#------------------------------------------------------------------------------
#$Date: 2020-06-18 02:17:08 +0300 (Thu, 18 Jun 2020) $
#$Revision: 253217 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/83/1558331.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1558331
loop_
_publ_author_name
'Xie, Shuangshuang'
'Tan, Xiaosheng'
'Liu, Yaping'
'Duan, Yulin'
'Chen, Gang'
'Feng, Hao'
'Sun, Lingjuan'
'Huang, Yingying'
'Guo, Yi'
'Shi, Zhengyi'
'Zhou, Yuan'
'Qi, Changxing'
'Zhang, Yonghui'
_publ_section_title
;
Hypersonins A-D, Polycyclic Polyprenylated Acylphloroglucinols with a
1,2-seco-Homoadamantane Architecture from Hypericum
wilsonii.
;
_journal_name_full 'Journal of natural products'
_journal_paper_doi 10.1021/acs.jnatprod.9b01187
_journal_year 2020
_chemical_absolute_configuration ad
_chemical_formula_moiety 'C31 H48 O6'
_chemical_formula_sum 'C31 H48 O6'
_chemical_formula_weight 516.69
_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 geom
_atom_sites_solution_primary direct
_audit_creation_date 2019-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 102.0033(13)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 10.90373(13)
_cell_length_b 9.73486(11)
_cell_length_c 14.2878(2)
_cell_measurement_reflns_used 30352
_cell_measurement_temperature 100.01(10)
_cell_measurement_theta_max 73.6840
_cell_measurement_theta_min 3.1610
_cell_volume 1483.44(3)
_computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100.01(10)
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w -60.00 -10.00 0.50 0.50 -- 0.00 -31.00 24.00 100
2 \w 36.00 61.00 0.50 0.50 -- 0.00 31.00-175.00 50
3 \w 94.00 132.00 0.50 0.50 -- 94.60 31.00-175.00 76
4 \w 31.00 106.00 0.50 0.50 -- 94.60 -31.00 24.00 150
5 \w 59.00 86.00 0.50 0.50 -- 0.00 57.00-180.00 54
6 \w -21.00 52.00 0.50 0.50 -- 0.00 57.00-180.00 146
7 \w -32.00 29.00 0.50 0.50 -- 0.00 -82.00 -30.00 122
8 \w -23.00 15.00 0.50 0.50 -- 0.00 -38.00 120.00 76
9 \w -88.00 -45.00 0.50 0.50 -- 0.00 -38.00 120.00 86
10 \w 39.00 88.00 0.50 0.50 -- 0.00 38.00 -30.00 98
11 \w -17.00 30.00 0.50 0.50 -- 0.00 38.00 -30.00 94
12 \w -24.00 30.00 0.50 0.50 -- 0.00 -82.00 30.00 108
13 \w -32.00 30.00 0.50 0.50 -- 0.00 -82.00-150.00 124
14 \w -16.00 62.00 0.50 0.50 -- 0.00 38.00 60.00 156
15 \w 67.00 93.00 0.50 0.50 -- 94.60 71.00-171.63 52
16 \w 77.00 184.00 0.50 0.50 -- 94.60 50.00 57.91 214
17 \w 67.00 93.00 0.50 0.50 -- 94.60 71.00 85.48 52
18 \w 67.00 93.00 0.50 0.50 -- 94.60 71.00-138.48 52
19 \w 41.00 125.00 0.50 0.50 -- 94.60 -82.00 -60.00 168
20 \w 156.00 181.00 0.50 0.50 -- 94.60 59.00 70.44 50
21 \w 101.00 174.00 0.50 0.50 -- 94.60 66.00 9.56 146
22 \w 159.00 184.00 0.50 0.50 -- 94.60 63.00 -14.37 50
23 \w 79.00 124.00 0.50 0.50 -- 94.60 -82.00 90.00 90
24 \w 70.00 108.00 0.50 0.50 -- 94.60 63.00 -14.37 76
25 \w 73.00 181.00 0.50 0.50 -- 94.60 61.00 30.00 216
26 \w 71.00 126.00 0.50 0.50 -- 94.60 -82.00-150.00 110
27 \w 72.00 116.00 0.50 0.50 -- 94.60 61.00 -90.00 88
28 \w 71.00 96.00 0.50 0.50 -- 94.60 61.00 0.00 50
29 \w 71.00 182.00 0.50 0.50 -- 94.60 60.00 -40.72 222
30 \w 75.00 120.00 0.50 0.50 -- 94.60 45.00-180.00 90
31 \w 74.00 184.00 0.50 0.50 -- 94.60 51.00 95.59 220
32 \w 72.00 183.00 0.50 0.50 -- 94.60 58.00 130.32 222
33 \w 72.00 102.00 0.50 0.50 -- 94.60 61.00-150.00 60
34 \w 67.00 93.00 0.50 0.50 -- 94.60 72.00 41.64 52
35 \w 71.00 148.00 0.50 0.50 -- 94.60 59.00 70.44 154
36 \w 53.00 78.00 0.50 0.50 -- 94.60 -82.00 90.00 50
37 \w 72.00 183.00 0.50 0.50 -- 94.60 57.00 -71.37 222
38 \w 69.00 96.00 0.50 0.50 -- 94.60 66.00 138.04 54
39 \w 69.00 139.00 0.50 0.50 -- 94.60 71.00-116.48 140
40 \w 12.00 126.00 0.50 0.50 -- 94.60 -82.00 0.00 228
41 \w 69.00 183.00 0.50 0.50 -- 94.60 66.00 173.48 228
42 \w 71.00 96.00 0.50 0.50 -- 94.60 61.00 90.00 50
43 \w 75.00 120.00 0.50 0.50 -- 94.60 45.00-120.00 90
44 \w 67.00 101.00 0.50 0.50 -- 94.60 72.00-127.04 68
45 \w 156.00 182.00 0.50 0.50 -- 94.60 71.00-138.48 52
46 \w 109.00 178.00 0.50 0.50 -- 94.60 71.00-171.63 138
47 \w 68.00 102.00 0.50 0.50 -- 94.60 -82.00 -30.00 68
48 \w 9.00 96.00 0.50 0.50 -- 94.60 -82.00-180.00 174
49 \w 69.00 95.00 0.50 0.50 -- 94.60 66.00 9.56 52
50 \w 71.00 97.00 0.50 0.50 -- 94.60 61.00 120.00 52
51 \w 69.00 95.00 0.50 0.50 -- 94.60 67.00 -69.14 52
52 \w 120.00 146.00 0.50 0.50 -- 94.60 67.00 -69.14 52
53 \w 11.00 81.00 0.50 0.50 -- 94.60 -77.00 120.00 140
54 \w 93.00 119.00 0.50 0.50 -- 94.60 -77.00 120.00 52
55 \w 71.00 119.00 0.50 0.50 -- 94.60 61.00 -30.00 96
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.1376765000
_diffrn_orient_matrix_UB_12 -0.0061033000
_diffrn_orient_matrix_UB_13 0.0105306000
_diffrn_orient_matrix_UB_21 -0.0120453000
_diffrn_orient_matrix_UB_22 -0.1460159000
_diffrn_orient_matrix_UB_23 -0.0423930000
_diffrn_orient_matrix_UB_31 0.0419526000
_diffrn_orient_matrix_UB_32 -0.0606765000
_diffrn_orient_matrix_UB_33 0.1012271000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0259
_diffrn_reflns_av_unetI/netI 0.0123
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 33591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.036
_diffrn_reflns_theta_min 3.162
_diffrn_source 'fine-focus sealed X-ray tube'
_diffrn_source_type 'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 0.626
