#------------------------------------------------------------------------------
#$Date: 2023-06-29 17:39:16 +0200 (Thu, 29 Jun 2023) $
#$Revision: 284686 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022778.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_2022778
loop_
_publ_author_name
'Tirkasheva, Sarvinoz I.'
'Ziyadullaev, Odiljon E.'
'Eshimbetov, Alisher G.'
'Ibragimov, Bakhtiyar T.'
'Ashurov, Jamshid M.'
_publ_section_title
;
Synthesis, crystal structure, Hirshfeld surface analysis and DFT study of
the 1,1′-(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)
;
_journal_coeditor_code ZV2024
_journal_issue 7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023004772
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C16 H22 O2'
_chemical_formula_moiety 'C16 H22 O2'
_chemical_formula_sum 'C16 H22 O2'
_chemical_formula_weight 246.33
_chemical_name_common
;
1-[4-(1-Hydroxycyclohexan-1-yl)buta-1,3-diyne-1-yl]cyclohexan-1-ol
;
_chemical_name_systematic
;
1,1'-(Buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 13
_space_group_name_Hall '-P 2yc'
_space_group_name_H-M_alt 'P 1 2/c 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha 90
_cell_angle_beta 90.308(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.4134(2)
_cell_length_b 6.9167(2)
_cell_length_c 20.4801(5)
_cell_measurement_reflns_used 4018
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.1670
_cell_measurement_theta_min 4.2390
_cell_volume 1475.09(6)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0382
_diffrn_reflns_av_unetI/netI 0.0276
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 13939
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 71.518
_diffrn_reflns_theta_min 4.246
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.559
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96014
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.109
_exptl_crystal_description block
_exptl_crystal_F_000 536
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.124
_refine_diff_density_min -0.157
_refine_ls_extinction_coef 0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 166
_refine_ls_number_reflns 2866
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0594
_refine_ls_R_factor_gt 0.0444
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.2398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1181
_refine_ls_wR_factor_ref 0.1291
_reflns_number_gt 2161
_reflns_number_total 2866
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zv2024sup1.cif
_cod_data_source_block I
_cod_database_code 2022778
_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_hkl_file
;
0 0 -2 690.57 14.61
0 0 -2 717.58 15.18
0 0 2 685.36 14.65
0 0 -2 681.13 14.92
0 0 2 694.65 15.19
0 0 3 0.09 0.17
0 0 -3 -0.18 0.32
0 0 -3 -0.14 0.23
0 0 -4 6943.27 143.84
0 0 4 6897.46 143.20
0 0 -4 7133.29 144.40
0 0 -5 -0.15 0.54
0 0 -5 0.12 0.41
0 0 -5 -0.15 0.60
0 0 -6 955.69 22.66
0 0 -6 941.92 21.99
0 0 -6 983.35 22.82
0 0 6 947.98 22.76
0 0 -7 0.45 0.61
0 0 -7 0.22 0.62
0 0 -7 -0.17 0.47
0 0 7 0.46 0.67
0 0 -8 1066.93 26.09
0 0 -8 1056.12 25.88
0 0 -8 1045.70 25.82
0 0 8 1062.34 26.19
0 0 -9 -0.31 0.75
0 0 -9 -0.30 0.72
0 0 -9 0.29 0.79
0 0 9 0.31 0.70
0 0 -10 56.78 4.19
0 0 -10 61.76 4.20
0 0 -10 69.94 4.45
0 0 10 60.88 4.34
0 0 -11 -0.41 0.78
