#------------------------------------------------------------------------------
#$Date: 2024-12-07 18:12:45 +0100 (Sat, 07 Dec 2024) $
#$Revision: 296788 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023287.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_2023287
loop_
_publ_author_name
'Peixoto de Abreu Lima, Alejandro'
'Pandolfi, Enrique'
'Schapiro, Valeria'
'Suescun, Leopoldo'
_publ_section_title
;
Synthesis, crystal structure and absolute configuration of
(3aS,4R,5S,7aR)-7-(but-3-en-1-yn-1-yl)-2,2-dimethyl-3a,4,5,7a-tetrahydro-2H-1,3-benzodioxole-4,5-diol
;
_journal_coeditor_code EE2008
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1165
_journal_page_last 1169
_journal_paper_doi 10.1107/S2056989024009733
_journal_volume 80
_journal_year 2024
_chemical_absolute_configuration syn
_chemical_formula_iupac 'C13 H16 O4'
_chemical_formula_moiety 'C13 H16 O4'
_chemical_formula_sum 'C13 H16 O4'
_chemical_formula_weight 236.26
_chemical_name_common
(1S,2R,3S,4R)-5-(But-3-en-1-ynyl)-1,2-dihydroxy-3,4-isopropylidenedioxocycle-5-hexene
_chemical_name_systematic
(3aS,4R,5S,7aR)-7-(But-3-en-1-yn-1-yl)-2,2-dimethyl-3a,4,5,7a-tetrahydro-2H-1,3-benzodioxole-4,5-diol
_space_group_crystal_system monoclinic
_space_group_IT_number 5
_space_group_name_Hall 'C 2y'
_space_group_name_H-M_alt 'C 1 2 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 109.652(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.4126(13)
_cell_length_b 5.0996(4)
_cell_length_c 14.9856(11)
_cell_measurement_reflns_used 7392
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 77.75
_cell_measurement_theta_min 5.225
_cell_volume 1253.17(16)
_computing_cell_refinement
;
SAINT V8.38A (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT V8.38A (Bruker, 2018)
;
_computing_molecular_graphics
;
ShelXle (H\"ubschle et al., 2011)
;
_computing_publication_material
;
ShelXle (H\"ubschle et al., 2011)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015)
;
_computing_structure_solution
;
olex2.solve 1.5 (Bourhis et al., 2015, Dolomanov et
al., 2009)
;
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type 'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method '\j and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0489
_diffrn_reflns_av_unetI/netI 0.0590
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 10420
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 81.635
_diffrn_reflns_theta_min 5.249
_diffrn_source 'Cu Incoatec microsource'
_exptl_absorpt_coefficient_mu 0.765
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.6456
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.252
_exptl_crystal_description plate
_exptl_crystal_F_000 504
_exptl_crystal_size_max 0.379
_exptl_crystal_size_mid 0.256
_exptl_crystal_size_min 0.120
_refine_diff_density_max 0.412
_refine_diff_density_min -0.206
_refine_ls_abs_structure_details
;
Flack x determined using 752 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.1(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.128
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 157
_refine_ls_number_reflns 2628
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.130
_refine_ls_R_factor_all 0.0908
_refine_ls_R_factor_gt 0.0804
_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^)+(0.1316P)^2^+0.6357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2344
_refine_ls_wR_factor_ref 0.2483
_reflns_number_gt 2138
_reflns_number_total 2628
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ee2008.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023287.cif.'
_cod_original_sg_symbol_H-M 'C 2'
_cod_database_code 2023287
_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 0.760
_shelx_estimated_absorpt_t_max 0.914
_shelx_hkl_file
;
2 0 0 441.13 36.23
4 0 0 1600.35 131.37
-6 0 0 1724.51 141.63
-8 0 0 1585.76 128.60
-8 0 0 1542.13 128.47
-10 0 0 111.84 8.49
10 0 0 88.06 8.76
-10 0 0 100.91 8.58
12 0 0 30.70 4.14
12 0 0 28.85 4.37
12 0 0 31.85 3.40
14 0 0 6.38 2.10
-14 0 0 1.46 0.60
-14 0 0 0.91 1.11
14 0 0 2.57 2.06
16 0 0 32.21 5.00
16 0 0 48.28 5.68
-16 0 0 42.74 4.64
16 0 0 44.59 4.54
-18 0 0 0.37 1.54
18 0 0 0.57 0.92
-18 0 0 0.14 0.50
18 0 0 -0.26 1.16
-20 0 0 0.58 0.67
20 0 0 0.14 0.38
20 0 0 2.20 1.66
-20 0 0 0.30 0.48
1 -1 0 5463.58 457.44
-1 -1 0 5607.88 456.69
1 -1 0 5335.12 456.40
1 1 0 5390.71 450.30
-3 -1 0 199.53 16.05
-3 -1 0 203.77 16.21
-3 -1 0 204.46 16.03
3 -1 0 170.40 16.05
3 1 0 192.83 16.05
-3 1 0 194.62 16.09
-3 1 0 196.25 16.29
-5 1 0 2516.93 206.90
-7 -1 0 126.30 10.23
7 -1 0 108.80 10.25
7 -1 0 130.33 10.21
-7 -1 0 122.31 10.52
-7 1 0 123.36 10.21
-7 1 0 118.19 10.12
-9 -1 0 1086.23 87.44
-9 -1 0 1050.53 87.80
