#------------------------------------------------------------------------------
#$Date: 2025-04-18 03:53:35 +0200 (Fri, 18 Apr 2025) $
#$Revision: 299328 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023472.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_2023472
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 'C10 H12 O3'
_chemical_formula_moiety 'C10 H12 O3'
_chemical_formula_sum 'C10 H12 O3'
_chemical_formula_weight 180.20
_chemical_name_systematic
;
4-Methoxybicyclo[3.3.1]non-3-ene-2,9-dione
;
_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
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 99.546(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.4819(4)
_cell_length_b 7.4766(5)
_cell_length_c 9.0627(5)
_cell_measurement_reflns_used 6064
_cell_measurement_temperature 153(2)
_cell_measurement_theta_max 27.90
_cell_measurement_theta_min 2.28
_cell_volume 433.12(5)
_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 153(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_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 0.0283
_diffrn_reflns_av_unetI/netI 0.0274
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 8258
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.896
_diffrn_reflns_theta_min 2.279
_diffrn_source 'INCOATEC I\^A\mS microfocus sealed tube'
_exptl_absorpt_coefficient_mu 0.102
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6992
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.382
_exptl_crystal_description rod
_exptl_crystal_F_000 192
_exptl_crystal_size_max 0.380
_exptl_crystal_size_mid 0.080
_exptl_crystal_size_min 0.060
_refine_diff_density_max 0.180
_refine_diff_density_min -0.151
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack 0.5
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 119
_refine_ls_number_reflns 2031
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0314
_refine_ls_R_factor_gt 0.0296
_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^)+(0.0364P)^2^+0.0624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0728
_refine_ls_wR_factor_ref 0.0744
_reflns_number_gt 1948
_reflns_number_total 2031
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ev2016.cif
_cod_data_source_block 1
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 2023472
_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 0.962
_shelx_estimated_absorpt_t_max 0.994
_shelx_hkl_file
;
-1 0 0 3394.86 99.09
-2 0 0 3975.20 125.09
-2 0 0 4740.53 153.58
-3 0 0 154.08 18.50
-3 0 0 151.58 23.00
-4 0 0 11.50 10.50
-4 0 0 21.90 14.00
-7 0 0 5.20 1.80
-8 0 0 30.90 3.50
0 -1 0 -0.30 0.40
0 -1 0 0.10 0.40
0 -1 0 0.30 0.30
0 1 0 0.10 0.40
0 1 0 0.10 0.30
0 1 0 0.30 0.40
-1 -1 0 4193.28 129.79
