#------------------------------------------------------------------------------
#$Date: 2025-04-18 03:53:35 +0200 (Fri, 18 Apr 2025) $
#$Revision: 299328 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023473.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_2023473
loop_
_publ_author_name
'K\"onig, Julien A.'
'Morgenstern, Bernd'
'Jauch, Johann'
_publ_section_title
;
Synthesis and crystal structure analysis of substituted
bicyclo[3.3.1]nonanones
;
_journal_coeditor_code EV2016
_journal_issue 5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025003299
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac 'C12 H20 O4'
_chemical_formula_moiety 'C12 H20 O4'
_chemical_formula_sum 'C12 H20 O4'
_chemical_formula_weight 228.28
_chemical_name_systematic
;
4,9,9-Trimethoxybicyclo[3.3.1]non-3-en-2-ol
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 101.984(5)
_cell_angle_beta 92.032(5)
_cell_angle_gamma 90.293(5)
_cell_formula_units_Z 4
_cell_length_a 7.7330(15)
_cell_length_b 10.976(2)
_cell_length_c 13.874(3)
_cell_measurement_reflns_used 1376
_cell_measurement_temperature 152(2)
_cell_measurement_theta_max 25.02
_cell_measurement_theta_min 3.00
_cell_volume 1151.1(4)
_computing_cell_refinement
;
SAINT (Bruker, 2021)
;
_computing_data_collection
;
APEX4 (Bruker, 2021)
;
_computing_data_reduction
;
SAINT (Bruker, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b) and
ShelXle (H\"ubschle et al., 2011)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 152(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0546
_diffrn_reflns_av_unetI/netI 0.1021
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 8885
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.372
_diffrn_reflns_theta_min 1.501
_diffrn_source 'INCOATEC I\^A\mS microfocus sealed tube'
_exptl_absorpt_coefficient_mu 0.097
_exptl_absorpt_correction_T_max 0.7455
_exptl_absorpt_correction_T_min 0.5782
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.317
_exptl_crystal_description plate
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.280
_exptl_crystal_size_mid 0.240
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.238
_refine_diff_density_min -0.239
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.981
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 301
_refine_ls_number_reflns 4662
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 0.981
_refine_ls_R_factor_all 0.1158
_refine_ls_R_factor_gt 0.0570
_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^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1178
_refine_ls_wR_factor_ref 0.1391
_reflns_number_gt 2677
_reflns_number_total 4662
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ev2016.cif
_cod_data_source_block 2
_cod_original_cell_volume 1151.2(4)
_cod_database_code 2023473
_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 0.973
_shelx_estimated_absorpt_t_max 0.996
_shelx_hkl_file
;
-1 0 0 -2.90 1.50
-1 0 0 -0.10 1.70
-1 0 0 0.10 1.80
1 0 0 0.30 1.90
1 0 0 -0.60 1.80
-2 0 0 0.70 2.50
-2 0 0 4.90 2.70
2 0 0 1.10 3.20
2 0 0 0.70 3.20
-3 0 0 -0.60 2.80
-3 0 0 -0.50 2.80
3 0 0 1.60 3.60
3 0 0 -0.90 4.00
4 0 0 167.28 11.20
4 0 0 156.58 11.50
5 0 0 8.30 5.00
5 0 0 -3.40 4.90
6 0 0 287.17 18.80
6 0 0 329.97 18.90
7 0 0 -2.40 6.50
7 0 0 -4.10 6.40
8 0 0 75.09 10.80
8 0 0 60.59 10.70
9 0 0 -11.40 8.30
9 0 0 -6.90 7.50
9 -1 0 59.59 11.20
9 -1 0 47.70 10.80
8 -1 0 70.89 10.60
8 -1 0 85.29 11.90
7 -1 0 5.00 6.80
7 -1 0 6.60 7.00
6 -1 0 237.18 16.10
6 -1 0 228.68 15.60
5 -1 0 5.50 5.00
5 -1 0 4.20 5.10
4 -1 0 8.00 4.90
4 -1 0 7.10 4.70
3 -1 0 3.70 3.90
3 -1 0 1.00 3.50
-3 1 0 0.60 2.50
2 -1 0 460.55 22.40
2 -1 0 456.45 22.50
-2 1 0 463.75 22.20
1 -1 0 6556.94 301.17
-1 1 0 6607.74 301.07
0 -1 0 2.50 1.30
0 -1 0 1.30 1.80
0 1 0 0.90 1.60
-1 -1 0 2037.30 94.59
-1 -1 0 2075.69 94.79
-1 -1 0 2110.79 94.89
1 1 0 2044.10 94.69
1 1 0 2120.89 94.79
1 1 0 2042.30 94.79
-2 -1 0 -2.00 2.30
-2 -1 0 5.20 3.50
-2 -1 0 3.10 3.10
2 1 0 1.30 3.30
2 1 0 -1.50 2.80
2 1 0 -1.80 2.60
-3 -1 0 209.88 12.20
-3 -1 0 203.78 11.40
-3 -1 0 210.78 11.50
3 1 0 178.48 11.40
3 1 0 206.68 12.10
3 1 0 204.98 11.80
-4 -1 0 21.90 6.00
4 1 0 22.20 5.10
4 1 0 21.30 5.20
-5 -1 0 39.60 7.50
5 1 0 48.40 6.50
5 1 0 38.60 6.80
6 1 0 26.70 7.40
6 1 0 35.40 6.80
7 1 0 59.19 10.10
7 1 0 51.99 8.70
8 1 0 219.78 18.30
8 1 0 227.68 18.00
9 1 0 111.89 14.90
9 1 0 87.19 12.80
9 -2 0 18.70 8.80
9 -2 0 33.50 10.40
8 -2 0 235.78 18.30
8 -2 0 253.07 19.50
7 -2 0 249.88 17.20
7 -2 0 239.68 17.40
6 -2 0 2.50 5.60
6 -2 0 2.10 6.10
5 -2 0 18.30 5.90
5 -2 0 23.10 5.50
4 -2 0 133.09 10.10
4 -2 0 139.49 10.30
3 -2 0 38.50 5.20
3 -2 0 39.60 5.50
-3 2 0 30.30 4.20
2 -2 0 1030.80 48.30
1 -2 0 751.82 35.70
1 -2 0 742.73 35.00
0 -2 0 697.03 33.50
0 -2 0 697.33 33.00
0 2 0 706.73 33.40
-1 -2 0 124.59 7.60
-1 -2 0 110.69 6.90
-1 -2 0 117.09 7.50
-1 -2 0 112.49 8.00
-1 -2 0 108.79 7.40
1 2 0 114.69 7.10
1 2 0 118.09 7.30
1 2 0 109.99 7.90
-2 -2 0 448.16 22.40
-2 -2 0 485.95 23.10
-2 -2 0 468.45 22.80
2 2 0 471.35 22.90
2 2 0 446.76 22.50
2 2 0 471.55 22.90
-3 -2 0 58.49 6.50
-3 -2 0 50.09 5.10
-3 -2 0 63.29 6.10
3 2 0 53.49 6.30
3 2 0 53.49 5.70
3 2 0 61.69 6.10
-4 -2 0 91.29 9.10
4 2 0 104.09 9.10
4 2 0 110.79 8.70
-5 -2 0 3.50 5.80
5 2 0 -3.70 4.60