9 -1 0 1050.96 87.55
9 1 0 1047.05 87.62
-9 1 0 1077.75 87.57
9 1 0 1067.44 87.71
-11 -1 0 60.02 5.69
11 -1 0 71.85 6.26
-11 -1 0 55.73 5.64
-11 -1 0 58.46 6.78
11 -1 0 71.82 6.04
-11 1 0 76.08 7.19
11 1 0 78.25 6.91
11 1 0 71.07 6.47
-11 1 0 60.74 6.34
-13 -1 0 86.24 8.19
-13 -1 0 94.07 7.98
13 -1 0 87.31 8.16
-13 1 0 93.97 8.03
13 1 0 82.04 7.93
-15 -1 0 7.19 1.59
15 -1 0 7.04 2.32
15 -1 0 6.97 1.66
15 -1 0 5.91 1.83
15 1 0 5.26 2.47
-15 1 0 1.99 2.17
17 -1 0 2.41 1.77
-17 -1 0 2.55 0.65
17 -1 0 6.42 2.36
-17 -1 0 2.71 1.72
-17 1 0 1.02 2.58
17 1 0 4.64 1.47
-17 1 0 1.58 1.13
-17 1 0 1.56 0.66
19 -1 0 4.43 1.99
19 -1 0 1.78 1.59
-19 -1 0 1.45 0.53
-19 -1 0 1.79 1.32
19 1 0 0.94 0.69
-19 1 0 0.71 0.75
-19 1 0 1.01 0.49
19 1 0 1.98 1.07
19 1 0 0.51 0.67
0 -2 0 375.56 30.58
0 -2 0 358.49 30.38
0 2 0 382.88 31.63
2 -2 0 739.02 63.23
2 -2 0 807.11 63.52
-2 -2 0 842.59 63.60
-2 -2 0 686.81 63.30
-2 2 0 637.37 53.99
2 2 0 654.52 53.97
2 2 0 674.25 54.23
-4 -2 0 712.05 65.53
-4 -2 0 850.80 65.97
4 -2 0 827.24 65.50
-4 2 0 829.81 67.07
4 2 0 798.70 66.98
-6 -2 0 577.51 47.85
6 -2 0 570.09 47.22
-6 2 0 600.97 48.72
6 2 0 580.28 48.61
-8 -2 0 481.14 41.42
-8 -2 0 545.87 40.71
-8 -2 0 504.79 40.59
8 -2 0 478.41 40.84
8 -2 0 421.59 41.21
8 -2 0 559.30 40.51
8 -2 0 448.06 40.95
-8 2 0 569.82 42.38
8 2 0 529.49 42.39
8 2 0 471.86 42.57
-8 2 0 552.61 42.46
-8 2 0 503.88 42.54
8 2 0 451.89 42.50
10 -2 0 26.49 4.26
10 -2 0 25.85 5.21
10 -2 0 26.38 3.39
-10 -2 0 24.96 6.33
10 -2 0 34.24 4.60
10 2 0 19.24 2.75
-10 2 0 15.01 2.05
10 2 0 24.56 3.03
-10 2 0 20.63 2.40
10 2 0 18.66 3.39
-10 2 0 21.14 2.85
12 -2 0 81.32 8.87
12 -2 0 90.91 8.35
-12 -2 0 85.45 7.56
-12 -2 0 71.47 8.37
12 -2 0 97.70 8.89
12 -2 0 93.09 7.95
-12 2 0 77.32 6.91
-12 2 0 75.84 7.21
12 2 0 77.73 7.28
12 2 0 83.73 7.26
-12 2 0 81.33 7.40
12 2 0 81.96 7.49
-14 -2 0 22.72 2.64
14 -2 0 19.58 4.61
14 -2 0 22.81 3.09
14 -2 0 24.16 4.08
-14 -2 0 27.08 2.31
14 -2 0 25.86 4.03
14 2 0 19.95 3.40
-14 2 0 15.08 2.50
-14 2 0 22.90 2.15
14 2 0 19.14 2.93
16 -2 0 6.82 2.80
16 -2 0 0.50 2.18
-16 -2 0 4.47 0.88
16 -2 0 5.00 1.02
-16 -2 0 4.79 1.22
16 2 0 -2.32 2.80
-16 2 0 2.71 0.76
-16 2 0 1.76 1.09
18 -2 0 2.46 0.59
-18 -2 0 3.41 1.23
18 -2 0 2.32 1.47
-18 -2 0 2.50 0.57
18 -2 0 2.71 1.51
18 2 0 2.82 1.29
-18 2 0 1.60 0.96
-18 2 0 2.56 0.57
-1 -3 0 163.74 16.02
1 -3 0 186.31 14.81
-1 -3 0 171.68 15.70
1 -3 0 181.99 15.95
-1 -3 0 181.78 14.80
1 -3 0 180.65 16.04
1 -3 0 182.91 15.70
1 3 0 208.08 17.14
1 3 0 210.19 16.91
1 3 0 200.34 17.31
-1 3 0 200.42 16.91
-1 3 0 216.96 17.18
1 3 0 195.65 17.12
-1 3 0 193.10 17.34
-3 -3 0 8.26 0.89
3 -3 0 8.19 0.95
3 3 0 13.22 1.90
3 3 0 10.86 1.29
-3 3 0 13.34 2.21
-3 3 0 9.70 1.41
-5 -3 0 28.28 6.05
-5 -3 0 21.49 5.62
-5 3 0 13.73 1.68
5 3 0 20.89 3.62
5 3 0 13.12 1.46
5 3 0 12.94 1.88
5 3 0 15.91 2.50
-5 3 0 15.06 3.03
5 3 0 17.11 3.11
7 -3 0 75.88 6.50
-7 -3 0 75.68 6.20
7 -3 0 75.64 6.27
-7 -3 0 68.46 6.53
-7 3 0 53.02 6.37
-7 3 0 73.38 5.85
7 3 0 75.27 5.67
-7 3 0 63.33 6.36
7 3 0 65.29 6.30
9 -3 0 38.73 3.40
-9 -3 0 36.25 3.83
9 -3 0 41.16 3.70
9 3 0 40.24 4.19
9 3 0 39.33 3.38
-9 3 0 37.61 4.28
-9 3 0 38.67 3.54
-9 3 0 34.50 4.17
11 -3 0 36.33 5.27
11 -3 0 49.66 5.86
11 -3 0 44.67 5.48
11 3 0 18.61 3.63
11 3 0 17.05 3.16
-11 3 0 17.30 2.86
13 -3 0 10.32 2.87
13 -3 0 7.35 1.18
-13 -3 0 6.42 1.26
13 -3 0 8.47 2.14
13 3 0 4.34 2.06
-13 3 0 5.22 1.58
-13 3 0 5.65 0.92
-15 -3 0 7.75 1.36
-15 -3 0 12.75 1.19
15 -3 0 10.52 1.25
15 -3 0 7.04 2.16
-15 3 0 4.16 1.37
15 3 0 1.49 2.52
-17 -3 0 2.75 1.11
17 -3 0 2.29 1.10
17 -3 0 2.28 1.48
-17 3 0 2.46 0.55
-17 3 0 2.34 1.26
17 3 0 0.72 3.09
0 -4 0 69.82 7.25
0 4 0 127.22 11.15
-2 -4 0 13.56 3.76
2 -4 0 16.60 3.52
-2 -4 0 19.45 1.66
2 -4 0 12.59 3.71
-2 -4 0 18.14 2.27
2 -4 0 19.37 1.69
-2 4 0 20.86 3.53
2 4 0 18.83 2.13
-2 4 0 22.83 2.16
2 4 0 22.82 3.06
2 4 0 21.33 4.37
-4 -4 0 20.54 2.37
-4 -4 0 20.41 1.75
4 -4 0 15.31 3.70
4 -4 0 14.70 3.44
4 -4 0 19.44 1.78
-4 4 0 22.00 2.14
4 4 0 17.69 2.83
-4 4 0 18.91 3.70
4 4 0 21.95 1.97
-6 -4 0 50.34 4.26
6 -4 0 48.61 5.89
6 -4 0 51.58 4.29
6 -4 0 48.30 6.17
-6 -4 0 50.29 4.63
6 4 0 53.82 5.05
-6 4 0 54.23 4.63
6 4 0 47.25 5.31
6 4 0 52.01 4.45
-8 -4 0 104.40 9.51
8 -4 0 118.32 9.31
8 4 0 116.08 9.51
-8 4 0 111.78 9.68
-10 -4 0 10.26 1.69
10 -4 0 9.73 2.91
10 -4 0 15.90 3.00
-10 -4 0 10.13 1.72
-10 4 0 11.36 1.36
-10 4 0 10.06 2.42
10 4 0 8.11 1.86
12 -4 0 1.95 2.16
12 -4 0 3.82 1.87
-12 -4 0 0.31 0.93
-12 -4 0 1.06 0.81
-12 4 0 1.48 0.65
12 4 0 2.34 1.63
-12 4 0 4.04 1.77
-14 -4 0 16.86 1.48
-14 -4 0 13.18 1.75
-14 4 0 10.58 2.23
-14 4 0 15.01 1.42
-16 -4 0 2.00 0.40
16 -4 0 0.72 0.70
-16 4 0 1.85 0.40