1 -1 0 3799.62 146.29
1 1 0 4642.54 130.59
-1 1 0 4333.77 151.58
-2 -1 0 4031.10 120.89
2 -1 0 4033.40 156.78
-2 1 0 4286.07 160.58
-3 -1 0 25.20 2.30
-3 1 0 19.30 1.60
-3 1 0 20.80 1.70
-4 -1 0 456.75 13.10
-4 1 0 430.16 12.60
-4 1 0 459.95 12.40
-5 -1 0 87.29 4.40
-5 1 0 85.29 3.90
-5 1 0 79.59 3.70
-6 -1 0 172.38 7.10
-6 1 0 166.48 6.40
-6 1 0 158.58 6.20
-7 -1 0 -0.90 1.10
-7 1 0 -0.40 1.00
-7 1 0 -0.70 1.00
-8 -1 0 9.40 2.30
-8 1 0 7.40 2.30
-8 1 0 9.90 2.00
-8 1 0 6.20 2.00
0 -2 0 5852.11 206.48
0 2 0 5226.78 199.48
-1 -2 0 266.07 8.10
1 -2 0 270.57 8.30
-1 -2 0 284.17 8.10
1 -2 0 282.27 8.40
-1 -2 0 276.67 8.40
-1 2 0 270.87 8.60
-1 2 0 289.07 8.60
-1 2 0 280.87 8.30
1 2 0 275.77 7.70
1 2 0 299.77 8.80
1 2 0 265.77 7.60
-2 -2 0 1206.78 30.90
2 -2 0 1196.68 30.50
2 -2 0 1157.88 30.00
2 -2 0 1147.29 30.60
2 2 0 1238.08 30.60
-2 2 0 1310.67 31.10
-2 2 0 1107.89 30.90
3 -2 0 47.20 2.30
-3 -2 0 49.70 3.00
3 -2 0 46.90 2.10
-3 2 0 43.70 3.00
-3 2 0 46.50 2.90
-4 -2 0 142.59 5.80
-4 2 0 147.39 5.70
-4 2 0 142.39 5.70
-5 -2 0 622.34 17.90
-5 -2 0 608.04 16.90
-5 2 0 612.74 17.50
-5 2 0 553.64 17.30
-6 -2 0 18.60 2.80
-6 2 0 19.30 2.30
-6 2 0 23.20 2.70
-7 -2 0 167.88 8.00
-7 2 0 165.68 7.60
-7 2 0 180.68 7.40
-8 -2 0 1.10 1.70
-8 2 0 7.80 2.20
0 -3 0 -0.30 0.80
0 -3 0 -0.10 0.60
0 -3 0 -0.40 1.00
0 3 0 0.30 0.70
0 3 0 0.90 1.10
0 3 0 1.40 1.00
1 -3 0 552.74 15.40
-1 -3 0 539.65 15.90
1 -3 0 527.55 15.00
-1 -3 0 497.45 14.60
-1 -3 0 532.15 15.10
-1 3 0 533.45 15.50
1 3 0 528.75 14.40
-1 3 0 528.25 15.10
-1 3 0 537.95 15.70
1 3 0 515.85 15.00
1 3 0 523.55 14.60
-2 -3 0 1318.47 35.00
2 -3 0 1392.76 35.80
2 -3 0 1353.06 35.20
-2 -3 0 1413.26 36.20
2 -3 0 1342.67 35.60
-2 -3 0 1415.96 35.50
2 3 0 1408.16 35.60
-2 3 0 1345.27 36.00
-2 3 0 1372.76 36.40
-3 -3 0 96.19 4.70
3 -3 0 92.19 3.80
3 -3 0 88.59 4.00
3 3 0 87.59 4.00
-3 3 0 101.49 4.60
-3 3 0 86.99 4.60
4 -3 0 369.36 10.90
-4 -3 0 352.76 12.10
4 -3 0 399.56 10.70
-4 3 0 369.96 12.40
-4 3 0 377.86 12.20
-5 -3 0 150.88 7.00
-5 3 0 149.79 6.90
-5 3 0 152.58 6.80
-6 -3 0 213.78 9.10
-6 -3 0 216.18 8.00
-6 3 0 214.58 8.80
-6 3 0 215.48 9.10
-7 -3 0 109.39 6.70
-7 3 0 122.99 6.90
-8 -3 0 60.39 5.50
-8 3 0 73.09 4.90
-8 3 0 64.29 6.00
0 -4 0 1870.21 48.70
0 -4 0 1881.11 48.50
0 -4 0 1847.02 47.90
0 4 0 1794.72 48.20
0 4 0 1903.81 47.90
0 4 0 1838.22 48.50
-1 -4 0 516.55 15.40
1 -4 0 523.35 15.80
1 -4 0 554.24 16.20
-1 -4 0 559.14 16.20
-1 -4 0 532.65 16.40
-1 4 0 544.75 16.50
-1 4 0 525.95 16.60
-1 4 0 546.05 16.00
1 4 0 539.35 15.50
1 4 0 525.65 16.00
1 4 0 524.85 15.10
2 -4 0 305.67 10.20
-2 -4 0 295.57 10.60
-2 -4 0 285.57 9.60
2 -4 0 304.57 9.90
2 -4 0 327.97 10.50
-2 -4 0 312.27 10.20
2 4 0 307.27 10.10