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.68141
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.157
_exptl_crystal_description block
_exptl_crystal_F_000 564
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.341
_refine_diff_density_min -0.169
_refine_diff_density_rms 0.035
_refine_ls_abs_structure_details
;
Flack x determined using 2719 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.06(4)
_refine_ls_extinction_coef 0.0117(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 348
_refine_ls_number_reflns 5937
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0275
_refine_ls_R_factor_gt 0.0274
_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^)+(0.0431P)^2^+0.2554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0722
_refine_ls_wR_factor_ref 0.0723
_reflns_Friedel_coverage 0.864
_reflns_Friedel_fraction_full 0.998
_reflns_Friedel_fraction_max 0.971
_reflns_number_gt 5912
_reflns_number_total 5937
_reflns_threshold_expression 'I > 2\s(I)'
_iucr_refine_instructions_details
;
20190308_xss30_5.res created by SHELXL-2014/7
TITL 20190308_XSS 30_5 in P21 #4
REM reset to P21 #4
CELL 1.54184 10.903735 9.734857 14.28781 90 102.0033 90
ZERR 2 0.00013 0.000106 0.000209 0 0.0013 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H O
UNIT 62 96 12
L.S. 4 0 0
PLAN 20
SIZE 0.12 0.1 0.1
HTAB O4 O5
BOND $H
HTAB
CONF
fmap 2 53
acta
REM
REM
REM
WGHT 0.043100 0.255400
EXTI 0.011667
FVAR 11.66991
O5 3 0.082083 0.460858 0.152538 11.00000 0.02534 0.02565 =
0.02858 -0.00173 -0.00321 0.00037
O6 3 0.654829 0.947890 0.041638 11.00000 0.02872 0.02454 =
0.02089 0.00375 0.00766 -0.00562
AFIX 147
H6 2 0.683454 1.009837 0.013688 11.00000 -1.50000
AFIX 0
O2 3 0.282407 0.683014 0.068543 11.00000 0.02155 0.02258 =
0.01956 -0.00466 0.00398 0.00064
O3 3 0.225641 0.895805 0.102379 11.00000 0.02068 0.02242 =
0.02039 -0.00252 -0.00103 0.00392
O1 3 0.374738 0.975985 0.321845 11.00000 0.03290 0.02413 =
0.02710 -0.00836 0.01260 -0.00853
O4 3 0.111441 0.689960 0.210176 11.00000 0.01788 0.02255 =
0.01956 -0.00085 -0.00060 0.00089
AFIX 147
H4 2 0.082836 0.624815 0.176178 11.00000 -1.50000
AFIX 0
C8 1 0.366861 0.471063 0.357321 11.00000 0.01837 0.02354 =
0.02049 0.00570 0.00265 0.00049
C25 1 0.493736 0.683016 0.230783 11.00000 0.01576 0.01833 =
0.01823 0.00135 0.00386 -0.00006
AFIX 13
H25 2 0.449455 0.601249 0.201209 11.00000 -1.20000
AFIX 0
C7 1 0.443080 0.600395 0.399467 11.00000 0.01727 0.02795 =
0.01557 0.00416 0.00032 -0.00012
AFIX 13
H7 2 0.495699 0.570201 0.460150 11.00000 -1.20000
AFIX 0
C9 1 0.210713 0.650122 0.272686 11.00000 0.01514 0.02296 =
0.01551 0.00179 0.00479 -0.00100
C24 1 0.535441 0.657924 0.339830 11.00000 0.01578 0.02521 =
0.01806 0.00129 0.00146 -0.00063
AFIX 23
H24A 2 0.566602 0.744776 0.368573 11.00000 -1.20000
H24B 2 0.606433 0.595724 0.348907 11.00000 -1.20000
AFIX 0
C1 1 0.253627 0.514577 0.278289 11.00000 0.01776 0.02262 =
0.01843 0.00300 0.00450 -0.00009
C22 1 0.156528 0.839607 0.583458 11.00000 0.04151 0.03923 =
0.02405 0.00056 0.00870 -0.00269
AFIX 137
H22A 2 0.106123 0.889297 0.619647 11.00000 -1.50000
H22B 2 0.207100 0.902986 0.556488 11.00000 -1.50000
H22C 2 0.209851 0.776426 0.624740 11.00000 -1.50000
AFIX 0
C3 1 0.406759 0.811259 0.203349 11.00000 0.01685 0.01830 =
0.01605 -0.00016 0.00349 0.00016
C28 1 0.725604 0.627635 0.229266 11.00000 0.02002 0.02958 =
0.03142 0.00807 0.00995 0.00415
AFIX 137
H28A 2 0.760541 0.664856 0.291302 11.00000 -1.50000
H28B 2 0.786973 0.631824 0.189937 11.00000 -1.50000
H28C 2 0.701721 0.533765 0.235780 11.00000 -1.50000
AFIX 0
C12 1 0.263342 0.241548 0.124691 11.00000 0.03647 0.02564 =
0.03682 -0.00063 0.01609 -0.00032
AFIX 137
H12A 2 0.285842 0.146385 0.122931 11.00000 -1.50000
H12B 2 0.337461 0.297157 0.132234 11.00000 -1.50000
H12C 2 0.206817 0.265564 0.066056 11.00000 -1.50000
AFIX 0
C2 1 0.298780 0.783940 0.118217 11.00000 0.01725 0.01925 =
0.01699 0.00060 0.00559 0.00030
C13 1 0.076909 0.185096 0.195534 11.00000 0.03034 0.02537 =
0.02675 0.00177 0.00485 -0.00454
AFIX 137
H13A 2 0.024131 0.209024 0.135229 11.00000 -1.50000
H13B 2 0.034694 0.206648 0.246331 11.00000 -1.50000
H13C 2 0.095054 0.088548 0.196465 11.00000 -1.50000
AFIX 0
C21 1 0.072745 0.761466 0.504357 11.00000 0.02357 0.02736 =
0.02686 0.00129 0.00892 0.00289
C14 1 0.490500 0.923926 0.171922 11.00000 0.02016 0.01868 =
0.02048 0.00142 0.00567 -0.00061
AFIX 23
H14A 2 0.464401 0.941611 0.103871 11.00000 -1.20000
H14B 2 0.484227 1.008754 0.206235 11.00000 -1.20000
AFIX 0
C23 1 -0.019833 0.667707 0.537029 11.00000 0.03739 0.04152 =
0.03665 0.00239 0.02063 -0.00319
AFIX 137
H23A 2 0.024534 0.597810 0.577978 11.00000 -1.50000
H23B 2 -0.072524 0.625565 0.482374 11.00000 -1.50000
H23C 2 -0.070549 0.719953 0.571573 11.00000 -1.50000
AFIX 0
C15 1 0.625601 0.869729 0.195348 11.00000 0.01899 0.02192 =
0.01737 0.00067 0.00337 -0.00323
AFIX 13
H15 2 0.657302 0.885977 0.263799 11.00000 -1.20000
AFIX 0
C26 1 0.609582 0.711671 0.182457 11.00000 0.01702 0.02082 =
0.02030 0.00218 0.00558 -0.00013
C16 1 0.710474 0.953398 0.141737 11.00000 0.02161 0.02457 =
0.02185 0.00144 0.00432 -0.00583
C27 1 0.575971 0.668119 0.076781 11.00000 0.02462 0.02090 =
0.02383 -0.00120 0.01067 -0.00138
AFIX 137
H27A 2 0.553933 0.572510 0.072643 11.00000 -1.50000
