#------------------------------------------------------------------------------
#$Date: 2024-05-06 07:21:16 +0300 (Mon, 06 May 2024) $
#$Revision: 291725 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/30/2023071.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_2023071
loop_
_publ_author_name
'Hanauer, Thomas'
'Seichter, Wilhelm'
'Mazik, Monika'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
4,4'-di-meth-oxy-biphenyl-3,3',5,5'-tetra-carb-oxy-lic acid dihydrate.
;
_journal_coeditor_code EX2080
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 413
_journal_page_last 417
_journal_paper_doi 10.1107/S2056989024002305
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C18 H14 O10, 2H2 O'
_chemical_formula_moiety 'C18 H14 O10, 2(H2 O)'
_chemical_formula_sum 'C18 H18 O12'
_chemical_formula_weight 426.32
_chemical_name_systematic
;
4,4'-Dimethoxybiphenyl-3,3',5,5'-tetracarboxylic acid dihydrate
;
_space_group_crystal_system tetragonal
_space_group_IT_number 110
_space_group_name_Hall 'I 4bw -2c'
_space_group_name_H-M_alt 'I 41 c d'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 24.069(3)
_cell_length_b 24.069(3)
_cell_length_c 6.4468(8)
_cell_measurement_reflns_used 1164
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max 23.31
_cell_measurement_theta_min 3.67
_cell_volume 3734.7(8)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010),
ShelXle
(H\"ubschle et al., 2011)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 123(2)
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'Stoe IPDS 2T'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0546
_diffrn_reflns_av_unetI/netI 0.0351
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_h_min -30
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 14573
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.481
_diffrn_reflns_theta_min 2.676
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current 40
_diffrn_source_power 2.000
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 0.130
_exptl_absorpt_correction_type none
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.516
_exptl_crystal_description needle
_exptl_crystal_F_000 1776
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.025
_exptl_crystal_size_min 0.025
_refine_diff_density_max 0.219
_refine_diff_density_min -0.196
_refine_ls_abs_structure_details
;
Flack x determined using 575 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -2.2(10)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.083
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 153
_refine_ls_number_reflns 1914
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.083
_refine_ls_R_factor_all 0.0617
_refine_ls_R_factor_gt 0.0394
_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^)+(0.0377P)^2^+2.9912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0824
_refine_ls_wR_factor_ref 0.0929
_reflns_number_gt 1502
_reflns_number_total 1914
