 -0.00375 0.00743 -0.00084
C23A 1 1.063646 0.723017 0.402470 11.00000 0.02377 0.02378 =
0.02655 -0.00438 -0.00076 -0.00205
AFIX 43
H23A 2 0.957047 0.709024 0.377368 11.00000 -1.20000
AFIX 0
C23B 1 1.509123 1.345603 0.126201 11.00000 0.02458 0.02507 =
0.02683 -0.00390 0.00239 0.00017
AFIX 43
H23B 2 1.622172 1.356047 0.148063 11.00000 -1.20000
AFIX 0
C24A 1 1.188847 0.879986 0.324631 11.00000 0.02751 0.02506 =
0.02886 -0.00415 0.00648 0.00079
C24B 1 1.411967 1.171842 0.205263 11.00000 0.02802 0.02616 =
0.03263 -0.00282 0.00824 0.00209
O25A 4 1.332532 0.941341 0.309736 11.00000 0.03008 0.04305 =
0.03529 0.00533 0.01028 -0.00240
O25B 4 1.277798 1.082934 0.216717 11.00000 0.03271 0.03679 =
0.03493 0.00196 0.01053 -0.00650
H25B 2 1.305835 1.026638 0.254316 11.00000 -1.50000
O26A 4 1.038059 0.878461 0.295178 11.00000 0.03549 0.04574 =
0.02403 0.00259 0.00078 -0.00755
O26B 4 1.554021 1.193337 0.236188 11.00000 0.02945 0.03993 =
0.03654 0.00720 0.00161 0.00011
N27A 3 1.545117 0.773868 0.517780 11.00000 0.02547 0.02576 =
0.04816 0.00174 -0.00723 -0.00001
N27B 3 0.999524 1.297745 0.025411 11.00000 0.03991 0.05028 =
0.06106 -0.01672 -0.01837 0.00453
O28A 4 1.673060 0.842464 0.500335 11.00000 0.02998 0.03602 =
0.07271 0.01591 -0.01242 -0.00793
O28B 4 0.884077 1.217767 0.045796 11.00000 0.03490 0.05210 =
0.10828 -0.01740 -0.02311 -0.00789
O29A 4 1.549934 0.716207 0.566735 11.00000 0.04159 0.05502 =
0.04163 0.00844 -0.01284 -0.00399
O29B 4 0.977251 1.362838 -0.022192 11.00000 0.05982 0.10287 =
0.06095 -0.00453 -0.03444 0.00277
N30A 3 0.924149 0.577795 0.477532 11.00000 0.02828 0.03440 =
0.03189 0.00490 -0.00119 -0.00626
N30B 3 1.615479 1.517532 0.051119 11.00000 0.04914 0.02756 =
0.02711 0.00117 0.00860 -0.00162
O31A 4 0.796947 0.542294 0.440795 11.00000 0.03497 0.06017 =
0.03507 0.01080 -0.00600 -0.02111
O31B 4 1.757324 1.537345 0.082944 11.00000 0.04020 0.04433 =
0.03950 0.00132 0.00353 -0.01049
O32A 4 0.929172 0.548225 0.529262 11.00000 0.04024 0.04986 =
0.03183 0.01671 0.00028 -0.01138
O32B 4 1.583747 1.572421 0.001804 11.00000 0.07337 0.04885 =
0.03323 0.01103 0.00305 -0.01214
HKLF 4
REM ACF in P2(1)
REM R1 = 0.0344 for 4841 Fo > 4sig(Fo) and 0.0353 for all 4966 data
REM 455 parameters refined using 8 restraints
END
WGHT 0.0458 0.4972
REM Highest difference peak 0.241, deepest hole -0.167, 1-sigma level 0.035
Q1 1 0.8714 0.9581 0.1257 11.00000 0.05 0.24
Q2 1 -0.1358 0.1379 0.3481 11.00000 0.05 0.19
Q3 1 0.8747 1.0333 0.1403 11.00000 0.05 0.19
Q4 1 0.6527 0.7869 0.1819 11.00000 0.05 0.17
Q5 1 1.3802 0.7390 0.4471 11.00000 0.05 0.17
Q6 1 0.3756 0.5819 0.2885 11.00000 0.05 0.17
Q7 1 0.2802 0.6710 0.1903 11.00000 0.05 0.17
Q8 1 -0.1145 0.2994 0.2783 11.00000 0.05 0.16
Q9 1 0.2089 0.4791 0.2839 11.00000 0.05 0.16
Q10 1 -0.0208 0.2852 0.3195 11.00000 0.05 0.16
Q11 1 -0.0242 0.5264 0.1786 11.00000 0.05 0.16
Q12 1 1.2018 1.0626 0.1910 11.00000 0.05 0.15
Q13 1 0.1190 0.6082 0.1909 11.00000 0.05 0.15
Q14 1 0.0958 0.5178 0.2373 11.00000 0.05 0.15
Q15 1 1.1847 0.6335 0.4663 11.00000 0.05 0.14
Q16 1 1.1013 0.6417 0.4226 11.00000 0.05 0.14
Q17 1 0.2476 0.5732 0.2351 11.00000 0.05 0.14
Q18 1 1.4740 1.5566 -0.0190 11.00000 0.05 0.14
Q19 1 1.2079 0.8057 0.3532 11.00000 0.05 0.14
Q20 1 1.0448 1.3961 -0.0463 11.00000 0.05 0.13
;
_shelx_res_checksum 67064
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1W -0.2535(3) 0.0353(4) 0.34754(12) 0.0551(7) Uani d 1 . .
