#------------------------------------------------------------------------------
#$Date: 2024-02-05 13:06:14 +0100 (Mon, 05 Feb 2024) $
#$Revision: 289687 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022985.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_2022985
loop_
_publ_author_name
'Sadikhova, Nurlana D.'
'Atioğlu, Zeliha'
'Guliyeva, Narmina A.'
'Podrezova, Alexandra G.'
'Nikitina, Eugeniya V.'
'Akkurt, Mehmet'
'Bhattarai, Ajaya'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of dieth-yl
(3aS,3a1R,4S,5S,6R,6aS,7R,9aS)-3a1,5,6,6a-tetra-hydro-1H,3H,4H,7H-3a,6:7,9a-di-epoxy-benzo[de]isochromene-4,5-di-carboxyl-ate.
;
_journal_coeditor_code JY2042
_journal_issue 'Pt 1'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 83
_journal_page_last 87
_journal_paper_doi 10.1107/S2056989023010794
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C18 H22 O7'
_chemical_formula_moiety 'C18 H22 O7'
_chemical_formula_sum 'C18 H22 O7'
_chemical_formula_weight 350.35
_chemical_name_systematic
'Diethyl (3aS,3a1R,4S,5S,6R,6aS,7R,9aS)-3a1,5,6,6a-tetrahydro-1H,3H,4H,7H-3a,6:7,9a-diepoxybenzo[de]isochromene-4,5-dicarboxylate'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 91.329(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.1566(4)
_cell_length_b 14.1907(9)
_cell_length_c 16.2737(10)
_cell_measurement_reflns_used 5852
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 29.93
_cell_measurement_theta_min 2.50
_cell_volume 1652.27(17)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker KAPPA APEXII area-detector diffractometer'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0511
_diffrn_reflns_av_unetI/netI 0.0421
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 28552
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.264
_diffrn_reflns_theta_min 2.871
_exptl_absorpt_coefficient_mu 0.109
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9411
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015).
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.408
_exptl_crystal_description bulk
_exptl_crystal_F_000 744
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.360
_exptl_crystal_size_min 0.340
_refine_diff_density_max 0.349
_refine_diff_density_min -0.296
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 226
_refine_ls_number_reflns 4921
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.026
_refine_ls_R_factor_all 0.0709
_refine_ls_R_factor_gt 0.0459
_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^)+(0.0541P)^2^+0.5731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1040
_refine_ls_wR_factor_ref 0.1185
_reflns_number_gt 3615
_reflns_number_total 4921
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jy2042sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022985.cif.'
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2022985
_cod_database_fobs_code 2022985
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.958
_shelx_estimated_absorpt_t_max 0.964
_shelx_hkl_file
;
-2 0 0 769.234 19.1064 1
-2 0 0 763.271 17.5911 5
-2 0 0 764.621 18.0743 6
-2 0 0 771.322 19.1804 9
-2 0 0 765.326 17.8238 12
2 0 0 777.096 19.5487 7
2 0 0 765.575 19.0363 13
-3 0 0 612.975 15.2661 6
3 0 0 610.615 16.6573 13
-3 0 0 632.032 16.9422 9
4 0 0 343.491 11.3553 13
-4 0 0 348.379 11.6289 9
-4 0 0 342.828 9.62436 6
-5 0 0 702.749 20.6526 9
5 0 0 650.871 19.9266 13
-6 0 0 20.8845 4.06555 9
6 0 0 18.1248 3.82588 13
-7 0 0 94.5917 7.34857 9
7 0 0 78.2140 6.22991 13
8 0 0 17.7247 5.52326 2
-8 0 0 15.6090 4.08569 9
8 0 0 8.03348 3.73951 13
9 0 0 41.5922 6.51222 13
9 0 0 18.0150 6.31358 2
-9 0 0 33.6485 6.05905 9
-9 0 0 25.7792 4.74560 3
10 0 0 31.1185 6.64186 13
-10 0 0 26.8796 6.41277 9
10 0 0 40.7519 8.14875 2
0 -1 0 0.18920 0.18905 11
0 -1 0 0.00372 0.12291 3
0 -1 0 -0.1441 0.10548 5
0 -1 0 -0.0815 0.09086 4
0 -1 0 -0.0847 0.09685 13
0 -1 0 -0.0038 0.03920 14
0 -1 0 0.07406 0.13662 10
-1 -1 0 1629.33 35.2746 6
-1 -1 0 1514.81 35.6109 1
-2 -1 0 542.570 13.7088 1
2 -1 0 520.885 14.1720 8
-2 -1 0 524.121 12.6033 6
2 -1 0 534.332 13.5390 13
2 -1 0 534.737 14.1057 1
2 -1 0 550.619 14.1509 7
-2 -1 0 537.143 13.8479 1
2 -1 0 555.029 14.3483 14
-2 -1 0 532.142 13.8612 9
-2 -1 0 502.756 12.1643 12
-2 1 0 553.130 14.1261 9
2 1 0 522.531 14.0445 13
2 1 0 497.365 14.2944 7
-2 1 0 528.077 13.9698 1
-2 1 0 543.906 13.2798 6
-2 1 0 524.175 12.9233 5
-3 -1 0 0.70271 1.00652 14
-3 -1 0 1.36239 1.27244 9
-3 -1 0 0.54807 0.55306 6
-3 -1 0 0.76958 1.06519 1
-3 -1 0 0.30064 0.38675 12
-3 -1 0 1.02947 1.20292 1
3 -1 0 0.21721 0.76792 13
3 1 0 -0.2787 0.96374 13
-3 1 0 0.45921 1.26607 9
-3 1 0 -0.0142 0.71451 6
-3 1 0 0.22291 0.60825 5
-4 -1 0 409.513 13.4140 9