H27B 2 0.646767 0.683017 0.047784 11.00000 -1.50000
H27C 2 0.506225 0.721634 0.043929 11.00000 -1.50000
AFIX 0
C4 1 0.350483 0.863206 0.288142 11.00000 0.01678 0.02045 =
0.01788 -0.00122 0.00286 -0.00048
C29 1 0.460663 0.370959 0.325812 11.00000 0.01983 0.02403 =
0.02952 0.00701 0.00324 0.00139
AFIX 137
H29A 2 0.477159 0.400232 0.265461 11.00000 -1.50000
H29B 2 0.425567 0.280157 0.319420 11.00000 -1.50000
H29C 2 0.537513 0.370324 0.372988 11.00000 -1.50000
AFIX 0
C5 1 0.269514 0.766569 0.337100 11.00000 0.01764 0.02119 =
0.01651 -0.00035 0.00428 -0.00083
C31 1 0.122981 0.889456 0.020340 11.00000 0.02435 0.03320 =
0.02273 -0.00246 -0.00492 0.00648
AFIX 137
H31A 2 0.155334 0.875130 -0.036461 11.00000 -1.50000
H31B 2 0.076969 0.974172 0.014845 11.00000 -1.50000
H31C 2 0.068387 0.814846 0.028093 11.00000 -1.50000
AFIX 0
C6 1 0.357912 0.710101 0.426027 11.00000 0.01827 0.03023 =
0.01523 -0.00015 0.00256 -0.00243
AFIX 23
H6A 2 0.408366 0.784387 0.459112 11.00000 -1.20000
H6B 2 0.309067 0.671547 0.469162 11.00000 -1.20000
AFIX 0
C20 1 0.077166 0.769352 0.411992 11.00000 0.01971 0.02567 =
0.02546 -0.00293 0.00720 -0.00001
AFIX 43
H20 2 0.019460 0.715788 0.370439 11.00000 -1.20000
AFIX 0
C17 1 0.844096 0.897877 0.156473 11.00000 0.02071 0.04097 =
0.04216 0.00893 0.00779 -0.00671
AFIX 137
H17A 2 0.843031 0.809370 0.126682 11.00000 -1.50000
H17B 2 0.878704 0.889476 0.223726 11.00000 -1.50000
H17C 2 0.894560 0.959878 0.128275 11.00000 -1.50000
AFIX 0
C10 1 0.176438 0.419286 0.213914 11.00000 0.02049 0.02500 =
0.02338 0.00104 0.00570 -0.00011
C18 1 0.714924 1.102978 0.175497 11.00000 0.03902 0.02778 =
0.03255 -0.00363 0.01150 -0.01367
AFIX 137
H18A 2 0.769733 1.154644 0.144178 11.00000 -1.50000
H18B 2 0.745650 1.106414 0.243485 11.00000 -1.50000
H18C 2 0.632179 1.141637 0.159990 11.00000 -1.50000
AFIX 0
C11 1 0.199239 0.266388 0.209188 11.00000 0.02483 0.02091 =
0.02243 0.00240 0.00383 -0.00126
AFIX 13
H11 2 0.255359 0.236784 0.268522 11.00000 -1.20000
AFIX 0
C19 1 0.164516 0.854703 0.366965 11.00000 0.02045 0.02334 =
0.02207 -0.00157 0.00715 0.00150
AFIX 23
H19A 2 0.202871 0.924682 0.411989 11.00000 -1.20000
H19B 2 0.116629 0.900740 0.310915 11.00000 -1.20000
AFIX 0
C30 1 0.316340 0.400481 0.438677 11.00000 0.02276 0.03402 =
0.02439 0.01157 0.00293 -0.00145
AFIX 137
H30A 2 0.383607 0.388356 0.493227 11.00000 -1.50000
H30B 2 0.281727 0.312535 0.417171 11.00000 -1.50000
H30C 2 0.252333 0.456752 0.456119 11.00000 -1.50000
AFIX 0
HKLF 4
REM 20190308_XSS 30_5 in P21 #4
REM R1 = 0.0274 for 5912 Fo > 4sig(Fo) and 0.0275 for all 5937 data
REM 348 parameters refined using 1 restraints
END
WGHT 0.0431 0.2554
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, y+1/2, -z
HTAB O6 O2_$1
HTAB O4 O5
REM Highest difference peak 0.341, deepest hole -0.169, 1-sigma level 0.035
Q1 1 0.0757 0.4170 0.2967 11.00000 0.05 0.34
Q2 1 0.1598 0.3799 0.2636 11.00000 0.05 0.22
Q3 1 0.3038 0.4934 0.3158 11.00000 0.05 0.17
Q4 1 0.6241 0.7939 0.1846 11.00000 0.05 0.17
Q5 1 0.3584 0.7974 0.1609 11.00000 0.05 0.17
Q6 1 0.4464 0.7528 0.2191 11.00000 0.05 0.17
Q7 1 0.4055 0.5385 0.3805 11.00000 0.05 0.16
Q8 1 0.4107 0.4261 0.3381 11.00000 0.05 0.16
Q9 1 0.5560 0.8936 0.1854 11.00000 0.05 0.15
Q10 1 0.6647 0.9031 0.1642 11.00000 0.05 0.15
Q11 1 0.7099 1.0294 0.1623 11.00000 0.05 0.15
Q12 1 0.2424 0.7109 0.3030 11.00000 0.05 0.15
Q13 1 0.5076 0.6761 0.2832 11.00000 0.05 0.15
Q14 1 0.3450 0.4290 0.3970 11.00000 0.05 0.14
Q15 1 0.1026 0.7427 0.4636 11.00000 0.05 0.14
Q16 1 0.5516 0.6920 0.2047 11.00000 0.05 0.14
Q17 1 0.4418 0.8779 0.1926 11.00000 0.05 0.14
Q18 1 0.7763 0.9270 0.1441 11.00000 0.05 0.14
Q19 1 0.2442 0.5857 0.2747 11.00000 0.05 0.13
Q20 1 0.5578 0.4136 0.3973 11.00000 0.05 0.13
REM The information below was added by Olex2.
REM
REM R1 = 0.0274 for 5912 Fo > 4sig(Fo) and 0.0275 for all 33630 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.34, deepest hole -0.17
REM Mean Shift 0, Max Shift -0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0275
REM R1_gt = 0.0274
REM wR_ref = 0.0723
REM GOOF = 1.046
REM Shift_max = -0.001
REM Shift_mean = 0
REM Reflections_all = 33630
REM Reflections_gt = 5912
REM Parameters = n/a
REM Hole = -0.17
REM Peak = 0.34
REM Flack = 0.06(4)
;
_cod_data_source_file np9b01187_si_002.cif
_cod_data_source_block 20190308_xss30_5
_cod_database_code 1558331
_shelx_shelxl_version_number 2014/7
_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_max 0.940
_shelx_estimated_absorpt_t_min 0.929
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
C25(H25), C7(H7), C15(H15), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
C24(H24A,H24B), C14(H14A,H14B), C6(H6A,H6B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
C20(H20)
2.d Idealised Me refined as rotating group:
C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C12(H12A,H12B,H12C), C13(H13A,H13B,
H13C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,
H31B,H31C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C)
2.e Idealised tetrahedral OH refined as rotating group:
O6(H6), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.580
_oxdiff_exptl_absorpt_empirical_full_min 0.746
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O5 O 0.08208(11) 0.46086(13) 0.15254(9) 0.0278(3) Uani 1 1 d . . . . .