H H2W -0.357(4) 0.046(7) 0.3268(19) 0.083 Uiso d 1 . .
H H1W -0.175(6) -0.016(6) 0.326(2) 0.083 Uiso d 1 . .
C C1 -0.0056(4) 0.4592(5) 0.21829(15) 0.0431(9) Uani d 1 . .
H H1A -0.094647 0.469846 0.186540 0.052 Uiso calc 1 . .
C C2 -0.0400(4) 0.3654(5) 0.26311(16) 0.0449(9) Uani d 1 . .
H H2A -0.149889 0.311245 0.261609 0.054 Uiso calc 1 . .
C C3 0.0934(5) 0.3494(4) 0.31315(15) 0.0407(8) Uani d 1 . .
C C4 0.2590(4) 0.4273(4) 0.31307(14) 0.0371(7) Uani d 1 . .
H H4A 0.346847 0.415927 0.345125 0.045 Uiso calc 1 . .
C C5 0.6678(4) 0.7653(4) 0.21974(13) 0.0349(7) Uani d 1 . .
H H5A 0.756458 0.750124 0.251324 0.042 Uiso calc 1 . .
C C6 0.7060(5) 0.8619(4) 0.17362(13) 0.0383(7) Uani d 1 . .
C C7 0.5686(5) 0.8829(5) 0.12475(14) 0.0405(8) Uani d 1 . .
H H7A 0.591623 0.946237 0.093398 0.049 Uiso calc 1 . .
C C8 0.4066(5) 0.8109(4) 0.12438(13) 0.0402(8) Uani d 1 . .
H H8A 0.319427 0.825608 0.092351 0.048 Uiso calc 1 . .
C C9 0.1977(5) 0.6385(4) 0.17188(14) 0.0409(8) Uani d 1 . .
H H9A 0.108400 0.654003 0.140510 0.049 Uiso calc 1 . .
N N10 0.4611(3) 0.5960(3) 0.26557(11) 0.0342(6) Uani d 1 . .
C C11 0.1604(4) 0.5423(4) 0.21744(14) 0.0380(8) Uani d 1 . .
C C12 0.2966(4) 0.5207(4) 0.26699(13) 0.0331(7) Uani d 1 . .
C C13 0.3637(4) 0.7126(4) 0.17135(14) 0.0359(7) Uani d 1 . .
C C14 0.5012(4) 0.6915(4) 0.21976(12) 0.0329(7) Uani d 1 . .
N N15 0.0558(4) 0.2637(4) 0.35971(14) 0.0497(8) Uani d 1 . .
H H15B 0.134(5) 0.240(6) 0.3886(15) 0.060 Uiso d 1 . .
H H15A -0.043(5) 0.204(5) 0.3581(18) 0.060 Uiso d 1 . .
C C16 0.5969(5) 0.5778(6) 0.31678(14) 0.0484(9) Uani d 1 . .
H H16A 0.547681 0.513918 0.345548 0.073 Uiso calc 0.5 . .
H H16B 0.629892 0.682553 0.332578 0.073 Uiso calc 0.5 . .
H H16C 0.702102 0.525118 0.305738 0.073 Uiso calc 0.5 . .
H H16D 0.705436 0.633808 0.310361 0.073 Uiso calc 0.5 . .