5 2 0 5.60 5.00
-6 -2 0 25.40 8.30
6 2 0 31.20 7.40
6 2 0 23.60 6.80
-7 -2 0 66.69 11.40
7 2 0 74.79 10.00
7 2 0 87.29 11.00
8 2 0 36.40 9.20
8 2 0 32.00 9.20
9 2 0 62.79 11.60
9 2 0 65.29 12.30
9 -3 0 66.79 11.80
9 -3 0 109.49 13.70
8 -3 0 20.60 9.00
8 -3 0 17.80 8.00
7 -3 0 25.60 8.00
7 -3 0 23.80 7.80
6 -3 0 1.00 6.50
6 -3 0 -1.20 5.30
5 -3 0 265.27 16.20
5 -3 0 259.47 16.00
4 -3 0 4.50 4.60
4 -3 0 2.70 4.40
3 -3 0 511.35 25.70
2 -3 0 477.85 24.10
2 -3 0 467.05 23.60
1 -3 0 609.04 29.30
0 -3 0 552.24 26.90
0 -3 0 523.15 26.10
-1 -3 0 5045.00 228.58
-1 -3 0 5010.00 229.48
-1 -3 0 4897.11 228.18
-1 -3 0 5092.09 228.78
1 3 0 5001.60 228.18
1 3 0 5011.90 228.48
1 3 0 4955.00 229.48
-2 -3 0 93.59 7.60
-2 -3 0 83.39 7.10
-2 -3 0 90.79 6.60
-2 -3 0 106.29 7.50
2 3 0 91.89 7.20
2 3 0 89.89 7.20
-3 -3 0 320.47 17.40
-3 -3 0 363.56 18.70
3 3 0 336.47 17.70
3 3 0 324.87 18.30
-4 -3 0 47.20 7.00
4 3 0 39.70 5.60
4 3 0 31.60 6.10
-5 -3 0 111.39 11.10
5 3 0 110.29 10.70
5 3 0 128.29 10.30
-6 -3 0 48.40 9.70
6 3 0 39.30 8.50
6 3 0 64.49 8.30
7 3 0 21.90 8.30
7 3 0 28.90 8.10
8 3 0 43.40 9.50
8 3 0 45.00 10.40
9 3 0 26.50 10.40
9 3 0 16.80 9.00
9 -4 0 5.00 8.60
9 -4 0 18.10 8.90
8 -4 0 101.49 12.30
8 -4 0 133.39 13.40
7 -4 0 30.60 8.80
7 -4 0 35.10 8.20
6 -4 0 55.19 8.60
6 -4 0 91.79 10.00
5 -4 0 68.39 8.10
5 -4 0 73.09 8.50
4 -4 0 171.08 11.90
3 -4 0 351.26 19.60
3 -4 0 350.06 19.10
2 -4 0 11.00 5.30
2 -4 0 11.60 3.80
1 -4 0 898.61 42.90
0 -4 0 38.30 5.20
0 -4 0 49.40 6.70
-1 -4 0 8.20 2.70
-1 -4 0 14.10 5.40
-1 -4 0 3.00 3.50
-1 -4 0 9.50 4.20
1 4 0 8.30 4.80
1 4 0 3.80 3.30
-2 -4 0 248.68 14.80
-2 -4 0 256.37 13.80
-2 -4 0 249.58 14.40
2 4 0 253.47 15.50
2 4 0 252.57 14.20
-3 -4 0 29.40 5.90
3 4 0 26.40 5.20
-4 -4 0 7.20 5.70
4 4 0 -0.40 5.20
4 4 0 7.50 4.80
-5 -4 0 92.29 10.80
5 4 0 93.19 9.20
5 4 0 112.99 10.70
-6 -4 0 4.60 8.10
6 4 0 -0.30 5.90
6 4 0 -0.90 6.90
-7 -4 0 21.80 10.00
7 4 0 26.40 9.40
7 4 0 20.70 7.60
-8 -4 0 16.00 10.80
8 4 0 11.20 9.60
8 4 0 23.70 8.50
9 4 0 20.80 10.60
9 4 0 15.10 8.80
9 -5 0 21.20 9.30
9 -5 0 33.00 10.30
8 -5 0 -6.60 7.10
8 -5 0 3.10 7.70
7 -5 0 1.50 6.80
7 -5 0 11.90 7.10
6 -5 0 51.89 8.40
6 -5 0 43.30 8.10
5 -5 0 71.09 8.80
5 -5 0 90.79 9.50
4 -5 0 24.20 6.00
3 -5 0 85.69 8.30
3 -5 0 73.99 9.00
2 -5 0 56.99 8.70
0 -5 0 7.10 5.60
-1 -5 0 662.33 32.10
-1 -5 0 616.04 31.10
-1 -5 0 669.73 33.80
-2 -5 0 94.89 10.10
-2 -5 0 87.89 8.20
2 5 0 80.99 7.20
-3 -5 0 178.68 12.40
3 5 0 154.88 11.20
-4 -5 0 158.88 12.80
4 5 0 155.98 11.30
-5 -5 0 141.29 13.00
5 5 0 136.79 11.70
-6 -5 0 11.80 8.80
6 5 0 10.40 6.70
6 5 0 22.30 8.00
-7 -5 0 73.29 12.90
7 5 0 77.49 10.30
7 5 0 94.09 12.90
-8 -5 0 25.20 11.00
8 5 0 -4.30 8.60
8 5 0 -3.70 7.60
-9 -5 0 29.60 12.50
9 5 0 3.20 8.70
9 5 0 8.70 11.10
8 -6 0 6.00 8.10
8 -6 0 -5.80 6.90
7 -6 0 27.60 8.10
7 -6 0 22.50 8.00
6 -6 0 136.39 13.30
6 -6 0 165.48 14.00
5 -6 0 20.00 6.40
4 -6 0 40.50 6.80
4 -6 0 59.69 8.50
3 -6 0 75.89 9.90
2 -6 0 133.19 13.40
0 -6 0 24.00 7.10
-1 -6 0 6.50 5.10
-1 -6 0 1.60 5.80
-2 -6 0 623.84 31.40
-2 -6 0 608.14 33.30
-3 -6 0 44.60 9.40
-3 -6 0 31.80 6.50
3 6 0 32.80 6.00
-4 -6 0 3.70 6.10
4 6 0 3.70 5.30
-5 -6 0 -2.70 7.20
5 6 0 9.70 6.00
-6 -6 0 95.09 12.80
6 6 0 105.29 10.70
-7 -6 0 111.19 15.00
7 6 0 115.39 12.20
-8 -6 0 19.70 10.90
8 6 0 5.90 8.40
8 -7 0 -4.80 7.10
8 -7 0 2.00 7.60
7 -7 0 34.80 8.80
7 -7 0 41.70 8.50
6 -7 0 -3.80 6.10
6 -7 0 -10.60 6.30
5 -7 0 11.40 6.70
4 -7 0 529.85 28.10
4 -7 0 504.55 29.00
3 -7 0 501.75 28.50
2 -7 0 10.50 6.60
1 -7 0 116.39 11.30
0 -7 0 48.50 9.10
-1 -7 0 23.40 7.80
-2 -7 0 103.59 9.60
-2 -7 0 89.49 11.70
-3 -7 0 73.19 8.80
3 7 0 71.59 8.00
-4 -7 0 127.09 12.10
4 7 0 123.09 11.30
-5 -7 0 6.50 8.10
5 7 0 -5.90 5.90
-6 -7 0 36.90 10.30
6 7 0 32.00 8.00
-7 -7 0 1.90 9.70
7 7 0 0.40 7.20
-8 -7 0 149.59 17.90
8 7 0 137.89 14.10
8 -8 0 80.79 11.70
8 -8 0 74.79 11.60
7 -8 0 17.60 8.40
7 -8 0 37.80 8.60
6 -8 0 19.50 7.70
6 -8 0 38.90 8.50
5 -8 0 8.60 6.30
5 -8 0 11.70 6.90
4 -8 0 717.13 38.90
4 -8 0 713.33 37.60
3 -8 0 436.96 26.50
2 -8 0 430.56 26.40
1 -8 0 106.19 13.20
0 -8 0 136.39 15.10
-1 -8 0 64.29 10.90
-2 -8 0 83.49 9.40
-2 -8 0 90.89 13.00
-3 -8 0 96.39 14.00
-3 -8 0 76.89 10.00
-4 -8 0 346.17 22.20
-5 -8 0 30.50 9.40
5 8 0 30.80 7.50
-6 -8 0 90.59 13.40
6 8 0 89.99 10.70
-7 -8 0 33.90 12.20
7 8 0 38.10 9.10
7 -9 0 1.90 7.10
7 -9 0 7.30 7.70
6 -9 0 22.90 8.20
6 -9 0 20.60 7.80
5 -9 0 -2.50 6.50
5 -9 0 6.40 7.00
4 -9 0 1.20 7.20
4 -9 0 -3.10 6.90
3 -9 0 25.20 8.90
2 -9 0 20.90 9.10
0 -9 0 376.26 24.90
-1 -9 0 10.30 8.50
-2 -9 0 52.49 11.90
-3 -9 0 -6.00 6.60
-3 -9 0 3.30 8.90
-4 -9 0 83.39 11.60
-4 -9 0 119.29 17.10
-5 -9 0 5.50 8.60
5 9 0 -2.20 6.50
-6 -9 0 22.10 10.60
6 9 0 3.50 6.90
-7 -9 0 64.09 13.70
7 9 0 27.80 8.50
6 -10 0 14.40 7.80
6 -10 0 25.10 8.80
6 -10 0 5.30 8.60
5 -10 0 19.50 8.40
5 -10 0 19.80 8.90
4 -10 0 10.60 8.00
4 -10 0 -2.00 7.30
3 -10 0 88.39 14.20
2 -10 0 295.57 22.50
1 -10 0 189.18 17.10
1 -10 0 186.28 17.90
0 -10 0 16.50 9.60
-1 -10 0 0.80 9.00
-2 -10 0 7.70 9.30
-2 -10 0 -6.60 6.30
-3 -10 0 16.60 8.00
-3 -10 0 38.20 12.20
-4 -10 0 47.60 10.20
-5 -10 0 5.10 9.30
-6 -10 0 75.49 13.60
6 -11 0 1.70 8.60
5 -11 0 79.59 13.80
5 -11 0 88.79 12.40
4 -11 0 19.70 10.00
4 -11 0 35.40 10.60
3 -11 0 156.98 19.00