1 -5 0 53.33 4.39
-1 -5 0 48.13 4.72
1 -5 0 50.80 4.78
-1 -5 0 54.76 4.41
-1 5 0 61.60 5.01
1 5 0 56.77 4.95
1 5 0 56.31 5.49
-1 5 0 56.69 5.57
-3 -5 0 10.39 1.59
3 -5 0 7.96 2.58
3 -5 0 6.39 3.10
-3 5 0 3.40 3.50
3 5 0 7.26 1.56
-3 5 0 10.50 2.32
-5 -5 0 1.47 2.65
5 -5 0 2.69 2.08
-5 -5 0 5.77 1.44
-5 5 0 10.02 1.62
5 5 0 7.03 1.79
-5 5 0 7.49 1.91
5 5 0 9.01 1.06
7 -5 0 10.45 0.92
-7 -5 0 7.22 1.57
-7 -5 0 7.32 1.40
-7 5 0 5.87 1.88
-9 -5 0 1.43 0.65
9 -5 0 -0.30 1.35
9 -5 0 -0.75 2.46
-9 -5 0 1.61 0.70
-9 5 0 2.14 0.58
-9 5 0 3.47 1.57
9 5 0 0.41 1.22
-11 -5 0 0.34 0.55
-11 -5 0 0.24 0.74
11 -5 0 0.92 1.55
11 -5 0 1.62 1.29
-11 5 0 0.69 1.63
-11 5 0 1.28 0.44
-13 -5 0 0.60 0.74
-13 -5 0 0.30 0.32
-13 5 0 1.11 0.34
0 6 0 20.53 2.35
-2 -6 0 0.78 0.71
-2 -6 0 0.81 3.07
2 -6 0 -0.18 1.39
-2 6 0 1.26 1.13
2 6 0 0.26 0.97
4 -6 0 0.57 1.17
4 6 0 -0.35 0.94
-4 6 0 1.31 0.91
6 -6 0 -0.89 1.70
-6 -6 0 -0.17 0.47
-6 6 0 1.00 1.09
-20 0 1 0.29 0.63
-20 0 1 -1.19 1.75
-20 0 1 1.01 0.47
20 0 -1 1.06 1.43
18 0 -1 -0.02 0.93
18 0 -1 1.71 1.38
-18 0 1 0.08 1.49
-18 0 1 0.67 0.54
16 0 -1 42.09 4.84
-16 0 1 45.31 3.96
-14 0 1 103.12 8.65
14 0 -1 95.44 8.67
14 0 -1 92.58 8.43
-14 0 1 89.91 8.74
12 0 -1 127.17 10.32
12 0 -1 112.67 9.92
12 0 -1 108.61 10.30
-12 0 1 112.09 9.92
-12 0 1 121.00 10.16
12 0 -1 130.35 10.81
-10 0 1 287.61 25.20
-10 0 1 320.25 25.35
10 0 -1 307.57 25.43
-8 0 1 185.70 14.01
-8 0 1 162.86 14.16
8 0 -1 156.06 13.93
-6 0 1 4323.48 368.04
6 0 -1 4413.33 367.57
4 0 -1 755.48 62.07
-2 0 1 5290.02 436.64
2 0 1 2205.47 182.71
-2 0 -1 2192.80 182.71
-4 0 -1 5.38 0.66
4 0 1 5.89 0.51
-4 0 -1 5.58 0.63
-6 0 -1 554.61 46.28
-6 0 -1 570.26 46.33
-8 0 -1 336.94 28.10
-8 0 -1 339.23 27.96
10 0 1 293.51 24.35
10 0 1 286.55 24.26
12 0 1 150.14 14.25
12 0 1 176.13 14.19
-14 0 -1 309.25 24.87
14 0 1 299.37 24.78
14 0 1 298.09 24.74
-14 0 -1 248.01 24.29
14 0 1 314.46 24.75
-16 0 -1 12.28 2.88
16 0 1 18.01 2.92
16 0 1 14.40 2.93
18 0 1 1.20 0.89
-18 0 -1 1.11 1.86
18 0 1 1.08 0.42
-18 0 -1 1.39 0.56
18 0 1 0.85 1.15
-20 0 -1 3.24 0.83
-20 0 -1 5.46 0.99
21 -1 -1 0.29 0.43
-21 -1 1 -0.49 1.01
-21 1 1 -0.05 0.86
21 1 -1 0.91 1.36
-19 -1 1 3.93 0.76
-19 -1 1 2.46 1.27
19 -1 -1 5.05 0.73
19 -1 -1 3.23 2.04
-19 1 1 2.50 0.80
-19 1 1 4.26 0.74
19 1 -1 1.97 1.23
17 -1 -1 10.47 1.98
17 -1 -1 11.35 2.39
-17 1 1 12.32 2.00
-17 1 1 11.93 1.90
15 -1 -1 86.44 8.49
-15 -1 1 80.49 6.98
-15 -1 1 74.52 7.22
15 -1 -1 88.31 7.54
15 -1 -1 82.12 7.82
-15 1 1 74.62 7.77
-15 1 1 89.07 6.90
15 1 -1 77.14 8.70
15 1 -1 73.97 7.15
-13 -1 1 51.67 5.35
13 -1 -1 62.40 6.94
-13 -1 1 54.66 5.00
13 1 -1 68.85 8.47
-13 1 1 76.28 6.83
13 1 -1 64.08 6.40
-13 1 1 60.23 6.20
11 -1 -1 248.74 20.95
-11 -1 1 259.16 20.43
11 -1 -1 253.50 20.22
-11 -1 1 250.58 20.30
11 -1 -1 220.99 21.19
11 -1 -1 243.38 20.53
-11 -1 1 230.35 20.99
11 1 -1 238.12 21.75
11 1 -1 270.01 21.53
-11 1 1 270.13 21.61
-11 1 1 273.50 21.77
11 1 -1 243.70 21.80
11 1 -1 266.41 22.03
-9 -1 1 1341.38 102.37
9 -1 -1 1108.20 102.06
9 -1 -1 1274.09 102.03
-9 -1 1 1238.27 102.01
-9 1 1 1311.59 112.19
9 1 -1 1458.53 112.07
-9 1 1 1316.37 111.97
-7 -1 1 372.01 28.47
7 -1 -1 309.55 28.50
7 -1 -1 351.63 28.45
-7 1 1 342.36 28.66
7 1 -1 329.89 28.44
-7 1 1 364.81 28.55
-5 -1 1 528.49 44.94
-5 -1 1 550.18 44.85
5 -1 -1 528.12 44.85
-5 -1 1 613.94 45.05
5 -1 -1 505.13 44.90
-5 1 1 561.57 45.23
5 1 -1 530.69 44.89
-3 -1 1 71.98 6.85
3 -1 -1 85.28 6.87
-3 -1 1 80.46 6.71
-3 -1 1 77.97 6.73
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4 0 9 -1.59 1.58
4 0 9 0.47 1.00
4 0 9 1.93 0.64
4 0 9 1.74 1.30
6 0 9 26.42 4.66
6 0 9 27.95 3.86
6 0 9 19.80 3.93
6 0 9 28.31 2.90
6 0 9 31.93 3.08
6 0 9 30.88 2.96
6 0 9 26.87 2.73
6 0 9 25.61 3.91
6 0 9 29.83 3.03
6 0 9 28.98 3.28
6 0 9 28.82 2.94
8 0 9 22.39 2.23
8 0 9 18.87 3.00
8 0 9 16.41 3.18
8 0 9 18.65 3.56
8 0 9 22.93 2.42
8 0 9 21.22 2.52
8 0 9 25.99 4.11
8 0 9 21.76 2.53
10 0 9 -0.74 1.41
10 0 9 -0.91 1.17
10 0 9 0.67 0.70
10 0 9 -0.87 1.03
10 0 9 0.58 0.61
12 0 9 12.83 1.59
14 0 9 11.61 1.36
21 -1 -9 5.50 1.18
-21 -1 9 5.52 1.86
-21 -1 9 5.74 1.29
-21 1 9 5.27 1.63
-19 -1 9 5.56 0.95
19 -1 -9 2.97 1.04
-19 -1 9 2.81 1.45
-19 -1 9 3.70 1.38
-19 1 9 0.64 1.31
-19 1 9 3.83 0.96
19 1 -9 1.34 1.03
19 1 -9 2.72 1.01
17 -1 -9 4.35 1.16
-17 -1 9 2.59 1.57
-17 -1 9 5.63 2.05
17 -1 -9 3.94 2.29
-17 1 9 5.94 1.47
-17 1 9 4.17 1.45
-17 1 9 4.42 1.72
17 1 -9 6.31 1.55
17 1 -9 2.87 1.38
-15 -1 9 72.69 6.41
-15 -1 9 75.37 6.76
15 -1 -9 71.12 6.54
15 -1 -9 65.77 6.76
15 -1 -9 66.76 6.17
-15 -1 9 68.36 6.13
-15 -1 9 83.73 7.21
-15 1 9 81.49 7.28
15 1 -9 65.04 6.29
-15 1 9 64.13 6.34
-15 1 9 79.06 7.20
-15 1 9 78.09 6.75
15 1 -9 80.23 6.76