-4 -1 0 457.962 11.4115 6
-4 -1 0 445.035 14.1563 14
4 -1 0 428.409 13.1943 13
-4 -1 0 440.296 14.2017 1
4 1 0 440.318 13.8455 13
-4 1 0 405.317 13.6321 9
5 -1 0 216.215 8.88637 13
-5 -1 0 221.038 6.86053 6
-5 -1 0 219.753 9.27638 9
-5 1 0 222.137 9.63151 9
5 1 0 222.198 9.57756 13
6 -1 0 51.1415 5.29895 13
6 -1 0 42.5215 5.54694 2
-6 -1 0 43.9598 5.37346 9
6 1 0 40.0379 5.09677 13
-6 1 0 48.8519 5.45959 9
-7 -1 0 -1.7616 2.44180 9
7 -1 0 2.26546 2.49001 2
7 -1 0 -1.3808 2.29043 13
7 1 0 0.03058 2.48029 13
-7 1 0 -1.2355 1.85118 9
8 -1 0 9.90945 3.86097 2
8 -1 0 11.5790 3.76328 13
-8 -1 0 3.19710 2.37897 9
8 1 0 3.89324 2.64273 13
-8 1 0 9.97841 4.25540 9
-8 1 0 11.1090 3.45661 3
9 -1 0 66.0262 8.98031 2
9 -1 0 54.4448 7.16111 13
-9 -1 0 59.5574 8.01470 9
9 1 0 55.3268 7.40539 13
-9 1 0 53.1394 6.71568 3
-9 1 0 50.6424 7.62666 9
10 -1 0 50.5574 8.21673 2
10 -1 0 50.2574 7.65004 13
-10 -1 0 47.9552 7.39466 9
10 1 0 35.7402 6.96277 13
-10 1 0 44.6430 7.29003 9
0 -2 0 389.401 9.76485 3
0 -2 0 391.138 9.75253 11
0 -2 0 398.188 9.78982 5
1 -2 0 2540.95 56.6460 7
1 -2 0 2563.08 57.1150 9
-1 -2 0 2511.06 56.4432 11
-1 -2 0 2548.21 57.0696 4
-1 -2 0 2610.03 57.0986 13
1 -2 0 2434.86 56.8312 1
-1 -2 0 2279.51 55.9688 1
-1 -2 0 2549.92 56.1430 5
2 -2 0 10.8002 1.61034 7
-2 -2 0 9.50290 1.38456 9
-2 -2 0 10.8639 0.94218 6
2 -2 0 9.42585 1.18616 13
2 -2 0 12.8636 1.71645 1
2 -2 0 12.3833 1.77622 8
2 -2 0 11.8479 1.85461 14
-2 -2 0 10.5654 0.59972 5
-2 -2 0 10.0508 1.39866 1
-2 -2 0 8.84044 1.25421 1
-2 2 0 12.8716 1.72895 9
2 2 0 11.7290 1.66948 13
-2 2 0 10.0398 1.50311 3
-2 2 0 9.45282 1.26240 5
-3 -2 0 4.00046 0.73983 6
-3 -2 0 3.13263 0.42492 12
-3 -2 0 1.16554 1.13358 1
-3 -2 0 2.35706 1.08632 1
3 -2 0 2.47418 1.30182 14
-3 -2 0 3.97768 1.24217 9
3 -2 0 3.12604 1.33398 8
3 -2 0 2.48874 1.14592 13
-3 2 0 3.77368 1.37447 9
3 2 0 3.47327 1.80892 13
-3 2 0 5.00079 1.12794 5
4 -2 0 39.6687 3.20203 13
-4 -2 0 46.9863 3.78360 1
-4 -2 0 39.1153 3.29200 9
-4 -2 0 41.5534 2.16001 6
-4 2 0 41.9021 2.57362 5
-4 2 0 47.2765 3.80767 9
4 2 0 43.9779 4.34138 13
-5 -2 0 2.06984 0.88908 6
-5 -2 0 4.24417 1.79942 9
5 -2 0 1.13316 1.83130 13
-5 -2 0 3.66851 2.19221 1
5 2 0 2.73208 1.95338 13
-5 2 0 2.99460 1.82067 9
-6 -2 0 263.411 11.3673 1
6 -2 0 275.367 10.8711 13
-6 -2 0 237.371 10.8333 9
-6 2 0 272.442 11.8180 9
6 2 0 273.948 11.9001 13
-7 -2 0 19.0307 4.45632 1
-7 -2 0 25.2637 4.43012 9
7 -2 0 24.4319 4.48629 2
7 -2 0 17.1776 3.81632 13
7 2 0 19.5828 4.30018 13
-7 2 0 18.9069 3.80868 3
-7 2 0 18.6474 4.05917 9
-8 -2 0 17.4417 4.70610 1
-8 -2 0 20.9063 4.37641 9
8 -2 0 20.8815 4.39019 13
8 -2 0 29.7814 6.00619 2
-8 2 0 14.4966 3.93929 3
8 2 0 26.8962 5.38338 13
-8 2 0 24.3547 5.24716 9
-9 -2 0 0.27739 3.36944 9
9 -2 0 -0.8752 2.61680 13
9 -2 0 -1.5331 2.53547 2
-9 2 0 7.74474 4.34845 9
9 2 0 -3.9279 2.80410 13
-9 2 0 -0.6391 2.51963 3
-10 -2 0 7.09756 5.12865 9
10 -2 0 31.0036 7.30619 2
10 2 0 29.9102 6.64439 13
-10 2 0 22.1162 6.10978 9
0 -3 0 -0.6754 0.54391 14
0 -3 0 -0.0185 0.52416 5
0 -3 0 0.06866 0.28084 1
0 -3 0 -0.1952 0.22771 1
0 -3 0 0.25292 0.63209 4
0 -3 0 -0.2745 0.51972 13
0 -3 0 0.05338 0.70020 11
0 -3 0 -0.2331 0.64611 10
0 -3 0 0.23262 0.52354 3
-1 -3 0 72.9842 2.93346 11
-1 -3 0 73.1563 2.12180 1
1 -3 0 71.8152 3.14963 14
1 -3 0 74.4801 3.34198 9
1 -3 0 80.5502 3.14775 1
-1 -3 0 73.4201 2.94801 3
-1 -3 0 71.2113 2.13283 1
-1 -3 0 76.2805 3.37015 4
-1 -3 0 67.9002 3.15336 10
-1 -3 0 71.9102 2.77459 5
1 -3 0 74.2659 3.01893 1
-1 -3 0 71.2864 3.28616 13
1 -3 0 70.7723 3.02419 8
1 -3 0 76.2966 2.98595 7
-1 3 0 77.3833 3.32204 5
2 -3 0 1.22782 0.93190 14
2 -3 0 1.49453 1.09366 8
-2 -3 0 0.54995 1.01882 7
2 -3 0 1.97701 1.04550 7
-2 -3 0 0.97915 0.75263 9
2 -3 0 0.49804 0.69164 13
2 -3 0 0.29618 1.07251 1
-2 -3 0 0.79500 0.65713 1
-2 -3 0 0.08128 0.73908 1
-2 -3 0 0.21947 0.48373 5
-2 3 0 0.54454 0.85137 3
-2 3 0 0.44598 0.93715 5
-3 -3 0 10.5896 2.90714 7
3 -3 0 10.1954 1.60371 13
3 -3 0 12.4939 2.31873 14
3 -3 0 10.5661 1.91374 8
-3 -3 0 12.1552 2.09209 9
-3 -3 0 11.8768 1.20957 6
-3 -3 0 9.02136 0.81394 12
-3 -3 0 9.80066 1.68705 1
-3 -3 0 11.2743 1.69118 1
-3 3 0 11.6262 1.73782 5
-3 3 0 8.79814 1.76372 3
-3 3 0 12.6602 2.33673 9
3 3 0 12.8305 2.24940 13
4 -3 0 103.551 5.94690 14
4 -3 0 110.932 6.12839 8
-4 -3 0 112.818 5.62515 1
4 -3 0 109.095 5.04621 13
-4 -3 0 106.090 3.77285 6
-4 -3 0 115.824 5.64778 9
-4 3 0 107.326 5.59853 3
-4 3 0 97.9527 5.71491 9
4 3 0 110.949 6.22745 13
-4 3 0 112.289 4.84836 5
-5 -3 0 57.0556 4.68995 9
5 -3 0 56.1916 4.13541 13
-5 -3 0 49.5028 2.45004 6
-5 -3 0 46.4002 4.09534 1
5 3 0 62.5044 5.39405 13
-5 3 0 50.3203 4.52831 3
-5 3 0 56.5535 4.76707 9
-6 -3 0 163.544 8.66811 9