2 -11 0 49.50 12.60
2 -11 0 54.79 11.90
1 -11 0 27.20 11.00
1 -11 0 13.30 9.00
0 -11 0 -3.60 8.20
-1 -11 0 84.49 15.00
-2 -11 0 15.00 10.40
-3 -11 0 5.10 10.50
-4 -11 0 -7.20 11.50
-4 -11 0 -6.90 8.20
-5 -11 0 -9.30 8.90
4 -12 0 59.69 12.60
4 -12 0 38.00 12.10
3 -12 0 2.10 9.20
3 -12 0 -2.80 7.60
2 -12 0 5.30 10.10
2 -12 0 -8.30 7.60
1 -12 0 54.49 12.90
1 -12 0 72.49 14.80
0 -12 0 -8.30 8.60
0 -12 0 21.20 10.20
-1 -12 0 4.70 10.50
-2 -12 0 -1.30 10.40
-3 -12 0 -1.60 8.60
-3 -12 0 -8.60 10.30
-4 -12 0 1.90 12.20
3 -13 0 28.50 12.90
3 -13 0 29.10 11.40
2 -13 0 -1.40 9.00
2 -13 0 3.20 10.60
1 -13 0 0.90 11.20
1 -13 0 -5.60 8.70
0 -13 0 3.20 10.20
0 -13 0 17.50 11.20
-1 -13 0 51.69 15.20
-1 -13 0 31.70 12.70
-2 -13 0 13.50 11.80
-3 -13 1 18.50 12.20
-3 -13 1 14.50 10.10
-2 -13 1 -1.70 10.40
-1 -13 1 -7.40 9.50
0 -13 1 18.00 11.30
0 -13 1 0.90 9.80
1 -13 1 5.40 10.10
1 -13 1 19.30 11.60
2 -13 1 19.90 12.10
2 -13 1 12.80 9.80
3 -13 1 34.00 12.50
-4 -12 1 39.20 15.10
-4 -12 1 32.60 10.80
-3 -12 1 37.60 14.00
-3 -12 1 18.40 9.40
-2 -12 1 64.19 15.10
-1 -12 1 13.60 11.10
0 -12 1 35.10 12.10
1 -12 1 154.98 19.70
1 -12 1 158.38 20.00
2 -12 1 -6.00 7.70
2 -12 1 4.40 9.80
3 -12 1 -1.40 8.90
4 -12 1 21.30 10.20
4 -12 1 7.40 9.20
5 -12 1 37.30 10.30
5 -12 1 50.29 12.10
-5 -11 1 -6.20 9.00
-4 -11 1 -3.70 8.80
-4 -11 1 -11.50 10.80
-3 -11 1 9.60 11.20
-3 -11 1 -7.20 7.20
-2 -11 1 4.90 9.90
-2 -11 1 1.30 7.50
-1 -11 1 -0.50 8.70
0 -11 1 -8.40 7.50
1 -11 1 18.70 9.50
2 -11 1 193.18 21.70
3 -11 1 99.99 15.50
4 -11 1 197.18 18.40
4 -11 1 176.38 19.80
5 -11 1 131.89 16.00
5 -11 1 146.89 15.20
6 -11 1 1.20 7.50
6 -11 1 4.20 7.40
6 -11 1 0.50 7.60
-6 -10 1 8.80 10.30
-5 -10 1 8.90 8.90
-4 -10 1 143.99 14.90
-3 -10 1 65.09 10.20
-3 -10 1 71.59 14.40
-2 -10 1 47.40 11.60
-1 -10 1 7.10 8.30
0 -10 1 31.20 10.00
1 -10 1 7.30 8.10
2 -10 1 229.88 19.30
3 -10 1 25.60 9.50
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3 4 -14 0.20 10.20
2 4 -14 35.00 11.40
1 4 -14 -5.30 9.00
0 4 -14 14.80 9.00
-1 4 -14 61.59 11.30
-2 4 -14 73.19 11.80
2 -4 14 64.09 11.70
-3 4 -14 -3.70 8.40
3 -4 14 7.30 9.40
-4 4 -14 26.50 9.40
4 -4 14 -6.60 9.60
5 -4 14 69.79 14.60
6 3 -14 8.70 10.50
6 3 -14 14.40 11.70
5 3 -14 8.30 11.50
5 3 -14 15.70 13.10
4 3 -14 18.40 9.80
4 3 -14 29.50 12.30
3 3 -14 9.00 8.80
3 3 -14 41.30 12.60
2 3 -14 12.60 11.10
2 3 -14 19.80 9.30
1 3 -14 3.60 8.30
1 3 -14 12.50 10.90
0 3 -14 12.90 8.20
-1 3 -14 35.50 9.80
1 -3 14 36.40 11.20
-2 3 -14 17.80 8.90
-3 3 -14 -1.00 8.30
-4 3 -14 0.70 8.60
5 -3 14 5.80 10.70
6 2 -14 44.00 14.60
6 2 -14 29.40 12.40
5 2 -14 4.30 9.90
5 2 -14 18.90 13.50
4 2 -14 7.10 9.50
4 2 -14 -4.50 10.80
3 2 -14 3.10 8.40
3 2 -14 28.40 11.70
2 2 -14 17.50 11.60
2 2 -14 4.80 8.30
-2 -2 14 9.00 9.80
1 2 -14 16.90 12.10
0 2 -14 154.98 18.10
0 -2 14 113.59 14.50
1 -2 14 40.70 11.30
-2 2 -14 52.19 10.50
-3 2 -14 2.00 8.40
3 -2 14 -3.50 9.10
-4 2 -14 10.90 9.00
4 -2 14 16.00 10.10
5 -2 14 3.30 10.50
6 1 -14 33.70 14.80
6 1 -14 16.50 11.00
6 1 -14 16.90 10.60
5 1 -14 30.90 14.70
5 1 -14 11.00 9.90
4 1 -14 11.60 11.90
3 1 -14 35.80 13.20
2 1 -14 35.80 13.20
-2 -1 14 24.30 10.30
1 1 -14 1.00 11.60
-1 -1 14 -3.20 10.20
0 1 -14 90.69 15.40
0 -1 14 61.29 12.50
-1 1 -14 176.28 18.70
1 -1 14 136.29 16.00
2 -1 14 5.30 9.40
-4 1 -14 0.70 8.70
4 -1 14 6.20 9.50
5 -1 14 -0.70 8.60
5 -1 14 -7.90 10.10
6 0 -14 2.70 13.50
6 0 -14 -5.40 9.70
5 0 -14 16.10 13.40
5 0 -14 1.70 9.90
4 0 -14 17.60 11.90
3 0 -14 9.10 10.90
2 0 -14 314.57 25.00
1 0 -14 16.80 11.10
-1 0 14 13.70 10.70
0 0 -14 17.90 12.10
0 0 14 0.00 10.50
-1 0 -14 19.20 11.80
2 0 14 25.90 10.90
3 0 14 7.40 9.60
4 0 14 -4.90 9.80
4 0 14 15.20 8.20
5 0 14 7.10 8.50
5 -1 -14 9.00 12.40
5 -1 -14 -8.10 9.30
4 -1 -14 39.80 14.10
3 -1 -14 65.89 15.40
2 -1 -14 12.30 12.00
-2 1 14 27.10 10.70
1 -1 -14 60.89 14.20
-1 1 14 66.39 12.90
0 -1 -14 -0.20 11.30
0 1 14 -2.90 10.10
-1 -1 -14 14.60 11.80
1 1 14 -2.00 10.10
2 1 14 -1.30 10.10
4 1 14 9.60 8.40
5 1 14 15.90 9.30
5 -2 -14 8.50 13.40
5 -2 -14 -15.40 10.20
4 -2 -14 26.70 14.20
3 -2 -14 85.39 16.20
2 -2 -14 61.99 15.60
1 -2 -14 -4.90 12.00
-1 2 14 -10.20 9.20
0 -2 -14 22.50 12.70
-1 -2 -14 9.80 11.80
1 2 14 -3.20 9.90
3 2 14 -20.40 9.50
5 -3 -14 -8.60 11.80
5 -3 -14 15.90 15.10
4 -3 -14 -2.00 10.10
4 -3 -14 -8.20 12.50
3 -3 -14 -2.00 12.60
2 -3 -14 6.30 13.10
1 -3 -14 112.19 17.90
-1 3 14 97.59 14.30
0 -3 -14 3.00 10.50
0 -3 -14 13.70 13.00
-1 -3 -14 -2.70 11.40
-1 -3 -14 27.00 13.10
-2 -3 -14 32.10 13.40
2 3 14 39.20 12.00
-3 -3 -14 7.90 11.50
3 3 14 0.90 10.10
-4 -3 -14 9.90 12.10
4 -4 -14 -0.60 13.10
4 -4 -14 -7.80 10.40
3 -4 -14 8.30 13.50
2 -4 -14 31.20 15.50
1 -4 -14 37.50 15.40
1 -4 -14 11.60 10.60
0 -4 -14 -5.20 13.40
0 -4 -14 5.70 10.30
0 4 14 12.60 10.10
-1 -4 -14 2.10 13.60
-1 -4 -14 16.00 11.40
-2 -4 -14 19.60 12.40
-3 -4 -14 60.49 14.50
3 -5 -14 21.60 15.20
2 -5 -14 8.30 14.90
1 -5 -14 -3.30 14.80
1 -5 -14 19.20 10.40
0 -5 -14 85.49 18.60
0 -5 -14 57.49 14.10
-1 -5 -14 26.20 12.30
-1 -5 -14 -5.60 14.10
-2 -5 -14 61.09 15.40
1 -6 -14 -3.20 14.90
1 -6 -14 38.60 12.10
0 -6 -14 2.10 14.50
0 -6 -14 42.00 13.20
2 9 -15 39.30 14.70
-2 -9 15 18.60 9.30
1 9 -15 2.60 12.20
-1 -9 15 6.00 8.60
0 9 -15 19.60 12.60
0 -9 15 11.80 9.00
-1 9 -15 37.00 12.10