-2 4 0 315.77 10.50
-2 4 0 309.87 10.90
-2 4 0 296.27 11.00
3 -4 0 46.40 3.10
3 -4 0 44.50 2.70
-3 -4 0 45.80 2.70
3 -4 0 41.80 3.00
-3 -4 0 42.70 3.00
-3 -4 0 44.20 3.70
3 4 0 43.30 3.10
-3 4 0 37.60 3.50
-3 4 0 41.70 3.80
-3 4 0 43.70 3.30
4 -4 0 140.99 5.80
-4 -4 0 142.79 6.90
4 -4 0 143.39 5.40
4 4 0 147.49 5.90
-4 4 0 136.49 9.10
-4 4 0 139.59 6.60
-5 -4 0 129.29 7.00
5 -4 0 134.59 5.20
5 -4 0 138.09 4.80
-5 4 0 147.99 7.00
-5 4 0 141.89 7.30
-6 -4 0 65.19 6.10
-6 4 0 69.79 6.10
-6 4 0 77.19 5.70
-7 -4 0 158.98 8.60
-7 -4 0 151.68 8.00
-7 4 0 158.48 7.90
-7 4 0 145.69 8.40
0 -5 0 3.40 1.20
0 -5 0 3.40 1.60
0 -5 0 3.80 1.60
0 5 0 3.80 1.20
0 5 0 3.20 1.60
0 5 0 1.70 1.30
-1 -5 0 545.25 16.60
-1 -5 0 510.75 15.70
1 -5 0 524.05 16.50
1 -5 0 491.75 15.90
-1 -5 0 524.45 16.80
1 5 0 512.75 15.20
1 5 0 515.05 15.70
-1 5 0 497.55 16.60
-1 5 0 535.45 16.30
1 5 0 531.75 16.40
-1 5 0 513.05 16.90
2 -5 0 227.88 8.70
-2 -5 0 236.18 9.60
-2 -5 0 238.28 8.60
2 -5 0 249.58 9.30
2 -5 0 237.18 9.00
-2 -5 0 255.47 9.40
2 5 0 255.27 8.60
-2 5 0 234.88 9.30
2 5 0 228.28 8.90
2 5 0 226.38 7.90
-3 -5 0 76.79 4.60
-3 -5 0 74.29 5.30
3 -5 0 71.99 4.40
3 -5 0 79.89 4.20
3 -5 0 64.99 4.80
-3 -5 0 73.69 4.00
3 5 0 72.49 4.50
-3 5 0 69.19 5.10
-3 5 0 72.69 5.50
-3 5 0 71.19 4.80
-4 -5 0 199.68 7.30
-4 -5 0 193.98 7.90
-4 -5 0 189.48 8.90
4 -5 0 180.48 10.30
4 -5 0 198.18 7.40
-4 5 0 181.28 8.50
-4 5 0 197.18 9.20
-4 5 0 205.68 9.70
4 5 0 186.38 7.60
-5 -5 0 46.70 4.70
5 -5 0 42.00 3.10
5 -5 0 44.70 2.80
-5 -5 0 45.80 3.10
-5 5 0 35.80 3.80
-5 5 0 38.60 4.80
-5 5 0 41.00 4.40
-6 -5 0 361.56 14.40
-6 5 0 383.26 14.30
-6 5 0 356.86 14.80
-6 5 0 392.36 16.00
-7 -5 0 82.99 5.30
-7 -5 0 87.79 6.60
-7 5 0 84.89 7.10
-7 5 0 83.29 5.80
0 -6 0 80.59 5.30
0 -6 0 80.69 5.50
0 -6 0 73.29 4.70
0 6 0 73.49 5.40
0 6 0 75.69 4.60
-1 -6 0 121.29 6.20
-1 -6 0 132.79 7.30
1 -6 0 122.19 6.30
1 -6 0 131.99 6.90
-1 -6 0 124.69 6.80
-1 6 0 126.99 7.00
1 6 0 135.49 7.00
1 6 0 137.99 6.50
-1 6 0 137.49 6.60
-1 6 0 128.49 7.40
1 6 0 134.89 5.90
2 -6 0 81.99 5.10
2 -6 0 85.89 5.40
2 -6 0 78.09 4.90
-2 -6 0 85.39 6.00
-2 -6 0 87.39 5.00
-2 -6 0 83.99 5.40
-2 6 0 78.29 5.60
2 6 0 81.29 4.40
2 6 0 82.69 4.00
2 6 0 86.19 5.40
-2 6 0 75.59 5.90
-2 6 0 83.49 5.30
3 -6 0 314.97 11.30
3 -6 0 297.07 10.50
-3 -6 0 292.17 11.30
-3 -6 0 293.67 12.60
3 -6 0 309.37 11.20
-3 -6 0 284.67 11.90
-3 6 0 299.07 12.40
3 6 0 276.57 10.80
-3 6 0 281.27 12.50
-3 6 0 278.67 12.90
-4 -6 0 74.99 5.90
4 -6 0 83.79 4.80
-4 -6 0 68.99 5.00
-4 -6 0 77.29 5.10
4 -6 0 78.39 4.80
-4 6 0 73.59 6.20
-4 6 0 68.89 5.80
4 6 0 77.79 5.10
-4 6 0 67.39 5.20
-5 -6 0 177.78 9.20
-5 -6 0 166.58 7.10
5 -6 0 168.68 7.30
-5 -6 0 174.68 8.00
5 -6 0 166.28 6.80