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ex2080.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023071.cif.'
_cod_original_cell_volume 3734.6(9)
_cod_database_code 2023071
_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 0.950
_shelx_estimated_absorpt_t_max 0.997
_shelx_hkl_file
;
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-7 -18 -5 123.25 10.72 0
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-6 -13 -5 106.06 10.20 0
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-5 -10 -5 25.96 6.84 0
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-2 -5 -5 15.51 10.32 0
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1 -11 4 156.50 12.21 0
1 -6 3 37.75 11.09 0
2 -23 5 60.72 13.23 0
2 -21 5 124.11 13.35 0
3 -16 5 23.71 10.04 0
3 -1 -6 20.42 7.73 0
6 2 2 16.51 10.26 0
7 4 -5 4.50 9.37 0
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8 1 3 9.48 9.94 0
8 6 -4 2.63 9.39 0
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10 -14 6 63.08 8.32 0
10 4 -6 5.46 10.06 0
11 2 -7 2.39 9.73 0
11 5 2 131.21 7.98 0
12 0 4 25.27 6.84 0
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15 9 -4 26.61 10.77 0
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16 2 4 -0.70 9.90 0
16 5 3 14.50 9.38 0
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25 6 3 80.67 11.74 0
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28 8 2 0.78 10.80 0
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0 -7 3 -5.19 10.09 0
1 -8 -7 4.96 9.10 0
2 -19 5 7.56 9.88 0
2 -7 -7 79.67 10.28 0
4 -13 5 21.42 9.79 0
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5 -5 4 3.66 7.58 0
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6 -4 4 25.16 7.77 0
7 -19 6 -8.02 9.61 0
7 -8 5 73.66 10.65 0
7 -3 4 26.56 8.07 0
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8 -2 4 35.54 10.41 0
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11 6 -5 74.29 10.91 0
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15 -2 5 8.48 6.96 0
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1 -9 4 -1.95 9.85 0
1 0 1 6.15 19.51 0
2 -15 5 20.40 9.08 0
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13 7 2 46.68 10.91 0
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-3 -19 -6 68.49 9.86 0
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3 1 -4 1413.46 14.41 0
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4 -4 4 305.51 10.91 0
4 3 1 158.26 12.86 0
4 4 0 352.21 22.80 0
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7 2 3 156.71 10.91 0
8 -3 -7 7.76 10.01 0
8 0 4 1076.24 13.27 0
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9 -2 -7 -4.95 10.13 0
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10 2 -6 -2.44 9.91 0
10 6 2 30.16 9.53 0
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12 -6 6 43.14 10.66 0
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17 10 1 10.13 9.51 0
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21 8 3 7.22 9.85 0
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22 10 -4 2.95 13.66 0