1 -9 15 8.00 8.60
3 8 -15 83.09 15.50
2 8 -15 76.69 15.50
-2 -8 15 80.39 11.80
1 8 -15 5.40 10.00
0 8 -15 -3.70 8.80
0 -8 15 9.60 8.10
-1 8 -15 7.70 9.20
1 -8 15 -1.30 8.10
-2 8 -15 67.49 11.90
-3 8 -15 6.40 9.40
4 7 -15 14.30 12.60
3 7 -15 4.40 12.10
2 7 -15 -8.80 11.90
1 7 -15 6.70 10.50
0 7 -15 -5.00 9.30
0 -7 15 14.90 7.90
-1 7 -15 27.10 10.20
-2 7 -15 23.10 10.30
-3 7 -15 16.50 9.30
4 6 -15 20.00 12.30
3 6 -15 23.50 12.60
2 6 -15 114.29 16.20
1 6 -15 14.60 10.70
0 6 -15 6.00 9.60
0 -6 15 -11.70 6.80
-1 6 -15 12.40 9.90
-2 6 -15 7.30 8.80
-3 6 -15 3.40 9.50
-4 6 -15 76.59 11.90
4 -6 15 24.40 12.10
5 5 -15 16.20 12.20
4 5 -15 1.70 11.30
3 5 -15 65.09 14.20
2 5 -15 1.50 11.10
1 5 -15 172.48 19.00
0 5 -15 -1.60 8.80
-1 5 -15 8.80 8.80
-2 5 -15 39.10 10.50
2 -5 15 21.20 10.40
-3 5 -15 0.90 8.60
-4 5 -15 18.10 9.70
4 -5 15 11.80 10.90
5 4 -15 16.60 12.10
4 4 -15 21.00 12.70
3 4 -15 6.40 11.90
2 4 -15 123.19 16.50
1 4 -15 -2.80 9.80
0 4 -15 0.70 8.70
-1 4 -15 16.70 9.60
1 -4 15 24.90 10.70
-2 4 -15 -7.30 8.40
-3 4 -15 8.00 9.60
3 -4 15 -4.50 9.30
-4 4 -15 -4.00 8.80
5 3 -15 42.90 13.70
5 3 -15 19.60 12.30
4 3 -15 -1.60 9.20
4 3 -15 10.60 11.80
3 3 -15 2.60 11.30
3 3 -15 6.90 9.30
2 3 -15 -2.00 8.70
2 3 -15 26.60 11.90
1 3 -15 140.39 17.40
1 3 -15 79.59 13.20
0 3 -15 14.20 8.90
-1 3 -15 -7.20 8.10
1 -3 15 5.40 9.90
-2 3 -15 4.10 9.00
2 -3 15 13.40 10.20
-3 3 -15 -2.70 8.70
3 -3 15 -22.30 8.90
-4 3 -15 -5.60 9.10
4 -3 15 -7.70 10.10
5 2 -15 26.30 13.40
5 2 -15 18.90 10.50
4 2 -15 10.00 11.50
4 2 -15 1.50 10.00
3 2 -15 25.00 10.00
3 2 -15 35.60 13.30
2 2 -15 7.20 11.80
2 2 -15 2.50 8.70
1 2 -15 36.40 13.00
1 2 -15 4.80 8.90
0 2 -15 94.59 15.70
0 2 -15 60.49 11.30
0 -2 15 78.79 13.50
-1 2 -15 18.60 9.00
1 -2 15 0.20 9.70
-2 2 -15 27.40 10.30
2 -2 15 12.30 10.60
-3 2 -15 10.30 9.80
3 -2 15 -9.10 9.40
-4 2 -15 -14.50 8.60
4 -2 15 -13.80 9.20
5 1 -15 1.70 9.80
5 1 -15 17.00 13.10
4 1 -15 10.80 9.80
4 1 -15 -0.10 11.70
3 1 -15 50.39 14.10
2 1 -15 38.00 13.50
1 1 -15 -1.50 11.50
-1 -1 15 11.70 11.00
0 1 -15 2.80 12.00
0 -1 15 -11.60 9.80
-1 1 -15 29.50 12.50
1 -1 15 4.80 10.50
2 -1 15 2.50 11.10
3 -1 15 -11.50 9.30
-4 1 -15 -2.90 9.20
4 -1 15 -2.10 7.60
5 0 -15 0.70 13.50
4 0 -15 30.70 13.30
3 0 -15 17.30 11.90
2 0 -15 43.70 13.70
-2 0 15 29.80 10.90
1 0 -15 6.40 11.70
-1 0 15 -13.90 9.90
0 0 -15 56.49 13.90
0 0 15 21.80 11.60
-1 0 -15 14.70 12.00
1 0 15 14.80 10.50
2 0 15 1.80 10.90
3 0 15 -12.50 9.50
4 0 15 -0.70 8.40
5 -1 -15 21.90 13.90
4 -1 -15 14.20 12.60
3 -1 -15 36.30 14.10
2 -1 -15 15.20 12.90
1 -1 -15 0.40 11.80
-1 1 15 1.20 10.30
0 -1 -15 8.20 11.80
0 1 15 6.00 11.20
-1 -1 -15 35.10 13.00
1 1 15 4.20 10.30
2 1 15 -13.20 9.50
3 1 15 0.50 10.50
4 1 15 26.00 11.10
4 -2 -15 29.70 13.50
3 -2 -15 15.00 12.70
2 -2 -15 4.10 13.00
1 -2 -15 23.00 13.40
-1 2 15 3.70 9.80
0 -2 -15 7.80 12.80
0 2 15 20.50 11.30
-1 -2 -15 25.90 13.00
3 2 15 31.00 12.20
3 -3 -15 7.50 13.10
2 -3 -15 -3.20 13.20
1 -3 -15 9.80 12.90
-1 3 15 21.70 10.60
0 -3 -15 113.19 17.80
0 3 15 119.19 15.40
-1 -3 -15 17.80 13.00
2 3 15 9.10 11.60
2 -4 -15 42.90 15.70
1 -4 -15 28.90 14.60
0 -4 -15 31.20 13.90
0 -4 -15 -12.60 12.60
0 4 15 -0.40 9.90
-1 -4 -15 8.00 13.20
-1 -4 -15 12.80 12.00
1 4 15 8.40 11.30
-2 -4 -15 17.70 12.60
1 8 -16 22.80 12.70
-1 -8 16 44.60 10.80
0 8 -16 46.40 12.70
0 -8 16 54.09 10.80
-1 8 -16 2.00 9.20
1 -8 16 11.80 8.70
3 7 -16 -5.70 12.50
2 7 -16 -8.50 11.60
1 7 -16 74.59 14.20
0 7 -16 11.60 10.60
0 -7 16 9.10 8.20
-1 7 -16 0.20 9.60
-2 7 -16 2.50 9.90
3 6 -16 9.10 12.00
2 6 -16 9.50 12.40
1 6 -16 4.60 10.40
0 6 -16 2.10 9.70
-1 6 -16 -2.60 9.50
-2 6 -16 20.50 10.20
-3 6 -16 -1.30 8.90
4 5 -16 -3.70 11.60
3 5 -16 -1.50 12.00
2 5 -16 11.40 12.30
1 5 -16 77.89 14.60
0 5 -16 26.30 10.50
-1 5 -16 9.40 9.20
-2 5 -16 13.80 9.70
-3 5 -16 45.40 11.80
4 4 -16 31.20 13.90
3 4 -16 -5.50 11.90
2 4 -16 3.80 12.50
1 4 -16 34.60 11.80
0 4 -16 -3.50 8.90
-1 4 -16 0.80 8.80
1 -4 16 -15.40 10.20
-2 4 -16 12.30 9.60
-3 4 -16 19.60 10.30
3 -4 16 31.80 12.30
4 3 -16 -0.60 10.00
4 3 -16 25.80 12.10
3 3 -16 -21.10 9.60
3 3 -16 7.90 12.00
2 3 -16 36.30 13.10
2 3 -16 -11.20 8.90
1 3 -16 100.69 14.20
0 3 -16 1.10 8.50
-1 3 -16 -6.20 8.30
1 -3 16 2.60 10.90
-2 3 -16 43.10 11.20
-3 3 -16 25.90 10.10
4 2 -16 31.10 12.70
4 2 -16 12.20 10.90
3 2 -16 -5.50 9.60
3 2 -16 23.30 13.30
2 2 -16 1.90 9.50
2 2 -16 5.00 11.90
1 2 -16 -1.30 8.50
1 2 -16 10.10 12.00
0 2 -16 7.90 11.70
0 2 -16 -5.00 8.00
0 -2 16 8.00 10.90
-1 2 -16 11.80 11.60
-1 2 -16 8.40 8.80
1 -2 16 -7.10 10.90
-2 2 -16 12.40 9.90
2 -2 16 -8.00 11.40
-3 2 -16 18.90 10.30
3 -2 16 13.80 11.60
4 1 -16 42.30 14.60
4 1 -16 -14.40 9.40
3 1 -16 68.19 15.80
2 1 -16 6.70 12.70
1 1 -16 19.80 12.90
0 1 -16 15.40 13.00
0 -1 16 -6.00 11.30
-1 1 -16 22.80 13.00
1 -1 16 12.50 12.00
2 -1 16 -16.60 10.80
4 0 -16 9.60 12.90
3 0 -16 13.70 12.80
2 0 -16 18.50 12.60
1 0 -16 15.10 12.50
-1 0 16 -2.20 11.40
0 0 -16 92.99 16.20
-1 0 -16 12.20 13.00
1 0 16 3.10 11.10
2 0 16 15.50 11.60
3 0 16 -0.60 11.10
3 -1 -16 20.90 12.90
2 -1 -16 10.80 12.60
1 -1 -16 57.99 14.50
-1 1 16 50.79 13.00
0 -1 -16 28.30 13.20
0 1 16 -4.30 10.60
-1 -1 -16 33.20 12.60
2 1 16 -6.80 11.10
3 -2 -16 14.90 12.50
2 -2 -16 14.00 13.50
1 -2 -16 42.30 14.60
-1 2 16 38.40 11.90
0 -2 -16 34.70 13.90