-5 6 0 164.28 8.70
-5 6 0 165.88 11.60
5 6 0 169.38 7.50
-5 6 0 184.08 10.30
-6 -6 0 7.00 2.70
6 -6 0 6.30 1.70
-6 -6 0 7.20 1.70
6 -6 0 8.90 1.50
-6 6 0 7.90 2.30
0 -7 0 4.80 1.80
0 -7 0 6.70 2.70
0 -7 0 7.40 2.60
0 7 0 3.60 2.20
0 7 0 9.00 2.50
0 7 0 8.30 1.90
1 -7 0 594.04 20.00
-1 -7 0 578.34 19.10
-1 -7 0 605.44 21.60
-1 -7 0 633.44 26.40
1 -7 0 599.94 19.50
1 7 0 616.74 19.20
-1 7 0 623.54 20.80
-1 7 0 588.04 20.30
1 7 0 590.24 18.30
1 7 0 607.24 20.00
-2 -7 0 67.99 4.70
2 -7 0 75.59 5.40
2 -7 0 65.59 4.90
2 -7 0 62.09 4.80
-2 -7 0 69.49 5.60
-2 7 0 62.39 5.50
2 7 0 66.89 3.80
2 7 0 67.79 5.40
-2 7 0 72.49 5.20
-2 7 0 54.69 5.70
2 7 0 64.89 4.30
-3 -7 0 8.10 2.60
3 -7 0 10.60 2.60
3 -7 0 3.30 1.80
-3 -7 0 8.50 2.30
-3 -7 0 9.70 2.20
3 -7 0 9.80 2.20
-3 7 0 6.40 2.10
3 7 0 8.10 2.50
-3 7 0 9.10 3.20
-3 7 0 7.30 2.70
4 -7 0 83.39 5.40
-4 -7 0 93.49 9.00
4 -7 0 83.69 5.30
4 -7 0 82.59 4.80
-4 -7 0 84.09 6.60
-4 -7 0 81.39 5.20
-4 7 0 76.19 6.60
4 7 0 83.99 5.60
-4 7 0 80.19 6.00
-4 7 0 86.89 7.50
-5 -7 0 56.19 5.00
-5 -7 0 53.99 5.60
5 -7 0 51.39 3.80
-5 -7 0 52.99 4.20
5 -7 0 59.29 4.40
-5 7 0 59.09 5.20
5 7 0 46.90 5.30
0 -8 0 157.18 11.20
0 -8 0 158.08 8.70
0 8 0 142.99 8.90
0 8 0 151.88 8.40
0 8 0 160.98 7.90
-1 -8 0 12.90 3.10
-1 -8 0 10.60 2.50
1 -8 0 12.90 2.90
1 -8 0 13.40 3.20
-1 -8 0 13.70 3.00
1 8 0 13.30 2.40
-1 8 0 13.60 2.70
-1 8 0 9.50 2.80
1 8 0 13.40 3.30
2 -8 0 11.20 2.60
-2 -8 0 5.70 2.10
-2 -8 0 4.20 2.30
2 -8 0 8.30 2.50
2 -8 0 5.80 2.40
-2 -8 0 4.20 2.40
2 8 0 6.80 2.80
-2 8 0 11.70 3.30
-2 8 0 10.10 2.90
2 8 0 6.70 1.70
-2 8 0 8.30 2.20
2 8 0 8.20 2.30
-3 -8 0 7.00 2.70
-3 -8 0 4.60 2.20
-3 -8 0 4.20 3.20
3 -8 0 3.30 2.10
3 -8 0 7.40 2.20
3 -8 0 5.30 2.20
-3 8 0 7.10 1.90
-3 8 0 10.80 4.20
-4 -8 0 57.89 6.00
4 -8 0 50.09 4.70
-4 -8 0 48.80 4.90
4 -8 0 54.19 4.30
4 -8 0 50.29 4.40
-4 8 0 61.29 6.70
4 8 0 58.09 5.40
0 -9 0 2.20 2.10
0 9 0 2.90 2.10
1 -9 0 92.89 6.90
-1 -9 0 84.09 6.90
-1 -9 0 92.09 6.90
1 -9 0 86.39 6.50
-1 9 0 88.19 6.20
1 9 0 123.99 13.20
-1 9 0 90.09 7.60
1 9 0 84.79 5.40
2 -9 0 7.00 2.70
2 -9 0 8.90 3.00
-2 -9 0 6.50 2.80
-2 -9 0 8.30 2.80
2 9 0 10.70 2.10
2 9 0 13.20 2.80
-2 9 0 6.70 2.50
3 -9 0 19.10 3.60
-3 -9 0 26.60 4.40
-3 -9 0 14.60 3.80
3 -9 0 15.60 3.70
-3 9 0 17.20 3.30
-8 0 1 10.00 2.20
-7 0 1 2.20 2.20
-4 0 1 28.00 1.60
-3 0 1 150.98 4.60
2 0 -1 226.58 6.40
-2 0 1 226.78 6.20
1 0 -1 1989.50 71.09
-1 0 1 2435.56 72.19
0 0 -1 760.22 18.50
0 0 1 769.52 18.70
0 0 1 739.23 18.50
0 0 -1 692.83 18.50
0 0 -1 775.62 18.70
-1 0 -1 3651.13 115.09
-3 0 -1 279.37 7.30
-3 0 -1 269.37 7.80
-4 0 -1 66.69 27.50
-4 0 -1 123.29 25.70
-6 0 -1 81.29 5.10
-6 0 -1 80.29 3.50
-7 0 -1 -1.00 1.20
-7 0 -1 -1.70 0.90
-8 0 -1 4.10 1.80