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24 11 1 6.46 9.60 0
24 12 -2 -5.43 12.66 0
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26 11 1 11.74 10.05 0
26 12 -2 0.44 10.78 0
28 10 2 4.01 9.29 0
28 11 1 61.92 10.36 0
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-2 -16 -6 19.17 8.90 0
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11 8 5 8.29 9.72 0
12 -12 -6 0.72 10.68 0
12 5 -3 421.22 10.95 0
12 9 -1 46.86 8.64 0
12 10 0 37.09 6.65 0
12 10 4 45.51 9.19 0
13 -2 -5 26.42 10.34 0
14 8 6 76.04 11.36 0
14 12 2 399.70 9.80 0
15 12 1 172.09 9.75 0
15 12 3 45.31 9.41 0
16 4 -4 45.85 8.97 0
16 7 -3 165.91 8.89 0
17 9 6 49.91 9.87 0
17 13 2 134.87 9.62 0
18 1 -5 5.56 8.24 0
18 10 -2 45.64 8.59 0
18 11 5 7.99 10.84 0
18 13 1 5.32 9.04 0
18 13 3 49.98 9.33 0
19 5 -4 5.37 9.26 0
19 8 -3 90.47 9.61 0
21 12 -1 20.44 8.72 0
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21 13 4 -2.22 9.78 0
22 6 -4 9.70 9.07 0
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23 11 -2 14.15 8.90 0
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25 11 -2 -9.69 9.26 0
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7 6 -1 132.75 13.83 0
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7 8 1 164.38 11.55 0
7 8 3 -0.47 8.66 0
8 8 0 1131.91 14.59 0
10 6 6 25.87 10.74 0
11 -15 -6 1.23 7.92 0
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11 7 -2 76.97 9.23 0
12 2 -4 0.39 9.13 0
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12 11 3 6.58 9.28 0
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14 -1 -5 26.56 10.53 0
15 9 -2 59.81 8.67 0
16 11 -1 143.34 7.08 0
16 12 0 331.01 7.67 0
16 12 4 53.95 9.94 0
19 12 -1 22.87 9.18 0
19 13 0 0.53 6.45 0
19 13 4 12.45 9.64 0
20 14 2 7.08 9.80 0
21 -3 -6 107.78 10.40 0
21 11 -2 47.41 9.83 0
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-6 -14 2 -3.65 9.23 0
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-5 -9 2 239.77 10.39 0
-4 -25 -1 119.42 9.48 0
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-1 -16 -3 16.31 8.53 0
0 -27 -3 -13.48 6.79 0
1 -10 7 5.93 13.21 0
1 -8 -3 13.91 8.10 0
2 -22 -4 231.04 9.58 0
3 2 5 127.31 14.15 0
4 -8 -4 65.07 9.95 0
4 3 5 45.20 11.21 0
6 5 5 2.17 8.37 0
7 6 5 11.06 9.55 0
8 7 -1 159.72 11.63 0
8 8 4 17.55 8.74 0
8 9 1 808.88 12.18 0
8 9 3 132.97 9.04 0
9 9 0 -3.70 9.32 0
11 -17 -6 68.76 9.44 0
11 11 2 344.46 10.20 0
12 5 7 13.10 10.79 0
12 8 -2 225.64 9.40 0
13 3 -4 83.49 9.78 0
13 6 -3 81.43 9.09 0
13 10 -1 71.92 7.14 0
13 10 5 23.78 11.14 0
13 11 4 65.92 9.79 0
15 9 6 49.99 10.07 0
15 13 2 317.87 9.99 0
16 10 -2 34.14 8.02 0
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16 13 1 66.05 6.51 0
16 13 3 8.85 8.88 0
17 -5 -6 19.43 11.65 0
17 8 -3 155.10 9.94 0
17 13 0 66.66 8.86 0
18 10 6 29.77 9.67 0
18 14 2 91.70 9.16 0
19 2 -5 11.68 9.16 0
19 11 -2 65.13 9.45 0
19 12 5 20.94 9.48 0
19 14 1 61.32 8.23 0
19 14 3 11.89 9.48 0
20 9 -3 29.51 9.35 0
22 3 -5 1.23 8.30 0
22 13 -1 -5.05 9.37 0