0 0 -11 -0.39 0.87
0 0 -11 0.38 0.86
0 0 11 -0.41 0.85
0 0 -12 42.50 4.05
0 0 -12 47.69 4.12
0 0 -12 42.04 3.92
0 0 12 41.29 3.99
0 0 -13 -0.52 0.99
0 0 -13 -0.48 1.01
0 0 13 -0.52 1.09
0 0 -14 22.35 3.16
0 0 -14 17.94 2.98
0 0 -14 22.26 3.37
0 0 14 15.72 2.87
0 0 -15 -0.58 1.11
0 0 -15 -0.64 1.21
0 0 -15 -0.64 1.09
0 0 15 -0.64 1.09
0 0 -16 20.14 3.25
0 0 -16 28.42 4.07
0 0 -16 24.25 3.81
0 0 -17 -0.67 1.13
0 0 -17 -0.73 1.08
0 0 -17 -0.74 0.89
0 0 -18 34.97 4.80
0 0 -18 32.99 4.35
0 0 -19 0.76 1.12
0 0 -19 0.69 1.01
0 0 -20 30.20 4.30
0 0 -21 -0.68 1.16
0 0 22 32.25 4.19
0 0 23 0.54 0.92
0 0 -23 1.03 0.98
0 0 -24 0.41 0.60
0 0 24 0.43 0.90
0 0 25 -0.63 0.65
0 0 -25 -0.29 0.60
0 -1 0 88.64 3.01
0 -1 0 87.21 2.94
0 -1 0 86.40 2.64
0 -1 -1 985.33 21.29
0 -1 1 955.27 21.12
0 1 -1 941.29 20.27
0 -1 1 984.09 21.04
0 1 -2 385.58 9.40
0 -1 2 370.23 9.23
0 -1 -2 383.99 9.39
0 1 -2 362.08 8.47
0 -1 2 374.11 9.27
0 1 2 372.79 9.48
0 1 3 894.20 20.10
0 -1 3 868.50 19.88
0 -1 -3 872.40 19.88
0 1 -3 874.43 19.89
0 1 3 862.64 19.76
0 1 -3 893.61 19.74
0 1 -3 862.44 19.14
0 -1 -3 851.99 18.48
0 1 -4 488.47 11.90
0 1 4 466.85 11.82
0 -1 -4 456.21 12.15
0 1 -4 474.95 12.08
0 -1 -4 475.42 12.09
0 1 4 488.51 12.29
0 -1 4 460.30 11.19
0 1 -4 465.60 11.49
0 1 5 143.16 5.02
0 -1 -5 151.53 5.50
0 1 -5 141.86 5.06
0 -1 -5 146.63 5.16
0 1 -5 141.29 5.25
0 -1 5 139.51 5.33
0 1 -5 141.15 4.90
0 -1 -5 140.69 5.10
0 1 6 11.38 1.34
0 -1 -6 7.08 1.23
0 -1 -6 7.47 1.13
0 1 -6 6.02 1.05
0 1 -6 7.38 1.27
0 -1 6 6.80 1.23
0 -1 -6 7.00 1.21
0 1 -6 6.69 1.08
0 -1 -7 228.26 8.20
0 1 -7 232.34 8.05
0 -1 -7 238.71 7.81
0 1 -7 231.67 7.84
0 -1 -7 230.12 8.04
0 1 -7 239.26 7.87
0 -1 7 216.54 8.09
0 -1 -8 77.75 4.44
0 1 -8 68.00 4.14
0 1 -8 65.49 3.92
0 -1 -8 69.65 3.90
0 -1 8 77.26 4.45
0 1 -8 74.95 4.10
0 -1 -8 78.98 4.40
0 1 -9 1101.79 27.75
0 1 -9 1131.55 28.21
0 -1 -9 1097.62 28.45
0 -1 9 1139.02 28.56
0 -1 -9 1166.28 28.47
0 1 -9 1102.41 27.84
0 1 -10 217.82 8.67
0 -1 -10 216.73 9.13
0 1 -10 220.17 8.91
0 -1 -10 224.46 9.21
0 1 -10 209.79 8.65
0 -1 -11 6.55 1.68
0 1 -11 7.63 1.71
0 -1 11 7.45 1.91
0 1 -11 7.12 1.58
0 -1 -11 7.66 1.78
0 -1 -12 -0.46 0.87
0 1 -12 0.45 1.01
0 1 -12 -0.45 0.85
0 -1 -12 -0.48 0.82
0 -1 12 -0.98 1.11
0 1 -13 218.08 10.15
0 -1 -13 229.20 10.60
0 -1 -13 210.75 10.08
0 1 -13 220.94 10.78
0 -1 -13 227.59 10.70
0 1 -13 216.23 10.15
0 -1 13 218.91 10.62
0 -1 14 17.03 2.98
0 -1 -14 9.70 2.29
0 1 -14 20.29 3.14
0 -1 -14 15.65 2.80
0 1 -14 7.83 2.03
0 -1 -14 10.18 2.46
0 1 -14 14.34 2.87
0 1 15 6.73 2.22
0 -1 15 7.34 2.13
0 1 15 9.27 2.52
0 -1 -15 1.87 1.19
0 1 -15 9.22 2.34
0 -1 -15 5.92 1.94
0 1 -15 5.45 1.93
0 1 16 1.44 1.84
0 -1 -16 4.69 1.89
0 -1 -16 3.37 1.62
0 -1 16 2.89 1.74
0 1 16 2.14 1.61
0 -1 -16 4.27 1.92
0 1 -16 1.33 1.50
0 1 -16 0.73 1.25
0 -1 -17 4.24 1.99
0 -1 -17 3.52 1.70
0 1 17 -0.76 1.44
0 -1 17 1.53 1.46
0 -1 -17 1.51 1.58
0 1 -17 0.77 1.32
0 -1 -18 163.27 10.27
0 -1 -18 173.08 10.43
0 1 -19 1.60 1.66
0 -1 -19 2.17 1.38
0 1 -20 112.35 8.46
0 1 20 97.83 7.82
0 -1 -20 93.68 7.52
0 1 21 5.51 2.11
0 1 -21 1.43 1.36
0 -1 -21 1.91 1.33
0 1 22 7.34 2.09
0 1 -22 10.71 2.58
0 -1 23 -0.51 0.97
0 1 23 -0.52 1.16
0 1 -23 -0.51 0.86
0 1 -23 -0.53 1.00
0 -1 24 0.40 0.76
0 1 24 0.41 0.92
0 1 -24 -0.40 0.90
0 1 -24 -0.41 0.78
0 1 -25 -0.28 0.64
0 -1 -25 0.28 0.53