-8 -1 1 45.30 4.10
-7 1 1 69.89 4.10
-6 -1 1 12.60 2.10
-5 -1 1 13.40 1.90
-4 -1 1 601.34 17.20
-4 -1 1 667.23 17.30
-3 -1 1 611.14 16.00
3 -1 -1 607.04 15.40
-3 1 1 591.44 15.80
-3 1 1 584.14 15.90
2 -1 -1 438.26 11.30
-2 -1 1 421.46 11.70
2 -1 -1 427.96 11.20
-2 1 1 406.16 11.70
-2 1 1 451.05 11.40
-2 1 1 450.75 11.50
1 -1 -1 879.11 22.80
1 -1 -1 926.51 22.40
1 -1 -1 930.41 22.40
-1 1 1 823.92 22.80
-1 1 1 896.11 22.90
-1 1 1 889.11 22.50
-1 1 1 894.11 22.50
0 -1 1 3520.45 124.29
0 -1 -1 2981.20 114.79
0 1 -1 3271.07 121.49
0 1 1 2879.41 112.39
-1 -1 -1 2313.37 92.99
1 1 1 2681.53 93.39
-1 1 -1 2353.26 110.09
-2 -1 -1 844.62 21.80
-2 -1 -1 869.51 21.90
-2 -1 -1 856.91 22.70
2 -1 1 864.61 21.80
-2 1 -1 883.41 22.60
-2 1 -1 909.01 23.10
-3 -1 -1 198.48 6.70
-3 1 -1 201.68 6.10
-3 1 -1 201.38 6.50
-4 -1 -1 865.31 23.10
-4 1 -1 834.92 22.10
-4 1 -1 835.12 22.70
-5 -1 -1 273.37 9.40
-5 1 -1 261.27 8.30
-5 1 -1 260.17 8.70
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-1 1 -11 170.68 10.20
-1 1 -11 210.78 8.80
1 1 11 182.58 9.30
-4 -2 11 26.60 3.50
4 -2 -11 20.90 3.50
-4 2 11 13.80 3.30
-4 2 11 19.20 3.10
3 -2 -11 222.58 10.90
-3 -2 11 247.78 10.10
3 -2 -11 243.78 8.90
-3 -2 11 210.18 10.10
-3 2 11 231.38 11.10
3 2 -11 243.48 9.80
-3 2 11 219.98 10.30
2 -2 -11 75.39 4.80
-2 -2 11 88.49 6.00
-2 -2 11 86.39 5.50
2 -2 -11 73.69 6.30
-2 2 11 98.49 7.70
2 2 -11 78.49 6.00
-1 -2 11 19.20 3.10
1 2 -11 17.70 3.40
1 2 -11 22.70 3.60
-1 2 11 20.80 3.70
0 -2 11 5.00 2.00
0 -2 11 4.30 1.70
0 2 -11 9.70 2.60
0 2 -11 7.40 2.80
0 2 11 6.70 2.50
-1 -2 -11 21.60 4.00
-1 -2 -11 28.50 4.20
1 -2 11 27.60 3.50
1 -2 11 30.60 3.40
-1 2 -11 23.10 4.10
1 2 11 26.10 4.10
3 -3 -11 1.30 2.00
-3 -3 11 -1.60 1.30
3 -3 -11 0.40 1.60
-3 3 11 1.40 1.50
3 3 -11 1.90 2.10
-3 3 11 2.80 2.00
3 3 -11 -4.10 2.10
2 -3 -11 27.00 4.50
-2 -3 11 32.20 3.20
-2 3 11 23.60 4.00
2 3 -11 33.30 4.50
2 3 -11 26.30 3.80
-2 3 11 21.90 3.50
-1 -3 11 6.60 1.80
-1 -3 11 4.40 1.90
-1 3 11 2.60 2.50
1 3 -11 2.80 2.00
-1 3 11 3.50 1.90
0 -3 -11 48.80 5.60
0 -3 11 39.80 3.60
0 -3 11 38.00 3.90
0 3 -11 59.49 9.60
0 3 11 40.90 4.30
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 16501
_shelx_res_file
;
TITL sh5023_a.res in P2(1)
sh5023_a.res
created by SHELXL-2019/3 at 12:04:01 on 01-Apr-2025
REM Old TITL sh5023 in P2(1)
REM SHELXT solution in P2(1): R1 0.081, Rweak 0.021, Alpha 0.001
REM 3.184 for 5 systematic absences, Orientation as input
REM Flack x = 0.404 ( 0.325 ) from 759 Parsons' quotients
REM Formula found by SHELXT: C10 O3
CELL 0.71073 6.4819 7.4766 9.0627 90.000 99.546 90.000
ZERR 2.000 0.0004 0.0005 0.0005 0.000 0.002 0.000
LATT -1
SYMM -X, 1/2+Y, -Z
SFAC C H O
UNIT 20 24 6
TEMP -120.150