6 -3 0 152.053 7.72340 13
-6 -3 0 166.879 8.78160 1
-6 3 0 160.767 8.50029 3
-6 3 0 178.039 9.56449 9
6 3 0 146.175 8.84702 13
7 -3 0 63.6347 5.44894 13
-7 -3 0 43.4495 5.90345 1
-7 -3 0 53.3794 6.01606 9
-7 3 0 55.1794 6.85924 9
7 3 0 61.2944 7.06654 13
-7 3 0 59.3338 6.30198 3
-8 -3 0 2.75318 2.60698 9
8 -3 0 -0.8571 3.44590 2
-8 -3 0 -0.3969 2.99365 1
8 -3 0 4.91976 2.99164 13
-8 3 0 1.00970 2.69471 3
8 3 0 9.08436 3.99146 13
-8 3 0 -0.4640 3.17138 9
-9 -3 0 7.35595 3.98303 1
9 -3 0 0.13585 2.63507 13
-9 -3 0 0.78087 3.23571 9
9 -3 0 2.89400 4.06204 2
9 3 0 -2.2804 3.55033 13
-9 3 0 1.29456 3.75268 9
-9 3 0 8.31203 3.49402 3
10 -3 0 67.7541 9.34687 2
-10 -3 0 80.6740 9.72871 9
-10 3 0 84.6300 9.94552 9
10 3 0 71.8840 9.66933 13
0 -4 0 2963.43 67.4105 10
0 -4 0 3026.07 67.0109 13
0 -4 0 2840.59 66.1217 1
0 -4 0 3064.36 67.7069 14
0 -4 0 2816.15 66.0949 1
0 -4 0 2907.29 67.5762 11
0 -4 0 3098.63 67.0468 4
0 -4 0 3048.61 67.7153 3
0 -4 0 2879.63 67.5558 8
0 -4 0 2960.87 67.6835 5
-1 -4 0 27.0219 0.89018 1
-1 -4 0 24.7512 2.16752 13
-1 -4 0 25.6813 1.81714 11
-1 -4 0 27.0851 1.95430 3
-1 -4 0 27.1167 2.30145 4
-1 -4 0 22.2468 1.88206 10
1 -4 0 27.6760 2.07992 14
1 -4 0 25.9079 1.86406 1
-1 -4 0 25.9765 0.90161 1
1 -4 0 24.9064 1.87761 1
-1 -4 0 27.1416 1.90306 5
1 -4 0 23.8892 1.88466 7
1 -4 0 30.8308 2.09144 8
-1 4 0 26.0174 2.09465 5
-2 -4 0 46.3058 3.33428 7
2 -4 0 50.2265 3.34119 14
-2 -4 0 47.7928 2.22586 1
2 -4 0 50.3582 3.05171 8
-2 -4 0 47.0353 2.63261 11
-2 -4 0 46.1306 2.28507 5
2 -4 0 44.1315 3.16534 1
-2 -4 0 48.2670 2.32006 1
2 -4 0 53.8720 3.26521 1
2 -4 0 48.7262 2.84327 7
-2 -4 0 46.7048 2.81700 9
-2 -4 0 50.7314 2.69900 3
-2 4 0 46.5471 3.02726 5
-2 4 0 51.8529 3.39809 3
-3 -4 0 136.581 5.15473 1
-3 -4 0 132.502 4.56010 6
-3 -4 0 135.757 4.05866 5
3 -4 0 134.270 4.88919 13
-3 -4 0 149.813 5.50804 1
-3 -4 0 134.738 5.74500 9
-3 -4 0 140.101 6.73635 7
3 -4 0 127.426 6.08750 14
3 -4 0 137.148 6.12101 8
-3 4 0 139.007 5.66122 5
-3 4 0 144.059 6.28918 3
-4 -4 0 10.9657 2.12606 1
-4 -4 0 8.85737 2.80654 7
-4 -4 0 9.17692 2.36464 9
4 -4 0 10.9131 2.40994 14
-4 -4 0 9.11565 1.20880 6
4 -4 0 13.0339 2.06137 13
-4 -4 0 9.59905 0.75610 12
-4 -4 0 11.4575 2.00713 1
4 -4 0 6.77686 2.27784 8
-4 -4 0 10.0640 0.79138 12
-4 4 0 9.20900 2.49648 3
-4 4 0 10.7662 2.02591 5
4 4 0 9.04367 2.38531 13
-4 4 0 9.96179 2.71662 9
5 -4 0 109.797 6.82363 14
-5 -4 0 98.8769 6.05383 1
-5 -4 0 106.307 6.31592 9
-5 -4 0 103.894 3.79250 6
5 -4 0 91.7488 5.15055 13
-5 4 0 105.962 6.33368 3
5 4 0 115.391 6.93642 13
-5 4 0 112.262 6.79742 9
-6 -4 0 7.17867 2.43588 9
-6 -4 0 13.3648 3.39468 1
6 -4 0 17.5258 3.09580 13
6 4 0 14.9645 3.56120 13
-6 4 0 12.9307 3.33939 9
-6 4 0 15.5913 3.62939 3
7 -4 0 19.5000 3.89117 13
-7 -4 0 22.3132 4.35973 1
-7 -4 0 15.4773 3.54732 9
-7 4 0 16.0851 4.03797 3
7 4 0 19.1372 4.72061 13
-7 4 0 21.0528 4.79547 9
-8 -4 0 17.8748 4.67436 9
8 -4 0 8.10003 3.56298 2
-8 -4 0 17.0216 4.56259 1
8 -4 0 13.0743 3.52981 13
8 4 0 10.7030 4.30508 13
-8 4 0 14.4059 3.96822 3
-8 4 0 13.2316 3.78613 9
9 -4 0 5.04676 3.75852 2
-9 -4 0 -2.1047 3.09221 1
-9 -4 0 1.20561 3.59917 9
-9 4 0 4.61608 3.01639 9
-9 4 0 3.14870 3.16643 3
9 4 0 -0.1824 2.79295 13
0 -5 0 0.27031 0.69673 10
0 -5 0 0.14067 0.86225 4
0 -5 0 -0.3709 0.96275 8
0 -5 0 0.13220 0.47578 1
0 -5 0 0.74231 1.07727 14
0 -5 0 1.64272 0.85815 13
0 -5 0 -0.3462 0.42454 1
1 -5 0 60.9775 2.94152 1
1 -5 0 57.0868 2.90425 1
1 -5 0 60.9699 3.09567 7
1 -5 0 61.8721 3.21539 8
1 -5 0 64.3031 3.53039 14
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-1 7 -20 1.66231 3.34903 10
2 -7 20 35.1579 6.84425 6
-2 7 -20 42.2972 7.38754 10
2 7 20 43.0490 7.73070 11
3 -7 20 2.78260 4.57224 6
-3 -7 -20 -7.3720 3.90195 1
-3 7 -20 0.60571 3.89201 10
3 7 20 1.36975 4.45189 11
-3 -8 20 0.20191 3.55710 1
3 8 -20 3.89194 4.03815 4
-3 8 20 -1.9122 3.73845 5
-2 -8 20 1.57909 4.17642 1
2 8 -20 2.65717 3.45945 4
-2 8 20 -0.8702 3.18875 5
2 8 -20 8.47624 4.34421 10
-2 8 20 4.72760 3.85627 11
-1 -8 20 19.3713 5.62034 1
-1 -8 20 14.3814 4.74622 6
1 8 -20 14.4552 5.86310 4
-1 8 20 15.4606 5.38633 11
1 8 -20 8.09194 4.73789 10
0 -8 20 6.31275 3.49698 6
0 8 20 -4.4087 3.23690 11
0 8 -20 2.86862 3.96491 10
1 -8 20 33.1046 6.95073 6
-1 8 -20 49.7004 7.83630 10
1 8 20 36.1863 6.58604 11
-2 -8 -20 10.8561 5.31050 1
2 -8 20 13.7420 5.39776 6
2 8 20 4.74871 4.76114 11
-2 8 -20 9.42473 4.80928 10
-2 -9 20 104.473 11.1359 1
2 9 -20 103.467 10.8917 10
2 9 -20 71.0481 9.74947 4
-2 9 20 82.6479 10.3040 5
-2 9 20 97.5376 10.3197 11
-1 -9 20 6.63824 4.13727 6
-1 -9 20 10.3369 5.09347 1
1 9 -20 12.5418 4.51651 10
-1 9 20 9.74289 4.81629 11
0 -9 -20 -0.2655 2.90400 1