H H16E 0.623225 0.465173 0.323331 0.073 Uiso calc 0.5 . .
H H16F 0.551015 0.622608 0.350171 0.073 Uiso calc 0.5 . .
N N17 0.8669(4) 0.9336(5) 0.17349(13) 0.0467(7) Uani d 1 . .
H H17A 0.943(5) 0.935(6) 0.2052(13) 0.056 Uiso d 1 . .
H H17B 0.876(5) 0.985(5) 0.1368(13) 0.056 Uiso d 1 . .
C C18A 1.2087(4) 0.8050(4) 0.38422(12) 0.0242(6) Uani d 1 . .
C C18B 1.3746(4) 1.2538(3) 0.14663(13) 0.0259(6) Uani d 1 . .
C C19A 1.3690(4) 0.8206(3) 0.42196(13) 0.0258(6) Uani d 1 . .
H H19A 1.468498 0.873246 0.410208 0.031 Uiso calc 1 . .
C C19B 1.2071(4) 1.2393(4) 0.11330(14) 0.0324(7) Uani d 1 . .
H H19B 1.116807 1.176785 0.126405 0.039 Uiso calc 1 . .
C C20A 1.3770(4) 0.7562(3) 0.47729(13) 0.0262(6) Uani d 1 . .
C C20B 1.1758(4) 1.3172(4) 0.06128(14) 0.0345(7) Uani d 1 . .
C C21A 1.2340(4) 0.6786(3) 0.49754(12) 0.0259(6) Uani d 1 . .
H H21A 1.241106 0.639468 0.535361 0.031 Uiso calc 1 . .
C C21B 1.3064(4) 1.4110(4) 0.03919(13) 0.0344(7) Uani d 1 . .
H H21B 1.282852 1.463916 0.003634 0.041 Uiso calc 1 . .
C C22A 1.0796(4) 0.6626(3) 0.45828(12) 0.0258(6) Uani d 1 . .
C C22B 1.4723(4) 1.4212(3) 0.07285(13) 0.0282(6) Uani d 1 . .
C C23A 1.0636(4) 0.7230(3) 0.40247(12) 0.0250(6) Uani d 1 . .
H H23A 0.957047 0.709024 0.377368 0.030 Uiso calc 1 . .
C C23B 1.5091(4) 1.3456(3) 0.12620(12) 0.0256(6) Uani d 1 . .
H H23B 1.622172 1.356047 0.148063 0.031 Uiso calc 1 . .
C C24A 1.1888(4) 0.8800(4) 0.32463(12) 0.0269(6) Uani d 1 . .
C C24B 1.4120(4) 1.1718(4) 0.20526(12) 0.0286(6) Uani d 1 . .
O O25A 1.3325(3) 0.9413(3) 0.30974(9) 0.0356(5) Uani d 1 . .
O O25B 1.2778(3) 1.0829(3) 0.21672(9) 0.0343(5) Uani d 1 . .
H H25B 1.306(5) 1.027(5) 0.2543(10) 0.051 Uiso d 1 . .
O O26A 1.0381(3) 0.8785(3) 0.29518(9) 0.0354(5) Uani d 1 . .
O O26B 1.5540(3) 1.1933(3) 0.23619(9) 0.0355(5) Uani d 1 . .
N N27A 1.5451(3) 0.7739(3) 0.51778(12) 0.0342(6) Uani d 1 . .
N N27B 0.9995(4) 1.2977(4) 0.02541(16) 0.0526(8) Uani d 1 . .
O O28A 1.6731(3) 0.8425(3) 0.50034(12) 0.0479(6) Uani d 1 . .
O O28B 0.8841(4) 1.2178(4) 0.04580(15) 0.0679(9) Uani d 1 . .
O O29A 1.5499(3) 0.7162(3) 0.56674(10) 0.0477(6) Uani d 1 . .
O O29B 0.9773(4) 1.3628(5) -0.02219(14) 0.0782(10) Uani d 1 . .
N N30A 0.9241(3) 0.5778(3) 0.47753(11) 0.0320(6) Uani d 1 . .
N N30B 1.6155(4) 1.5175(3) 0.05112(11) 0.0343(6) Uani d 1 . .
O O31A 0.7969(3) 0.5423(3) 0.44079(10) 0.0443(6) Uani d 1 . .
O O31B 1.7573(3) 1.5373(3) 0.08294(10) 0.0415(5) Uani d 1 . .