0 2 16 1.30 10.70
-1 -2 -16 21.90 12.90
1 2 16 -8.50 10.90
1 -3 -16 14.30 14.50
0 -3 -16 -4.80 13.20
-1 -3 -16 47.10 14.70
1 6 -17 30.00 12.80
0 6 -17 9.10 10.90
-1 6 -17 12.20 10.20
2 5 -17 19.40 13.50
1 5 -17 -3.90 10.70
0 5 -17 9.10 10.50
-1 5 -17 52.09 12.00
2 4 -17 -5.40 11.90
1 4 -17 -4.40 10.20
0 4 -17 1.70 9.70
0 -4 17 0.50 11.50
-1 4 -17 3.50 9.20
-2 4 -17 -2.50 9.50
3 3 -17 25.70 12.20
2 3 -17 23.90 11.30
1 3 -17 27.40 9.90
0 3 -17 9.00 9.10
-1 3 -17 27.10 10.30
-2 3 -17 -9.10 9.70
3 2 -17 15.00 12.20
2 2 -17 21.10 12.70
2 2 -17 3.80 9.50
1 2 -17 28.30 13.80
1 2 -17 35.70 11.30
0 2 -17 28.30 12.50
0 2 -17 -16.00 8.10
-1 2 -17 7.60 9.00
1 -2 17 -4.10 11.40
-2 2 -17 0.10 10.10
2 -2 17 -2.40 12.30
2 1 -17 48.40 14.40
1 1 -17 23.10 13.40
-1 -1 17 25.20 12.60
0 1 -17 4.80 12.80
0 -1 17 8.80 12.40
2 -1 17 -9.50 12.10
2 0 -17 10.40 12.90
1 0 -17 28.50 13.80
-1 0 17 6.80 12.00
0 0 -17 31.40 14.20
0 0 17 -1.20 12.30
-1 0 -17 18.30 13.40
1 0 17 -4.60 11.70
1 -1 -17 46.90 14.60
0 -1 -17 18.30 13.10
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 3569
_shelx_res_file
;
TITL sh4913_a.res in P-1
sh4913_a.res
created by SHELXL-2019/3 at 17:59:43 on 01-Apr-2025
REM Old TITL sh4913 in P-1
REM SHELXT solution in P-1: R1 0.186, Rweak 0.011, Alpha 0.041
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C24 O8
CELL 0.71073 7.7330 10.9765 13.8741 101.984 92.032 90.293
ZERR 4.000 0.0015 0.0023 0.0028 0.005 0.005 0.005
LATT 1
SFAC C H O
UNIT 48 80 16
TEMP -120.500
SIZE 0.04 0.24 0.28
L.S. 10
BOND $H
EQIV $1 1+x, y, z
DFIX 0.84 0.01 O2 H2O O6 H6O
HTAB O6 O4_$1
HTAB O2 O8
SHEL 10000 0.80
LIST 4
ACTA
CONF
FMAP 2
PLAN -5
WGHT 0.051300
FVAR 0.72994
O3 3 0.225005 0.370700 0.139783 11.00000 0.02545 0.01881 =
0.03059 0.00990 -0.00625 0.00420
O2 3 0.747639 0.613008 0.271913 11.00000 0.02177 0.01607 =
0.05218 0.01485 0.00371 -0.00085
H2O 2 0.741069 0.690881 0.278199 11.00000 -1.50000
O1 3 0.554317 0.278717 0.403361 11.00000 0.03233 0.01695 =
0.02884 0.01410 -0.00469 0.00296
O4 3 0.237192 0.507890 0.292099 11.00000 0.02105 0.01451 =
0.03181 0.00808 0.00541 0.00375
O5 3 1.060014 1.164407 0.393678 11.00000 0.03105 0.01457 =
0.02970 0.00525 -0.00462 0.00010
O6 3 1.248606 0.759063 0.264456 11.00000 0.02420 0.01811 =
0.05463 0.01453 0.00801 0.01019
H6O 2 1.233956 0.685385 0.271479 11.00000 -1.50000
O7 3 0.719390 0.927845 0.138914 11.00000 0.02632 0.02117 =
0.02961 0.01017 -0.00620 -0.00206
O8 3 0.742440 0.877535 0.293170 11.00000 0.02002 0.01677 =
0.02784 0.00914 0.00334 0.00460
C1 1 0.412710 0.316688 0.259749 11.00000 0.02228 0.01350 =
0.02886 0.01059 -0.00066 0.00139
AFIX 13
H1 2 0.317759 0.267373 0.281279 11.00000 -1.20000
AFIX 0
C2 1 0.534502 0.365211 0.345824 11.00000 0.02247 0.01506 =
0.02708 0.01046 0.00433 0.00686
C3 1 0.615156 0.474936 0.359246 11.00000 0.02028 0.01939 =
0.02602 0.01018 -0.00125 0.00311
AFIX 43
H3 2 0.695548 0.498054 0.413456 11.00000 -1.20000
AFIX 0
C4 1 0.583490 0.563532 0.291639 11.00000 0.01922 0.01481 =
0.03095 0.00862 0.00513 0.00223
AFIX 13
H4 2 0.514429 0.634247 0.327706 11.00000 -1.20000
AFIX 0
C5 1 0.482437 0.506090 0.196393 11.00000 0.02096 0.01444 =
0.03197 0.01189 0.00361 0.00662
AFIX 13
H5 2 0.430621 0.575362 0.168691 11.00000 -1.20000
AFIX 0
C6 1 0.591020 0.426307 0.116079 11.00000 0.02915 0.02620 =
0.02678 0.01197 0.00482 0.00321
AFIX 23
H6A 2 0.520091 0.406174 0.053892 11.00000 -1.20000
H6B 2 0.692026 0.476413 0.104437 11.00000 -1.20000
AFIX 0
C7 1 0.655976 0.304827 0.141091 11.00000 0.02706 0.02464 =
0.03098 0.00471 0.00295 0.00773
AFIX 23
H7A 2 0.749392 0.323841 0.192827 11.00000 -1.20000
H7B 2 0.705050 0.252400 0.081777 11.00000 -1.20000
AFIX 0
C8 1 0.510693 0.232603 0.177296 11.00000 0.02901 0.01555 =
0.02892 0.00581 -0.00359 0.00747
AFIX 23
H8A 2 0.560293 0.161608 0.202263 11.00000 -1.20000
H8B 2 0.428924 0.198770 0.121522 11.00000 -1.20000
AFIX 0
C9 1 0.334651 0.426153 0.221032 11.00000 0.01815 0.01692 =
0.02594 0.00707 0.00046 0.00284
C10 1 0.125967 0.454426 0.094066 11.00000 0.03364 0.02650 =
0.04039 0.01603 -0.00949 0.00816
AFIX 137
H10A 2 0.054707 0.406678 0.039144 11.00000 -1.50000
H10B 2 0.204374 0.510236 0.069224 11.00000 -1.50000
H10C 2 0.051003 0.503695 0.142526 11.00000 -1.50000
AFIX 0
C11 1 0.099458 0.452518 0.335037 11.00000 0.02434 0.02881 =
0.04267 0.01537 0.01025 0.00366
AFIX 137
H11A 2 0.019317 0.517320 0.364698 11.00000 -1.50000
H11B 2 0.147237 0.411031 0.385985 11.00000 -1.50000
H11C 2 0.037487 0.391278 0.283835 11.00000 -1.50000
AFIX 0
C12 1 0.680374 0.307921 0.482991 11.00000 0.03794 0.02856 =
0.02944 0.01256 -0.00253 0.00763
AFIX 137
H12A 2 0.682747 0.240840 0.519879 11.00000 -1.50000
H12B 2 0.650051 0.386227 0.526962 11.00000 -1.50000
H12C 2 0.794670 0.316700 0.456675 11.00000 -1.50000
AFIX 0
C13 1 0.918492 1.047312 0.250911 11.00000 0.02366 0.01079 =
0.03128 0.00997 -0.00307 0.00346
AFIX 13
H13 2 0.826248 1.109938 0.271311 11.00000 -1.20000
AFIX 0
C14 1 1.041028 1.047329 0.336912 11.00000 0.02242 0.01467 =
0.02484 0.00623 0.00240 -0.00080
C15 1 1.121040 0.945432 0.351179 11.00000 0.01942 0.01857 =
0.02360 0.00825 -0.00097 0.00270
AFIX 43
H15 2 1.203910 0.952686 0.404336 11.00000 -1.20000
AFIX 0
C16 1 1.086178 0.819679 0.287062 11.00000 0.01795 0.01515 =
0.03797 0.01269 0.00568 0.00797