22 14 4 22.92 10.14 0
24 12 -2 11.44 9.70 0
25 10 -3 15.73 9.13 0
25 15 2 66.09 6.98 0
26 12 -2 -22.95 10.45 0
26 15 1 3.36 6.95 0
-6 -22 2 121.45 7.02 0
-6 -20 2 45.30 9.07 0
-6 -19 1 272.17 7.13 0
-6 -17 1 232.59 7.17 0
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-5 -26 1 24.72 8.17 0
-5 -26 3 38.62 7.20 0
-5 -23 0 2.13 8.17 0
-5 -21 4 78.83 9.39 0
-5 -19 4 8.58 8.99 0
-5 -17 4 129.62 9.74 0
-5 -15 4 44.44 9.12 0
-5 -10 1 518.62 9.68 0
-4 -29 1 14.88 9.65 0
-4 -28 0 8.13 6.39 0
-4 -23 -1 34.32 7.54 0
-4 -21 -1 57.89 9.33 0
-4 -21 5 56.71 8.93 0
-4 -19 5 -6.56 9.25 0
-4 -13 -1 381.27 7.98 0
-4 -7 1 61.33 13.15 0
-4 -7 3 69.57 9.49 0
-3 -10 5 -7.08 8.70 0
-2 -14 6 15.52 9.80 0
-2 -7 5 37.20 10.92 0
-2 -2 2 1.95 16.47 0
-1 -29 -2 40.66 6.99 0
-1 -9 6 53.73 10.02 0
0 -25 -3 17.69 8.23 0
0 -15 7 -8.50 8.61 0
1 -28 -3 21.40 7.88 0
2 -20 -4 44.97 8.61 0
2 -18 -4 8.48 9.22 0
2 4 2 143.66 17.46 0
3 -25 -4 1.03 8.85 0
3 -11 -4 52.38 7.94 0
3 5 2 727.02 16.23 0
4 6 2 670.26 13.19 0
5 7 2 145.22 11.92 0
6 -19 -5 6.54 8.73 0
6 -17 -5 61.59 9.14 0
6 -15 -5 57.93 7.52 0
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9 8 -1 774.06 12.28 0
9 9 4 -7.11 8.67 0
9 10 1 9.78 8.84 0
10 10 0 557.98 10.58 0
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12 12 2 2.15 8.66 0
14 7 -3 11.30 7.92 0
14 11 -1 70.85 9.07 0
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15 0 -5 4.95 8.12 0
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23 10 -3 49.00 9.37 0
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-4 -26 0 8.11 8.52 0
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-2 -16 6 8.12 8.66 0
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-1 -27 -2 53.79 9.72 0
0 -23 -3 11.08 8.47 0
0 -21 -3 0.36 8.03 0
0 -13 -3 1.56 8.98 0
1 -26 -3 29.84 8.90 0
4 -26 -4 -5.23 8.73 0
7 -12 -5 6.48 8.93 0
7 9 2 394.78 10.97 0
9 8 5 -0.94 9.45 0
9 10 3 59.73 6.59 0
10 9 -1 9.61 8.77 0
10 10 4 137.00 8.89 0
10 11 1 95.07 8.80 0
12 -14 -6 -2.18 8.50 0
12 8 6 85.50 9.44 0
13 6 7 0.89 10.72 0
13 9 -2 81.06 8.98 0
14 4 -4 6.62 7.60 0
14 11 5 57.16 9.47 0
14 13 1 213.76 10.01 0
14 13 3 19.80 9.13 0
15 13 0 73.67 9.28 0
16 1 -5 8.67 8.75 0
16 10 6 27.11 9.82 0
16 14 2 465.55 10.73 0
17 14 3 35.46 7.04 0
18 -4 -6 7.35 9.38 0
18 9 -3 41.75 8.94 0
18 14 0 -3.83 9.09 0
18 14 4 151.94 9.16 0
19 15 2 -2.31 9.84 0
20 3 -5 0.67 8.15 0
20 12 -2 14.70 8.21 0
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20 15 3 -6.62 9.08 0
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21 15 0 -0.74 8.60 0
23 4 -5 40.20 9.95 0
23 14 -1 7.53 6.90 0
23 15 0 2.41 6.40 0
24 8 -4 51.03 9.83 0
24 16 2 24.35 10.79 0
25 13 -2 -9.46 9.22 0
25 16 1 4.74 9.75 0
26 11 -3 -5.82 9.91 0
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-5 -11 2 124.40 6.85 0
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-4 -10 0 1037.52 14.65 0
-3 -27 0 -5.40 9.04 0
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-3 -22 5 5.76 9.23 0
-3 -12 5 5.08 8.95 0