SIZE 0.06 0.08 0.38
L.S. 10
BOND $H
ACTA
CONF
TWIN
LIST 4
FMAP 2
PLAN -5
WGHT 0.036400 0.062400
FVAR 1.90924
O1 3 0.635581 0.202195 0.731439 11.00000 0.04172 0.01892 =
0.04816 0.00263 0.01123 0.00006
O2 3 0.801226 0.733878 0.492089 11.00000 0.02876 0.02634 =
0.02249 -0.00020 0.00778 -0.00412
O3 3 0.274031 0.709800 0.734838 11.00000 0.02589 0.03724 =
0.04229 0.00587 0.01090 0.00779
C1 1 0.630488 0.754789 0.700262 11.00000 0.02345 0.01867 =
0.02185 0.00099 0.00331 0.00188
AFIX 13
H1 2 0.578127 0.868685 0.649526 11.00000 -1.20000
AFIX 0
C2 1 0.720259 0.636870 0.592579 11.00000 0.01897 0.02372 =
0.01888 0.00076 0.00150 -0.00120
C10 1 0.888415 0.636819 0.379323 11.00000 0.03381 0.03710 =
0.02741 -0.00609 0.01392 -0.00488
AFIX 137
H10A 2 0.930016 0.721305 0.306964 11.00000 -1.50000
H10B 2 0.783321 0.554093 0.327603 11.00000 -1.50000
H10C 2 1.011125 0.569139 0.426813 11.00000 -1.50000
AFIX 0
C3 1 0.717048 0.456434 0.598904 11.00000 0.02474 0.02266 =
0.02497 -0.00391 0.00407 0.00055
AFIX 43
H3 2 0.773987 0.388629 0.526623 11.00000 -1.20000
AFIX 0
C4 1 0.627791 0.364739 0.714629 11.00000 0.02224 0.02047 =
0.02914 0.00026 0.00199 -0.00036
C5 1 0.521101 0.477991 0.820674 11.00000 0.02356 0.02310 =
0.02639 0.00409 0.00703 -0.00170
AFIX 13
H5 2 0.397653 0.412087 0.846504 11.00000 -1.20000
AFIX 0
C6 1 0.677878 0.519609 0.965732 11.00000 0.03477 0.02820 =
0.02265 0.00560 0.00504 -0.00075
AFIX 23
H6A 2 0.604837 0.586413 1.036072 11.00000 -1.20000
H6B 2 0.729428 0.405919 1.014438 11.00000 -1.20000
AFIX 0
C7 1 0.863640 0.629587 0.932943 11.00000 0.02704 0.03154 =
0.02298 0.00079 -0.00069 -0.00013
AFIX 23
H7A 2 0.951032 0.665124 1.028598 11.00000 -1.20000
H7B 2 0.950543 0.554829 0.877127 11.00000 -1.20000
AFIX 0
C8 1 0.793806 0.796960 0.841792 11.00000 0.02831 0.02348 =
0.02371 -0.00300 0.00420 -0.00371
AFIX 23
H8A 2 0.917481 0.854469 0.810933 11.00000 -1.20000
H8B 2 0.732289 0.882757 0.905492 11.00000 -1.20000
AFIX 0
C9 1 0.451146 0.654033 0.748728 11.00000 0.02358 0.02251 =
0.02188 -0.00117 0.00574 0.00213
HKLF 4
REM sh5023_a.res in P2(1)
REM wR2 = 0.0744, GooF = S = 1.078, Restrained GooF = 1.077 for all data
REM R1 = 0.0296 for 1948 Fo > 4sig(Fo) and 0.0314 for all 2031 data
REM 119 parameters refined using 1 restraints
END
WGHT 0.0364 0.0624
REM Highest difference peak 0.180, deepest hole -0.151, 1-sigma level 0.037
Q1 1 0.6666 0.6974 0.6403 11.00000 0.05 0.18
Q2 1 0.4820 0.5586 0.7806 11.00000 0.05 0.17
Q3 1 0.5421 0.7000 0.7214 11.00000 0.05 0.15
Q4 1 0.7614 0.5710 0.9382 11.00000 0.05 0.15
Q5 1 0.6748 0.4211 0.6553 11.00000 0.05 0.15
;
_shelx_res_checksum 828
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.6356(2) 0.20219(18) 0.73144(16) 0.0358(3) Uani d 1 . .