0 -2 0 698.83 17.00
0 -2 0 682.22 16.81
0 -2 0 667.44 15.95
0 -2 -1 1.84 0.68
0 -2 1 1.62 0.67
0 -2 1 1.57 0.71
0 -2 -1 0.80 0.43
0 -2 1 1.56 0.57
0 -2 -2 1700.14 36.68
0 -2 2 1577.91 36.37
0 -2 -2 1631.65 36.45
0 -2 2 1606.97 36.26
0 -2 2 1598.85 35.98
0 -2 -3 777.96 19.40
0 -2 3 796.96 19.23
0 -2 3 778.67 19.14
0 -2 -4 680.70 17.84
0 -2 4 699.34 17.67
0 2 4 714.98 18.31
0 2 5 374.31 11.44
0 -2 -5 385.50 11.57
0 -2 5 379.48 11.11
0 2 5 378.72 11.66
0 -2 -6 457.36 13.78
0 2 6 453.61 13.39
0 2 -6 462.78 13.57
0 -2 6 473.92 13.27
0 -2 -6 463.86 13.63
0 -2 -6 441.95 12.61
0 2 6 470.95 13.95
0 2 -7 0.30 0.86
0 -2 -7 0.30 0.91
0 -2 -7 -0.66 0.94
0 -2 7 0.54 0.69
0 -2 -7 -0.25 0.64
0 -2 7 0.32 0.81
0 2 -8 0.34 0.95
0 -2 -8 0.74 0.89
0 -2 -8 0.65 0.87
0 -2 8 1.81 0.89
0 -2 -8 0.89 0.76
0 2 8 1.48 1.04
0 -2 8 0.72 0.86
0 -2 -9 181.29 7.75
0 2 -9 177.47 7.99
0 -2 -9 183.39 7.95
0 -2 -9 176.53 8.32
0 2 9 169.19 8.16
0 -2 9 190.03 8.50
0 -2 -10 149.54 7.26
0 -2 -10 124.42 7.22
0 2 -10 144.09 7.34
0 2 10 144.93 7.66
0 -2 10 135.95 7.44
0 -2 -11 1.33 1.00
0 2 -11 3.21 1.30
0 -2 -11 2.04 1.23
0 -2 11 4.00 1.65
0 2 11 1.52 1.14
0 -2 -12 0.56 1.17
0 2 -12 1.52 1.22
0 2 12 0.56 1.06
0 -2 -12 0.50 0.85
0 2 -12 0.55 0.93
0 2 -13 69.07 6.25
0 -2 -13 68.51 5.87
0 2 -13 84.54 6.24
0 2 13 73.44 6.19
0 -2 13 84.20 6.53
0 -2 -13 82.38 6.18
0 2 -13 81.12 6.40
0 2 -14 42.17 5.01
0 -2 -14 40.12 4.65
0 2 -14 43.10 4.62
0 -2 -14 47.84 4.98
0 -2 14 45.20 5.11
0 -2 14 46.78 4.91
0 2 14 44.13 4.98
0 2 -14 43.67 4.96
0 2 15 9.34 2.60
0 -2 15 9.32 2.45
0 -2 -15 9.44 2.44
0 2 -15 9.74 2.56
0 -2 -15 5.33 1.89
0 2 -15 7.14 2.11
0 2 16 53.74 5.67
0 2 -16 43.16 5.38
0 -2 -16 47.09 5.41
0 -2 -16 40.29 5.00
0 2 16 47.17 5.46
0 -2 16 44.87 5.34
0 2 -16 41.69 5.24
0 2 16 45.90 5.63
0 2 -17 69.14 6.80
0 -2 -17 73.93 6.71
0 2 17 75.03 6.83
0 -2 -17 65.33 6.55
0 2 -17 88.27 7.62
0 2 17 73.41 7.17
0 2 -18 0.80 0.96
0 -2 -18 2.24 1.68
0 2 18 -0.75 1.11
0 2 -18 2.39 1.92
0 2 18 0.82 1.39
0 -2 -18 1.54 1.74
0 2 19 -0.73 1.40
0 2 -19 0.78 1.49
0 2 19 -0.79 1.51
0 -2 -19 0.75 1.42
0 2 20 4.84 1.77
0 2 -20 1.48 1.26
0 2 20 0.74 1.54
0 -2 -20 0.70 1.19
0 2 21 2.50 1.51
0 2 -21 5.38 2.14
0 2 21 3.93 1.77
0 -2 -21 4.99 1.68
0 2 -22 11.99 2.32
0 2 22 9.70 2.16
0 2 -22 12.26 2.54
0 2 22 13.78 2.70
0 -2 -22 9.53 2.12
0 -2 -23 0.42 0.63
0 2 23 0.88 0.91
0 2 -23 0.42 0.81
0 2 -23 -0.96 1.08
0 -2 -24 -0.32 0.60
0 2 -24 0.73 0.82
0 2 24 0.98 0.73
0 2 -24 -0.32 0.60
0 -3 0 619.76 17.43
0 -3 0 655.86 17.71
0 -3 -1 5.47 1.33
0 -3 1 8.42 1.55
0 -3 -1 6.50 1.41
0 -3 1 8.60 1.51
0 -3 2 393.03 12.28
0 -3 -2 401.83 12.59
0 -3 -2 417.64 12.79
0 -3 2 397.71 12.52
0 -3 3 223.68 8.40
0 -3 -3 229.23 8.71
0 -3 3 227.59 8.61
0 -3 4 0.30 0.73
0 -3 -4 1.67 0.94
0 -3 4 0.31 0.89
0 -3 -5 2.15 1.01
0 -3 5 3.50 1.24
0 -3 5 2.32 1.13
0 -3 6 457.91 14.30
0 -3 -6 460.47 14.90
0 3 6 441.94 14.78
0 -3 -7 348.27 12.70
0 -3 7 345.41 12.58
0 -3 -7 343.62 12.92
0 -3 -7 333.43 12.40
0 -3 8 88.52 5.86
0 -3 -8 86.21 5.96
0 -3 -8 104.02 6.23
0 -3 9 732.70 22.29
0 3 9 719.10 22.54
0 -3 -9 742.14 22.70
0 -3 -9 717.85 21.86
0 3 10 23.51 3.43
0 -3 10 17.30 2.83
0 -3 -10 22.93 3.12
0 -3 -10 17.22 2.92
0 3 11 1.21 1.26
0 -3 11 0.59 1.00
0 3 -11 -0.65 0.96
0 -3 -11 -0.55 0.94
0 3 11 -0.63 1.42
0 -3 -11 -0.62 0.75
0 -3 -12 -0.67 0.99