-3 -10 -1 1019.75 12.02 0
-2 -30 0 347.65 10.19 0
-2 -27 -1 -1.27 9.15 0
-2 -20 -2 493.36 10.46 0
-2 -18 -2 19.56 8.72 0
-2 -14 -2 2.89 8.46 0
-1 -30 -1 22.59 7.86 0
-1 -25 -2 36.59 9.24 0
0 -28 -2 50.63 8.96 0
0 -19 -3 2.66 9.25 0
0 -17 -3 3.57 8.45 0
0 -15 -3 6.16 8.48 0
1 -12 7 7.67 11.11 0
3 -21 -4 41.55 8.68 0
3 -13 -4 88.76 8.44 0
8 3 -3 509.90 12.56 0
8 10 2 63.71 9.41 0
9 4 -3 -4.20 9.79 0
10 9 5 25.53 9.59 0
10 11 3 18.10 8.44 0
11 10 -1 85.12 8.70 0
11 11 0 4.19 5.76 0
11 11 4 6.89 9.04 0
12 -16 -6 14.82 8.94 0
13 9 6 66.35 9.44 0
13 13 2 586.39 9.03 0
14 10 -2 81.17 8.95 0
15 5 -4 28.56 8.85 0
15 8 -3 48.05 8.55 0
15 12 -1 185.28 7.45 0
15 12 5 10.73 8.51 0
15 13 4 29.32 9.90 0
17 2 -5 11.34 8.41 0
17 11 6 85.42 10.01 0
17 15 2 26.21 7.55 0
18 13 5 16.60 9.23 0
18 15 1 5.26 7.82 0
18 15 3 142.33 9.96 0
19 7 -4 141.73 9.91 0
19 10 -3 5.10 8.52 0
21 14 -1 9.07 6.77 0
21 15 4 67.41 10.45 0
21 16 1 37.20 8.05 0
22 8 -4 34.95 9.85 0
22 16 2 31.01 7.95 0
23 13 -2 6.46 9.19 0
23 16 1 63.89 7.27 0
23 16 3 10.63 6.77 0
24 11 -3 -1.38 9.39 0
26 15 -1 8.74 9.67 0
26 16 0 -4.43 10.31 0
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24 16 0 172.19 7.70 0
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26 14 -2 7.83 9.71 0
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-2 -25 -1 -3.17 6.55 0
-1 -28 -1 14.84 6.52 0
1 -22 -3 176.08 7.51 0
9 7 -2 391.05 8.79 0
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;
_shelx_hkl_checksum 88795
_shelx_res_file
;
TITL I in I4(1)cd
I.res
created by SHELXL-2018/3 at 10:35:37 on 12-Mar-2020
CELL 0.71073 24.0686 24.0686 6.4468 90.000 90.000 90.000
ZERR 8.000 0.0025 0.0025 0.0008 0.000 0.000 0.000
LATT -2
SYMM 1/2-X, 1/2-Y, 1/2+Z
SYMM -Y, 1/2+X, 1/4+Z
SYMM 1/2+Y, -X, 3/4+Z
SYMM X, -Y, 1/2+Z
SYMM 1/2-X, 1/2+Y, Z
SYMM -Y, 1/2-X, 3/4+Z
SYMM 1/2+Y, X, 1/4+Z
SFAC C H O
UNIT 144 144 96
L.S. 10
BOND $h
conf
omit -3 53
size 0.4 0.025 0.025
temp -150.15
acta
EQIV $2 -y+1, -x+1/2, z-1/4
HTAB O2 O5_$2
EQIV $3 -y+1/2, -x+1, z+1/4
HTAB O4 O1_$3
EQIV $4 y, -x+1/2, z+1/4
HTAB O6 O6_$4
HTAB O6 O3
LIST 4
FMAP 2
PLAN 20
WGHT 0.037700 2.991200
FVAR 0.23677
mole 1
O1 3 0.518329 0.314548 0.233939 11.00000 0.01492 0.01480 =
0.04128 -0.00359 0.00217 0.00360
O2 3 0.429950 0.286011 0.218562 11.00000 0.01790 0.01099 =
0.04281 -0.00736 0.00221 -0.00204
H1O2 2 0.448653 0.255744 0.184820 11.00000 0.05365
O3 3 0.351369 0.357986 0.316536 11.00000 0.01361 0.01313 =
0.02705 -0.00213 0.00026 -0.00320
dfix 0.88 o4 h1o4
O4 3 0.283378 0.437599 0.426497 11.00000 0.01008 0.01681 =
0.04749 -0.00431 0.00383 0.00043
H1O4 2 0.249514 0.450153 0.442996 11.00000 0.07070
O5 3 0.313785 0.524962 0.409341 11.00000 0.01258 0.01696 =
0.03712 -0.00097 0.00379 0.00364
C1 1 0.392689 0.396593 0.326378 11.00000 0.01134 0.01591 =
0.01460 0.00038 -0.00116 -0.00218
C2 1 0.379957 0.452885 0.367322 11.00000 0.01256 0.01327 =
0.01624 -0.00197 -0.00091 0.00193
C3 1 0.422436 0.492503 0.366148 11.00000 0.01313 0.01187 =