O O32A 0.9292(3) 0.5482(3) 0.52926(9) 0.0410(6) Uani d 1 . .
O O32B 1.5837(4) 1.5724(3) 0.00180(10) 0.0521(6) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1W 0.0384(13) 0.0737(19) 0.0508(15) 0.0081(14) -0.0034(11) -0.0028(15)
C1 0.0385(18) 0.047(2) 0.0392(19) 0.0128(16) -0.0127(14) -0.0126(16)
C2 0.0307(17) 0.049(2) 0.053(2) 0.0052(15) -0.0024(14) -0.0178(18)
C3 0.0398(18) 0.0398(19) 0.0413(19) 0.0117(15) 0.0004(14) -0.0094(15)
C4 0.0282(15) 0.0399(18) 0.0406(18) 0.0083(13) -0.0051(13) -0.0132(15)
C5 0.0352(16) 0.0393(18) 0.0269(15) 0.0098(14) -0.0087(12) -0.0097(13)
C6 0.0490(19) 0.0396(17) 0.0253(15) 0.0139(15) 0.0012(13) -0.0048(13)
C7 0.0479(19) 0.0437(19) 0.0283(16) 0.0139(16) -0.0005(13) -0.0024(14)
C8 0.052(2) 0.0397(18) 0.0250(16) 0.0208(16) -0.0086(13) -0.0082(14)
C9 0.0449(19) 0.0406(18) 0.0324(17) 0.0179(15) -0.0133(14) -0.0136(14)
N10 0.0299(13) 0.0347(14) 0.0347(14) 0.0026(11) -0.0088(10) -0.0095(11)
C11 0.0298(15) 0.0391(18) 0.0419(18) 0.0092(14) -0.0075(12) -0.0187(15)
C12 0.0357(16) 0.0286(15) 0.0326(15) 0.0116(13) -0.0048(12) -0.0132(13)
C13 0.0340(16) 0.0358(17) 0.0341(16) 0.0079(14) -0.0108(13) -0.0144(14)
C14 0.0438(17) 0.0278(15) 0.0244(14) 0.0123(14) -0.0055(12) -0.0093(13)
N15 0.0369(16) 0.061(2) 0.0487(19) -0.0013(15) -0.0037(13) -0.0035(17)
C16 0.0383(17) 0.069(3) 0.0336(17) -0.0040(18) -0.0101(14) 0.0078(18)
N17 0.0392(16) 0.065(2) 0.0339(15) 0.0013(15) -0.0017(12) 0.0031(15)
C18A 0.0265(13) 0.0211(13) 0.0251(14) 0.0027(11) 0.0038(11) -0.0050(11)
C18B 0.0228(13) 0.0240(14) 0.0318(15) 0.0012(11) 0.0072(11) -0.0056(12)
C19A 0.0239(13) 0.0184(13) 0.0358(16) 0.0010(11) 0.0070(11) -0.0058(12)
C19B 0.0259(14) 0.0277(15) 0.0435(18) -0.0007(12) 0.0040(12) -0.0090(13)
C20A 0.0238(13) 0.0206(13) 0.0322(15) 0.0032(11) -0.0038(11) -0.0043(11)
C20B 0.0289(15) 0.0313(16) 0.0407(18) 0.0013(13) -0.0059(13) -0.0125(14)
C21A 0.0280(14) 0.0198(13) 0.0288(14) 0.0018(11) -0.0006(11) 0.0021(11)
C21B 0.0446(18) 0.0307(17) 0.0255(15) 0.0087(14) -0.0049(12) -0.0071(13)
C22A 0.0259(14) 0.0230(14) 0.0279(14) -0.0027(11) 0.0012(11) -0.0008(12)
C22B 0.0337(15) 0.0205(13) 0.0313(15) -0.0008(12) 0.0074(12) -0.0038(12)
C23A 0.0238(13) 0.0238(14) 0.0265(14) -0.0021(11) -0.0008(10) -0.0044(11)
C23B 0.0246(13) 0.0251(14) 0.0268(15) 0.0002(11) 0.0024(11) -0.0039(11)
C24A 0.0275(14) 0.0251(14) 0.0289(15) 0.0008(12) 0.0065(11) -0.0042(12)
C24B 0.0280(15) 0.0262(15) 0.0326(15) 0.0021(12) 0.0082(12) -0.0028(13)