0 -9 20 -2.2047 4.03785 1
0 -9 20 -0.8584 3.32549 6
0 9 20 1.01080 3.06747 11
0 9 -20 2.87927 4.04010 10
1 -9 20 3.50700 4.16912 6
-1 -9 -20 -2.1950 3.42611 1
-1 9 -20 -2.7768 3.66531 10
1 9 20 2.18472 3.32152 11
-2 9 -20 4.41137 4.44672 10
0 10 -20 -1.6546 2.63596 10
4 0 -21 2.81783 3.93523 4
3 0 -21 4.43178 3.17039 4
2 0 -21 -2.7317 2.28148 4
1 0 -21 -4.8693 3.27082 4
0 0 -21 -1.8771 2.30419 4
0 0 21 -0.0728 2.57608 11
-1 0 -21 -2.4349 3.88206 4
1 0 21 1.67694 2.77437 11
2 0 21 -0.9348 2.98825 11
3 0 21 1.86603 3.72398 11
4 -1 -21 16.7266 5.11843 4
-4 1 21 24.4412 6.53567 5
4 1 -21 21.7139 5.92463 4
3 -1 -21 94.4598 10.0488 4
3 1 -21 84.2302 9.96462 4
2 -1 -21 6.89405 4.77446 4
2 1 -21 5.67504 4.64179 4
1 -1 -21 -6.8033 3.07153 4
1 1 -21 2.53915 2.81986 4
0 -1 -21 10.3417 4.21337 4
0 -1 21 3.04621 3.48218 11
0 1 -21 1.63410 3.17026 4
0 1 21 5.05814 3.40273 11
1 -1 21 -0.2777 2.92477 11
1 1 21 -1.8333 2.17004 11
-1 1 -21 8.68026 4.67644 4
2 -1 21 18.7293 5.10854 6
2 -1 21 32.3296 6.10264 11
2 1 21 18.3849 5.48761 11
3 -1 21 3.47401 3.78394 11
3 -1 21 6.40104 4.79029 6
3 1 21 3.15519 4.20721 11
-4 2 21 4.85813 3.55732 5
4 2 -21 -1.4736 2.63256 4
3 -2 -21 2.62772 3.60793 4
-3 2 21 -5.8154 3.21579 5
3 2 -21 -1.5067 2.42728 4
2 -2 -21 10.8928 4.56848 4
2 2 -21 10.3622 4.99283 4
1 -2 -21 -3.3866 3.45110 4
1 2 -21 6.14643 3.92668 4
0 -2 -21 -3.8763 3.25111 4
0 2 -21 3.54275 3.55209 4
0 2 21 2.36011 3.56019 11
1 -2 21 27.5955 5.93919 6
1 -2 21 33.3507 5.81387 11
1 2 21 33.4339 5.99122 11
-1 2 -21 28.3375 6.91001 4
2 -2 21 6.96621 3.73013 11
2 -2 21 6.22259 4.52648 6
2 2 21 2.73241 3.04847 11
3 -2 21 24.1285 5.16855 11
3 -2 21 21.5300 6.81938 6
3 2 21 18.2406 5.16026 11
4 3 -21 38.7347 8.08459 4
-4 3 21 43.2787 7.58986 5
3 -3 -21 14.3869 4.33276 4
-3 3 21 9.79919 5.08501 5
3 3 -21 11.1060 5.04113 4
2 -3 -21 68.6990 8.24447 4
2 3 -21 48.7456 8.11377 4
-2 3 21 46.5359 8.07528 5
1 -3 -21 4.98801 4.09090 4
1 3 -21 7.92103 3.87474 4
-1 3 21 4.23968 3.81325 11
0 -3 21 16.6320 4.91563 6
0 -3 -21 18.4175 5.51253 4
0 3 -21 16.3738 5.20329 4
0 3 21 12.7937 4.67379 11
1 -3 21 0.97918 2.99855 6
1 -3 21 1.16673 2.93402 11
-1 3 -21 4.63685 4.25240 4
1 3 21 5.41822 4.20665 11
2 -3 21 11.9198 4.27474 11
2 -3 21 12.6833 5.60822 6
-2 3 -21 16.0502 6.27961 4
2 3 21 2.80614 3.11721 11
3 -3 21 28.1315 6.37864 11
3 -3 21 37.1553 7.33115 6
3 3 21 65.1833 8.56119 11
-3 4 21 24.3006 6.69677 5
3 4 -21 37.3468 7.09544 4
2 -4 -21 8.88502 4.07692 4
-2 4 21 9.21536 3.85363 5
2 4 -21 11.1462 4.25359 4
1 -4 -21 1.04425 3.57428 4
-1 -4 21 4.08116 3.64309 6
-1 4 21 7.71358 3.92604 11
1 4 -21 5.52624 3.85967 4
0 -4 -21 46.6658 7.12491 4
0 -4 21 45.7643 7.71987 6
0 4 -21 51.9504 8.45811 4
0 4 21 36.9477 6.43608 11
1 -4 21 48.6891 7.53237 6
1 -4 21 41.8366 6.23950 11
-1 4 -21 36.8463 6.95994 4
1 4 21 40.7410 7.00333 11
2 -4 21 1.46467 3.13685 6
2 -4 21 -1.1334 3.12285 11
-2 4 -21 -3.9612 2.43655 4
2 4 21 1.14322 3.61802 11
3 -4 21 -3.7762 3.83018 6
3 -4 21 2.87046 3.60080 11
3 4 21 4.58943 4.57806 11
3 5 -21 18.1706 5.74636 4
-3 5 21 21.1776 6.44994 5
2 5 -21 4.74749 4.20774 4
-2 5 21 10.5297 4.55572 5
-1 -5 21 -1.8893 3.24107 6
1 -5 -21 -1.0473 3.09337 4
1 5 -21 5.39160 3.78231 10
-1 5 21 -0.9901 2.86864 11
1 5 -21 -0.1310 3.13246 4
0 -5 21 -0.7687 2.77018 6
0 -5 -21 -5.6766 3.15336 4
0 5 -21 -1.6327 3.87406 4
0 5 21 3.13770 3.82234 11
0 5 -21 -0.0891 3.36973 10
1 -5 21 35.0570 7.11828 6
-1 5 -21 42.9975 6.66039 10
-1 5 -21 35.7628 7.02122 4
1 5 21 27.7591 6.33328 11
2 -5 21 20.8949 6.67570 6
2 -5 21 21.2974 5.26643 11
-2 5 -21 22.0997 5.60435 10
2 5 21 21.4366 6.00340 11
3 -5 21 -1.4874 3.31541 6
3 6 -21 31.9604 6.58958 4
-3 6 21 39.4634 7.57445 5
-2 -6 21 -3.1983 2.44108 6
-2 6 21 -5.2603 2.60683 5
2 6 -21 -1.7871 2.77906 4
-1 -6 21 -3.3152 3.22982 6
-1 6 21 4.52009 3.50215 11
1 6 -21 2.15955 4.55614 4
1 6 -21 1.64682 3.19242 10
0 -6 -21 -2.8467 3.44369 4
0 -6 21 1.37704 3.95388 6
0 6 21 1.88149 4.25557 11
0 6 -21 -0.5059 4.49218 4
0 6 -21 -3.4014 3.08968 10
1 -6 21 17.3573 5.38960 6
1 6 21 30.0099 6.53428 11
-1 6 -21 24.3496 5.50068 10
-1 6 -21 19.5574 6.89409 4
2 -6 21 -4.3313 3.22178 11
2 -6 21 0.59293 3.36076 6
-2 6 -21 3.17085 3.70134 10
2 6 21 2.03763 4.55996 11
2 7 -21 6.94223 3.80129 4
-2 7 21 2.87683 3.25718 5
-1 -7 21 23.2223 5.87108 6
-1 7 21 33.2979 6.47621 11
1 7 -21 37.9815 7.69491 4
1 7 -21 28.6918 6.47850 10
0 -7 21 0.04162 3.15718 6
0 7 -21 0.03168 3.58076 4
0 7 21 -2.4834 3.21209 11
0 7 -21 -1.4802 3.29955 10
1 -7 21 16.7421 5.90818 6
-1 7 -21 39.3059 7.11676 10
1 7 21 18.1984 5.19807 11
-2 7 -21 72.6236 9.36919 10
-1 -8 21 18.1458 5.27933 6
1 8 -21 9.36334 4.93505 10
1 8 -21 5.51074 5.12508 4
0 -8 21 -1.0367 3.80958 6