AFIX 13
H16 2 1.019848 0.769528 0.326094 11.00000 -1.20000
AFIX 0
C17 1 0.978504 0.822128 0.191700 11.00000 0.02129 0.01285 =
0.03103 0.00705 0.00125 0.00146
AFIX 13
H17 2 0.923065 0.738204 0.168204 11.00000 -1.20000
AFIX 0
C18 1 1.081432 0.852688 0.107478 11.00000 0.03044 0.02259 =
0.02831 0.00635 0.00823 0.00143
AFIX 23
H18A 2 1.005550 0.839472 0.047137 11.00000 -1.20000
H18B 2 1.178675 0.793939 0.094485 11.00000 -1.20000
AFIX 0
C19 1 1.154120 0.986138 0.127797 11.00000 0.03107 0.02862 =
0.02734 0.01179 0.00460 -0.00361
AFIX 23
H19A 2 1.249799 0.994633 0.178169 11.00000 -1.20000
H19B 2 1.201510 1.003598 0.066630 11.00000 -1.20000
AFIX 0
C20 1 1.014053 1.080627 0.164092 11.00000 0.02578 0.02601 =
0.03092 0.01503 -0.00272 -0.00423
AFIX 23
H20A 2 0.929714 1.083264 0.109210 11.00000 -1.20000
H20B 2 1.067692 1.164458 0.185194 11.00000 -1.20000
AFIX 0
C21 1 0.834388 0.917652 0.217585 11.00000 0.02010 0.01664 =
0.02419 0.00840 -0.00154 0.00058
C22 1 0.619630 0.817948 0.096156 11.00000 0.03853 0.02537 =
0.03870 0.00598 -0.01395 -0.00504
AFIX 137
H22A 2 0.531624 0.838293 0.049607 11.00000 -1.50000
H22B 2 0.563015 0.786549 0.148393 11.00000 -1.50000
H22C 2 0.696186 0.754021 0.061296 11.00000 -1.50000
AFIX 0
C23 1 0.605977 0.956620 0.336023 11.00000 0.02548 0.02441 =
0.03980 0.01210 0.01056 0.01083
AFIX 137
H23A 2 0.535246 0.912043 0.375069 11.00000 -1.50000
H23B 2 0.533485 0.979948 0.283521 11.00000 -1.50000
H23C 2 0.656028 1.031866 0.378740 11.00000 -1.50000
AFIX 0
C24 1 1.174423 1.178051 0.478117 11.00000 0.03429 0.02912 =
0.02853 0.00786 -0.00173 -0.00543
AFIX 137
H24A 2 1.172238 1.264278 0.515319 11.00000 -1.50000
H24B 2 1.292245 1.157427 0.457040 11.00000 -1.50000
H24C 2 1.137482 1.121833 0.520074 11.00000 -1.50000
AFIX 0
HKLF 4
REM sh4913_a.res in P-1
REM wR2 = 0.1391, GooF = S = 0.981, Restrained GooF = 0.981 for all data
REM R1 = 0.0570 for 2677 Fo > 4sig(Fo) and 0.1158 for all 4662 data
REM 301 parameters refined using 2 restraints
END
WGHT 0.0510 0.0000
REM Highest difference peak 0.238, deepest hole -0.239, 1-sigma level 0.056
Q1 1 0.3534 0.3583 0.2412 11.00000 0.05 0.24
Q2 1 0.0046 0.4508 0.2822 11.00000 0.05 0.22
Q3 1 0.8609 0.8963 0.3400 11.00000 0.05 0.22
Q4 1 0.5249 0.4546 0.3851 11.00000 0.05 0.22
Q5 1 1.3788 0.8605 0.2820 11.00000 0.05 0.21
;
_shelx_res_checksum 13020
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 O3 0.2250(2) 0.37070(16) 0.13978(14) 0.0244(5) Uani d 1 . .
O O2 0.7476(2) 0.61301(17) 0.27191(16) 0.0288(5) Uani d 1 . .
H H2O 0.741(4) 0.6909(10) 0.278(2) 0.043 Uiso d 1 . .
O O1 0.5543(2) 0.27872(16) 0.40336(14) 0.0248(5) Uani d 1 . .
O O4 0.2372(2) 0.50789(16) 0.29210(14) 0.0219(4) Uani d 1 . .
O O5 1.0600(2) 1.16441(16) 0.39368(14) 0.0252(5) Uani d 1 . .
O O6 1.2486(2) 0.75906(17) 0.26446(16) 0.0311(5) Uani d 1 . .
H H6O 1.234(4) 0.6854(14) 0.271(2) 0.047 Uiso d 1 . .
O O7 0.7194(2) 0.92784(17) 0.13891(14) 0.0252(5) Uani d 1 . .
O O8 0.7424(2) 0.87754(16) 0.29317(13) 0.0208(4) Uani d 1 . .
C C1 0.4127(3) 0.3167(2) 0.2597(2) 0.0207(6) Uani d 1 . .
H H1 0.317759 0.267373 0.281279 0.025 Uiso calc 1 . .
C C2 0.5345(3) 0.3652(2) 0.3458(2) 0.0206(6) Uani d 1 . .
C C3 0.6152(3) 0.4749(2) 0.3592(2) 0.0211(6) Uani d 1 . .
H H3 0.695548 0.498054 0.413456 0.025 Uiso calc 1 . .
C C4 0.5835(3) 0.5635(2) 0.2916(2) 0.0210(6) Uani d 1 . .
H H4 0.514429 0.634247 0.327706 0.025 Uiso calc 1 . .
C C5 0.4824(3) 0.5061(2) 0.1964(2) 0.0213(6) Uani d 1 . .
H H5 0.430621 0.575362 0.168691 0.026 Uiso calc 1 . .
C C6 0.5910(3) 0.4263(3) 0.1161(2) 0.0263(7) Uani d 1 . .
H H6A 0.520091 0.406174 0.053892 0.032 Uiso calc 1 . .
H H6B 0.692026 0.476413 0.104437 0.032 Uiso calc 1 . .
C C7 0.6560(3) 0.3048(3) 0.1411(2) 0.0276(7) Uani d 1 . .
H H7A 0.749392 0.323841 0.192827 0.033 Uiso calc 1 . .
H H7B 0.705050 0.252400 0.081777 0.033 Uiso calc 1 . .
C C8 0.5107(3) 0.2326(2) 0.1773(2) 0.0244(7) Uani d 1 . .
H H8A 0.560293 0.161608 0.202263 0.029 Uiso calc 1 . .
H H8B 0.428924 0.198770 0.121522 0.029 Uiso calc 1 . .
C C9 0.3347(3) 0.4262(2) 0.2210(2) 0.0200(6) Uani d 1 . .
C C10 0.1260(4) 0.4544(3) 0.0941(2) 0.0324(7) Uani d 1 . .
H H10A 0.054707 0.406678 0.039144 0.049 Uiso calc 1 . .
H H10B 0.204374 0.510236 0.069224 0.049 Uiso calc 1 . .
H H10C 0.051003 0.503695 0.142526 0.049 Uiso calc 1 . .
C C11 0.0995(3) 0.4525(3) 0.3350(2) 0.0306(7) Uani d 1 . .
H H11A 0.019317 0.517320 0.364698 0.046 Uiso calc 1 . .
H H11B 0.147237 0.411031 0.385985 0.046 Uiso calc 1 . .
H H11C 0.037487 0.391278 0.283835 0.046 Uiso calc 1 . .
C C12 0.6804(4) 0.3079(3) 0.4830(2) 0.0311(7) Uani d 1 . .
H H12A 0.682747 0.240840 0.519879 0.047 Uiso calc 1 . .
H H12B 0.650051 0.386227 0.526962 0.047 Uiso calc 1 . .
H H12C 0.794670 0.316700 0.456675 0.047 Uiso calc 1 . .
C C13 0.9185(3) 1.0473(2) 0.2509(2) 0.0212(6) Uani d 1 . .
H H13 0.826248 1.109938 0.271311 0.025 Uiso calc 1 . .
C C14 1.0410(3) 1.0473(2) 0.3369(2) 0.0203(6) Uani d 1 . .
C C15 1.1210(3) 0.9454(2) 0.3512(2) 0.0200(6) Uani d 1 . .
H H15 1.203910 0.952686 0.404336 0.024 Uiso calc 1 . .
C C16 1.0862(3) 0.8197(2) 0.2871(2) 0.0225(6) Uani d 1 . .
H H16 1.019848 0.769528 0.326094 0.027 Uiso calc 1 . .
C C17 0.9785(3) 0.8221(2) 0.1917(2) 0.0214(6) Uani d 1 . .
H H17 0.923065 0.738204 0.168204 0.026 Uiso calc 1 . .