0 -3 -12 -0.60 0.72
0 3 -12 -0.70 1.47
0 3 12 0.65 1.24
0 -3 12 0.64 1.22
0 -3 -13 440.64 18.03
0 3 13 422.90 17.65
0 -3 -14 122.42 8.95
0 3 14 120.74 8.74
0 -3 14 121.71 8.79
0 -3 14 133.87 8.96
0 3 -14 123.61 9.00
0 3 15 48.01 5.54
0 -3 15 51.61 5.68
0 -3 15 37.69 4.93
0 3 -15 33.79 5.03
0 3 -16 132.87 9.73
0 3 -16 124.85 8.97
0 3 16 142.07 10.01
0 -3 -16 144.48 9.80
0 3 -17 71.14 7.02
0 3 -17 52.77 5.91
0 3 17 51.86 6.17
0 -3 -17 74.32 6.94
0 3 -18 36.38 5.00
0 3 -18 41.37 5.07
0 3 18 53.60 6.05
0 -3 -18 50.74 5.70
0 3 -19 1.51 1.57
0 3 -19 0.70 1.33
0 3 19 0.76 1.59
0 -3 -19 0.72 1.23
0 3 -20 1.27 1.33
0 3 20 4.12 1.94
0 -3 -20 2.61 1.36
0 3 21 0.59 1.01
0 -3 -21 0.57 0.96
0 3 22 2.40 1.23
0 -3 -22 4.64 1.48
0 3 23 0.36 0.75
0 3 -23 1.41 0.90
0 -4 0 16.27 2.40
0 -4 0 13.56 2.27
0 -4 -1 28.96 3.18
0 -4 -1 20.65 2.76
0 -4 1 24.30 2.92
0 -4 -2 190.31 8.89
0 -4 2 190.68 8.76
0 -4 2 189.46 8.74
0 -4 3 8.36 1.92
0 -4 -3 8.63 1.86
0 -4 -4 75.89 5.50
0 -4 4 64.34 4.85
0 4 4 69.64 5.52
0 4 -4 68.02 5.51
0 -4 -5 6.02 1.76
0 4 5 5.77 1.79
0 4 -5 3.08 1.45
0 4 6 0.54 0.79
0 4 -6 1.73 1.48
0 -4 -6 0.53 1.01
0 4 -7 35.45 4.21
0 -4 -7 38.98 4.36
0 -4 -7 36.44 4.18
0 -4 7 35.47 3.97
0 4 -7 31.68 4.08
0 4 7 37.08 4.48
0 -4 -7 38.64 4.27
0 4 -8 0.63 1.08
0 -4 -8 0.63 0.93
0 -4 -8 -0.60 1.35
0 -4 8 0.57 1.18
0 4 8 0.63 1.31
0 4 -8 -1.28 1.72
0 4 8 -0.67 1.14
0 4 -9 39.78 4.69
0 -4 -9 37.66 4.48
0 -4 -9 37.42 4.58
0 -4 9 39.30 4.47
0 4 -9 35.60 4.50
0 4 9 43.91 5.18
0 4 -10 -0.72 1.22
0 -4 -10 0.66 0.79
0 -4 -10 -0.71 1.05
0 -4 10 -0.64 0.78
0 4 -10 -0.70 1.46
0 4 10 0.74 1.27
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11 -1 -3 15.82 3.11
11 -1 -3 11.72 2.69
11 -1 -3 15.75 3.02
11 1 -3 14.67 2.86
11 -1 -2 -0.64 1.33
11 -1 -2 -0.64 1.33
11 -1 -2 2.44 1.64
11 1 -2 -0.62 1.41
11 -1 -1 14.65 2.89
11 -1 -1 18.82 3.29
11 -1 -1 16.44 3.04
11 1 -1 18.39 3.26
11 -1 0 0.63 0.93
11 -1 0 -0.58 0.99
11 1 0 1.88 1.51
11 -1 0 1.96 1.47
11 -1 0 1.21 1.36
11 1 0 1.28 1.21
11 -1 1 6.73 2.15
11 -1 1 5.34 1.83
11 1 1 3.13 1.41
11 -1 1 5.84 2.07
11 -1 1 5.34 1.82
11 1 1 7.02 2.11
11 -1 2 2.94 1.50
11 -1 2 5.21 1.78
11 1 2 2.53 1.53
11 -1 2 2.39 1.44
11 1 2 2.47 1.29
11 -1 2 4.46 1.88
11 1 3 41.85 4.69
11 -1 3 36.42 4.28
11 1 3 32.71 4.13
11 -1 3 35.13 4.39
11 1 4 58.55 5.54
11 -1 4 67.53 5.88
11 -1 4 74.34 6.11
11 1 4 67.01 5.82
11 1 5 46.08 4.81
11 -1 5 47.89 4.83
11 1 5 46.82 4.73
11 1 6 -0.57 0.96
11 -1 6 0.56 0.95
11 1 6 0.53 0.91
11 -1 7 36.65 3.80
11 1 7 26.69 3.54
11 -1 7 33.50 3.89
11 1 7 23.91 3.20
11 -1 8 0.88 1.06
11 1 8 1.49 1.34
11 -1 8 0.50 0.85
11 1 8 0.91 1.10
11 -1 9 1.23 1.04
11 1 9 0.91 1.02
11 -1 9 1.38 1.24
11 -1 10 2.96 1.14
11 1 10 2.43 1.14
11 -1 10 2.07 1.00
11 1 11 11.56 1.92
11 -1 11 9.41 1.67
11 -1 11 11.17 1.95
-11 1 -11 7.67 1.66
11 -1 12 0.30 0.57
-11 1 -12 -0.32 0.67
11 -2 -11 28.92 2.84
11 2 -11 28.69 2.99
11 -2 -10 0.34 0.82
11 2 -10 0.66 0.68
11 2 -10 0.78 0.81
11 -2 -10 0.36 0.80
11 -2 -9 12.38 2.14
11 2 -9 15.91 2.29
11 2 -9 12.48 2.24
11 -2 -9 9.76 1.93
11 -2 -8 -0.45 0.85
11 2 -8 -0.42 0.80
11 -2 -8 2.10 1.43
11 2 -8 0.47 1.05
11 -2 -8 1.25 1.18
11 -2 -7 -1.96 1.32
11 2 -7 -0.92 0.96
11 -2 -7 -0.45 0.93
11 2 -7 1.97 1.39
11 -2 -7 -0.44 1.11
11 -2 -6 2.09 1.41
11 2 -6 1.47 1.18
11 -2 -6 -0.47 0.98
11 2 -6 1.54 1.16