O6 O 0.65483(11) 0.94789(13) 0.04164(8) 0.0244(3) Uani 1 1 d . . . . .
H6 H 0.6835 1.0098 0.0137 0.037 Uiso 1 1 calc GR . . . .
O2 O 0.28241(10) 0.68301(12) 0.06854(8) 0.0213(2) Uani 1 1 d . . . . .
O3 O 0.22564(10) 0.89581(12) 0.10238(8) 0.0219(2) Uani 1 1 d . . . . .
O1 O 0.37474(12) 0.97598(13) 0.32185(9) 0.0271(3) Uani 1 1 d . . . . .
O4 O 0.11144(10) 0.68996(12) 0.21018(8) 0.0206(2) Uani 1 1 d . . . . .
H4 H 0.0828 0.6248 0.1762 0.031 Uiso 1 1 calc GR . . . .
C8 C 0.36686(14) 0.47106(17) 0.35732(11) 0.0210(3) Uani 1 1 d . . . . .
C25 C 0.49374(13) 0.68302(16) 0.23078(11) 0.0174(3) Uani 1 1 d . . . . .
H25 H 0.4495 0.6012 0.2012 0.021 Uiso 1 1 calc R . . . .
C7 C 0.44308(15) 0.60040(17) 0.39947(11) 0.0207(3) Uani 1 1 d . . . . .
H7 H 0.4957 0.5702 0.4602 0.025 Uiso 1 1 calc R . . . .
C9 C 0.21071(14) 0.65012(16) 0.27269(11) 0.0176(3) Uani 1 1 d . . . . .
C24 C 0.53544(14) 0.65792(17) 0.33983(11) 0.0200(3) Uani 1 1 d . . . . .
H24A H 0.5666 0.7448 0.3686 0.024 Uiso 1 1 calc R . . . .
H24B H 0.6064 0.5957 0.3489 0.024 Uiso 1 1 calc R . . . .
C1 C 0.25363(14) 0.51458(17) 0.27829(11) 0.0195(3) Uani 1 1 d . . . . .
C22 C 0.1565(2) 0.8396(2) 0.58346(13) 0.0347(4) Uani 1 1 d . . . . .
H22A H 0.1061 0.8893 0.6196 0.052 Uiso 1 1 calc GR . . . .
H22B H 0.2071 0.9030 0.5565 0.052 Uiso 1 1 calc GR . . . .
H22C H 0.2099 0.7764 0.6247 0.052 Uiso 1 1 calc GR . . . .
C3 C 0.40676(14) 0.81126(16) 0.20335(11) 0.0171(3) Uani 1 1 d . . . . .
C28 C 0.72560(15) 0.62763(19) 0.22927(13) 0.0263(4) Uani 1 1 d . . . . .
H28A H 0.7605 0.6649 0.2913 0.040 Uiso 1 1 calc GR . . . .
H28B H 0.7870 0.6318 0.1899 0.040 Uiso 1 1 calc GR . . . .
H28C H 0.7017 0.5338 0.2358 0.040 Uiso 1 1 calc GR . . . .
C12 C 0.26334(19) 0.2415(2) 0.12469(15) 0.0317(4) Uani 1 1 d . . . . .
H12A H 0.2858 0.1464 0.1229 0.048 Uiso 1 1 calc GR . . . .
H12B H 0.3375 0.2972 0.1322 0.048 Uiso 1 1 calc GR . . . .
H12C H 0.2068 0.2656 0.0661 0.048 Uiso 1 1 calc GR . . . .
C2 C 0.29878(14) 0.78394(16) 0.11822(10) 0.0175(3) Uani 1 1 d . . . . .
C13 C 0.07691(17) 0.18510(19) 0.19553(13) 0.0276(4) Uani 1 1 d . . . . .
H13A H 0.0241 0.2090 0.1352 0.041 Uiso 1 1 calc GR . . . .
H13B H 0.0347 0.2066 0.2463 0.041 Uiso 1 1 calc GR . . . .
H13C H 0.0951 0.0885 0.1965 0.041 Uiso 1 1 calc GR . . . .
C21 C 0.07274(16) 0.76147(18) 0.50436(13) 0.0254(4) Uani 1 1 d . . . . .
C14 C 0.49050(14) 0.92393(16) 0.17192(11) 0.0196(3) Uani 1 1 d . . . . .
H14A H 0.4644 0.9416 0.1039 0.023 Uiso 1 1 calc R . . . .
H14B H 0.4842 1.0088 0.2062 0.023 Uiso 1 1 calc R . . . .
C23 C -0.01983(19) 0.6677(2) 0.53703(15) 0.0366(4) Uani 1 1 d . . . . .
H23A H 0.0245 0.5978 0.5780 0.055 Uiso 1 1 calc GR . . . .
H23B H -0.0725 0.6256 0.4824 0.055 Uiso 1 1 calc GR . . . .
H23C H -0.0705 0.7200 0.5716 0.055 Uiso 1 1 calc GR . . . .
C15 C 0.62560(14) 0.86973(16) 0.19535(11) 0.0195(3) Uani 1 1 d . . . . .
H15 H 0.6573 0.8860 0.2638 0.023 Uiso 1 1 calc R . . . .
C26 C 0.60958(14) 0.71167(16) 0.18246(11) 0.0191(3) Uani 1 1 d . . . . .
C16 C 0.71047(15) 0.95340(18) 0.14174(11) 0.0227(3) Uani 1 1 d . . . . .
C27 C 0.57597(15) 0.66812(17) 0.07678(11) 0.0223(3) Uani 1 1 d . . . . .
H27A H 0.5539 0.5725 0.0726 0.033 Uiso 1 1 calc GR . . . .
H27B H 0.6468 0.6830 0.0478 0.033 Uiso 1 1 calc GR . . . .
H27C H 0.5062 0.7216 0.0439 0.033 Uiso 1 1 calc GR . . . .
C4 C 0.35048(14) 0.86321(16) 0.28814(11) 0.0185(3) Uani 1 1 d . . . . .
C29 C 0.46066(15) 0.37096(17) 0.32581(12) 0.0247(3) Uani 1 1 d . . . . .
H29A H 0.4772 0.4002 0.2655 0.037 Uiso 1 1 calc GR . . . .
H29B H 0.4256 0.2802 0.3194 0.037 Uiso 1 1 calc GR . . . .
H29C H 0.5375 0.3703 0.3730 0.037 Uiso 1 1 calc GR . . . .
C5 C 0.26951(14) 0.76657(16) 0.33710(11) 0.0183(3) Uani 1 1 d . . . . .
C31 C 0.12298(16) 0.8895(2) 0.02034(12) 0.0282(4) Uani 1 1 d . . . . .
H31A H 0.1553 0.8751 -0.0365 0.042 Uiso 1 1 calc GR . . . .
H31B H 0.0770 0.9742 0.0148 0.042 Uiso 1 1 calc GR . . . .
H31C H 0.0684 0.8148 0.0281 0.042 Uiso 1 1 calc GR . . . .
C6 C 0.35791(14) 0.71010(18) 0.42603(11) 0.0214(3) Uani 1 1 d . . . . .