C C18 1.0814(3) 0.8527(2) 0.1075(2) 0.0268(7) Uani d 1 . .
H H18A 1.005550 0.839472 0.047137 0.032 Uiso calc 1 . .
H H18B 1.178675 0.793939 0.094485 0.032 Uiso calc 1 . .
C C19 1.1541(3) 0.9861(3) 0.1278(2) 0.0281(7) Uani d 1 . .
H H19A 1.249799 0.994633 0.178169 0.034 Uiso calc 1 . .
H H19B 1.201510 1.003598 0.066630 0.034 Uiso calc 1 . .
C C20 1.0141(3) 1.0806(3) 0.1641(2) 0.0264(7) Uani d 1 . .
H H20A 0.929714 1.083264 0.109210 0.032 Uiso calc 1 . .
H H20B 1.067692 1.164458 0.185194 0.032 Uiso calc 1 . .
C C21 0.8344(3) 0.9177(2) 0.2176(2) 0.0198(6) Uani d 1 . .
C C22 0.6196(4) 0.8179(3) 0.0962(2) 0.0347(8) Uani d 1 . .
H H22A 0.531624 0.838293 0.049607 0.052 Uiso calc 1 . .
H H22B 0.563015 0.786549 0.148393 0.052 Uiso calc 1 . .
H H22C 0.696186 0.754021 0.061296 0.052 Uiso calc 1 . .
C C23 0.6060(3) 0.9566(3) 0.3360(2) 0.0288(7) Uani d 1 . .
H H23A 0.535246 0.912043 0.375069 0.043 Uiso calc 1 . .
H H23B 0.533485 0.979948 0.283521 0.043 Uiso calc 1 . .
H H23C 0.656028 1.031866 0.378740 0.043 Uiso calc 1 . .
C C24 1.1744(4) 1.1781(3) 0.4781(2) 0.0305(7) Uani d 1 . .
H H24A 1.172238 1.264278 0.515319 0.046 Uiso calc 1 . .
H H24B 1.292245 1.157427 0.457040 0.046 Uiso calc 1 . .
H H24C 1.137482 1.121833 0.520074 0.046 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
O3 0.0254(10) 0.0188(10) 0.0306(12) 0.0042(7) -0.0063(9) 0.0099(9)
O2 0.0218(10) 0.0161(10) 0.0522(15) -0.0008(8) 0.0037(9) 0.0149(10)
O1 0.0323(10) 0.0170(10) 0.0288(12) 0.0030(8) -0.0047(9) 0.0141(9)
O4 0.0210(9) 0.0145(10) 0.0318(12) 0.0038(7) 0.0054(8) 0.0081(8)
O5 0.0311(10) 0.0146(10) 0.0297(12) 0.0001(8) -0.0046(9) 0.0052(9)
O6 0.0242(10) 0.0181(11) 0.0546(15) 0.0102(8) 0.0080(10) 0.0145(10)
O7 0.0263(10) 0.0212(11) 0.0296(12) -0.0021(8) -0.0062(9) 0.0102(9)
O8 0.0200(9) 0.0168(10) 0.0278(12) 0.0046(7) 0.0033(8) 0.0091(8)
C1 0.0223(13) 0.0135(14) 0.0289(17) 0.0014(10) -0.0007(12) 0.0106(12)
C2 0.0225(13) 0.0151(14) 0.0271(17) 0.0069(10) 0.0043(12) 0.0105(12)
C3 0.0203(13) 0.0194(15) 0.0260(17) 0.0031(11) -0.0013(12) 0.0102(12)
C4 0.0192(13) 0.0148(14) 0.0310(17) 0.0022(10) 0.0051(12) 0.0086(12)
C5 0.0210(13) 0.0144(14) 0.0320(17) 0.0066(10) 0.0036(12) 0.0119(12)
C6 0.0291(15) 0.0262(16) 0.0268(17) 0.0032(12) 0.0048(13) 0.0120(14)
C7 0.0271(15) 0.0246(16) 0.0310(18) 0.0077(12) 0.0030(13) 0.0047(14)
C8 0.0290(15) 0.0155(14) 0.0289(18) 0.0075(11) -0.0036(13) 0.0058(13)
C9 0.0182(13) 0.0169(14) 0.0259(16) 0.0028(10) 0.0005(12) 0.0071(12)
C10 0.0336(16) 0.0265(17) 0.040(2) 0.0082(13) -0.0095(14) 0.0160(15)
C11 0.0243(14) 0.0288(17) 0.043(2) 0.0037(12) 0.0103(14) 0.0154(15)
C12 0.0379(17) 0.0286(17) 0.0294(18) 0.0076(13) -0.0025(14) 0.0126(14)
C13 0.0237(13) 0.0108(13) 0.0313(17) 0.0035(10) -0.0031(12) 0.0100(12)
C14 0.0224(13) 0.0147(14) 0.0248(16) -0.0008(10) 0.0024(12) 0.0062(12)
C15 0.0194(13) 0.0186(14) 0.0236(16) 0.0027(10) -0.0010(11) 0.0083(12)
C16 0.0179(13) 0.0152(14) 0.0380(18) 0.0080(10) 0.0057(12) 0.0127(13)
C17 0.0213(13) 0.0129(13) 0.0310(17) 0.0015(10) 0.0012(12) 0.0071(12)
C18 0.0304(15) 0.0226(16) 0.0283(18) 0.0014(12) 0.0082(13) 0.0063(13)
C19 0.0311(15) 0.0286(17) 0.0273(18) -0.0036(12) 0.0046(13) 0.0118(14)
C20 0.0258(14) 0.0260(16) 0.0309(18) -0.0042(12) -0.0027(13) 0.0150(14)
C21 0.0201(13) 0.0166(14) 0.0242(16) 0.0006(10) -0.0015(12) 0.0084(12)
C22 0.0385(17) 0.0254(17) 0.039(2) -0.0050(13) -0.0139(15) 0.0060(15)
C23 0.0255(15) 0.0244(16) 0.040(2) 0.0108(11) 0.0106(13) 0.0121(14)
C24 0.0343(16) 0.0291(17) 0.0285(18) -0.0054(13) -0.0017(14) 0.0079(14)
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
C9 O3 C10 . . 116.1(2) ?
C4 O2 H2O . . 110(2) ?
C2 O1 C12 . . 116.2(2) ?
C9 O4 C11 . . 116.6(2) ?
C14 O5 C24 . . 116.6(2) ?
C16 O6 H6O . . 106(2) ?
C21 O7 C22 . . 116.0(2) ?
C21 O8 C23 . . 116.4(2) ?
C2 C1 C9 . . 109.6(2) ?
C2 C1 C8 . . 109.8(2) ?
C9 C1 C8 . . 109.5(2) ?
C2 C1 H1 . . 109.3 ?
C9 C1 H1 . . 109.3 ?
C8 C1 H1 . . 109.3 ?
C3 C2 O1 . . 126.4(2) ?
C3 C2 C1 . . 123.2(2) ?
O1 C2 C1 . . 110.3(2) ?
C2 C3 C4 . . 122.2(2) ?
C2 C3 H3 . . 118.9 ?
C4 C3 H3 . . 118.9 ?
O2 C4 C3 . . 108.1(2) ?
O2 C4 C5 . . 111.5(2) ?
C3 C4 C5 . . 113.9(2) ?
O2 C4 H4 . . 107.7 ?
C3 C4 H4 . . 107.7 ?
C5 C4 H4 . . 107.7 ?
C4 C5 C9 . . 108.7(2) ?
C4 C5 C6 . . 114.8(2) ?
C9 C5 C6 . . 109.0(2) ?
C4 C5 H5 . . 108.0 ?
C9 C5 H5 . . 108.0 ?
C6 C5 H5 . . 108.0 ?
C7 C6 C5 . . 114.4(2) ?
C7 C6 H6A . . 108.7 ?
C5 C6 H6A . . 108.7 ?
C7 C6 H6B . . 108.7 ?
C5 C6 H6B . . 108.7 ?
H6A C6 H6B . . 107.6 ?
C6 C7 C8 . . 111.6(2) ?
C6 C7 H7A . . 109.3 ?
C8 C7 H7A . . 109.3 ?
C6 C7 H7B . . 109.3 ?
C8 C7 H7B . . 109.3 ?
H7A C7 H7B . . 108.0 ?
C7 C8 C1 . . 111.1(2) ?
C7 C8 H8A . . 109.4 ?
C1 C8 H8A . . 109.4 ?
C7 C8 H8B . . 109.4 ?
C1 C8 H8B . . 109.4 ?
H8A C8 H8B . . 108.0 ?
O3 C9 O4 . . 109.76(19) ?
O3 C9 C5 . . 115.0(2) ?
O4 C9 C5 . . 105.4(2) ?
O3 C9 C1 . . 105.0(2) ?
O4 C9 C1 . . 113.5(2) ?
C5 C9 C1 . . 108.5(2) ?
O3 C10 H10A . . 109.5 ?
O3 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
O3 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
O4 C11 H11A . . 109.5 ?
O4 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
O4 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O1 C12 H12A . . 109.5 ?
O1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
O1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C14 C13 C21 . . 109.5(2) ?
C14 C13 C20 . . 110.8(2) ?