13 -1 -9 77.44 6.81
-13 -1 9 80.59 6.71
-13 -1 9 73.09 7.11
13 -1 -9 72.77 7.38
-13 -1 9 67.76 7.40
-13 1 9 86.85 6.59
-13 1 9 71.43 7.32
13 1 -9 70.67 6.87
-13 1 9 82.39 6.96
-13 1 9 67.26 7.37
-11 -1 9 74.09 6.84
-11 -1 9 79.31 6.56
-11 -1 9 75.82 6.66
-11 -1 9 69.32 7.08
11 -1 -9 82.75 6.58
-11 1 9 69.50 6.72
-11 1 9 70.21 6.07
11 1 -9 58.55 6.25
-11 1 9 66.48 6.80
-11 1 9 72.80 6.36
11 1 -9 72.71 5.84
9 -1 -9 135.71 11.91
-9 -1 9 125.75 11.72
-9 -1 9 138.57 11.60
-9 -1 9 138.23 11.46
-9 -1 9 144.17 11.88
9 -1 -9 141.45 11.36
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-9 1 9 127.34 10.75
9 1 -9 130.46 10.55
-9 1 9 123.58 11.20
-9 1 9 139.32 11.02
9 1 -9 123.27 11.19
-9 1 9 125.94 10.97
-9 1 9 114.89 11.31
9 1 -9 126.31 11.16
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7 -1 -9 112.79 9.56
-7 -1 9 102.95 9.93
-7 -1 9 109.27 9.47
-7 -1 9 106.61 9.44
7 -1 -9 112.05 9.10
-7 -1 9 110.03 9.36
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7 1 -9 112.74 9.27
-7 1 9 109.13 9.06
-7 1 9 104.68 8.91
7 1 -9 109.54 9.27
-7 1 9 96.59 9.28
-7 1 9 112.46 9.34
-7 1 9 97.94 9.35
-7 1 9 108.82 8.96
7 1 -9 103.60 8.76
-7 1 9 105.83 9.17
-5 -1 9 142.91 13.37
-5 -1 9 182.03 13.70
5 -1 -9 161.88 13.72
-5 -1 9 151.57 14.04
-5 -1 9 158.30 13.41
-5 -1 9 150.19 13.64
-5 -1 9 171.42 13.63
-5 1 9 147.26 12.49
-5 1 9 143.75 12.24
5 1 -9 137.08 13.11
5 1 -9 156.83 12.53
-5 1 9 131.19 12.58
-5 1 9 146.74 12.22
-5 1 9 152.24 12.29
3 -1 -9 193.45 16.48
-3 -1 9 187.51 16.04
3 -1 -9 211.13 16.44
-3 -1 9 175.80 16.72
-3 -1 9 195.57 16.37
-3 1 9 195.26 16.89
-3 1 9 212.79 16.98
-3 1 9 209.32 16.95
3 1 -9 222.69 17.26
3 1 -9 211.12 17.03
-3 1 9 193.21 17.24
-3 1 9 184.77 16.92
-3 1 9 191.85 16.88
1 -1 -9 0.28 1.12
-1 -1 9 0.41 1.96
-1 -1 9 0.14 0.46
1 -1 -9 1.38 2.14
-1 -1 9 0.59 0.89
-1 -1 9 0.25 0.73
-1 -1 9 1.11 1.29
-1 -1 9 3.12 3.54
-1 -1 9 0.69 0.83
-1 -1 9 -0.01 1.50
-1 1 9 2.44 0.87
1 1 -9 1.19 1.26
-1 1 9 2.22 1.12
-1 1 9 1.65 1.43
-1 1 9 0.83 0.73
-1 1 9 1.49 1.17
-1 1 9 1.25 2.07
1 -1 9 51.24 5.14
1 -1 9 49.46 4.48
1 -1 9 54.12 5.67
1 -1 9 48.30 4.33
1 -1 9 49.21 4.81
-1 -1 -9 48.00 5.23
1 -1 9 42.60 4.72
1 -1 9 48.26 4.34
1 -1 9 47.78 4.36
1 -1 9 50.43 4.34
1 -1 9 48.50 4.66
1 -1 9 43.71 6.18
1 -1 9 50.59 5.79
1 1 9 39.67 5.11
1 1 9 43.07 4.09
-1 1 -9 48.49 4.71
1 1 9 44.91 4.22
1 1 9 46.83 4.21
1 1 9 42.76 4.54
1 1 9 42.37 4.10
1 1 9 40.68 4.31
1 1 9 49.74 4.19
1 1 9 45.91 4.17
3 -1 9 24.97 2.69
3 -1 9 26.16 3.46
3 -1 9 20.05 4.03
3 -1 9 25.72 4.23
-3 -1 -9 24.93 4.95
3 -1 9 26.76 3.42
3 -1 9 26.53 3.09
3 -1 9 25.50 2.66
3 1 9 21.48 3.47
3 1 9 31.18 6.08
3 1 9 22.31 2.63
3 1 9 19.74 3.21
3 1 9 24.97 3.53
3 1 9 24.56 2.68
-3 1 -9 29.13 3.31
3 1 9 16.72 2.92
3 1 9 22.32 3.45
3 1 9 23.41 3.05
3 1 9 28.52 2.69
5 -1 9 13.91 2.12
5 -1 9 18.77 2.19
5 -1 9 21.07 3.51
5 -1 9 18.39 2.48
5 -1 9 17.99 2.83
5 -1 9 21.94 4.05
5 -1 9 24.05 3.80
5 -1 9 17.21 2.08
5 -1 9 18.63 3.01
5 1 9 14.47 2.68
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5 1 9 13.41 1.98
5 1 9 15.33 2.27
5 1 9 14.19 2.00
5 1 9 16.39 2.16
5 1 9 17.53 2.93
5 1 9 13.47 1.86
5 1 9 15.48 2.41
7 -1 9 31.49 4.40
7 -1 9 27.51 3.49
7 -1 9 28.43 3.17
7 -1 9 26.03 4.08
7 -1 9 30.03 2.87
7 -1 9 30.01 2.83
7 -1 9 31.40 3.05
7 -1 9 26.76 3.66
7 1 9 31.19 5.41
7 1 9 33.88 3.08
7 1 9 27.44 2.96
7 1 9 29.76 3.35
7 1 9 28.95 3.33
7 1 9 25.45 3.99
7 1 9 26.85 3.54
9 -1 9 3.74 0.96
9 -1 9 0.28 1.65
9 -1 9 2.29 0.87
9 -1 9 0.94 1.86
9 -1 9 -0.21 1.47
9 1 9 -0.88 1.43
9 1 9 1.58 2.52
9 1 9 0.10 1.80
9 1 9 3.55 0.96
9 1 9 2.18 1.07
11 -1 9 -0.74 1.68
11 -1 9 0.08 0.75
11 -1 9 2.03 1.41
11 -1 9 1.00 1.16
11 -1 9 -2.06 1.64
11 1 9 0.55 0.69
11 1 9 2.06 1.09
11 1 9 -0.13 1.04
11 1 9 1.13 2.35
13 -1 9 2.80 0.68
13 -1 9 1.89 1.59
13 -1 9 1.49 0.89
13 -1 9 -0.21 1.00
13 1 9 2.70 2.91
13 1 9 1.42 0.59
13 1 9 0.65 0.90
-20 -2 9 0.84 1.68
-20 -2 9 -0.47 1.45
20 -2 -9 0.99 0.98
20 -2 -9 -1.00 2.27
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18 -2 -9 5.26 1.22
-18 -2 9 7.22 1.39
18 -2 -9 7.37 0.82
-18 -2 9 4.34 1.54
-18 -2 9 8.65 1.11
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18 2 -9 5.26 1.10
-18 2 9 6.79 1.73
18 2 -9 8.03 0.82
16 -2 -9 2.75 1.31
-16 -2 9 0.71 2.11
-16 -2 9 0.38 0.57
-16 -2 9 2.94 1.56
-16 -2 9 3.13 1.11
16 -2 -9 0.38 0.48
16 -2 -9 1.61 1.95
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16 2 -9 2.43 1.37
16 2 -9 1.00 0.44
16 2 -9 1.46 1.05
-16 2 9 1.19 1.01
-16 2 9 0.93 0.72
-14 -2 9 3.91 1.75
-14 -2 9 4.96 2.37
-14 -2 9 5.65 1.17
14 -2 -9 5.01 1.29
-14 2 9 2.76 1.61
14 2 -9 4.31 1.21
14 2 -9 4.74 1.74
-14 2 9 5.38 1.20
12 -2 -9 10.31 1.83
-12 -2 9 5.75 1.16
-12 -2 9 9.49 1.87
-12 -2 9 8.91 3.17