O25A 0.0301(11) 0.0431(13) 0.0353(12) -0.0024(10) 0.0103(9) 0.0053(10)
O25B 0.0327(11) 0.0368(12) 0.0349(11) -0.0065(9) 0.0105(9) 0.0020(10)
O26A 0.0355(11) 0.0457(13) 0.0240(11) -0.0075(10) 0.0008(9) 0.0026(10)
O26B 0.0294(11) 0.0399(12) 0.0365(11) 0.0001(10) 0.0016(9) 0.0072(10)
N27A 0.0255(13) 0.0258(14) 0.0482(17) 0.0000(11) -0.0072(11) 0.0017(12)
N27B 0.0399(17) 0.0503(19) 0.061(2) 0.0045(16) -0.0184(15) -0.0167(17)
O28A 0.0300(12) 0.0360(13) 0.0727(17) -0.0079(10) -0.0124(11) 0.0159(12)
O28B 0.0349(14) 0.0521(17) 0.108(2) -0.0079(13) -0.0231(14) -0.0174(17)
O29A 0.0416(13) 0.0550(16) 0.0416(13) -0.0040(12) -0.0128(10) 0.0084(12)
O29B 0.0598(19) 0.103(3) 0.061(2) 0.0028(19) -0.0344(15) -0.0045(19)
N30A 0.0283(12) 0.0344(14) 0.0319(13) -0.0063(11) -0.0012(10) 0.0049(11)
N30B 0.0491(16) 0.0276(13) 0.0271(13) -0.0016(12) 0.0086(11) 0.0012(11)
O31A 0.0350(11) 0.0602(16) 0.0351(11) -0.0211(12) -0.0060(9) 0.0108(11)
O31B 0.0402(12) 0.0443(13) 0.0395(12) -0.0105(11) 0.0035(10) 0.0013(11)
O32A 0.0402(12) 0.0499(15) 0.0318(12) -0.0114(11) 0.0003(9) 0.0167(11)
O32B 0.0734(17) 0.0488(15) 0.0332(13) -0.0121(13) 0.0030(11) 0.0110(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
H2W O1W H1W . . 110(5) ?
C2 C1 C11 . . 122.9(3) ?
C2 C1 H1A . . 118.6 ?
C11 C1 H1A . . 118.6 ?
C1 C2 C3 . . 119.8(3) ?
C1 C2 H2A . . 120.1 ?
C3 C2 H2A . . 120.1 ?
N15 C3 C4 . . 121.2(3) ?
N15 C3 C2 . . 120.1(3) ?
C4 C3 C2 . . 118.6(3) ?
C12 C4 C3 . . 122.0(3) ?
C12 C4 H4A . . 119.0 ?
C3 C4 H4A . . 119.0 ?
C14 C5 C6 . . 121.7(3) ?
C14 C5 H5A . . 119.2 ?
C6 C5 H5A . . 119.2 ?
N17 C6 C5 . . 121.8(3) ?
N17 C6 C7 . . 119.5(3) ?
C5 C6 C7 . . 118.6(3) ?
C8 C7 C6 . . 120.0(3) ?
C8 C7 H7A . . 120.0 ?
C6 C7 H7A . . 120.0 ?
C7 C8 C13 . . 122.4(3) ?
C7 C8 H8A . . 118.8 ?
C13 C8 H8A . . 118.8 ?
C11 C9 C13 . . 122.1(3) ?
C11 C9 H9A . . 118.9 ?
C13 C9 H9A . . 118.9 ?
C12 N10 C14 . . 123.7(3) ?
C12 N10 C16 . . 117.3(3) ?
C14 N10 C16 . . 119.0(3) ?
C9 C11 C1 . . 123.6(3) ?
C9 C11 C12 . . 119.4(3) ?
C1 C11 C12 . . 117.1(3) ?
C4 C12 N10 . . 122.8(3) ?
C4 C12 C11 . . 119.7(3) ?
N10 C12 C11 . . 117.5(3) ?
C9 C13 C8 . . 123.2(3) ?
C9 C13 C14 . . 119.4(3) ?
C8 C13 C14 . . 117.4(3) ?
C5 C14 N10 . . 122.2(3) ?
C5 C14 C13 . . 119.9(3) ?
N10 C14 C13 . . 117.8(3) ?
C3 N15 H15B . . 124(3) ?
C3 N15 H15A . . 121(3) ?
H15B N15 H15A . . 113(4) ?
N10 C16 H16A . . 109.5 ?
N10 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
N10 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N10 C16 H16D . . 109.5 ?