C21 C13 C20 . . 109.1(2) ?
C14 C13 H13 . . 109.1 ?
C21 C13 H13 . . 109.1 ?
C20 C13 H13 . . 109.1 ?
C15 C14 O5 . . 126.7(2) ?
C15 C14 C13 . . 122.6(2) ?
O5 C14 C13 . . 110.7(2) ?
C14 C15 C16 . . 122.8(2) ?
C14 C15 H15 . . 118.6 ?
C16 C15 H15 . . 118.6 ?
O6 C16 C15 . . 108.7(2) ?
O6 C16 C17 . . 110.7(2) ?
C15 C16 C17 . . 114.2(2) ?
O6 C16 H16 . . 107.7 ?
C15 C16 H16 . . 107.7 ?
C17 C16 H16 . . 107.7 ?
C18 C17 C21 . . 109.5(2) ?
C18 C17 C16 . . 114.9(2) ?
C21 C17 C16 . . 108.0(2) ?
C18 C17 H17 . . 108.1 ?
C21 C17 H17 . . 108.1 ?
C16 C17 H17 . . 108.1 ?
C17 C18 C19 . . 114.0(2) ?
C17 C18 H18A . . 108.8 ?
C19 C18 H18A . . 108.8 ?
C17 C18 H18B . . 108.8 ?
C19 C18 H18B . . 108.8 ?
H18A C18 H18B . . 107.6 ?
C20 C19 C18 . . 111.1(2) ?
C20 C19 H19A . . 109.4 ?
C18 C19 H19A . . 109.4 ?
C20 C19 H19B . . 109.4 ?
C18 C19 H19B . . 109.4 ?
H19A C19 H19B . . 108.0 ?
C19 C20 C13 . . 111.6(2) ?
C19 C20 H20A . . 109.3 ?
C13 C20 H20A . . 109.3 ?
C19 C20 H20B . . 109.3 ?
C13 C20 H20B . . 109.3 ?
H20A C20 H20B . . 108.0 ?
O7 C21 O8 . . 109.84(19) ?
O7 C21 C17 . . 115.2(2) ?
O8 C21 C17 . . 104.9(2) ?
O7 C21 C13 . . 105.2(2) ?
O8 C21 C13 . . 113.6(2) ?
C17 C21 C13 . . 108.3(2) ?
O7 C22 H22A . . 109.5 ?
O7 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
O7 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
O8 C23 H23A . . 109.5 ?
O8 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
O8 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
O5 C24 H24A . . 109.5 ?
O5 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
O5 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 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
O3 C9 . 1.415(3) ?
O3 C10 . 1.431(3) ?
O2 C4 . 1.435(3) ?
O2 H2O . 0.843(10) ?
O1 C2 . 1.367(3) ?
O1 C12 . 1.431(3) ?
O4 C9 . 1.427(3) ?
O4 C11 . 1.431(3) ?
O5 C14 . 1.365(3) ?
O5 C24 . 1.425(3) ?
O6 C16 . 1.438(3) ?
O6 H6O . 0.842(10) ?
O7 C21 . 1.406(3) ?
O7 C22 . 1.436(3) ?
O8 C21 . 1.429(3) ?
O8 C23 . 1.435(3) ?
C1 C2 . 1.499(4) ?
C1 C9 . 1.533(3) ?
C1 C8 . 1.538(4) ?
C1 H1 . 1.0000 ?
C2 C3 . 1.329(3) ?
C3 C4 . 1.500(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.526(4) ?
C4 H4 . 1.0000 ?
C5 C9 . 1.528(3) ?
C5 C6 . 1.543(4) ?
C5 H5 . 1.0000 ?
C6 C7 . 1.529(4) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.529(4) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 C14 . 1.497(4) ?
C13 C21 . 1.536(3) ?
C13 C20 . 1.541(4) ?
C13 H13 . 1.0000 ?
C14 C15 . 1.328(3) ?
C15 C16 . 1.496(4) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.543(4) ?
C16 H16 . 1.0000 ?
C17 C18 . 1.529(3) ?
C17 C21 . 1.534(3) ?
C17 H17 . 1.0000 ?
C18 C19 . 1.533(4) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 C20 . 1.528(4) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 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
O6 H6O O4 1_655 0.842(10) 2.027(11) 2.863(3) 172(3) yes
O2 H2O O8 . 0.843(10) 2.016(10) 2.858(3) 176(3) 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
C12 O1 C2 C3 . . . . -3.0(4) ?
C12 O1 C2 C1 . . . . 174.1(2) ?
C9 C1 C2 C3 . . . . -25.6(4) ?
C8 C1 C2 C3 . . . . 94.7(3) ?
C9 C1 C2 O1 . . . . 157.2(2) ?
C8 C1 C2 O1 . . . . -82.5(3) ?
O1 C2 C3 C4 . . . . -179.8(2) ?
C1 C2 C3 C4 . . . . 3.4(4) ?
C2 C3 C4 O2 . . . . -136.6(3) ?
C2 C3 C4 C5 . . . . -12.2(4) ?
O2 C4 C5 C9 . . . . 165.22(19) ?
C3 C4 C5 C9 . . . . 42.6(3) ?
O2 C4 C5 C6 . . . . 42.8(3) ?
C3 C4 C5 C6 . . . . -79.8(3) ?
C4 C5 C6 C7 . . . . 68.5(3) ?
C9 C5 C6 C7 . . . . -53.7(3) ?
C5 C6 C7 C8 . . . . 48.6(3) ?
C6 C7 C8 C1 . . . . -50.6(3) ?
C2 C1 C8 C7 . . . . -60.8(3) ?
C9 C1 C8 C7 . . . . 59.5(3) ?
C10 O3 C9 O4 . . . . 53.5(3) ?
C10 O3 C9 C5 . . . . -65.1(3) ?
C10 O3 C9 C1 . . . . 175.8(2) ?
C11 O4 C9 O3 . . . . 61.6(3) ?
C11 O4 C9 C5 . . . . -174.1(2) ?
C11 O4 C9 C1 . . . . -55.6(3) ?
C4 C5 C9 O3 . . . . 177.56(19) ?
C6 C5 C9 O3 . . . . -56.6(3) ?
C4 C5 C9 O4 . . . . 56.6(2) ?
C6 C5 C9 O4 . . . . -177.5(2) ?
C4 C5 C9 C1 . . . . -65.2(3) ?
C6 C5 C9 C1 . . . . 60.6(3) ?
C2 C1 C9 O3 . . . . 179.1(2) ?
C8 C1 C9 O3 . . . . 58.6(2) ?
C2 C1 C9 O4 . . . . -61.0(3) ?
C8 C1 C9 O4 . . . . 178.5(2) ?
C2 C1 C9 C5 . . . . 55.7(3) ?
C8 C1 C9 C5 . . . . -64.8(3) ?
C24 O5 C14 C15 . . . . -1.5(4) ?
C24 O5 C14 C13 . . . . -179.6(2) ?
C21 C13 C14 C15 . . . . 27.9(4) ?
C20 C13 C14 C15 . . . . -92.4(3) ?
C21 C13 C14 O5 . . . . -153.9(2) ?
C20 C13 C14 O5 . . . . 85.8(3) ?
O5 C14 C15 C16 . . . . 177.4(2) ?
C13 C14 C15 C16 . . . . -4.7(4) ?
C14 C15 C16 O6 . . . . 135.7(3) ?
C14 C15 C16 C17 . . . . 11.7(4) ?
O6 C16 C17 C18 . . . . -41.7(3) ?
C15 C16 C17 C18 . . . . 81.3(3) ?
O6 C16 C17 C21 . . . . -164.30(19) ?
C15 C16 C17 C21 . . . . -41.3(3) ?
C21 C17 C18 C19 . . . . 54.7(3) ?
C16 C17 C18 C19 . . . . -67.0(3) ?
C17 C18 C19 C20 . . . . -49.6(3) ?
C18 C19 C20 C13 . . . . 51.3(3) ?
C14 C13 C20 C19 . . . . 61.2(3) ?
C21 C13 C20 C19 . . . . -59.4(3) ?
C22 O7 C21 O8 . . . . -55.6(3) ?
C22 O7 C21 C17 . . . . 62.5(3) ?
C22 O7 C21 C13 . . . . -178.3(2) ?
C23 O8 C21 O7 . . . . -59.8(3) ?
C23 O8 C21 C17 . . . . 175.9(2) ?
C23 O8 C21 C13 . . . . 57.7(3) ?
C18 C17 C21 O7 . . . . 56.6(3) ?
C16 C17 C21 O7 . . . . -177.58(19) ?
C18 C17 C21 O8 . . . . 177.5(2) ?
C16 C17 C21 O8 . . . . -56.7(2) ?
C18 C17 C21 C13 . . . . -60.9(3) ?
C16 C17 C21 C13 . . . . 64.9(3) ?
C14 C13 C21 O7 . . . . 178.6(2) ?
C20 C13 C21 O7 . . . . -60.0(3) ?
C14 C13 C21 O8 . . . . 58.4(3) ?
C20 C13 C21 O8 . . . . 179.81(19) ?
C14 C13 C21 C17 . . . . -57.7(3) ?
C20 C13 C21 C17 . . . . 63.7(3) ?