0.01314 -0.00040 -0.00297 -0.00066
AFIX 43
H3 2 0.413302 0.530267 0.392110 11.00000 -1.20000
AFIX 0
C4 1 0.477727 0.478542 0.328218 11.00000 0.01174 0.01368 =
0.01175 -0.00014 -0.00300 0.00072
C5 1 0.489532 0.422645 0.287760 11.00000 0.00933 0.01626 =
0.01552 -0.00014 -0.00019 0.00340
AFIX 43
H5 2 0.526771 0.412055 0.259073 11.00000 -1.20000
AFIX 0
C6 1 0.448160 0.382018 0.288357 11.00000 0.01861 0.01058 =
0.01353 -0.00024 0.00035 -0.00018
C7 1 0.467848 0.323824 0.243451 11.00000 0.01566 0.01245 =
0.01860 0.00060 0.00313 -0.00117
C8 1 0.339487 0.329757 0.511301 11.00000 0.02188 0.02449 =
0.03480 0.01041 0.00394 -0.00261
AFIX 137
H8A 2 0.308463 0.303926 0.491492 11.00000 -1.50000
H8B 2 0.329565 0.357244 0.617154 11.00000 -1.50000
H8C 2 0.372435 0.309100 0.556346 11.00000 -1.50000
AFIX 0
C9 1 0.322194 0.474626 0.402687 11.00000 0.01376 0.01664 =
0.01595 0.00159 -0.00118 0.00237
mole 2
dfix 0.88 h1o6 o6
dfix 0.88 h2o6 o6
O6 3 0.304314 0.287672 -0.012704 11.00000 0.04503 0.03656 =
0.03872 -0.00289 -0.00628 -0.00507
H1O6 2 0.301858 0.257047 0.070086 11.00000 0.04223
H2O6 2 0.321017 0.309042 0.084405 11.00000 0.09244
HKLF 4
REM H09_01 in I4(1)cd
REM wR2 = 0.0929, GooF = S = 1.083, Restrained GooF = 1.083 for all data
REM R1 = 0.0394 for 1502 Fo > 4sig(Fo) and 0.0617 for all 1914 data
REM 153 parameters refined using 4 restraints
END
WGHT 0.0377 2.9911
REM Highest difference peak 0.219, deepest hole -0.196, 1-sigma level 0.045
Q1 1 0.3511 0.4600 0.3450 11.00000 0.05 0.22
Q2 1 0.3823 0.4349 0.3694 11.00000 0.05 0.21
Q3 1 0.4536 0.3576 0.2378 11.00000 0.05 0.21
Q4 1 0.4210 0.3893 0.2702 11.00000 0.05 0.21
Q5 1 0.5000 0.5000 0.3321 10.50000 0.05 0.20
Q6 1 0.4839 0.4511 0.2983 11.00000 0.05 0.19
Q7 1 0.4566 0.3508 0.3140 11.00000 0.05 0.19
Q8 1 0.4514 0.4866 0.3959 11.00000 0.05 0.18
Q9 1 0.3078 0.4236 0.3107 11.00000 0.05 0.18
Q10 1 0.3725 0.4265 0.2778 11.00000 0.05 0.18
Q11 1 0.2824 0.5345 0.4480 11.00000 0.05 0.17
Q12 1 0.4495 0.4888 0.3176 11.00000 0.05 0.16
Q13 1 0.5258 0.2892 0.2068 11.00000 0.05 0.16
Q14 1 0.3442 0.5383 0.4089 11.00000 0.05 0.16
Q15 1 0.4580 0.4084 0.2493 11.00000 0.05 0.16
Q16 1 0.5378 0.3493 0.2428 11.00000 0.05 0.16
Q17 1 0.4392 0.3803 0.3573 11.00000 0.05 0.15
Q18 1 0.3380 0.3649 0.8739 11.00000 0.05 0.15
Q19 1 0.3878 0.3502 0.2739 11.00000 0.05 0.15
Q20 1 0.4020 0.4691 0.3706 11.00000 0.05 0.14
;
_shelx_res_checksum 32021
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'
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 0.51833(11) 0.31455(13) 0.2339(6) 0.0237(8) Uani d 1 . .
O O2 0.42995(12) 0.28601(12) 0.2186(6) 0.0239(8) Uani d 1 . .
H H1O2 0.449(3) 0.256(3) 0.185(12) 0.05(2) Uiso d 1 . .
O O3 0.35137(11) 0.35799(11) 0.3165(6) 0.0179(5) Uani d 1 . .
O O4 0.28338(12) 0.43760(11) 0.4265(6) 0.0248(8) Uani d 1 . .
H H1O4 0.2495(15) 0.450(3) 0.443(13) 0.07(2) Uiso d 1 . .
O O5 0.31378(12) 0.52496(11) 0.4093(6) 0.0222(7) Uani d 1 . .
C C1 0.39269(17) 0.39659(18) 0.3264(9) 0.0140(6) Uani d 1 . .