O O2 0.80123(19) 0.73388(16) 0.49209(12) 0.0255(3) Uani d 1 . .
O O3 0.2740(2) 0.7098(2) 0.73484(15) 0.0345(3) Uani d 1 . .
C C1 0.6305(3) 0.7548(2) 0.70026(17) 0.0214(3) Uani d 1 . .
H H1 0.578127 0.868685 0.649526 0.026 Uiso calc 1 . .
C C2 0.7203(2) 0.6369(2) 0.59258(16) 0.0207(3) Uani d 1 . .
C C10 0.8884(3) 0.6368(3) 0.3793(2) 0.0318(4) Uani d 1 . .
H H10A 0.930016 0.721305 0.306964 0.048 Uiso calc 1 . .
H H10B 0.783321 0.554093 0.327603 0.048 Uiso calc 1 . .
H H10C 1.011125 0.569139 0.426813 0.048 Uiso calc 1 . .
C C3 0.7170(3) 0.4564(2) 0.59890(18) 0.0241(3) Uani d 1 . .
H H3 0.773987 0.388629 0.526623 0.029 Uiso calc 1 . .
C C4 0.6278(3) 0.3647(2) 0.71463(18) 0.0242(3) Uani d 1 . .
C C5 0.5211(3) 0.4780(2) 0.82067(18) 0.0240(3) Uani d 1 . .
H H5 0.397653 0.412087 0.846504 0.029 Uiso calc 1 . .
C C6 0.6779(3) 0.5196(2) 0.96573(19) 0.0285(4) Uani d 1 . .
H H6A 0.604837 0.586413 1.036072 0.034 Uiso calc 1 . .
H H6B 0.729428 0.405919 1.014438 0.034 Uiso calc 1 . .
C C7 0.8636(3) 0.6296(2) 0.93294(18) 0.0277(4) Uani d 1 . .
H H7A 0.951032 0.665124 1.028598 0.033 Uiso calc 1 . .
H H7B 0.950543 0.554829 0.877127 0.033 Uiso calc 1 . .
C C8 0.7938(3) 0.7970(2) 0.84179(19) 0.0252(4) Uani d 1 . .
H H8A 0.917481 0.854469 0.810933 0.030 Uiso calc 1 . .
H H8B 0.732289 0.882757 0.905492 0.030 Uiso calc 1 . .
C C9 0.4511(3) 0.6540(2) 0.74873(17) 0.0224(3) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0417(8) 0.0189(6) 0.0482(8) 0.0001(6) 0.0112(6) 0.0026(5)
O2 0.0288(7) 0.0263(6) 0.0225(5) -0.0041(5) 0.0078(4) -0.0002(4)
O3 0.0259(7) 0.0372(7) 0.0423(7) 0.0078(6) 0.0109(5) 0.0059(6)
C1 0.0235(8) 0.0187(8) 0.0219(7) 0.0019(6) 0.0033(6) 0.0010(6)
C2 0.0190(7) 0.0237(7) 0.0189(6) -0.0012(6) 0.0015(6) 0.0008(6)
C10 0.0338(10) 0.0371(9) 0.0274(8) -0.0049(8) 0.0139(7) -0.0061(8)
C3 0.0247(8) 0.0227(8) 0.0250(8) 0.0005(6) 0.0041(6) -0.0039(6)
C4 0.0222(9) 0.0205(8) 0.0291(8) -0.0004(6) 0.0020(6) 0.0003(6)
C5 0.0236(9) 0.0231(8) 0.0264(8) -0.0017(6) 0.0070(6) 0.0041(6)
C6 0.0348(10) 0.0282(9) 0.0227(7) -0.0008(7) 0.0050(6) 0.0056(6)
C7 0.0270(9) 0.0315(9) 0.0230(7) -0.0001(7) -0.0007(6) 0.0008(7)
C8 0.0283(9) 0.0235(8) 0.0237(8) -0.0037(7) 0.0042(6) -0.0030(6)
C9 0.0236(8) 0.0225(7) 0.0219(7) 0.0021(6) 0.0057(6) -0.0012(6)
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
C2 O2 C10 . . 116.97(14) ?