11 -2 -5 13.12 2.60
11 -2 -5 13.40 2.48
11 2 -5 11.33 2.41
11 2 -5 11.63 2.52
11 -2 -4 1.13 1.27
11 -2 -4 4.28 1.64
11 2 -4 2.14 1.51
11 -2 -3 10.30 2.39
11 -2 -3 7.35 2.05
11 2 -3 11.49 2.47
11 -2 -3 8.43 2.03
11 2 -3 7.51 2.00
11 2 -3 11.78 2.35
11 -2 -2 13.19 2.65
11 -2 -2 14.65 2.79
11 -2 -2 14.34 2.67
11 2 -2 17.57 3.13
11 2 -2 14.87 2.69
11 -2 -1 3.96 1.60
11 -2 -1 2.99 1.61
11 -2 -1 1.57 1.09
11 2 -1 2.56 1.44
11 2 -1 1.63 1.23
11 -2 0 8.28 2.21
11 -2 0 3.19 1.43
11 2 0 6.41 2.04
11 2 0 2.77 1.57
11 -2 0 7.23 2.18
11 -2 1 1.07 1.11
11 2 1 0.63 1.32
11 2 1 3.91 1.50
11 -2 1 -0.60 1.14
11 -2 2 0.53 1.01
11 2 2 0.62 1.06
11 2 2 0.56 0.82
11 -2 2 -0.59 1.00
11 -2 3 1.05 1.10
11 2 3 1.10 1.24
11 -2 3 1.69 1.36
11 -2 4 40.22 4.20
11 2 4 41.66 4.39
11 -2 4 36.81 4.17
11 -2 4 39.61 4.11
11 -2 5 1.00 1.04
11 2 5 2.10 1.26
11 -2 5 -0.49 0.94
11 -2 6 1.43 1.00
11 2 6 4.03 1.48
11 -2 6 2.87 1.47
11 -2 7 14.87 2.41
11 2 7 14.26 2.45
11 -2 7 14.13 2.41
11 -2 8 1.25 0.87
11 2 8 2.65 1.30
11 -2 8 0.43 0.81
11 2 9 4.43 1.42
11 -2 9 4.56 1.41
-11 2 -9 3.67 1.35
11 -2 9 5.48 1.49
11 2 10 0.36 0.68
11 -2 10 0.34 0.57
-11 2 -10 0.72 0.86
11 -2 10 -0.35 0.67
11 2 11 1.23 0.78
11 -2 11 0.30 0.57
-11 2 -11 -0.30 0.81
11 -2 11 1.44 0.78
11 -3 -9 5.56 1.32
11 -3 -8 13.68 1.99
11 -3 -8 17.04 2.30
11 3 -8 12.42 1.92
11 -3 -7 4.11 1.28
11 -3 -7 5.10 1.60
11 3 -7 4.06 1.30
11 -3 -6 1.88 1.06
11 3 -6 1.15 0.92
11 -3 -6 2.95 1.24
11 3 -6 1.59 1.12
11 -3 -5 2.42 1.14
11 3 -5 0.42 1.07
11 -3 -5 0.88 0.92
11 3 -5 1.67 0.94
11 -3 -4 11.80 2.23
11 -3 -4 11.83 2.22
11 3 -4 11.67 2.22
11 3 -4 16.41 2.63
11 -3 -4 13.66 2.28
11 3 -4 10.31 2.14
11 3 -3 28.26 3.39
11 -3 -3 32.06 3.58
11 -3 -3 25.33 3.25
11 -3 -3 27.59 3.27
11 3 -3 32.04 3.68
11 3 -3 26.57 3.38
11 -3 -2 -0.45 0.95
11 -3 -2 1.83 1.10
11 3 -2 0.49 1.10
11 3 -2 0.52 1.09
11 3 -2 0.44 0.85
11 -3 -2 0.49 1.02
11 -3 -1 7.94 1.95
11 3 -1 7.50 1.94
11 3 -1 4.42 1.51
11 -3 -1 4.03 1.55
11 -3 0 5.18 1.61
11 3 0 4.31 1.66
11 3 0 1.73 1.05
11 -3 0 3.55 1.56
11 -3 1 0.94 0.98
11 3 1 0.53 0.79
11 -3 1 -0.50 0.96
11 -3 2 0.46 0.97
11 3 2 -0.52 1.17
11 -3 2 -0.49 1.02
11 3 3 2.49 1.34
11 -3 3 0.91 1.16
11 3 3 -0.49 0.94
11 -3 3 1.86 1.12
11 3 4 16.39 2.71
11 -3 4 14.02 2.34
11 3 4 5.51 1.62
11 -3 4 9.56 2.04
11 3 5 0.39 0.87
-11 3 -5 1.59 1.01
11 3 5 0.97 1.17
11 -3 5 0.42 0.79
11 3 6 45.53 3.80
11 -3 6 48.94 4.04
11 3 7 3.09 1.13
-11 3 -7 3.64 1.32
11 -3 7 4.33 1.27
11 3 8 3.12 1.13
11 -3 8 2.27 0.92
-11 3 -8 2.68 1.11
11 -3 9 0.28 0.68
-11 3 -9 0.30 0.76
11 -4 -4 16.96 2.09
11 4 -4 8.87 1.68
11 -4 -3 -0.32 0.61
11 4 -3 -0.34 0.71
11 -4 -3 0.32 0.66
11 -4 -2 6.88 1.58
11 4 -2 5.84 1.53
11 -4 -2 5.27 1.38
11 -4 -1 3.57 1.18
11 4 -1 3.79 1.25
11 -4 -1 3.69 1.18
11 -4 0 0.36 0.81
11 4 0 1.53 0.86
11 -4 0 1.34 0.90
11 -4 1 0.36 0.74
11 4 1 -0.38 0.79
11 -4 1 1.66 0.94
11 -4 2 -0.34 0.82
11 4 2 0.36 0.62
11 -4 2 0.32 0.73
11 -4 3 5.73 1.46
11 4 3 6.38 1.49
11 -4 3 5.55 1.32
11 -4 4 19.08 2.21
12 0 -8 12.81 1.93
12 0 -7 -0.72 0.91
12 0 -6 5.45 1.49
12 0 -5 -0.83 1.06
12 0 -4 27.06 3.29
12 0 -3 -0.45 0.94
12 0 -2 2.31 1.24
12 0 -1 1.40 1.12
12 0 0 2.33 1.26
12 0 1 0.46 1.04
12 0 2 12.61 2.28
12 0 2 11.70 2.21
12 0 3 -0.44 0.75
12 0 3 0.87 0.98
12 0 4 1.71 1.26
12 0 4 0.41 0.93
12 0 5 -0.81 0.91
12 0 5 0.38 0.80
12 0 6 0.76 0.72