12 -2 -9 6.52 1.12
-12 2 9 8.32 1.49
-12 2 9 6.81 1.22
12 2 -9 9.76 2.15
12 2 -9 5.48 0.91
12 2 -9 10.72 1.99
-10 -2 9 119.87 10.47
-10 -2 9 115.10 11.20
10 -2 -9 141.11 10.55
-10 -2 9 122.13 10.91
10 -2 -9 105.78 10.85
-10 -2 9 137.34 10.63
-10 -2 9 126.96 10.67
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10 2 -9 133.01 10.31
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8 -2 -9 106.18 10.02
-8 -2 9 121.40 9.86
-8 -2 9 120.19 10.05
-8 -2 9 122.06 10.21
-8 -2 9 91.96 9.42
8 2 -9 119.30 10.67
-8 2 9 124.41 10.37
-8 2 9 125.57 10.17
-8 2 9 113.73 10.02
-8 2 9 110.78 9.91
8 2 -9 100.24 9.61
-6 -2 9 7.82 1.60
6 -2 -9 7.54 1.44
-6 -2 9 6.70 2.26
-6 -2 9 4.70 1.76
-6 -2 9 5.96 2.02
-6 -2 9 9.75 1.24
-6 2 9 5.86 1.84
-6 2 9 7.75 1.52
-6 2 9 6.50 1.37
6 2 -9 6.92 1.03
-6 2 9 5.16 1.88
4 -2 -9 47.20 5.41
-4 -2 9 52.12 4.51
-4 -2 9 47.52 4.70
-4 -2 9 51.83 5.59
-4 -2 9 51.79 5.15
-4 -2 9 51.62 5.02
4 2 -9 47.68 4.07
-4 2 9 51.75 4.31
-4 2 9 37.93 5.24
4 2 -9 41.90 5.27
-4 2 9 46.36 4.41
2 -2 -9 595.73 50.70
-2 -2 9 597.05 50.24
-2 -2 9 622.68 50.17
-2 -2 9 589.93 50.51
-2 -2 9 626.06 50.05
-2 -2 9 615.14 50.37
-2 2 9 631.91 52.60
-2 2 9 649.12 52.86
-2 2 9 633.45 52.69
0 -2 9 16.00 3.42
0 -2 9 11.37 2.64
0 -2 9 9.71 3.33
0 -2 9 13.56 2.41
0 -2 9 9.21 1.82
0 -2 9 10.45 1.38
0 2 9 10.83 2.41
0 2 9 11.55 1.73
2 -2 9 45.05 4.39
2 -2 9 51.78 5.31
2 -2 9 45.61 4.71
2 -2 9 43.22 4.14
2 -2 9 44.28 4.23
2 -2 9 43.36 5.76
2 2 9 45.89 5.06
2 2 9 60.15 5.53
2 2 9 57.27 4.90
2 2 9 53.13 4.88
2 2 9 61.32 5.33
2 2 9 52.73 6.27
2 2 9 49.63 5.35
4 -2 9 23.10 3.21
4 -2 9 25.96 2.47
4 -2 9 22.89 2.68
4 -2 9 19.52 2.99
4 -2 9 18.59 4.13
4 -2 9 25.27 2.49
4 -2 9 24.76 4.12
4 -2 9 24.49 2.42
4 2 9 27.72 3.46
4 2 9 28.82 2.76
4 2 9 21.69 3.10
-4 2 -9 23.97 4.20
4 2 9 23.88 2.83
4 2 9 20.04 2.95
4 2 9 24.79 2.67
6 -2 9 88.26 6.84
6 -2 9 75.52 6.86
6 -2 9 83.27 7.91
6 -2 9 76.98 7.28
6 -2 9 68.98 7.73
6 -2 9 79.37 7.02
6 2 9 78.03 7.30
6 2 9 77.07 7.42
6 2 9 81.06 7.03
6 2 9 86.18 7.15
8 -2 9 22.85 2.46
8 -2 9 18.36 3.07
8 -2 9 22.52 2.21
8 -2 9 16.63 2.78
8 -2 9 18.87 3.70
8 2 9 11.73 2.45
8 2 9 13.36 2.54
8 2 9 18.43 1.90
10 -2 9 -0.91 1.09
10 -2 9 0.32 0.96
10 -2 9 0.19 1.44
10 -2 9 -0.32 0.37
10 -2 9 -0.63 1.68
10 -2 9 1.25 0.74
10 2 9 0.26 0.89
10 2 9 -0.03 0.73
10 2 9 0.13 1.17
12 -2 9 0.05 0.32
12 -2 9 1.21 1.21
12 -2 9 -0.88 1.13
12 -2 9 1.34 1.44
12 2 9 -0.23 0.53
12 2 9 0.54 0.79
19 3 -9 -0.34 0.71
-17 -3 9 0.47 0.77
17 -3 -9 0.62 1.14
17 -3 -9 1.11 1.18
-17 -3 9 -0.72 1.21
17 -3 -9 0.46 0.29
17 -3 -9 0.60 3.32
17 3 -9 0.21 0.28
17 3 -9 0.08 0.68
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15 -3 -9 8.71 1.70
15 -3 -9 7.78 4.29
-15 -3 9 9.66 1.70
15 -3 -9 8.54 0.97
15 -3 -9 7.82 1.95
-15 -3 9 7.32 1.21
15 3 -9 4.94 1.19
15 3 -9 5.45 1.37
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-13 -3 9 9.97 1.47
-13 -3 9 11.53 2.04
13 -3 -9 14.32 6.23
13 -3 -9 13.71 1.32
13 -3 -9 8.27 2.40
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-11 -3 9 55.11 4.49
-11 -3 9 59.65 4.81
11 -3 -9 42.08 5.89
11 -3 -9 47.27 5.45
-11 -3 9 44.88 5.11
-11 3 9 51.48 4.75
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11 3 -9 49.99 5.00
-9 -3 9 20.87 2.89
-9 -3 9 20.10 2.38
-9 -3 9 24.38 2.29
9 -3 -9 16.96 4.00
9 -3 -9 20.09 2.09
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-7 -3 9 30.36 4.31
7 -3 -9 39.18 3.05
-7 -3 9 26.96 3.80
7 -3 -9 26.58 4.89
-7 -3 9 32.24 4.30
-7 -3 9 37.04 3.30
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7 3 -9 41.38 3.36
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5 -3 -9 158.10 11.35
5 -3 -9 122.32 12.78
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-5 -3 9 154.17 11.49
-5 -3 9 116.36 11.91
-5 -3 9 119.45 11.76
5 3 -9 167.50 13.73
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3 -3 -9 186.71 13.58
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-3 -3 9 145.48 14.00
-3 -3 9 141.56 14.05
-3 -3 9 182.49 13.76
-3 -3 9 150.75 14.23
3 3 -9 153.94 15.51
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3 3 -9 191.51 14.68
1 -3 -9 41.50 4.01
-1 -3 9 45.29 4.77
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-1 -3 9 42.96 4.67
-1 -3 9 47.13 4.10
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1 3 -9 48.81 4.29
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-1 3 9 50.74 4.53
1 3 -9 43.03 6.06
1 -3 9 23.83 2.62
1 -3 9 22.40 3.10
1 -3 9 18.51 3.07
1 -3 9 24.14 4.92
1 3 9 30.25 4.06
1 3 9 29.51 3.94
1 3 9 45.40 3.78
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1 3 9 38.01 4.37
3 -3 9 0.84 2.03
3 -3 9 3.70 1.48
3 -3 9 2.11 1.94
3 -3 9 5.39 2.65
3 3 9 4.90 1.80
3 3 9 5.18 1.68