0 8 21 5.08994 3.26332 11
0 8 -21 -3.1918 2.04463 10
3 0 -22 32.7169 6.94681 4
2 0 -22 193.121 13.0927 4
1 0 -22 104.609 10.9764 4
0 0 -22 1.23837 2.88231 4
-1 0 -22 62.4618 9.45563 4
1 0 22 78.3028 8.61655 11
2 0 22 5.77297 3.94073 11
3 -1 -22 63.2097 8.53405 4
3 1 -22 71.0314 8.97256 4
2 -1 -22 -4.1316 3.33033 4
2 1 -22 -3.5351 3.59541 4
1 -1 -22 26.7974 6.45435 4
1 1 -22 8.16162 4.34007 4
0 -1 -22 0.59912 3.64831 4
0 1 -22 -2.0428 2.89957 4
0 1 22 -0.2596 3.26994 11
-1 -1 -22 35.4774 7.65726 4
1 -1 22 66.6856 8.00515 11
-1 1 -22 59.4288 9.16950 4
1 1 22 50.0227 7.41491 11
2 -1 22 58.2629 7.79928 11
2 1 22 63.0359 8.32698 11
3 -2 -22 2.28715 3.67126 4
-3 2 22 -4.9126 3.54152 5
3 2 -22 3.09759 4.25527 4
2 -2 -22 132.582 10.7247 4
2 2 -22 141.821 11.0425 4
1 -2 -22 56.9480 8.49332 4
1 2 -22 59.8806 8.90520 4
0 -2 -22 -0.3987 3.51916 4
0 2 22 -0.0036 3.31537 11
0 2 -22 -0.9786 2.94039 4
1 -2 22 -0.4281 3.20402 6
1 -2 22 6.40821 3.81344 11
-1 2 -22 11.7067 5.65172 4
1 2 22 2.22055 2.85660 11
2 -2 22 24.4138 6.29591 6
2 -2 22 18.4507 5.35818 11
-2 2 -22 17.7197 6.42501 4
2 2 22 11.9115 5.08477 11
2 -3 -22 34.1579 6.74195 4
2 3 -22 40.6415 7.66977 4
-2 3 22 37.6972 7.71985 5
1 -3 -22 -1.8988 3.65542 4
1 3 -22 2.78357 4.60449 4
0 -3 22 9.20772 4.86327 6
0 -3 -22 11.4795 4.90932 4
0 3 -22 13.7727 4.98714 4
0 3 22 10.1593 4.39713 11
1 -3 22 0.63735 2.76558 6
1 -3 22 -1.3910 2.04520 11
1 3 22 -1.3141 3.46269 11
-1 3 -22 3.74882 4.62894 4
2 -3 22 56.4806 8.57380 6
2 -3 22 53.8714 7.62473 11
2 3 22 46.3513 7.27671 11
-2 3 -22 38.5704 8.11378 4
2 4 -22 3.12410 4.33766 4
-2 4 22 1.45648 4.00068 5
1 -4 -22 44.4789 7.45118 4
1 4 -22 27.5869 7.25349 4
0 -4 22 31.5005 6.43496 6
0 -4 -22 50.1142 7.76897 4
0 4 22 33.5079 6.38200 11
0 4 -22 48.3914 8.01729 4
1 -4 22 7.11336 5.20297 6
1 4 22 3.62422 4.38881 11
-1 4 -22 14.0625 5.62353 4
2 -4 22 2.32145 4.87241 6
-1 -5 22 11.6413 4.54322 6
1 -5 -22 5.78331 4.08232 4
-1 5 22 9.08501 3.80311 11
1 5 -22 13.2723 6.19436 4
0 -5 22 55.9805 8.55631 6
0 -5 -22 51.4347 8.05140 4
0 5 -22 48.2206 8.11171 4
0 5 22 34.7099 6.53403 11
1 -5 22 2.91683 3.69181 6
1 5 22 -1.8698 3.40605 11
-1 5 -22 0.81986 3.33244 4
0 0 -23 0.09741 3.24259 4
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 7856
_shelx_res_file
;
TITL PA-79 in P2(1)/c
shelx.res
created by SHELXL-2018/3 at 11:23:56 on 21-Dec-2023
CELL 0.71073 7.1566 14.1907 16.2737 90.000 91.329 90.000
ZERR 4.00 0.0004 0.0009 0.0010 0.000 0.002 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H O
UNIT 72 88 28
MERG 2
OMIT 0 1 1
OMIT 1 1 0
HTAB C3 O13
EQIV $1 -x+1, y-1/2, -z+1/2
HTAB C9 O13_$1
EQIV $2 x, -y+1/2, z-1/2
HTAB C13 O2_$2
HTAB C13 O10_$2
HTAB C14 O15_$1
HTAB
FMAP 2
PLAN 3
SIZE 0.340 0.360 0.400
ACTA
BOND $H
CONF
L.S. 13
TEMP -173.00
WGHT 0.054100 0.573100
FVAR 0.45633
O2 3 0.650031 0.146896 0.397845 11.00000 0.01177 0.02703 =
0.01666 0.00411 -0.00192 0.00225
O10 3 0.322308 0.272159 0.414236 11.00000 0.01298 0.01894 =
0.01102 -0.00185 0.00189 0.00059
O11 3 0.281227 0.085687 0.448806 11.00000 0.01425 0.02044 =
0.01503 0.00331 0.00166 0.00319
O12 3 0.200086 0.287451 0.145092 11.00000 0.01619 0.05364 =
0.01679 -0.00394 -0.00227 0.00014
O13 3 0.510889 0.301907 0.166012 11.00000 0.01360 0.03515 =
0.01206 -0.00418 0.00208 -0.00258
O15 3 0.207491 0.506036 0.328093 11.00000 0.02675 0.01687 =
0.03940 -0.00379 0.00966 -0.00214
O16 3 -0.065446 0.451341 0.374261 11.00000 0.02073 0.01449 =
0.02599 -0.00188 0.00691 0.00475
C1 1 0.567028 0.058982 0.373257 11.00000 0.01423 0.02255 =
0.02041 0.00271 0.00136 0.00704
AFIX 23
H1A 2 0.604785 0.009304 0.412996 11.00000 -1.20000
H1B 2 0.613288 0.040808 0.318629 11.00000 -1.20000
AFIX 0
C3B 1 0.285851 0.151484 0.317374 11.00000 0.01055 0.01499 =
0.01255 -0.00062 -0.00003 0.00161
AFIX 13
H3BA 2 0.276226 0.137729 0.257158 11.00000 -1.20000
AFIX 0
C3A 1 0.397159 0.241331 0.337316 11.00000 0.01129 0.01715 =
0.01020 -0.00123 0.00148 0.00084
C3 1 0.605318 0.223354 0.343888 11.00000 0.01085 0.02438 =
0.01475 0.00336 0.00057 0.00059
AFIX 23
H3A 2 0.652818 0.209205 0.288583 11.00000 -1.20000
H3B 2 0.668881 0.281058 0.364234 11.00000 -1.20000
AFIX 0
C4 1 0.328128 0.323043 0.280485 11.00000 0.01287 0.01481 =
0.01197 -0.00050 0.00172 -0.00050
AFIX 13
H4A 2 0.406592 0.379971 0.292317 11.00000 -1.20000
AFIX 0
C5 1 0.130321 0.340338 0.313900 11.00000 0.01254 0.01428 =
0.01487 -0.00101 0.00193 0.00144
AFIX 13
H5A 2 0.033387 0.321017 0.271973 11.00000 -1.20000
AFIX 0
C6 1 0.128006 0.271880 0.388717 11.00000 0.01145 0.01644 =
0.01535 0.00062 0.00281 0.00237
AFIX 13
H6A 2 0.040849 0.291342 0.432769 11.00000 -1.20000
AFIX 0
C6A 1 0.093896 0.171519 0.356181 11.00000 0.01027 0.01465 =