H6A H 0.4084 0.7844 0.4591 0.026 Uiso 1 1 calc R . . . .
H6B H 0.3091 0.6715 0.4692 0.026 Uiso 1 1 calc R . . . .
C20 C 0.07717(15) 0.76935(18) 0.41199(12) 0.0232(3) Uani 1 1 d . . . . .
H20 H 0.0195 0.7158 0.3704 0.028 Uiso 1 1 calc R . . . .
C17 C 0.84410(16) 0.8979(2) 0.15647(15) 0.0344(4) Uani 1 1 d . . . . .
H17A H 0.8430 0.8094 0.1267 0.052 Uiso 1 1 calc GR . . . .
H17B H 0.8787 0.8895 0.2237 0.052 Uiso 1 1 calc GR . . . .
H17C H 0.8946 0.9599 0.1283 0.052 Uiso 1 1 calc GR . . . .
C10 C 0.17644(15) 0.41929(18) 0.21391(12) 0.0228(3) Uani 1 1 d . . . . .
C18 C 0.71492(19) 1.1030(2) 0.17550(14) 0.0325(4) Uani 1 1 d . . . . .
H18A H 0.7697 1.1546 0.1442 0.049 Uiso 1 1 calc GR . . . .
H18B H 0.7456 1.1064 0.2435 0.049 Uiso 1 1 calc GR . . . .
H18C H 0.6322 1.1416 0.1600 0.049 Uiso 1 1 calc GR . . . .
C11 C 0.19924(15) 0.26639(17) 0.20919(12) 0.0229(3) Uani 1 1 d . . . . .
H11 H 0.2554 0.2368 0.2685 0.027 Uiso 1 1 calc R . . . .
C19 C 0.16452(15) 0.85470(17) 0.36697(12) 0.0216(3) Uani 1 1 d . . . . .
H19A H 0.2029 0.9247 0.4120 0.026 Uiso 1 1 calc R . . . .
H19B H 0.1166 0.9007 0.3109 0.026 Uiso 1 1 calc R . . . .
C30 C 0.31634(16) 0.4005(2) 0.43868(12) 0.0273(4) Uani 1 1 d . . . . .
H30A H 0.3836 0.3884 0.4932 0.041 Uiso 1 1 calc GR . . . .
H30B H 0.2817 0.3125 0.4172 0.041 Uiso 1 1 calc GR . . . .
H30C H 0.2523 0.4568 0.4561 0.041 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O5 0.0253(6) 0.0256(6) 0.0286(6) -0.0017(5) -0.0032(5) 0.0004(5)
O6 0.0287(6) 0.0245(6) 0.0209(5) 0.0038(5) 0.0077(5) -0.0056(5)
O2 0.0216(5) 0.0226(5) 0.0196(5) -0.0047(5) 0.0040(4) 0.0006(4)
O3 0.0207(5) 0.0224(6) 0.0204(5) -0.0025(4) -0.0010(4) 0.0039(4)
O1 0.0329(6) 0.0241(6) 0.0271(6) -0.0084(5) 0.0126(5) -0.0085(5)
O4 0.0179(5) 0.0226(6) 0.0196(5) -0.0009(5) -0.0006(4) 0.0009(4)
C8 0.0184(7) 0.0235(8) 0.0205(7) 0.0057(6) 0.0026(6) 0.0005(6)
C25 0.0158(6) 0.0183(7) 0.0182(7) 0.0013(6) 0.0039(5) -0.0001(6)
C7 0.0173(7) 0.0279(8) 0.0156(7) 0.0042(6) 0.0003(6) -0.0001(6)
C9 0.0151(6) 0.0230(8) 0.0155(7) 0.0018(6) 0.0048(5) -0.0010(6)
C24 0.0158(7) 0.0252(8) 0.0181(7) 0.0013(6) 0.0015(5) -0.0006(6)
C1 0.0178(7) 0.0226(7) 0.0184(7) 0.0030(6) 0.0045(6) -0.0001(6)
C22 0.0415(10) 0.0392(10) 0.0241(8) 0.0006(8) 0.0087(8) -0.0027(8)
C3 0.0168(7) 0.0183(7) 0.0161(7) -0.0002(5) 0.0035(5) 0.0002(6)
C28 0.0200(8) 0.0296(9) 0.0314(9) 0.0081(7) 0.0100(7) 0.0041(7)
C12 0.0365(10) 0.0256(9) 0.0368(10) -0.0006(7) 0.0161(8) -0.0003(7)
C2 0.0173(7) 0.0193(7) 0.0170(7) 0.0006(6) 0.0056(5) 0.0003(5)
C13 0.0303(8) 0.0254(8) 0.0267(8) 0.0018(7) 0.0049(7) -0.0045(7)
C21 0.0236(8) 0.0274(8) 0.0269(9) 0.0013(7) 0.0089(7) 0.0029(7)
C14 0.0202(7) 0.0187(7) 0.0205(7) 0.0014(6) 0.0057(6) -0.0006(6)
C23 0.0374(10) 0.0415(11) 0.0367(10) 0.0024(9) 0.0206(8) -0.0032(9)
C15 0.0190(7) 0.0219(8) 0.0174(7) 0.0007(6) 0.0034(6) -0.0032(6)
C26 0.0170(7) 0.0208(8) 0.0203(7) 0.0022(6) 0.0056(6) -0.0001(6)
C16 0.0216(7) 0.0246(8) 0.0218(8) 0.0014(6) 0.0043(6) -0.0058(6)
C27 0.0246(7) 0.0209(8) 0.0238(8) -0.0012(6) 0.0107(6) -0.0014(6)
C4 0.0168(7) 0.0205(7) 0.0179(7) -0.0012(6) 0.0029(5) -0.0005(6)
C29 0.0198(7) 0.0240(8) 0.0295(8) 0.0070(7) 0.0032(6) 0.0014(6)
C5 0.0176(7) 0.0212(8) 0.0165(7) -0.0003(6) 0.0043(6) -0.0008(6)
C31 0.0244(8) 0.0332(9) 0.0227(8) -0.0025(7) -0.0049(6) 0.0065(7)
C6 0.0183(7) 0.0302(9) 0.0152(7) -0.0002(6) 0.0026(6) -0.0024(6)
C20 0.0197(7) 0.0257(8) 0.0255(8) -0.0029(7) 0.0072(6) 0.0000(6)
C17 0.0207(8) 0.0410(11) 0.0422(10) 0.0089(9) 0.0078(7) -0.0067(8)
C10 0.0205(7) 0.0250(8) 0.0234(8) 0.0010(6) 0.0057(6) -0.0001(6)
C18 0.0390(10) 0.0278(9) 0.0325(9) -0.0036(7) 0.0115(8) -0.0137(8)
C11 0.0248(8) 0.0209(8) 0.0224(8) 0.0024(6) 0.0038(6) -0.0013(6)
C19 0.0204(7) 0.0233(8) 0.0221(7) -0.0016(6) 0.0072(6) 0.0015(6)
C30 0.0228(8) 0.0340(9) 0.0244(8) 0.0116(7) 0.0029(6) -0.0015(7)
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'
O O 0.0492 0.0322 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 O6 H6 109.5 . . ?
C2 O3 C31 115.83(12) . . ?
C9 O4 H4 109.5 . . ?
C1 C8 C7 109.93(13) . . ?
C29 C8 C7 106.84(12) . . ?