C2 C1 C9 . . 107.21(13) ?
C2 C1 C8 . . 111.78(13) ?
C9 C1 C8 . . 108.24(12) ?
C2 C1 H1 . . 109.8 ?
C9 C1 H1 . . 109.8 ?
C8 C1 H1 . . 109.8 ?
O2 C2 C3 . . 125.52(15) ?
O2 C2 C1 . . 111.23(14) ?
C3 C2 C1 . . 123.25(14) ?
O2 C10 H10A . . 109.5 ?
O2 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
O2 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C2 C3 C4 . . 120.89(15) ?
C2 C3 H3 . . 119.6 ?
C4 C3 H3 . . 119.6 ?
O1 C4 C3 . . 123.06(16) ?
O1 C4 C5 . . 119.00(15) ?
C3 C4 C5 . . 117.94(14) ?
C9 C5 C4 . . 110.31(13) ?
C9 C5 C6 . . 107.41(13) ?
C4 C5 C6 . . 110.00(14) ?
C9 C5 H5 . . 109.7 ?
C4 C5 H5 . . 109.7 ?
C6 C5 H5 . . 109.7 ?
C7 C6 C5 . . 111.67(13) ?
C7 C6 H6A . . 109.3 ?
C5 C6 H6A . . 109.3 ?
C7 C6 H6B . . 109.3 ?
C5 C6 H6B . . 109.3 ?
H6A C6 H6B . . 107.9 ?
C8 C7 C6 . . 111.97(15) ?
C8 C7 H7A . . 109.2 ?
C6 C7 H7A . . 109.2 ?
C8 C7 H7B . . 109.2 ?
C6 C7 H7B . . 109.2 ?
H7A C7 H7B . . 107.9 ?
C7 C8 C1 . . 112.38(14) ?
C7 C8 H8A . . 109.1 ?
C1 C8 H8A . . 109.1 ?
C7 C8 H8B . . 109.1 ?
C1 C8 H8B . . 109.1 ?
H8A C8 H8B . . 107.9 ?
O3 C9 C5 . . 124.04(16) ?
O3 C9 C1 . . 124.16(15) ?
C5 C9 C1 . . 111.78(14) ?
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
O1 C4 . 1.225(2) ?
O2 C2 . 1.3377(19) ?
O2 C10 . 1.443(2) ?
O3 C9 . 1.208(2) ?
C1 C2 . 1.502(2) ?
C1 C9 . 1.510(2) ?
C1 C8 . 1.554(2) ?
C1 H1 . 1.0000 ?
C2 C3 . 1.351(2) ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C3 C4 . 1.451(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.529(2) ?
C5 C9 . 1.505(2) ?
C5 C6 . 1.554(2) ?
C5 H5 . 1.0000 ?
C6 C7 . 1.527(3) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.526(2) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
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
C10 O2 C2 C3 . . . . 1.4(2) ?
C10 O2 C2 C1 . . . . -178.52(14) ?
C9 C1 C2 O2 . . . . 149.74(13) ?
C8 C1 C2 O2 . . . . -91.79(15) ?
C9 C1 C2 C3 . . . . -30.1(2) ?
C8 C1 C2 C3 . . . . 88.33(19) ?
O2 C2 C3 C4 . . . . 179.00(15) ?
C1 C2 C3 C4 . . . . -1.1(3) ?
C2 C3 C4 O1 . . . . -174.35(17) ?
C2 C3 C4 C5 . . . . 5.1(2) ?
O1 C4 C5 C9 . . . . -157.28(16) ?
C3 C4 C5 C9 . . . . 23.2(2) ?
O1 C4 C5 C6 . . . . 84.41(19) ?
C3 C4 C5 C6 . . . . -95.07(17) ?
C9 C5 C6 C7 . . . . -57.61(19) ?
C4 C5 C6 C7 . . . . 62.47(18) ?
C5 C6 C7 C8 . . . . 52.43(19) ?
C6 C7 C8 C1 . . . . -50.79(18) ?
C2 C1 C8 C7 . . . . -63.52(18) ?
C9 C1 C8 C7 . . . . 54.34(18) ?
C4 C5 C9 O3 . . . . 125.58(18) ?
C6 C5 C9 O3 . . . . -114.54(18) ?
C4 C5 C9 C1 . . . . -56.12(18) ?
C6 C5 C9 C1 . . . . 63.76(17) ?
C2 C1 C9 O3 . . . . -123.17(17) ?
C8 C1 C9 O3 . . . . 116.10(18) ?
C2 C1 C9 C5 . . . . 58.54(16) ?
C8 C1 C9 C5 . . . . -62.20(17) ?