12 0 6 0.35 0.73
12 0 7 -0.34 0.59
12 0 8 43.72 3.41
12 -1 -7 7.69 1.62
12 1 -7 10.76 1.80
12 -1 -7 8.91 1.61
12 -1 -6 15.15 2.25
12 1 -6 15.59 2.20
12 -1 -6 15.91 2.31
12 1 -6 20.66 2.49
12 -1 -5 4.00 1.32
12 1 -5 1.79 0.92
12 -1 -5 5.37 1.50
12 1 -5 3.38 1.24
12 -1 -4 0.85 1.08
12 1 -4 -0.38 0.73
12 -1 -4 -0.40 0.90
12 1 -4 0.40 0.83
12 -1 -3 19.70 2.73
12 -1 -3 17.26 2.49
12 1 -3 21.02 2.79
12 -1 -2 10.83 2.04
12 1 -2 5.66 1.74
12 -1 -1 3.33 1.37
12 1 -1 3.11 1.31
12 -1 0 1.23 0.99
12 1 0 -0.45 0.76
12 -1 1 0.40 0.77
12 1 1 0.90 1.26
12 -1 2 3.25 1.20
12 1 2 2.64 1.19
12 -1 3 1.21 0.97
12 1 3 0.43 0.82
12 -1 4 1.18 0.95
12 1 4 1.23 1.05
12 -1 5 11.29 1.99
12 1 5 10.87 1.94
12 -1 6 16.64 2.29
12 1 6 21.57 2.59
12 -1 7 -0.33 0.55
12 1 7 0.98 0.87
12 -1 8 9.84 1.63
12 -2 -6 4.69 1.28
12 2 -6 4.34 1.13
12 -2 -5 8.48 1.67
12 2 -5 10.47 1.76
12 -2 -4 2.14 1.05
12 2 -4 1.69 1.12
12 -2 -3 0.72 0.81
12 2 -3 -0.71 0.74
12 -2 -2 9.94 1.78
12 -2 -2 5.74 1.57
12 2 -2 8.00 1.76
12 2 -2 10.71 1.79
12 -2 -1 -0.36 0.75
12 2 -1 1.40 0.94
12 2 -1 -0.37 0.77
12 -2 -1 -0.79 0.82
12 2 0 1.43 0.91
12 2 0 0.36 0.69
12 -2 0 2.00 1.02
12 2 1 2.17 1.07
12 2 1 1.43 0.91
12 -2 1 4.34 1.30
12 2 2 1.79 0.97
12 -2 2 3.04 1.21
12 -2 3 0.31 0.65
12 2 3 0.70 0.79
12 -2 3 1.07 0.86
12 2 4 37.18 3.25
12 -2 4 31.83 2.91
12 2 5 5.10 1.36
-12 2 -5 2.44 1.13
12 -2 5 3.67 1.08
12 2 6 3.24 1.00
0 0 0 0.00 0.00
TITL exp_872+B11-23 in P2/c
REM P2/c (#13 in standard setting)
CELL 1.54184 10.413377 6.916659 20.480115 90.0000 90.3077 90.0000
ZERR 6.00 0.000211 0.000169 0.000461 0.0000 0.0020 0.0000
LATT 1
SYMM -x, y,-z+1/2
SFAC C H N O
UNIT 66.00 60.00 6.00 6.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 66714
_shelx_res_file
;
TITL exp_872+b11-23.81-2_a.res in P2/c
exp_872+b11-23.81-2.res
created by SHELXL-2019/2 at 10:58:06 on 26-Jul-2022
REM Old TITL exp_872+b11-23.81-2_a.res in P2/c
REM SHELXT solution in P2/c: R1 0.189, Rweak 0.007, Alpha 0.022
REM 0.231 for 251 systematic absences, Orientation as input
REM Formula found by SHELXT: C1B N2 O1B
CELL 1.54184 10.4134 6.9167 20.4801 90 90.308 90
ZERR 4 0.0002 0.0002 0.0005 0 0.002 0
LATT 1
SYMM -X,+Y,0.5-Z
SFAC C H O
UNIT 64 88 8
L.S. 4 0 0
PLAN 5
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta NOHKL
REM
REM
REM
WGHT 0.056500 0.239800
EXTI 0.001807
FVAR 0.69925
O1A 3 0.612986 0.285040 0.675298 11.00000 0.04440 0.05960 =
0.04598 0.01277 -0.00053 -0.00770
AFIX 147
H1A 2 0.534651 0.297081 0.675485 11.00000 -1.50000
AFIX 0
O1B 3 0.350984 0.289216 0.690556 11.00000 0.04577 0.06456 =
0.04391 -0.00674 0.00072 -0.01256
AFIX 147
H1B 2 0.352776 0.275754 0.730331 11.00000 -1.50000
AFIX 0
C8B 1 0.055022 0.126033 0.731325 11.00000 0.03698 0.05565 =
0.03812 -0.00070 0.00164 -0.00007
C7B 1 0.150862 0.131234 0.699532 11.00000 0.03913 0.05112 =
0.03821 -0.00057 0.00197 -0.00129
C7A 1 0.595866 0.464291 0.577363 11.00000 0.03995 0.05321 =
0.03806 0.00286 -0.00207 -0.00307
C1A 1 0.668990 0.440057 0.638462 11.00000 0.03712 0.04885 =
0.03271 0.00554 -0.00290 -0.00366
C1B 1 0.271318 0.141584 0.662004 11.00000 0.03357 0.04724 =
0.03720 -0.00161 0.00379 -0.00369
C8A 1 0.535289 0.487522 0.528420 11.00000 0.04101 0.05674 =
0.03825 0.00529 -0.00388 -0.00433
C6B 1 0.244417 0.202546 0.591939 11.00000 0.05399 0.06113 =
0.03937 0.00633 0.00268 -0.01335