C C2 0.37996(17) 0.45289(16) 0.3673(7) 0.0140(9) Uani d 1 . .
C C3 0.42244(16) 0.49250(17) 0.3661(6) 0.0127(9) Uani d 1 . .
H H3 0.413302 0.530267 0.392110 0.015 Uiso calc 1 . .
C C4 0.47773(17) 0.47854(17) 0.3282(9) 0.0124(5) Uani d 1 . .
C C5 0.48953(17) 0.42264(17) 0.2878(7) 0.0137(9) Uani d 1 . .
H H5 0.526771 0.412055 0.259073 0.016 Uiso calc 1 . .
C C6 0.44816(17) 0.38202(16) 0.2884(7) 0.0142(9) Uani d 1 . .
C C7 0.46785(15) 0.32382(17) 0.2435(7) 0.0156(9) Uani d 1 . .
C C8 0.33949(17) 0.32976(16) 0.5113(7) 0.0271(9) Uani d 1 . .
H H8A 0.308463 0.303926 0.491492 0.041 Uiso calc 1 . .
H H8B 0.329565 0.357244 0.617154 0.041 Uiso calc 1 . .
H H8C 0.372435 0.309100 0.556346 0.041 Uiso calc 1 . .
C C9 0.32219(16) 0.47463(15) 0.4027(8) 0.0155(9) Uani d 1 . .
O O6 0.30431(14) 0.28767(14) -0.0127(6) 0.0401(8) Uani d 1 . .
H H1O6 0.302(2) 0.2570(16) 0.070(7) 0.042(15) Uiso d 1 . .
H H2O6 0.321(3) 0.309(3) 0.084(9) 0.09(3) Uiso 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 0.0149(13) 0.0148(15) 0.041(2) 0.0036(10) 0.0022(14) -0.0036(15)
O2 0.0179(13) 0.0110(15) 0.043(2) -0.0020(11) 0.0022(14) -0.0074(15)
O3 0.0136(13) 0.0131(13) 0.0270(12) -0.0032(9) 0.0003(12) -0.0021(12)
O4 0.0101(14) 0.0168(14) 0.047(2) 0.0004(10) 0.0038(15) -0.0043(14)
O5 0.0126(13) 0.0170(13) 0.037(2) 0.0036(10) 0.0038(15) -0.0010(14)
C1 0.0113(19) 0.0159(19) 0.0146(14) -0.0022(11) -0.0012(17) 0.0004(17)
C2 0.0126(19) 0.0133(18) 0.016(2) 0.0019(15) -0.0009(17) -0.0020(17)
C3 0.0131(17) 0.0119(18) 0.013(2) -0.0007(14) -0.0030(18) -0.0004(17)
C4 0.0117(19) 0.0137(19) 0.0118(14) 0.0007(10) -0.0030(16) -0.0001(17)
C5 0.0093(17) 0.0163(19) 0.016(2) 0.0034(14) -0.0002(17) -0.0001(19)
C6 0.019(2) 0.0106(19) 0.014(2) -0.0002(15) 0.0004(18) -0.0002(17)
C7 0.0157(17) 0.0125(19) 0.019(2) -0.0012(15) 0.0031(19) 0.0006(17)
C8 0.022(2) 0.024(2) 0.035(2) -0.0026(16) 0.0039(18) 0.0104(18)
C9 0.0138(19) 0.0166(18) 0.016(2) 0.0024(15) -0.0012(18) 0.0016(17)
O6 0.045(2) 0.0366(18) 0.039(2) -0.0051(15) -0.0063(16) -0.0029(16)
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
C7 O2 H1O2 . . 105(4) ?
C1 O3 C8 . . 114.9(4) ?
C9 O4 H1O4 . . 117(5) ?
O3 C1 C6 . . 121.1(4) ?
O3 C1 C2 . . 120.3(4) ?
C6 C1 C2 . . 118.6(2) ?
C3 C2 C1 . . 119.6(4) ?
C3 C2 C9 . . 116.1(3) ?