0.01750 0.00273 0.00158 0.00111
AFIX 13
H6AA 2 -0.012435 0.168001 0.315333 11.00000 -1.20000
AFIX 0
C7 1 0.088274 0.091473 0.421864 11.00000 0.01166 0.01782 =
0.02239 0.00429 0.00233 0.00113
AFIX 13
H7A 2 -0.003793 0.100706 0.466452 11.00000 -1.20000
AFIX 0
C8 1 0.067384 0.000208 0.373335 11.00000 0.02044 0.01551 =
0.03100 0.00488 -0.00313 -0.00267
AFIX 43
H8A 2 -0.041834 -0.037460 0.367396 11.00000 -1.20000
AFIX 0
C9A 1 0.356559 0.065942 0.369214 11.00000 0.01431 0.01637 =
0.01577 0.00028 0.00047 0.00369
C9 1 0.233464 -0.016041 0.340912 11.00000 0.02448 0.01318 =
0.02512 0.00092 -0.00332 0.00301
AFIX 43
H9A 2 0.267854 -0.067681 0.307329 11.00000 -1.20000
AFIX 0
C12 1 0.333748 0.302305 0.189443 11.00000 0.01464 0.01261 =
0.01344 0.00221 0.00071 0.00083
C13 1 0.550020 0.287380 0.079085 11.00000 0.02028 0.02948 =
0.01026 -0.00187 0.00249 0.00354
AFIX 23
H13A 2 0.568211 0.348732 0.051437 11.00000 -1.20000
H13B 2 0.444317 0.254289 0.051389 11.00000 -1.20000
AFIX 0
C14 1 0.724244 0.229181 0.074890 11.00000 0.02763 0.03076 =
0.01944 -0.00067 0.00477 0.00904
AFIX 33
H14A 2 0.754364 0.218155 0.017244 11.00000 -1.50000
H14B 2 0.827848 0.262688 0.102366 11.00000 -1.50000
H14C 2 0.704464 0.168635 0.102318 11.00000 -1.50000
AFIX 0
C15 1 0.100273 0.441869 0.338703 11.00000 0.01804 0.01656 =
0.01325 0.00064 0.00085 0.00349
C16 1 -0.112784 0.545382 0.403268 11.00000 0.02670 0.01540 =
0.02261 -0.00264 0.00133 0.00930
AFIX 23
H16A 2 -0.109745 0.591211 0.357452 11.00000 -1.20000
H16B 2 -0.022582 0.565926 0.446699 11.00000 -1.20000
AFIX 0
C17 1 -0.305809 0.539335 0.436788 11.00000 0.02798 0.03204 =
0.05116 -0.01119 0.01021 0.01146
AFIX 33
H17A 2 -0.343372 0.601375 0.457067 11.00000 -1.50000
H17B 2 -0.393486 0.518921 0.393188 11.00000 -1.50000
H17C 2 -0.306732 0.493754 0.482017 11.00000 -1.50000
AFIX 0
HKLF 4
REM PA-79 in P2(1)/c
REM wR2 = 0.1185, GooF = S = 1.026, Restrained GooF = 1.026 for all data
REM R1 = 0.0459 for 3615 Fo > 4sig(Fo) and 0.0709 for all 4921 data
REM 226 parameters refined using 0 restraints
END
WGHT 0.0541 0.5731
REM Instructions for potential hydrogen bonds
HTAB C3 O13
HTAB C9 O13_$1
HTAB C13 O2_$2
HTAB C13 O10_$2
HTAB C14 O15_$1
REM Highest difference peak 0.349, deepest hole -0.296, 1-sigma level 0.076
Q1 1 0.3239 0.3121 0.2378 11.00000 0.05 0.35
Q2 1 0.4974 0.2354 0.3395 11.00000 0.05 0.34
Q3 1 0.4591 0.0625 0.3759 11.00000 0.05 0.33
;
_shelx_res_checksum 49237
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O2 0.65003(13) 0.14690(7) 0.39784(6) 0.0185(2) Uani d 1 . .
O O10 0.32231(13) 0.27216(6) 0.41424(6) 0.01429(19) Uani d 1 . .
O O11 0.28123(13) 0.08569(7) 0.44881(6) 0.0166(2) Uani d 1 . .
O O12 0.20009(15) 0.28745(9) 0.14509(7) 0.0289(3) Uani d 1 . .
O O13 0.51089(13) 0.30191(7) 0.16601(6) 0.0202(2) Uani d 1 . .
O O15 0.20749(15) 0.50604(7) 0.32809(7) 0.0275(3) Uani d 1 . .
O O16 -0.06545(14) 0.45134(7) 0.37426(6) 0.0203(2) Uani d 1 . .
C C1 0.56703(19) 0.05898(10) 0.37326(9) 0.0190(3) Uani d 1 . .
H H1A 0.604785 0.009304 0.412996 0.023 Uiso calc 1 . .
H H1B 0.613288 0.040808 0.318629 0.023 Uiso calc 1 . .
C C3B 0.28585(17) 0.15148(9) 0.31737(8) 0.0127(2) Uani d 1 . .
H H3BA 0.276226 0.137729 0.257158 0.015 Uiso calc 1 . .
C C3A 0.39716(17) 0.24133(9) 0.33732(8) 0.0129(2) Uani d 1 . .
C C3 0.60532(18) 0.22335(10) 0.34389(8) 0.0167(3) Uani d 1 . .
H H3A 0.652818 0.209205 0.288583 0.020 Uiso calc 1 . .
H H3B 0.668881 0.281058 0.364234 0.020 Uiso calc 1 . .
C C4 0.32813(18) 0.32304(9) 0.28048(8) 0.0132(2) Uani d 1 . .
H H4A 0.406592 0.379971 0.292317 0.016 Uiso calc 1 . .
C C5 0.13032(18) 0.34034(9) 0.31390(8) 0.0139(2) Uani d 1 . .
H H5A 0.033387 0.321017 0.271973 0.017 Uiso calc 1 . .
C C6 0.12801(18) 0.27188(9) 0.38872(8) 0.0144(3) Uani d 1 . .
H H6A 0.040849 0.291342 0.432769 0.017 Uiso calc 1 . .
C C6A 0.09390(18) 0.17152(9) 0.35618(8) 0.0141(2) Uani d 1 . .
H H6AA -0.012435 0.168001 0.315333 0.017 Uiso calc 1 . .
C C7 0.08827(19) 0.09147(9) 0.42186(9) 0.0173(3) Uani d 1 . .
H H7A -0.003793 0.100706 0.466452 0.021 Uiso calc 1 . .
C C8 0.0674(2) 0.00021(10) 0.37333(10) 0.0224(3) Uani d 1 . .
H H8A -0.041834 -0.037460 0.367396 0.027 Uiso calc 1 . .
C C9A 0.35656(18) 0.06594(9) 0.36921(8) 0.0155(3) Uani d 1 . .
C C9 0.2335(2) -0.01604(9) 0.34091(9) 0.0210(3) Uani d 1 . .
H H9A 0.267854 -0.067681 0.307329 0.025 Uiso calc 1 . .
C C12 0.33375(18) 0.30231(9) 0.18944(8) 0.0136(2) Uani d 1 . .
C C13 0.5500(2) 0.28738(11) 0.07909(8) 0.0200(3) Uani d 1 . .
H H13A 0.568211 0.348732 0.051437 0.024 Uiso calc 1 . .
H H13B 0.444317 0.254289 0.051389 0.024 Uiso calc 1 . .
C C14 0.7242(2) 0.22918(11) 0.07489(10) 0.0259(3) Uani d 1 . .
H H14A 0.754364 0.218155 0.017244 0.039 Uiso calc 1 . .