AFIX 23
H6BA 2 0.325069 0.226105 0.569837 11.00000 -1.20000
H6BB 2 0.195840 0.322206 0.591871 11.00000 -1.20000
AFIX 0
C2A 1 0.806869 0.381232 0.624387 11.00000 0.04152 0.07677 =
0.05334 0.01591 0.00125 0.00590
AFIX 23
H2AA 2 0.806869 0.268548 0.596191 11.00000 -1.20000
H2AB 2 0.849339 0.346281 0.664971 11.00000 -1.20000
AFIX 0
C6A 1 0.665163 0.627286 0.677718 11.00000 0.07353 0.05610 =
0.04377 -0.00287 -0.00478 -0.00293
AFIX 23
H6AA 2 0.576503 0.666216 0.683656 11.00000 -1.20000
H6AB 2 0.702445 0.604832 0.720557 11.00000 -1.20000
AFIX 0
C2B 1 0.339647 -0.052690 0.663222 11.00000 0.04785 0.05564 =
0.07085 0.00577 0.01131 0.00776
AFIX 23
H2BA 2 0.423514 -0.038974 0.643367 11.00000 -1.20000
H2BB 2 0.352351 -0.092677 0.708192 11.00000 -1.20000
AFIX 0
C5B 1 0.169194 0.047997 0.555146 11.00000 0.08479 0.09703 =
0.03957 0.00004 -0.00447 -0.03551
AFIX 23
H5BA 2 0.084237 0.036283 0.573930 11.00000 -1.20000
H5BB 2 0.159152 0.086946 0.509906 11.00000 -1.20000
AFIX 0
C3B 1 0.264779 -0.206573 0.627336 11.00000 0.08274 0.04839 =
0.10652 -0.01401 0.02123 -0.00054
AFIX 23
H3BA 2 0.184876 -0.230967 0.650026 11.00000 -1.20000
H3BB 2 0.313885 -0.325736 0.627015 11.00000 -1.20000
AFIX 0
C3A 1 0.881235 0.544249 0.591649 11.00000 0.04234 0.11994 =
0.08168 0.03522 0.00730 -0.00861
AFIX 23
H3AA 2 0.845971 0.567268 0.548409 11.00000 -1.20000
H3AB 2 0.970324 0.506143 0.586823 11.00000 -1.20000
AFIX 0
C5A 1 0.737821 0.789020 0.644180 11.00000 0.12068 0.05622 =
0.06855 -0.00014 -0.01297 -0.02640
AFIX 23
H5AA 2 0.695858 0.820426 0.603132 11.00000 -1.20000
H5AB 2 0.736769 0.903581 0.671491 11.00000 -1.20000
AFIX 0
C4A 1 0.874233 0.730183 0.631589 11.00000 0.09750 0.11367 =
0.08687 0.02562 -0.02037 -0.06397
AFIX 23
H4AA 2 0.918322 0.711258 0.672939 11.00000 -1.20000
H4AB 2 0.917728 0.833008 0.608294 11.00000 -1.20000
AFIX 0
C4B 1 0.235874 -0.146024 0.557979 11.00000 0.11247 0.09047 =
0.08374 -0.04361 0.02470 -0.03384
AFIX 23
H4BA 2 0.181703 -0.242772 0.537411 11.00000 -1.20000
H4BB 2 0.315449 -0.139078 0.533687 11.00000 -1.20000
AFIX 0
HKLF 4
REM exp_872+b11-23.81-2_a.res in P2/c
REM wR2 = 0.1291, GooF = S = 1.066, Restrained GooF = 1.066 for all data
REM R1 = 0.0444 for 2161 Fo > 4sig(Fo) and 0.0594 for all 2866 data
REM 166 parameters refined using 0 restraints
END
WGHT 0.0565 0.2398
REM Highest difference peak 0.124, deepest hole -0.157, 1-sigma level 0.030
Q1 1 0.2019 0.1190 0.6783 11.00000 0.05 0.12
Q2 1 0.7382 0.4091 0.6247 11.00000 0.05 0.12
Q3 1 0.8959 0.4200 0.5777 11.00000 0.05 0.12
Q4 1 0.3015 0.0400 0.6607 11.00000 0.05 0.12
Q5 1 0.9530 0.5955 0.6190 11.00000 0.05 0.11
;
_shelx_res_checksum 64878
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1A 0.61299(10) 0.28504(18) 0.67530(5) 0.0500(3) Uani d 1 . .
H H1A 0.534651 0.297081 0.675485 0.075 Uiso calc 1 . .
O O1B 0.35098(10) 0.28922(18) 0.69056(5) 0.0514(3) Uani d 1 . .
H H1B 0.352776 0.275754 0.730331 0.077 Uiso calc 1 . .
C C8B 0.05502(14) 0.1260(2) 0.73133(7) 0.0436(4) Uani d 1 . .
C C7B 0.15086(14) 0.1312(2) 0.69953(7) 0.0428(4) Uani d 1 . .
C C7A 0.59587(14) 0.4643(3) 0.57736(7) 0.0438(4) Uani d 1 . .
C C1A 0.66899(13) 0.4401(2) 0.63846(7) 0.0396(4) Uani d 1 . .
C C1B 0.27132(13) 0.1416(2) 0.66200(7) 0.0393(4) Uani d 1 . .
C C8A 0.53529(14) 0.4875(2) 0.52842(7) 0.0454(4) Uani d 1 . .