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3 3 9 8.88 1.32
3 3 9 3.66 1.61
5 -3 9 10.11 2.20
5 -3 9 9.94 1.57
5 -3 9 10.74 2.32
5 -3 9 8.61 1.58
5 -3 9 13.73 2.80
5 3 9 9.87 1.52
5 3 9 6.01 1.69
5 3 9 6.25 1.73
5 3 9 7.14 1.75
7 -3 9 1.01 0.54
7 -3 9 2.91 2.25
7 -3 9 1.61 1.07
7 -3 9 0.78 1.98
7 -3 9 1.74 1.34
7 -3 9 1.31 0.73
7 3 9 3.49 1.92
7 3 9 0.81 0.79
7 3 9 0.46 1.11
7 3 9 0.89 0.95
7 3 9 1.35 1.35
9 -3 9 3.76 1.70
9 -3 9 3.00 1.67
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9 3 9 -1.10 0.94
9 3 9 0.61 0.74
11 -3 9 1.94 0.88
11 -3 9 1.97 0.87
11 -3 9 3.28 1.48
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16 -4 -9 1.48 1.16
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14 -4 -9 4.72 1.57
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-12 -4 9 1.19 1.33
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-10 -4 9 0.99 1.51
10 -4 -9 1.90 0.46
10 4 -9 1.69 1.14
10 4 -9 1.01 0.39
10 4 -9 2.19 1.34
8 -4 -9 17.12 4.13
-8 -4 9 24.10 3.75
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6 -4 -9 8.22 0.94
6 -4 -9 5.57 3.17
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-2 -4 9 29.05 4.43
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0 -4 -9 10.00 1.02
0 -4 9 6.06 2.13
0 -4 9 5.20 2.02
0 -4 9 7.77 1.51
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2 -4 9 11.07 2.29
2 -4 9 8.89 1.81
2 -4 9 10.46 1.62
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4 -4 9 8.68 1.37
4 -4 9 5.21 1.98
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4 4 9 9.85 1.36
6 -4 9 4.88 1.56
6 -4 9 9.62 1.15
6 -4 9 6.02 2.10
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8 -4 9 7.63 1.15
8 -4 9 4.45 1.12
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-5 -5 9 1.08 1.05
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1 -5 -9 3.14 0.46
1 5 -9 1.18 0.37
1 5 -9 0.03 1.03
1 5 -9 -0.19 1.36
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-1 5 9 0.71 1.57
-1 5 9 1.68 0.75
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-1 -5 -9 5.83 1.06
1 -5 9 1.60 1.09
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-1 5 -9 3.80 1.34
1 5 9 2.21 1.30
1 5 9 1.90 0.64
3 -5 9 0.43 0.71
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3 -5 9 0.49 0.75
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3 5 9 1.26 1.11
3 5 9 1.16 0.64
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20 0 -10 5.52 1.10
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0 0 0
_cell_measurement_reflns_used 7392
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 77.75
_cell_measurement_theta_min 5.225
_exptl_absorpt_correction_T_max 0.7543
_exptl_absorpt_correction_T_min 0.6456
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_crystal_colour colourless
_exptl_crystal_description plate
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_source 'Cu Incoatec microsource'
_diffrn_measurement_device_type 'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method '\j and \w scans'
_diffrn_detector_area_resol_mean 10.4167
_computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection 'APEX III (Bruker, 2018)'
_computing_data_reduction 'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics 'SHELXLE (Hubschle et al., 2011'
_computing_publication_material 'SHELXLE (Hubschle et al., 2011'
_computing_structure_refinement 'SHELXL (Sheldrick, 2015)'
_computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)'
_chemical_absolute_configuration syn
;
_shelx_hkl_checksum 67074
_shelx_res_file
;
TITL cu_190910_AP_127d_0m_a.res in C2
AP_127d_final.res
created by SHELXL-2019/3 at 18:00:12 on 28-Jun-2024
REM Old TITL cu_190910_AP_127d_0m in C2
REM SHELXT solution in C2
REM R1 0.156, Rweak 0.058, Alpha 0.008, Orientation as input
REM Flack x = 0.292 ( 0.316 ) from Parsons' quotients
REM Formula found by SHELXT: C12 O5
REM #####
CELL 1.54178 17.4126 5.0996 14.9856 90 109.652 90
ZERR 4 0.0013 0.0004 0.0011 0 0.002 0
LATT -7
SYMM -X,+Y,-Z
SFAC C H O
UNIT 52 64 16
L.S. 10
PLAN 1
SIZE 0.12 0.256 0.379
TEMP 23
CONF
BOND $H
LIST 4
EQIV $1 0.5-X,-0.5+Y,1-Z
EQIV $2 1-X,Y,1-Z
HTAB O1 O1_$1
HTAB O2 O3_$2
fmap 2
PLAN -5
mpla 5 c1 c3 c4 c5 c6 c2 c7 c8 c9 c10 o1 o2 o3 o4
acta
WGHT 0.131600 0.635700
FVAR 0.84508
C2 1 0.374560 0.111630 0.410958 11.00000 0.06362 0.07298 =
0.06988 0.00389 0.02439 -0.00191
AFIX 13
H2 2 0.398970 0.279483 0.437829 11.00000 -1.20000
AFIX 0
C1 1 0.284382 0.118827 0.388945 11.00000 0.06404 0.07246 =
0.08484 0.00156 0.03660 -0.00069
AFIX 13
H1A 2 0.261212 -0.053188 0.365494 11.00000 -1.20000
AFIX 0
O1 3 0.264545 0.185258 0.470217 11.00000 0.11257 0.09093 =
0.10932 -0.00920 0.07135 -0.00609
AFIX 147
H1 2 0.252857 0.051859 0.493396 11.00000 -1.50000
AFIX 0