C29 C8 C1 115.81(13) . . ?
C29 C8 C30 107.42(14) . . ?
C30 C8 C7 108.24(14) . . ?
C30 C8 C1 108.35(12) . . ?
C24 C25 H25 108.7 . . ?
C24 C25 C3 114.39(12) . . ?
C24 C25 C26 111.84(12) . . ?
C3 C25 H25 108.7 . . ?
C3 C25 C26 104.26(12) . . ?
C26 C25 H25 108.7 . . ?
C8 C7 H7 105.5 . . ?
C24 C7 C8 115.71(13) . . ?
C24 C7 H7 105.5 . . ?
C6 C7 C8 111.16(13) . . ?
C6 C7 H7 105.5 . . ?
C6 C7 C24 112.62(14) . . ?
O4 C9 C1 122.55(14) . . ?
O4 C9 C5 112.18(13) . . ?
C1 C9 C5 125.26(14) . . ?
C25 C24 C7 121.37(12) . . ?
C25 C24 H24A 107.0 . . ?
C25 C24 H24B 107.0 . . ?
C7 C24 H24A 107.0 . . ?
C7 C24 H24B 107.0 . . ?
H24A C24 H24B 106.7 . . ?
C9 C1 C8 120.46(14) . . ?
C9 C1 C10 115.19(14) . . ?
C10 C1 C8 123.94(15) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
C2 C3 C25 112.70(12) . . ?
C2 C3 C14 107.13(12) . . ?
C2 C3 C4 108.26(12) . . ?
C14 C3 C25 105.87(12) . . ?
C14 C3 C4 110.33(12) . . ?
C4 C3 C25 112.40(12) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
O2 C2 O3 123.60(14) . . ?
O2 C2 C3 127.30(14) . . ?
O3 C2 C3 108.99(12) . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
C22 C21 C23 114.55(16) . . ?
C20 C21 C22 125.01(17) . . ?
C20 C21 C23 120.44(17) . . ?
C3 C14 H14A 110.4 . . ?
C3 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
C15 C14 C3 106.84(12) . . ?
C15 C14 H14A 110.4 . . ?
C15 C14 H14B 110.4 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 C15 H15 106.6 . . ?
C14 C15 C26 103.61(12) . . ?
C14 C15 C16 110.87(13) . . ?
C26 C15 H15 106.6 . . ?
C16 C15 H15 106.6 . . ?
C16 C15 C26 121.69(14) . . ?
C28 C26 C25 112.02(13) . . ?
C28 C26 C15 114.38(13) . . ?
C15 C26 C25 101.69(12) . . ?
C27 C26 C25 109.30(12) . . ?
C27 C26 C28 106.67(13) . . ?
C27 C26 C15 112.78(13) . . ?
O6 C16 C15 107.52(12) . . ?
O6 C16 C17 108.54(14) . . ?
O6 C16 C18 109.20(14) . . ?
C17 C16 C15 113.36(14) . . ?
C17 C16 C18 109.04(15) . . ?
C18 C16 C15 109.09(14) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C4 C3 121.25(14) . . ?
O1 C4 C5 118.02(14) . . ?
C3 C4 C5 120.56(13) . . ?
C8 C29 H29A 109.5 . . ?
C8 C29 H29B 109.5 . . ?
C8 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C9 C5 C4 112.83(12) . . ?
C9 C5 C6 110.47(13) . . ?
C9 C5 C19 109.61(12) . . ?
C4 C5 C19 107.97(12) . . ?
C6 C5 C4 105.85(12) . . ?
C6 C5 C19 110.02(12) . . ?
O3 C31 H31A 109.5 . . ?
O3 C31 H31B 109.5 . . ?
O3 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C7 C6 C5 111.03(12) . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C21 C20 H20 116.2 . . ?
C21 C20 C19 127.69(16) . . ?
C19 C20 H20 116.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C10 C1 120.99(15) . . ?
O5 C10 C11 113.54(15) . . ?
C1 C10 C11 125.45(15) . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C11 H11 109.2 . . ?
C13 C11 C12 110.25(14) . . ?
C13 C11 H11 109.2 . . ?
C10 C11 C12 107.22(14) . . ?
C10 C11 C13 111.59(14) . . ?
C10 C11 H11 109.2 . . ?
C5 C19 H19A 109.1 . . ?
C5 C19 H19B 109.2 . . ?
C20 C19 C5 112.27(13) . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C8 C30 H30A 109.5 . . ?
C8 C30 H30B 109.5 . . ?
C8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 C10 1.271(2) . ?
O6 H6 0.8200 . ?
O6 C16 1.4337(19) . ?
O2 C2 1.203(2) . ?
O3 C2 1.3409(19) . ?
O3 C31 1.4440(19) . ?
O1 C4 1.206(2) . ?
O4 H4 0.8200 . ?
O4 C9 1.3106(18) . ?
C8 C7 1.559(2) . ?
C8 C1 1.549(2) . ?
C8 C29 1.546(2) . ?
C8 C30 1.547(2) . ?
C25 H25 0.9800 . ?
C25 C24 1.549(2) . ?
C25 C3 1.567(2) . ?
C25 C26 1.585(2) . ?
C7 H7 0.9800 . ?
C7 C24 1.553(2) . ?
C7 C6 1.514(2) . ?
C9 C1 1.397(2) . ?
C9 C5 1.516(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C1 C10 1.447(2) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 C21 1.504(3) . ?
C3 C2 1.530(2) . ?
C3 C14 1.552(2) . ?
C3 C4 1.552(2) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 C26 1.538(2) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 C11 1.535(2) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 C11 1.528(2) . ?
C21 C23 1.505(2) . ?
C21 C20 1.333(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.535(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C15 H15 0.9800 . ?
C15 C26 1.555(2) . ?
C15 C16 1.550(2) . ?
C26 C27 1.537(2) . ?
C16 C17 1.527(2) . ?
C16 C18 1.532(3) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C4 C5 1.553(2) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C5 C6 1.528(2) . ?
C5 C19 1.560(2) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C20 H20 0.9300 . ?
C20 C19 1.505(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C10 C11 1.513(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C11 H11 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O5 0.82 1.63 2.3760(17) 149.8 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 C10 C11 C12 78.47(18) . . . . ?
O5 C10 C11 C13 -42.4(2) . . . . ?
O1 C4 C5 C9 161.37(14) . . . . ?
O1 C4 C5 C6 -77.71(17) . . . . ?
O1 C4 C5 C19 40.08(19) . . . . ?
O4 C9 C1 C8 -176.42(13) . . . . ?
O4 C9 C1 C10 -3.5(2) . . . . ?
O4 C9 C5 C4 -78.76(16) . . . . ?
O4 C9 C5 C6 162.99(12) . . . . ?
O4 C9 C5 C19 41.59(16) . . . . ?
C8 C7 C24 C25 48.6(2) . . . . ?
C8 C7 C6 C5 -66.04(16) . . . . ?
C8 C1 C10 O5 177.61(15) . . . . ?
C8 C1 C10 C11 -4.5(2) . . . . ?
C25 C3 C2 O2 -6.7(2) . . . . ?
C25 C3 C2 O3 176.99(12) . . . . ?
C25 C3 C14 C15 -8.32(16) . . . . ?
C25 C3 C4 O1 116.81(16) . . . . ?
C25 C3 C4 C5 -58.34(17) . . . . ?
C7 C8 C1 C9 -18.56(19) . . . . ?