H H14B 0.827848 0.262688 0.102366 0.039 Uiso calc 1 . .
H H14C 0.704464 0.168635 0.102318 0.039 Uiso calc 1 . .
C C15 0.10027(19) 0.44187(9) 0.33870(8) 0.0159(3) Uani d 1 . .
C C16 -0.1128(2) 0.54538(10) 0.40327(9) 0.0216(3) Uani d 1 . .
H H16A -0.109745 0.591211 0.357452 0.026 Uiso calc 1 . .
H H16B -0.022582 0.565926 0.446699 0.026 Uiso calc 1 . .
C C17 -0.3058(2) 0.53933(13) 0.43679(13) 0.0369(4) Uani d 1 . .
H H17A -0.343372 0.601375 0.457067 0.055 Uiso calc 1 . .
H H17B -0.393486 0.518921 0.393188 0.055 Uiso calc 1 . .
H H17C -0.306732 0.493754 0.482017 0.055 Uiso calc 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
O2 0.0118(4) 0.0270(5) 0.0167(5) 0.0022(4) -0.0019(4) 0.0041(4)
O10 0.0130(4) 0.0189(4) 0.0110(4) 0.0006(3) 0.0019(3) -0.0018(3)
O11 0.0142(4) 0.0204(5) 0.0150(5) 0.0032(4) 0.0017(4) 0.0033(4)
O12 0.0162(5) 0.0536(7) 0.0168(5) 0.0001(5) -0.0023(4) -0.0039(5)
O13 0.0136(5) 0.0351(6) 0.0121(5) -0.0026(4) 0.0021(4) -0.0042(4)
O15 0.0267(6) 0.0169(5) 0.0394(7) -0.0021(4) 0.0097(5) -0.0038(4)
O16 0.0207(5) 0.0145(4) 0.0260(6) 0.0047(4) 0.0069(4) -0.0019(4)
C1 0.0142(6) 0.0225(7) 0.0204(7) 0.0070(5) 0.0014(5) 0.0027(5)
C3B 0.0105(5) 0.0150(6) 0.0126(6) 0.0016(4) 0.0000(5) -0.0006(4)
C3A 0.0113(6) 0.0171(6) 0.0102(6) 0.0008(4) 0.0015(5) -0.0012(4)
C3 0.0108(6) 0.0244(7) 0.0148(6) 0.0006(5) 0.0006(5) 0.0034(5)
C4 0.0129(6) 0.0148(6) 0.0120(6) -0.0005(4) 0.0017(5) -0.0005(4)
C5 0.0125(6) 0.0143(6) 0.0149(6) 0.0014(5) 0.0019(5) -0.0010(5)
C6 0.0115(6) 0.0164(6) 0.0153(6) 0.0024(5) 0.0028(5) 0.0006(5)
C6A 0.0103(6) 0.0147(6) 0.0175(6) 0.0011(4) 0.0016(5) 0.0027(5)
C7 0.0117(6) 0.0178(6) 0.0224(7) 0.0011(5) 0.0023(5) 0.0043(5)
C8 0.0204(7) 0.0155(6) 0.0310(8) -0.0027(5) -0.0031(6) 0.0049(6)
C9A 0.0143(6) 0.0164(6) 0.0158(6) 0.0037(5) 0.0005(5) 0.0003(5)
C9 0.0245(7) 0.0132(6) 0.0251(7) 0.0030(5) -0.0033(6) 0.0009(5)
C12 0.0146(6) 0.0126(6) 0.0134(6) 0.0008(4) 0.0007(5) 0.0022(4)
C13 0.0203(7) 0.0295(7) 0.0103(6) 0.0035(6) 0.0025(5) -0.0019(5)
C14 0.0276(8) 0.0308(8) 0.0194(7) 0.0090(6) 0.0048(6) -0.0007(6)
C15 0.0180(6) 0.0166(6) 0.0132(6) 0.0035(5) 0.0008(5) 0.0006(5)
C16 0.0267(7) 0.0154(6) 0.0226(7) 0.0093(5) 0.0013(6) -0.0026(5)
C17 0.0280(9) 0.0320(9) 0.0512(12) 0.0115(7) 0.0102(8) -0.0112(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
C3 O2 C1 . . 113.82(10) ?
C3A O10 C6 . . 97.15(9) ?
C7 O11 C9A . . 96.51(10) ?
C12 O13 C13 . . 118.82(11) ?
C15 O16 C16 . . 116.54(11) ?
O2 C1 C9A . . 111.20(10) ?
O2 C1 H1A . . 109.4 ?
C9A C1 H1A . . 109.4 ?
O2 C1 H1B . . 109.4 ?
C9A C1 H1B . . 109.4 ?
H1A C1 H1B . . 108.0 ?
C3A C3B C6A . . 102.82(10) ?
C3A C3B C9A . . 111.90(10) ?
C6A C3B C9A . . 101.66(10) ?
C3A C3B H3BA . . 113.2 ?
C6A C3B H3BA . . 113.1 ?
C9A C3B H3BA . . 113.1 ?
O10 C3A C3 . . 112.03(10) ?
O10 C3A C3B . . 103.56(10) ?
C3 C3A C3B . . 112.36(10) ?
O10 C3A C4 . . 99.83(9) ?
C3 C3A C4 . . 117.78(11) ?
C3B C3A C4 . . 109.72(10) ?
O2 C3 C3A . . 112.21(11) ?
O2 C3 H3A . . 109.2 ?
C3A C3 H3A . . 109.2 ?
O2 C3 H3B . . 109.2 ?
C3A C3 H3B . . 109.2 ?
H3A C3 H3B . . 107.9 ?
C12 C4 C5 . . 114.86(11) ?
C12 C4 C3A . . 114.96(10) ?
C5 C4 C3A . . 100.93(10) ?
C12 C4 H4A . . 108.6 ?
C5 C4 H4A . . 108.6 ?
C3A C4 H4A . . 108.6 ?
C15 C5 C4 . . 112.43(11) ?
C15 C5 C6 . . 112.40(11) ?
C4 C5 C6 . . 101.66(10) ?
C15 C5 H5A . . 110.0 ?
C4 C5 H5A . . 110.0 ?
C6 C5 H5A . . 110.0 ?
O10 C6 C6A . . 104.25(10) ?
O10 C6 C5 . . 101.29(10) ?
C6A C6 C5 . . 108.24(11) ?
O10 C6 H6A . . 114.0 ?
C6A C6 H6A . . 114.0 ?
C5 C6 H6A . . 114.0 ?
C6 C6A C3B . . 100.08(10) ?
C6 C6A C7 . . 116.41(11) ?
C3B C6A C7 . . 100.52(10) ?
C6 C6A H6AA . . 112.8 ?
C3B C6A H6AA . . 112.8 ?
C7 C6A H6AA . . 112.8 ?
O11 C7 C8 . . 101.02(10) ?
O11 C7 C6A . . 102.12(10) ?
C8 C7 C6A . . 105.52(11) ?
O11 C7 H7A . . 115.4 ?
C8 C7 H7A . . 115.4 ?
C6A C7 H7A . . 115.4 ?
C9 C8 C7 . . 105.96(12) ?
C9 C8 H8A . . 127.0 ?
C7 C8 H8A . . 127.0 ?
O11 C9A C1 . . 111.53(11) ?
O11 C9A C9 . . 101.20(11) ?
C1 C9A C9 . . 122.17(11) ?
O11 C9A C3B . . 102.22(10) ?
C1 C9A C3B . . 112.73(11) ?
C9 C9A C3B . . 104.67(11) ?
C8 C9 C9A . . 105.25(12) ?
C8 C9 H9A . . 127.4 ?
C9A C9 H9A . . 127.4 ?
O12 C12 O13 . . 125.17(12) ?
O12 C12 C4 . . 125.66(12) ?