O3 3 0.476919 0.093513 0.337508 11.00000 0.05245 0.09330 =
0.08957 0.01580 0.02598 0.00723
O4 3 0.412043 0.429848 0.240491 11.00000 0.05906 0.07296 =
0.09985 0.01336 0.03590 0.00482
C3 1 0.392691 0.052682 0.321476 11.00000 0.05444 0.06366 =
0.07412 0.00125 0.02398 0.00316
AFIX 13
H3 2 0.377713 -0.128755 0.301629 11.00000 -1.20000
AFIX 0
C4 1 0.350420 0.242032 0.239879 11.00000 0.05847 0.06939 =
0.07093 -0.00030 0.02258 -0.00101
AFIX 13
H4 2 0.333731 0.145670 0.179805 11.00000 -1.20000
AFIX 0
C5 1 0.277584 0.390805 0.248532 11.00000 0.05699 0.07213 =
0.08419 0.00401 0.02266 0.00542
O2 3 0.408047 -0.097891 0.476643 11.00000 0.10179 0.09943 =
0.07554 0.01774 0.02313 0.00941
AFIX 143
H2A 2 0.433176 -0.036444 0.528898 11.00000 -1.50000
AFIX 0
C6 1 0.246909 0.323449 0.314978 11.00000 0.05837 0.07700 =
0.10893 0.00344 0.03747 -0.00073
AFIX 43
H6 2 0.199730 0.407119 0.315916 11.00000 -1.20000
AFIX 0
C7 1 0.239515 0.587180 0.176680 11.00000 0.06791 0.07855 =
0.08667 -0.00378 0.02101 -0.00494
C8 1 0.208535 0.737996 0.116704 11.00000 0.07827 0.09794 =
0.10259 0.00964 0.01528 -0.00329
DELU 0.01 0.005 C9 C10
DFIX 1.34 C9 C10
C9 1 0.173249 0.917533 0.040317 11.00000 0.15772 0.11416 =
0.11648 0.01600 0.00829 -0.01921
AFIX 43
H9 2 0.190917 0.900463 -0.011464 11.00000 -1.20000
AFIX 0
C10 1 0.121295 1.096057 0.033943 11.00000 0.19559 0.12370 =
0.21886 0.05711 0.00150 0.00916
AFIX 93
H10A 2 0.101128 1.123418 0.083313 11.00000 -1.50000
H10B 2 0.103243 1.200024 -0.020116 11.00000 -1.50000
AFIX 0
C11 1 0.485919 0.280551 0.271383 11.00000 0.06270 0.07470 =
0.09590 0.00761 0.03774 0.00235
C12 1 0.555207 0.461704 0.320754 11.00000 0.06880 0.08604 =
0.18256 0.00815 0.01608 -0.00830
AFIX 137
H12A 2 0.562490 0.585508 0.276005 11.00000 -1.50000
H12B 2 0.604292 0.361554 0.347503 11.00000 -1.50000
H12C 2 0.543123 0.553832 0.370311 11.00000 -1.50000
AFIX 0
C13 1 0.500463 0.130918 0.190701 11.00000 0.11061 0.13808 =
0.11071 0.00688 0.06388 0.03517
AFIX 137
H13A 2 0.459372 -0.001682 0.167864 11.00000 -1.50000
H13B 2 0.553287 0.049946 0.213143 11.00000 -1.50000
H13C 2 0.497907 0.250061 0.140183 11.00000 -1.50000
REM #####
AFIX 0
HKLF 4
REM cu_190910_AP_127d_0m_a.res in C2
REM wR2 = 0.2483, GooF = S = 1.128, Restrained GooF = 1.130 for all data
REM R1 = 0.0804 for 2138 Fo > 4sig(Fo) and 0.0908 for all 2628 data
REM 157 parameters refined using 3 restraints
END
WGHT 0.1316 0.6357
REM Highest difference peak 0.412, deepest hole -0.206, 1-sigma level 0.054
Q1 1 0.2118 0.3327 0.1074 11.00000 0.05 0.41
Q2 1 0.2611 0.2077 0.1983 11.00000 0.05 0.28
Q3 1 0.3493 0.0855 0.2205 11.00000 0.05 0.25
Q4 1 0.2058 0.5383 0.0785 11.00000 0.05 0.22
Q5 1 0.3872 0.2826 0.3907 11.00000 0.05 0.18
;
_shelx_res_checksum 31197
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, 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
C C2 0.3746(3) 0.1116(12) 0.4110(3) 0.0683(11) Uani d 1 . .
H H2 0.398970 0.279483 0.437829 0.082 Uiso calc 1 . .
C C1 0.2844(3) 0.1188(12) 0.3889(4) 0.0709(12) Uani d 1 . .
H H1A 0.261212 -0.053188 0.365494 0.085 Uiso calc 1 . .
O O1 0.2645(3) 0.1853(10) 0.4702(3) 0.0957(14) Uani d 1 . .
H H1 0.252857 0.051859 0.493396 0.144 Uiso calc 1 . .
O O3 0.47692(19) 0.0935(9) 0.3375(3) 0.0779(11) Uani d 1 . .
O O4 0.4120(2) 0.4298(8) 0.2405(3) 0.0750(10) Uani d 1 . .
C C3 0.3927(3) 0.0527(10) 0.3215(3) 0.0635(11) Uani d 1 . .
H H3 0.377713 -0.128755 0.301629 0.076 Uiso calc 1 . .
C C4 0.3504(3) 0.2420(11) 0.2399(3) 0.0661(11) Uani d 1 . .
H H4 0.333731 0.145670 0.179805 0.079 Uiso calc 1 . .
C C5 0.2776(3) 0.3908(12) 0.2485(4) 0.0714(12) Uani d 1 . .
O O2 0.4080(3) -0.0979(11) 0.4766(3) 0.0939(13) Uani d 1 . .
H H2A 0.433176 -0.036444 0.528898 0.141 Uiso calc 1 . .
C C6 0.2469(3) 0.3234(12) 0.3150(5) 0.0791(15) Uani d 1 . .
H H6 0.199730 0.407119 0.315916 0.095 Uiso calc 1 . .
C C7 0.2395(3) 0.5872(13) 0.1767(4) 0.0790(14) Uani d 1 . .
C C8 0.2085(4) 0.7380(16) 0.1167(5) 0.0968(19) Uani d 1 . .
C C9 0.1732(7) 0.918(2) 0.0403(7) 0.139(4) Uani d 1 . .
H H9 0.190917 0.900463 -0.011464 0.167 Uiso calc 1 . .
C C10 0.1213(9) 1.096(3) 0.0339(11) 0.197(7) Uani d 1 . .
H H10A 0.101128 1.123418 0.083313 0.295 Uiso calc 1 . .
H H10B 0.103243 1.200024 -0.020116 0.295 Uiso calc 1 . .
C C11 0.4859(3) 0.2806(12) 0.2714(4) 0.0750(14) Uani d 1 . .
C C12 0.5552(4) 0.4617(17) 0.3208(8) 0.119(3) Uani d 1 . .
H H12A 0.562490 0.585508 0.276005 0.179 Uiso calc 1 . .
H H12B 0.604292 0.361554 0.347503 0.179 Uiso calc 1 . .
H H12C 0.543123 0.553832 0.370311 0.179 Uiso calc 1 . .
C C13 0.5005(5) 0.131(2) 0.1907(5) 0.113(3) Uani d 1 . .
H H13A 0.459372 -0.001682 0.167864 0.170 Uiso calc 1 . .
H H13B 0.553287 0.049946 0.213143 0.170 Uiso calc 1 . .