C7 C8 C1 C10 169.17(14) . . . . ?
C9 C1 C10 O5 5.0(2) . . . . ?
C9 C1 C10 C11 -177.12(15) . . . . ?
C9 C5 C6 C7 46.58(17) . . . . ?
C9 C5 C19 C20 54.53(17) . . . . ?
C24 C25 C3 C2 -138.50(13) . . . . ?
C24 C25 C3 C14 104.69(14) . . . . ?
C24 C25 C3 C4 -15.83(17) . . . . ?
C24 C25 C26 C28 35.14(19) . . . . ?
C24 C25 C26 C15 -87.43(15) . . . . ?
C24 C25 C26 C27 153.14(13) . . . . ?
C24 C7 C6 C5 65.66(17) . . . . ?
C1 C8 C7 C24 -80.70(16) . . . . ?
C1 C8 C7 C6 49.40(16) . . . . ?
C1 C9 C5 C4 102.21(17) . . . . ?
C1 C9 C5 C6 -16.0(2) . . . . ?
C1 C9 C5 C19 -137.44(15) . . . . ?
C1 C10 C11 C12 -99.58(19) . . . . ?
C1 C10 C11 C13 139.59(16) . . . . ?
C22 C21 C20 C19 0.4(3) . . . . ?
C3 C25 C24 C7 73.70(19) . . . . ?
C3 C25 C26 C28 159.26(13) . . . . ?
C3 C25 C26 C15 36.69(14) . . . . ?
C3 C25 C26 C27 -82.74(14) . . . . ?
C3 C14 C15 C26 31.71(15) . . . . ?
C3 C14 C15 C16 163.84(12) . . . . ?
C3 C4 C5 C9 -23.33(19) . . . . ?
C3 C4 C5 C6 97.60(15) . . . . ?
C3 C4 C5 C19 -144.62(13) . . . . ?
C2 C3 C14 C15 -128.82(13) . . . . ?
C2 C3 C4 O1 -118.05(16) . . . . ?
C2 C3 C4 C5 66.80(17) . . . . ?
C21 C20 C19 C5 104.82(19) . . . . ?
C14 C3 C2 O2 109.35(17) . . . . ?
C14 C3 C2 O3 -66.97(15) . . . . ?
C14 C3 C4 O1 -1.1(2) . . . . ?
C14 C3 C4 C5 -176.26(12) . . . . ?
C14 C15 C26 C25 -41.96(14) . . . . ?
C14 C15 C26 C28 -162.89(13) . . . . ?
C14 C15 C26 C27 74.97(15) . . . . ?
C14 C15 C16 O6 -55.87(17) . . . . ?
C14 C15 C16 C17 -175.85(15) . . . . ?
C14 C15 C16 C18 62.43(17) . . . . ?
C23 C21 C20 C19 -178.74(16) . . . . ?
C26 C25 C24 C7 -168.06(14) . . . . ?
C26 C25 C3 C2 99.03(13) . . . . ?
C26 C25 C3 C14 -17.77(15) . . . . ?
C26 C25 C3 C4 -138.29(12) . . . . ?
C26 C15 C16 O6 66.22(18) . . . . ?
C26 C15 C16 C17 -53.8(2) . . . . ?
C26 C15 C16 C18 -175.47(15) . . . . ?
C16 C15 C26 C25 -167.43(13) . . . . ?
C16 C15 C26 C28 71.64(19) . . . . ?
C16 C15 C26 C27 -50.50(18) . . . . ?
C4 C3 C2 O2 -131.67(16) . . . . ?
C4 C3 C2 O3 52.02(16) . . . . ?
C4 C3 C14 C15 113.54(13) . . . . ?
C4 C5 C6 C7 -75.86(15) . . . . ?
C4 C5 C19 C20 177.80(13) . . . . ?
C29 C8 C7 C24 45.72(17) . . . . ?
C29 C8 C7 C6 175.82(13) . . . . ?
C29 C8 C1 C9 -139.74(15) . . . . ?
C29 C8 C1 C10 48.0(2) . . . . ?
C5 C9 C1 C8 2.5(2) . . . . ?
C5 C9 C1 C10 175.43(14) . . . . ?
C31 O3 C2 O2 0.0(2) . . . . ?
C31 O3 C2 C3 176.49(13) . . . . ?
C6 C7 C24 C25 -80.76(18) . . . . ?
C6 C5 C19 C20 -67.14(17) . . . . ?
C19 C5 C6 C7 167.73(13) . . . . ?
C30 C8 C7 C24 161.13(13) . . . . ?
C30 C8 C7 C6 -68.77(16) . . . . ?
C30 C8 C1 C9 99.55(17) . . . . ?
C30 C8 C1 C10 -72.72(19) . . . . ?
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 -12 0 16235.1 266.009 45
0 -12 -1 2052.25 93.0286 4
0 -12 -1 2006.41 93.2569 45
0 -12 2 2545.67 100.341 45
0 -11 0 40.4452 50.0368 53
0 -11 0 17.7344 61.604 45
0 -11 -1 6334.13 220.824 4
0 -11 1 5780.25 210.168 4
0 -11 -1 6072.44 207.326 53
0 -11 -2 6138.94 211.713 53
0 -11 2 6341.11 213.32 4
0 -11 2 5823.82 178.962 53
0 -11 -2 6475.73 221.574 4
0 -11 2 6138.24 214.044 45
0 -11 -3 7201.71 231.215 39
0 -11 -3 6973.16 216.484 4
0 -11 4 14179.4 267.899 40
0 -11 -4 15561.8 333.136 39
0 -11 4 14753.3 280.926 4
0 -11 4 14571.5 303.772 45
0 -11 -4 15743.8 298.688 4
0 -11 5 9674.93 194.436 4
0 -11 5 10487.4 233.785 45
0 -11 5 10071.5 223.904 40
0 -11 -5 10830.9 268.811 39
0 -11 -5 9659.52 199.782 4
0 -11 6 1046.24 72.2533 40
0 -11 6 1067.76 79.082 36
0 -11 7 6877.47 159.097 36
0 -11 -7 5917.62 165.479 39
0 -10 0 63469.8 831.667 39
0 -10 1 3644.35 201.591 4
0 -10 1 3506.55 183.651 53
0 -10 -1 3821.65 205.496 39
0 -10 -1 3749.16 207.979 4
0 -10 2 823.552 97.5132 53
0 -10 2 810.78 99.1235 40
0 -10 -2 906.496 119.348 39
0 -10 2 776.981 107.863 4
0 -10 -2 897.701 114.371 4
0 -10 3 20641.3 434.77 4
0 -10 -3 21152.5 476.596 39
0 -10 3 19520.7 394.706 53
0 -10 -3 21601.8 460.247 4
0 -10 3 20652.6 452.032 45
0 -10 3 19916.4 433.143 40
0 -10 4 5069.68 206.772 4
0 -10 -4 5171.3 215.216 4
0 -10 -4 5218.64 240.088 39
0 -10 4 5082.83 228.841 40
0 -10 4 5068.25 219.366 45
0 -10 4 4803.61 181.618 53
0 -10 5 24914.7 420.978 4
0 -10 5 26610.6 507.786 40
0 -10 5 26055.5 464.756 45
0 -10 6 9017.95 217.407 4
0 -10 6 9197.85 255.532 45
0 -10 6 9740.87 301.364 40
0 -10 7 13271.2 304.303 36
0 -10 7 13161.5 331.105 40
0 -10 -7 14017.1 341.703 39