H16A C16 H16D . . 141.1 ?
H16B C16 H16D . . 56.3 ?
H16C C16 H16D . . 56.3 ?
N10 C16 H16E . . 109.5 ?
H16A C16 H16E . . 56.3 ?
H16B C16 H16E . . 141.1 ?
H16C C16 H16E . . 56.3 ?
H16D C16 H16E . . 109.5 ?
N10 C16 H16F . . 109.5 ?
H16A C16 H16F . . 56.3 ?
H16B C16 H16F . . 56.3 ?
H16C C16 H16F . . 141.1 ?
H16D C16 H16F . . 109.5 ?
H16E C16 H16F . . 109.5 ?
C6 N17 H17A . . 120(3) ?
C6 N17 H17B . . 111(2) ?
H17A N17 H17B . . 129(4) ?
C23A C18A C19A . . 119.5(3) ?
C23A C18A C24A . . 119.5(2) ?
C19A C18A C24A . . 120.9(2) ?
C19B C18B C23B . . 119.7(3) ?
C19B C18B C24B . . 120.7(3) ?
C23B C18B C24B . . 119.6(3) ?
C20A C19A C18A . . 118.6(3) ?
C20A C19A H19A . . 120.7 ?
C18A C19A H19A . . 120.7 ?
C20B C19B C18B . . 119.5(3) ?
C20B C19B H19B . . 120.2 ?
C18B C19B H19B . . 120.2 ?
C21A C20A C19A . . 123.5(3) ?
C21A C20A N27A . . 117.4(3) ?
C19A C20A N27A . . 119.0(3) ?
C19B C20B C21B . . 122.8(3) ?
C19B C20B N27B . . 119.2(3) ?
C21B C20B N27B . . 117.9(3) ?
C20A C21A C22A . . 115.9(3) ?
C20A C21A H21A . . 122.1 ?
C22A C21A H21A . . 122.1 ?
C22B C21B C20B . . 116.4(3) ?
C22B C21B H21B . . 121.8 ?
C20B C21B H21B . . 121.8 ?
C23A C22A C21A . . 123.3(3) ?
C23A C22A N30A . . 118.8(2) ?
C21A C22A N30A . . 117.9(2) ?
C21B C22B C23B . . 122.7(3) ?
C21B C22B N30B . . 118.5(3) ?
C23B C22B N30B . . 118.8(3) ?
C22A C23A C18A . . 119.1(2) ?
C22A C23A H23A . . 120.4 ?
C18A C23A H23A . . 120.4 ?
C22B C23B C18B . . 118.9(3) ?
C22B C23B H23B . . 120.5 ?
C18B C23B H23B . . 120.5 ?
O26A C24A O25A . . 126.2(3) ?
O26A C24A C18A . . 118.5(2) ?
O25A C24A C18A . . 115.3(2) ?
O26B C24B O25B . . 126.9(3) ?
O26B C24B C18B . . 120.8(3) ?
O25B C24B C18B . . 112.4(2) ?
C24A O25A H25B . . 114.1(15) ?
C24B O25B H25B . . 112(2) ?
O28A N27A O29A . . 123.7(3) ?
O28A N27A C20A . . 118.1(3) ?
O29A N27A C20A . . 118.2(3) ?
O29B N27B O28B . . 124.4(3) ?
O29B N27B C20B . . 118.1(3) ?
O28B N27B C20B . . 117.4(3) ?
O32A N30A O31A . . 124.0(2) ?
O32A N30A C22A . . 117.9(2) ?
O31A N30A C22A . . 118.2(2) ?
O31B N30B O32B . . 124.3(3) ?
O31B N30B C22B . . 118.4(2) ?
O32B N30B C22B . . 117.3(3) ?
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
O1W H2W . 0.86(3) ?
O1W H1W . 0.91(3) ?
C1 C2 . 1.347(6) ?
C1 C11 . 1.418(5) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.434(5) ?
C2 H2A . 0.9300 ?
C3 N15 . 1.350(5) ?
C3 C4 . 1.393(5) ?
C4 C12 . 1.376(5) ?
C4 H4A . 0.9300 ?
C5 C14 . 1.383(5) ?
C5 C6 . 1.393(5) ?
C5 H5A . 0.9300 ?
C6 N17 . 1.338(5) ?
C6 C7 . 1.437(5) ?
C7 C8 . 1.345(5) ?
C7 H7A . 0.9300 ?
C8 C13 . 1.428(5) ?