C1 C2 C9 . . 124.2(3) ?
C4 C3 C2 . . 122.3(4) ?
C4 C3 H3 . . 118.8 ?
C2 C3 H3 . . 118.8 ?
C3 C4 C5 . . 117.3(2) ?
C3 C4 C4 . 10_554 121.3(5) ?
C5 C4 C4 . 10_554 121.4(5) ?
C6 C5 C4 . . 121.9(4) ?
C6 C5 H5 . . 119.1 ?
C4 C5 H5 . . 119.1 ?
C5 C6 C1 . . 120.3(4) ?
C5 C6 C7 . . 115.2(4) ?
C1 C6 C7 . . 124.5(3) ?
O1 C7 O2 . . 123.9(4) ?
O1 C7 C6 . . 119.1(4) ?
O2 C7 C6 . . 117.0(3) ?
O3 C8 H8A . . 109.5 ?
O3 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
O3 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
O5 C9 O4 . . 123.6(4) ?
O5 C9 C2 . . 120.1(4) ?
O4 C9 C2 . . 116.4(3) ?
H1O6 O6 H2O6 . . 95(6) ?
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 C7 . 1.237(4) ?
O2 C7 . 1.298(5) ?
O2 H1O2 . 0.88(6) ?
O3 C1 . 1.363(4) ?
O3 C8 . 1.456(5) ?
O4 C9 . 1.300(5) ?
O4 H1O4 . 0.88(3) ?
O5 C9 . 1.229(4) ?
C1 C6 . 1.402(6) ?
C1 C2 . 1.414(6) ?
C2 C3 . 1.398(6) ?
C2 C9 . 1.503(6) ?
C3 C4 . 1.394(6) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.400(6) ?
C4 C4 10_554 1.489(6) ?
C5 C6 . 1.396(6) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.507(6) ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
O6 H1O6 . 0.91(3) ?
O6 H2O6 . 0.90(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H1O2 O5 7_654 0.88(6) 1.80(6) 2.663(4) 166(7) yes
O4 H1O4 O1 15_554 0.88(3) 1.74(3) 2.611(4) 174(7) yes
O6 H1O6 O6 12_454 0.91(3) 1.86(3) 2.768(4) 173(5) yes
O6 H2O6 O3 . 0.90(3) 2.04(3) 2.941(5) 174(7) 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
C8 O3 C1 C6 . . . . 90.3(6) ?
C8 O3 C1 C2 . . . . -92.3(6) ?
O3 C1 C2 C3 . . . . -176.6(5) ?
C6 C1 C2 C3 . . . . 0.9(9) ?
O3 C1 C2 C9 . . . . 0.1(8) ?
C6 C1 C2 C9 . . . . 177.6(4) ?
C1 C2 C3 C4 . . . . -0.8(8) ?
C9 C2 C3 C4 . . . . -177.8(4) ?
C2 C3 C4 C5 . . . . 0.9(8) ?
C2 C3 C4 C4 . . . 10_554 -179.9(3) ?
C3 C4 C5 C6 . . . . -1.1(8) ?
C4 C4 C5 C6 10_554 . . . 179.7(3) ?
C4 C5 C6 C1 . . . . 1.2(8) ?
C4 C5 C6 C7 . . . . -179.6(5) ?
O3 C1 C6 C5 . . . . 176.4(4) ?
C2 C1 C6 C5 . . . . -1.1(9) ?
O3 C1 C6 C7 . . . . -2.7(8) ?
C2 C1 C6 C7 . . . . 179.8(4) ?
C5 C6 C7 O1 . . . . 8.4(7) ?
C1 C6 C7 O1 . . . . -172.4(5) ?
C5 C6 C7 O2 . . . . -172.1(4) ?
C1 C6 C7 O2 . . . . 7.1(7) ?
C3 C2 C9 O5 . . . . 6.7(7) ?
C1 C2 C9 O5 . . . . -170.1(5) ?
C3 C2 C9 O4 . . . . -172.8(4) ?
C1 C2 C9 O4 . . . . 10.4(7) ?