O13 C12 C4 . . 109.17(11) ?
O13 C13 C14 . . 107.45(12) ?
O13 C13 H13A . . 110.2 ?
C14 C13 H13A . . 110.2 ?
O13 C13 H13B . . 110.2 ?
C14 C13 H13B . . 110.2 ?
H13A C13 H13B . . 108.5 ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
O15 C15 O16 . . 124.01(12) ?
O15 C15 C5 . . 125.88(12) ?
O16 C15 C5 . . 110.11(11) ?
O16 C16 C17 . . 106.76(12) ?
O16 C16 H16A . . 110.4 ?
C17 C16 H16A . . 110.4 ?
O16 C16 H16B . . 110.4 ?
C17 C16 H16B . . 110.4 ?
H16A C16 H16B . . 108.6 ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O2 C3 . 1.4274(16) ?
O2 C1 . 1.4347(17) ?
O10 C3A . 1.4410(15) ?
O10 C6 . 1.4420(15) ?
O11 C7 . 1.4414(16) ?
O11 C9A . 1.4420(16) ?
O12 C12 . 1.2035(16) ?
O13 C12 . 1.3323(16) ?
O13 C13 . 1.4630(16) ?
O15 C15 . 1.2058(17) ?
O16 C15 . 1.3384(16) ?
O16 C16 . 1.4581(16) ?
C1 C9A . 1.5094(18) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C3B C3A . 1.5341(18) ?
C3B C6A . 1.5515(17) ?
C3B C9A . 1.5561(18) ?
C3B H3BA . 1.0000 ?
C3A C3 . 1.5127(17) ?
C3A C4 . 1.5565(18) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C12 . 1.5120(18) ?
C4 C5 . 1.5478(18) ?
C4 H4A . 1.0000 ?
C5 C15 . 1.5130(18) ?
C5 C6 . 1.5580(18) ?
C5 H5A . 1.0000 ?
C6 C6A . 1.5370(18) ?
C6 H6A . 1.0000 ?
C6A C7 . 1.5609(18) ?
C6A H6AA . 1.0000 ?
C7 C8 . 1.522(2) ?
C7 H7A . 1.0000 ?
C8 C9 . 1.332(2) ?
C8 H8A . 0.9500 ?
C9A C9 . 1.5241(19) ?
C9 H9A . 0.9500 ?
C13 C14 . 1.498(2) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 H14A . 0.9800 ?
C14 H14B . 0.9800 ?
C14 H14C . 0.9800 ?
C16 C17 . 1.499(2) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
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
C3 H3A O13 . 0.99 2.58 3.1604(17) 117.5 yes
C9 H9A O13 2_645 0.95 2.47 3.1692(17) 130.6 yes
C13 H13A O2 4_565 0.99 2.58 3.1905(17) 119.8 yes
C13 H13B O10 4_565 0.99 2.41 3.2193(17) 138.9 yes
C14 H14C O15 2_645 0.98 2.64 3.5669(19) 157.8 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
C3 O2 C1 C9A . . . . -59.58(14) ?
C6 O10 C3A C3 . . . . -173.99(10) ?
C6 O10 C3A C3B . . . . -52.67(11) ?
C6 O10 C3A C4 . . . . 60.53(10) ?
C6A C3B C3A O10 . . . . 31.09(12) ?
C9A C3B C3A O10 . . . . -77.27(12) ?
C6A C3B C3A C3 . . . . 152.18(11) ?
C9A C3B C3A C3 . . . . 43.82(14) ?
C6A C3B C3A C4 . . . . -74.76(12) ?
C9A C3B C3A C4 . . . . 176.89(10) ?
C1 O2 C3 C3A . . . . 59.76(14) ?
O10 C3A C3 O2 . . . . 64.99(14) ?
C3B C3A C3 O2 . . . . -51.11(15) ?
C4 C3A C3 O2 . . . . 179.91(11) ?
O10 C3A C4 C12 . . . . -163.65(10) ?
C3 C3A C4 C12 . . . . 74.92(15) ?
C3B C3A C4 C12 . . . . -55.30(14) ?
O10 C3A C4 C5 . . . . -39.44(11) ?
C3 C3A C4 C5 . . . . -160.87(11) ?
C3B C3A C4 C5 . . . . 68.91(12) ?
C12 C4 C5 C15 . . . . -110.49(13) ?
C3A C4 C5 C15 . . . . 125.24(11) ?
C12 C4 C5 C6 . . . . 129.10(11) ?
C3A C4 C5 C6 . . . . 4.83(12) ?
C3A O10 C6 C6A . . . . 54.98(11) ?
C3A O10 C6 C5 . . . . -57.36(10) ?
C15 C5 C6 O10 . . . . -89.24(12) ?
C4 C5 C6 O10 . . . . 31.18(12) ?
C15 C5 C6 C6A . . . . 161.48(10) ?
C4 C5 C6 C6A . . . . -78.09(12) ?
O10 C6 C6A C3B . . . . -34.93(12) ?
C5 C6 C6A C3B . . . . 72.31(12) ?
O10 C6 C6A C7 . . . . 72.24(13) ?
C5 C6 C6A C7 . . . . 179.48(10) ?
C3A C3B C6A C6 . . . . 2.12(12) ?
C9A C3B C6A C6 . . . . 118.07(10) ?
C3A C3B C6A C7 . . . . -117.38(11) ?
C9A C3B C6A C7 . . . . -1.44(12) ?
C9A O11 C7 C8 . . . . 50.63(11) ?
C9A O11 C7 C6A . . . . -58.08(11) ?
C6 C6A C7 O11 . . . . -70.74(13) ?
C3B C6A C7 O11 . . . . 36.17(12) ?
C6 C6A C7 C8 . . . . -175.97(11) ?
C3B C6A C7 C8 . . . . -69.05(12) ?
O11 C7 C8 C9 . . . . -32.10(14) ?
C6A C7 C8 C9 . . . . 73.94(14) ?
C7 O11 C9A C1 . . . . 177.58(10) ?
C7 O11 C9A C9 . . . . -51.00(11) ?
C7 O11 C9A C3B . . . . 56.88(11) ?
O2 C1 C9A O11 . . . . -63.19(14) ?
O2 C1 C9A C9 . . . . 177.15(12) ?
O2 C1 C9A C3B . . . . 51.15(15) ?
C3A C3B C9A O11 . . . . 75.48(12) ?
C6A C3B C9A O11 . . . . -33.62(12) ?
C3A C3B C9A C1 . . . . -44.38(15) ?
C6A C3B C9A C1 . . . . -153.48(11) ?
C3A C3B C9A C9 . . . . -179.32(11) ?
C6A C3B C9A C9 . . . . 71.58(12) ?
C7 C8 C9 C9A . . . . -0.35(15) ?
O11 C9A C9 C8 . . . . 32.70(14) ?
C1 C9A C9 C8 . . . . 157.22(13) ?
C3B C9A C9 C8 . . . . -73.26(14) ?
C13 O13 C12 O12 . . . . 3.4(2) ?
C13 O13 C12 C4 . . . . -177.31(11) ?
C5 C4 C12 O12 . . . . -9.39(19) ?
C3A C4 C12 O12 . . . . 107.12(15) ?
C5 C4 C12 O13 . . . . 171.36(10) ?
C3A C4 C12 O13 . . . . -72.14(13) ?
C12 O13 C13 C14 . . . . -143.18(13) ?
C16 O16 C15 O15 . . . . -1.7(2) ?
C16 O16 C15 C5 . . . . 178.70(11) ?
C4 C5 C15 O15 . . . . 6.3(2) ?
C6 C5 C15 O15 . . . . 120.28(15) ?
C4 C5 C15 O16 . . . . -174.16(11) ?
C6 C5 C15 O16 . . . . -60.17(14) ?
C15 O16 C16 C17 . . . . 177.50(13) ?