C8 H8A . 0.9300 ?
C9 C11 . 1.379(5) ?
C9 C13 . 1.382(5) ?
C9 H9A . 0.9300 ?
N10 C12 . 1.379(4) ?
N10 C14 . 1.387(4) ?
N10 C16 . 1.466(4) ?
C11 C12 . 1.444(4) ?
C13 C14 . 1.430(4) ?
N15 H15B . 0.85(3) ?
N15 H15A . 0.88(3) ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
C16 H16D . 0.9600 ?
C16 H16E . 0.9600 ?
C16 H16F . 0.9600 ?
N17 H17A . 0.87(2) ?
N17 H17B . 0.96(2) ?
C18A C23A . 1.387(4) ?
C18A C19A . 1.394(4) ?
C18A C24A . 1.504(4) ?
C18B C19B . 1.387(4) ?
C18B C23B . 1.388(4) ?
C18B C24B . 1.513(4) ?
C19A C20A . 1.383(4) ?
C19A H19A . 0.9300 ?
C19B C20B . 1.361(5) ?
C19B H19B . 0.9300 ?
C20A C21A . 1.377(4) ?
C20A N27A . 1.474(4) ?
C20B C21B . 1.392(5) ?
C20B N27B . 1.471(4) ?
C21A C22A . 1.379(4) ?
C21A H21A . 0.9300 ?
C21B C22B . 1.378(4) ?
C21B H21B . 0.9300 ?
C22A C23A . 1.378(4) ?
C22A N30A . 1.471(4) ?
C22B C23B . 1.382(4) ?
C22B N30B . 1.471(4) ?
C23A H23A . 0.9300 ?
C23B H23B . 0.9300 ?
C24A O26A . 1.238(3) ?
C24A O25A . 1.272(3) ?
C24B O26B . 1.213(4) ?
C24B O25B . 1.296(4) ?
O25B H25B . 0.987(14) ?
N27A O28A . 1.222(4) ?
N27A O29A . 1.228(4) ?
N27B O29B . 1.220(4) ?
N27B O28B . 1.227(5) ?
N30A O32A . 1.220(3) ?
N30A O31A . 1.226(3) ?
N30B O31B . 1.220(3) ?
N30B O32B . 1.225(3) ?
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
O1W H1W O26A 1_445 0.92(5) 2.02(5) 2.925(4) 167(4) yes
O1W H2W O25A 1_345 0.86(4) 2.46(4) 3.194(5) 144(5) yes
O1W H2W O26B 1_345 0.86(4) 2.45(5) 3.079(4) 131(4) yes
N15 H15A O1W . 0.88(4) 2.09(4) 2.966(4) 171(4) yes
N15 H15B O29A 2_745 0.85(4) 2.46(4) 3.227(3) 151(3) yes
N15 H15B O32A 2_646 0.85(4) 2.57(4) 3.121(3) 124(3) yes
N17 H17A O26A . 0.87(3) 2.17(4) 2.979(4) 155(4) yes
O25B H25B O25A . 0.99(3) 1.46(3) 2.442(4) 176(4) yes
C2 H2A O26B 1_345 0.93 2.42 3.330(4) 167 yes
C5 H5A O26A . 0.93 2.45 3.212(4) 139 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
C11 C1 C2 C3 . . . . 1.2(5) ?
C1 C2 C3 N15 . . . . 176.0(3) ?
C1 C2 C3 C4 . . . . -2.3(5) ?
N15 C3 C4 C12 . . . . -177.2(3) ?
C2 C3 C4 C12 . . . . 1.1(5) ?
C14 C5 C6 N17 . . . . 179.9(3) ?
C14 C5 C6 C7 . . . . -0.7(5) ?
N17 C6 C7 C8 . . . . 179.8(3) ?
C5 C6 C7 C8 . . . . 0.4(5) ?
C6 C7 C8 C13 . . . . 0.1(5) ?
C13 C9 C11 C1 . . . . -177.3(3) ?
C13 C9 C11 C12 . . . . 1.5(5) ?
C2 C1 C11 C9 . . . . 179.9(3) ?
C2 C1 C11 C12 . . . . 1.1(5) ?
C3 C4 C12 N10 . . . . -178.6(3) ?
C3 C4 C12 C11 . . . . 1.3(4) ?
C14 N10 C12 C4 . . . . -179.5(3) ?
C16 N10 C12 C4 . . . . -2.0(4) ?