H H13C 0.497907 0.250061 0.140183 0.170 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
C2 0.064(2) 0.073(3) 0.070(2) -0.002(2) 0.024(2) 0.004(2)
C1 0.064(3) 0.072(3) 0.085(3) -0.001(2) 0.037(2) 0.002(3)
O1 0.113(3) 0.091(3) 0.109(3) -0.006(3) 0.071(3) -0.009(2)
O3 0.0525(16) 0.093(3) 0.090(2) 0.0072(17) 0.0260(15) 0.016(2)
O4 0.0591(17) 0.073(2) 0.100(2) 0.0048(16) 0.0359(16) 0.0134(19)
C3 0.054(2) 0.064(3) 0.074(3) 0.0032(19) 0.0240(19) 0.001(2)
C4 0.058(2) 0.069(3) 0.071(2) -0.001(2) 0.0226(19) 0.000(2)
C5 0.057(2) 0.072(3) 0.084(3) 0.005(2) 0.023(2) 0.004(3)
O2 0.102(3) 0.099(3) 0.076(2) 0.009(3) 0.0231(19) 0.018(2)
C6 0.058(2) 0.077(3) 0.109(4) -0.001(2) 0.037(3) 0.003(3)
C7 0.068(3) 0.079(3) 0.087(3) -0.005(3) 0.021(2) -0.004(3)
C8 0.078(4) 0.098(4) 0.103(4) -0.003(4) 0.015(3) 0.010(4)
C9 0.158(9) 0.114(7) 0.116(6) -0.019(6) 0.008(6) 0.016(6)
C10 0.196(13) 0.124(9) 0.219(14) 0.009(9) 0.002(10) 0.057(11)
C11 0.063(3) 0.075(3) 0.096(3) 0.002(2) 0.038(2) 0.008(3)
C12 0.069(3) 0.086(5) 0.183(8) -0.008(3) 0.016(4) 0.008(5)
C13 0.111(5) 0.138(6) 0.111(5) 0.035(5) 0.064(4) 0.007(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 C2 C1 . . 108.9(4) ?
O2 C2 C3 . . 107.6(5) ?
C1 C2 C3 . . 109.1(4) ?
O2 C2 H2 . . 110.4 ?
C1 C2 H2 . . 110.4 ?
C3 C2 H2 . . 110.4 ?
O1 C1 C2 . . 111.0(4) ?
O1 C1 C6 . . 107.3(5) ?
C2 C1 C6 . . 110.1(4) ?
O1 C1 H1A . . 109.4 ?
C2 C1 H1A . . 109.4 ?
C6 C1 H1A . . 109.4 ?
C1 O1 H1 . . 109.5 ?
C3 O3 C11 . . 109.3(4) ?
C11 O4 C4 . . 103.6(4) ?
O3 C3 C2 . . 109.5(4) ?
O3 C3 C4 . . 103.5(4) ?
C2 C3 C4 . . 113.2(4) ?
O3 C3 H3 . . 110.1 ?
C2 C3 H3 . . 110.1 ?
C4 C3 H3 . . 110.1 ?
O4 C4 C5 . . 108.0(4) ?
O4 C4 C3 . . 104.9(4) ?
C5 C4 C3 . . 115.8(4) ?
O4 C4 H4 . . 109.3 ?
C5 C4 H4 . . 109.3 ?
C3 C4 H4 . . 109.3 ?
C6 C5 C7 . . 122.4(5) ?
C6 C5 C4 . . 119.6(5) ?
C7 C5 C4 . . 117.7(5) ?
C2 O2 H2A . . 109.5 ?
C5 C6 C1 . . 123.4(5) ?
C5 C6 H6 . . 118.3 ?
C1 C6 H6 . . 118.3 ?
C8 C7 C5 . . 177.7(7) ?
C7 C8 C9 . . 176.9(10) ?
C10 C9 C8 . . 128.6(13) ?
C10 C9 H9 . . 115.7 ?
C8 C9 H9 . . 115.7 ?
C9 C10 H10A . . 120.0 ?
C9 C10 H10B . . 120.0 ?
H10A C10 H10B . . 120.0 ?
O3 C11 O4 . . 106.5(4) ?
O3 C11 C12 . . 109.1(5) ?
O4 C11 C12 . . 108.5(5) ?
O3 C11 C13 . . 107.7(6) ?
O4 C11 C13 . . 112.4(5) ?
C12 C11 C13 . . 112.3(6) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C13 H13A . . 109.5 ?
C11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 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
C2 O2 . 1.437(7) ?
C2 C1 . 1.492(6) ?
C2 C3 . 1.508(7) ?
C2 H2 . 0.9800 ?
C1 O1 . 1.414(7) ?
C1 C6 . 1.502(8) ?
C1 H1A . 0.9800 ?
O1 H1 . 0.8200 ?
O3 C3 . 1.420(5) ?
O3 C11 . 1.422(7) ?
O4 C11 . 1.431(6) ?
O4 C4 . 1.436(6) ?
C3 C4 . 1.538(7) ?
C3 H3 . 0.9800 ?
C4 C5 . 1.520(7) ?
C4 H4 . 0.9800 ?
C5 C6 . 1.324(8) ?
C5 C7 . 1.457(8) ?
O2 H2A . 0.8200 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.168(9) ?
C8 C9 . 1.433(12) ?
C9 C10 . 1.264(16) ?
C9 H9 . 0.9300 ?
C10 H10A . 0.9300 ?
C10 H10B . 0.9300 ?
C11 C12 . 1.502(9) ?
C11 C13 . 1.521(10) ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C12 H12C . 0.9600 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
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
O1 H1 O1 4_546 0.82 2.00 2.803(3) 166.8 yes
O2 H2A O3 2_656 0.82 2.19 2.995(6) 167.7 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
O2 C2 C1 O1 . . . . 65.4(6) ?
C3 C2 C1 O1 . . . . -177.4(5) ?
O2 C2 C1 C6 . . . . -175.9(5) ?
C3 C2 C1 C6 . . . . -58.7(6) ?
C11 O3 C3 C2 . . . . -122.7(5) ?
C11 O3 C3 C4 . . . . -1.7(5) ?
O2 C2 C3 O3 . . . . -72.8(5) ?
C1 C2 C3 O3 . . . . 169.2(4) ?
O2 C2 C3 C4 . . . . 172.3(4) ?
C1 C2 C3 C4 . . . . 54.2(6) ?
C11 O4 C4 C5 . . . . 156.9(4) ?
C11 O4 C4 C3 . . . . 32.8(5) ?
O3 C3 C4 O4 . . . . -19.4(5) ?
C2 C3 C4 O4 . . . . 99.0(5) ?
O3 C3 C4 C5 . . . . -138.4(4) ?
C2 C3 C4 C5 . . . . -19.9(6) ?
O4 C4 C5 C6 . . . . -127.6(5) ?
C3 C4 C5 C6 . . . . -10.4(7) ?
O4 C4 C5 C7 . . . . 58.1(6) ?
C3 C4 C5 C7 . . . . 175.4(5) ?
C7 C5 C6 C1 . . . . 179.1(5) ?
C4 C5 C6 C1 . . . . 5.1(9) ?
O1 C1 C6 C5 . . . . 151.3(6) ?
C2 C1 C6 C5 . . . . 30.3(8) ?
C3 O3 C11 O4 . . . . 22.5(6) ?
C3 O3 C11 C12 . . . . 139.5(5) ?
C3 O3 C11 C13 . . . . -98.3(5) ?
C4 O4 C11 O3 . . . . -34.5(5) ?
C4 O4 C11 C12 . . . . -151.9(6) ?
C4 O4 C11 C13 . . . . 83.2(6) ?