0 -10 8 7494.3 232.93 40
0 -10 8 7169.92 201.21 36
0 -10 -8 7217.03 224.201 39
0 -10 9 7358.95 168.273 36
0 -10 9 7755.61 211.484 40
0 -9 0 36.3908 66.9374 39
0 -9 0 83.803 59.7465 40
0 -9 0 65.6457 74.2022 46
0 -9 1 6811.95 278.141 39
0 -9 1 6651.87 267.612 40
0 -9 1 7245.64 292.896 4
0 -9 -1 7066.24 291.126 4
0 -9 1 6961.79 295.416 46
0 -9 -1 6704.69 283.602 39
0 -9 -1 7012.83 278.311 46
0 -9 2 41201.5 699.485 40
0 -9 2 40802.8 656.48 53
0 -9 -2 41553.7 649.985 46
0 -9 2 44121.3 701.561 4
0 -9 -2 43629.2 713.893 4
0 -9 2 43309.4 745.318 46
0 -9 -2 43261.8 726.025 39
0 -9 3 18294.2 482.928 40
0 -9 -3 19575.6 449.888 27
0 -9 3 19324.1 451.107 4
0 -9 3 19920.2 503.848 46
0 -9 -3 19869.9 501.119 39
0 -9 3 18670.5 425.002 53
0 -9 -3 20744.8 483.095 4
0 -9 -4 23243.3 500.532 27
0 -9 -4 23221 540.592 39
0 -9 -4 24031.2 500.661 4
0 -9 4 24818 565.457 40
0 -9 4 23755.2 508.196 45
0 -9 4 24197.7 486.711 4
0 -9 4 24028.2 563.908 46
0 -9 4 23580.4 462.085 53
0 -9 -4 22741.1 441.664 37
0 -9 5 6104.28 252.358 45
0 -9 -5 5682.14 252.134 27
0 -9 -5 5885.1 231.94 37
0 -9 5 6269.68 236.535 4
0 -9 5 6215.62 289.993 40
0 -9 -5 6087.91 243.481 4
0 -9 5 6006.37 219.186 53
0 -9 6 7610.51 266.393 45
0 -9 6 6951.69 228.294 4
0 -9 6 7767.85 318.551 40
0 -9 -6 6811.92 289.329 39
0 -9 -6 6782.45 277.973 27
0 -9 -6 6472.54 228.557 4
0 -9 -6 6784.65 252.975 37
0 -9 7 6158.33 281.753 40
0 -9 -7 6108.05 263.223 27
0 -9 7 5856.85 220.489 45
0 -9 -7 6147.56 269.666 39
0 -9 -7 6317 243.641 37
0 -9 -8 3429.14 195.225 39
0 -9 -8 3430.11 179.411 37
0 -9 8 3290.65 205.92 40
0 -9 8 3297.25 171.983 36
0 -9 -8 3543.9 195.57 27
0 -9 9 729.38 81.7278 36
0 -9 -9 638.49 86.0476 37
0 -9 -9 607.945 89.6521 39
0 -9 -9 582.675 90.4768 27
0 -9 10 1310.76 83.8761 36
0 -9 -10 1374.29 102.873 37
0 -9 -10 1291.05 100.925 39
0 -9 -10 1456.47 112.19 27
0 -9 11 2946.1 132.591 40
0 -9 -11 2662.28 109.766 39
0 -9 -11 3112.01 129.486 37
0 -8 0 5328.72 249.396 46
0 -8 0 5020.08 229.583 40
0 -8 0 5244.25 244.265 39
0 -8 -1 35425.9 637.091 4
0 -8 1 38727 685.145 41
0 -8 1 36310.2 667.816 46
0 -8 1 37202.2 631.373 39
0 -8 1 35458.7 641.673 40
0 -8 -1 35060.9 583.11 27
0 -8 -1 35652.3 626 46
0 -8 1 36682.8 634.762 4
0 -8 -1 36773.9 649.558 39
0 -8 -2 3421.82 190.16 27
0 -8 -2 3651.07 212.252 39
0 -8 2 4362.53 223.667 4
0 -8 2 4439.13 218.539 39
0 -8 2 4264.39 243.218 46
0 -8 -2 3280 203 4
0 -8 -2 3418.66 191.918 46
0 -8 2 4371.67 244.164 41
0 -8 2 4092.67 231.388 40
0 -8 3 30118.4 543.284 53
0 -8 -3 28996.6 564.321 27
0 -8 3 31463.5 579.018 4
0 -8 -3 29704.2 574.504 4
0 -8 3 30910.4 634.499 46
0 -8 -3 28370.2 506.001 37
0 -8 -3 29381.4 595.938 39
0 -8 3 30606 632.064 40
0 -8 -4 18282.3 438.782 4
0 -8 4 15914.1 395.735 4
0 -8 4 14690.1 373.138 53
0 -8 -4 17142.2 410.434 37
0 -8 4 16058.6 434.239 19
0 -8 4 14937.6 458.728 40
0 -8 -4 17837 452.695 27
0 -8 4 14686.1 445.355 46
0 -8 5 42046.5 634.276 4
0 -8 -5 41153.2 723.308 27
0 -8 5 40653.3 614.351 53
0 -8 -5 42062.1 657.222 4
0 -8 5 41830 675.091 45
0 -8 -5 40611.7 623.378 51
0 -8 5 41813.6 715.79 19
0 -8 -5 40440.8 667.082 37
0 -8 5 41845.4 777.636 40
0 -8 6 17235.9 447.384 19
0 -8 6 15702.9 364.455 4
0 -8 6 16456 366.602 53
0 -8 -6 16398.4 402.465 51
0 -8 -6 16505.1 453.948 27
0 -8 -6 15953.4 379.778 4
0 -8 -6 16755.4 439.202 37
0 -8 6 17080.9 502.007 40
0 -8 6 17190.9 415.437 45
0 -8 6 17526.9 478.53 46
0 -8 -6 16927.9 470.077 39
0 -8 -7 16269.5 454.571 39
0 -8 -7 16540.4 455.238 27
0 -8 7 17693.7 409.104 45
0 -8 7 17206.1 434.966 19
0 -8 -7 17132.3 421.355 51
0 -8 -7 17577.2 454.048 37
0 -8 7 18237.2 513.662 40
0 -8 8 16984.7 414.043 19
0 -8 -8 18327.6 482.623 27
0 -8 -8 17875.2 465.038 39
0 -8 -8 18211.9 459.715 37
0 -8 9 12769.4 334.27 36
0 -8 -9 11810 375.672 27
0 -8 9 12707.5 337.469 19
0 -8 -9 12623.5 373.184 39
0 -8 -9 12345.7 373.12 37
0 -8 -9 12046.3 350.066 51
0 -8 -10 6921.9 268.457 37
0 -8 -10 6612.96 253.888 39
0 -8 10 6901.55 225.569 19
0 -8 10 6867.91 221.642 36
0 -8 -10 6754.91 253.363 51
0 -8 10 6938.6 280.265 40
0 -8 11 4075.08 144.469 36
0 -8 -11 4650.4 187.482 39
0 -8 -11 4265.86 199.462 27
0 -8 -11 4787.66 172.668 29
0 -8 11 4338.1 202.548 40
0 -8 -11 4957.27 211.14 37
0 -8 -11 4838.29 199.335 51
0 -8 -12 2052.95 115.921 51
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