C14 N10 C12 C11 . . . . 0.6(4) ?
C16 N10 C12 C11 . . . . 178.1(3) ?
C9 C11 C12 C4 . . . . 178.8(3) ?
C1 C11 C12 C4 . . . . -2.4(4) ?
C9 C11 C12 N10 . . . . -1.3(4) ?
C1 C11 C12 N10 . . . . 177.5(3) ?
C11 C9 C13 C8 . . . . 179.1(3) ?
C11 C9 C13 C14 . . . . -0.9(5) ?
C7 C8 C13 C9 . . . . 179.6(3) ?
C7 C8 C13 C14 . . . . -0.4(5) ?
C6 C5 C14 N10 . . . . -179.6(3) ?
C6 C5 C14 C13 . . . . 0.4(4) ?
C12 N10 C14 C5 . . . . 180.0(3) ?
C16 N10 C14 C5 . . . . 2.5(4) ?
C12 N10 C14 C13 . . . . 0.0(4) ?
C16 N10 C14 C13 . . . . -177.5(3) ?
C9 C13 C14 C5 . . . . -179.9(3) ?
C8 C13 C14 C5 . . . . 0.1(4) ?
C9 C13 C14 N10 . . . . 0.1(4) ?
C8 C13 C14 N10 . . . . -179.9(3) ?
C23A C18A C19A C20A . . . . -1.3(4) ?
C24A C18A C19A C20A . . . . 176.8(3) ?
C23B C18B C19B C20B . . . . -0.9(4) ?
C24B C18B C19B C20B . . . . 178.6(3) ?
C18A C19A C20A C21A . . . . -0.8(4) ?
C18A C19A C20A N27A . . . . -179.2(2) ?
C18B C19B C20B C21B . . . . 0.7(5) ?
C18B C19B C20B N27B . . . . 178.4(3) ?
C19A C20A C21A C22A . . . . 2.2(4) ?
N27A C20A C21A C22A . . . . -179.3(2) ?
C19B C20B C21B C22B . . . . 0.3(5) ?
N27B C20B C21B C22B . . . . -177.4(3) ?
C20A C21A C22A C23A . . . . -1.7(4) ?
C20A C21A C22A N30A . . . . 178.9(3) ?
C20B C21B C22B C23B . . . . -1.0(4) ?
C20B C21B C22B N30B . . . . 179.4(3) ?
C21A C22A C23A C18A . . . . -0.3(4) ?
N30A C22A C23A C18A . . . . 179.1(2) ?
C19A C18A C23A C22A . . . . 1.8(4) ?
C24A C18A C23A C22A . . . . -176.4(3) ?
C21B C22B C23B C18B . . . . 0.8(4) ?
N30B C22B C23B C18B . . . . -179.6(2) ?
C19B C18B C23B C22B . . . . 0.2(4) ?
C24B C18B C23B C22B . . . . -179.3(2) ?
C23A C18A C24A O26A . . . . 6.1(4) ?
C19A C18A C24A O26A . . . . -172.1(3) ?
C23A C18A C24A O25A . . . . -174.6(3) ?
C19A C18A C24A O25A . . . . 7.2(4) ?
C19B C18B C24B O26B . . . . -174.9(3) ?
C23B C18B C24B O26B . . . . 4.5(4) ?
C19B C18B C24B O25B . . . . 4.5(4) ?
C23B C18B C24B O25B . . . . -176.1(2) ?
C21A C20A N27A O28A . . . . 180.0(3) ?
C19A C20A N27A O28A . . . . -1.5(4) ?
C21A C20A N27A O29A . . . . 1.3(4) ?
C19A C20A N27A O29A . . . . 179.9(3) ?
C19B C20B N27B O29B . . . . -176.8(3) ?
C21B C20B N27B O29B . . . . 1.0(5) ?
C19B C20B N27B O28B . . . . 3.8(5) ?
C21B C20B N27B O28B . . . . -178.5(3) ?
C23A C22A N30A O32A . . . . -168.4(3) ?
C21A C22A N30A O32A . . . . 11.0(4) ?
C23A C22A N30A O31A . . . . 11.1(4) ?
C21A C22A N30A O31A . . . . -169.5(3) ?
C21B C22B N30B O31B . . . . 174.1(3) ?
C23B C22B N30B O31B . . . . -5.5(4) ?
C21B C22B N30B O32B . . . . -6.0(4) ?
C23B C22B N30B O32B . . . . 174.3(3) ?