C C6B 0.24442(16) 0.2025(3) 0.59194(7) 0.0515(4) Uani d 1 . .
H H6BA 0.325069 0.226105 0.569837 0.062 Uiso calc 1 . .
H H6BB 0.195840 0.322206 0.591871 0.062 Uiso calc 1 . .
C C2A 0.80687(15) 0.3812(3) 0.62439(9) 0.0572(5) Uani d 1 . .
H H2AA 0.806869 0.268548 0.596191 0.069 Uiso calc 1 . .
H H2AB 0.849339 0.346281 0.664971 0.069 Uiso calc 1 . .
C C6A 0.66516(19) 0.6273(3) 0.67772(8) 0.0578(5) Uani d 1 . .
H H6AA 0.576503 0.666216 0.683656 0.069 Uiso calc 1 . .
H H6AB 0.702445 0.604832 0.720557 0.069 Uiso calc 1 . .
C C2B 0.33965(16) -0.0527(3) 0.66322(10) 0.0581(5) Uani d 1 . .
H H2BA 0.423514 -0.038974 0.643367 0.070 Uiso calc 1 . .
H H2BB 0.352351 -0.092677 0.708192 0.070 Uiso calc 1 . .
C C5B 0.1692(2) 0.0480(4) 0.55515(9) 0.0738(6) Uani d 1 . .
H H5BA 0.084237 0.036283 0.573930 0.089 Uiso calc 1 . .
H H5BB 0.159152 0.086946 0.509906 0.089 Uiso calc 1 . .
C C3B 0.2648(2) -0.2066(3) 0.62734(12) 0.0791(7) Uani d 1 . .
H H3BA 0.184876 -0.230967 0.650026 0.095 Uiso calc 1 . .
H H3BB 0.313885 -0.325736 0.627015 0.095 Uiso calc 1 . .
C C3A 0.88123(18) 0.5442(4) 0.59165(11) 0.0813(7) Uani d 1 . .
H H3AA 0.845971 0.567268 0.548409 0.098 Uiso calc 1 . .
H H3AB 0.970324 0.506143 0.586823 0.098 Uiso calc 1 . .
C C5A 0.7378(2) 0.7890(3) 0.64418(11) 0.0819(7) Uani d 1 . .
H H5AA 0.695858 0.820426 0.603132 0.098 Uiso calc 1 . .
H H5AB 0.736769 0.903581 0.671491 0.098 Uiso calc 1 . .
C C4A 0.8742(3) 0.7302(4) 0.63159(13) 0.0994(9) Uani d 1 . .
H H4AA 0.918322 0.711258 0.672939 0.119 Uiso calc 1 . .
H H4AB 0.917728 0.833008 0.608294 0.119 Uiso calc 1 . .
C C4B 0.2359(3) -0.1460(4) 0.55798(13) 0.0955(9) Uani d 1 . .
H H4BA 0.181703 -0.242772 0.537411 0.115 Uiso calc 1 . .
H H4BB 0.315449 -0.139078 0.533687 0.115 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
O1A 0.0444(6) 0.0596(7) 0.0460(6) -0.0077(5) -0.0005(5) 0.0128(5)
O1B 0.0458(6) 0.0646(8) 0.0439(6) -0.0126(5) 0.0007(5) -0.0067(6)
C8B 0.0370(7) 0.0557(10) 0.0381(8) -0.0001(7) 0.0016(6) -0.0007(7)
C7B 0.0391(8) 0.0511(9) 0.0382(8) -0.0013(7) 0.0020(6) -0.0006(7)
C7A 0.0400(8) 0.0532(10) 0.0381(8) -0.0031(7) -0.0021(6) 0.0029(7)
C1A 0.0371(7) 0.0488(9) 0.0327(7) -0.0037(6) -0.0029(6) 0.0055(6)
C1B 0.0336(7) 0.0472(9) 0.0372(8) -0.0037(6) 0.0038(6) -0.0016(6)
C8A 0.0410(8) 0.0567(10) 0.0382(8) -0.0043(7) -0.0039(6) 0.0053(7)
C6B 0.0540(9) 0.0611(11) 0.0394(8) -0.0133(8) 0.0027(7) 0.0063(8)
C2A 0.0415(8) 0.0768(13) 0.0533(10) 0.0059(8) 0.0012(7) 0.0159(9)
C6A 0.0735(12) 0.0561(11) 0.0438(9) -0.0029(9) -0.0048(8) -0.0029(8)
C2B 0.0479(9) 0.0556(11) 0.0708(12) 0.0078(8) 0.0113(8) 0.0058(9)
C5B 0.0848(14) 0.0970(17) 0.0396(9) -0.0355(13) -0.0045(9) 0.0000(10)
C3B 0.0827(14) 0.0484(11) 0.1065(19) -0.0005(10) 0.0212(13) -0.0140(12)
C3A 0.0423(10) 0.120(2) 0.0817(14) -0.0086(11) 0.0073(9) 0.0352(15)
C5A 0.121(2) 0.0562(13) 0.0686(13) -0.0264(13) -0.0130(13) -0.0001(10)
C4A 0.0975(19) 0.114(2) 0.0869(17) -0.0640(17) -0.0204(14) 0.0256(16)
C4B 0.112(2) 0.0905(19) 0.0837(17) -0.0338(16) 0.0247(14) -0.0436(15)
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
C1A O1A H1A . . 109.5 ?
C1B O1B H1B . . 109.5 ?
C7B C8B C8B . 2_556 178.17(13) ?
C8B C7B C1B . . 178.07(17) ?
C8A C7A C1A . . 178.52(18) ?
O1A C1A C7A . . 108.79(12) ?
O1A C1A C2A . . 106.62(13) ?
O1A C1A C6A . . 110.19(12) ?
C7A C1A C2A . . 110.74(13) ?
C7A C1A C6A . . 109.69(14) ?
C2A C1A C6A . . 110.76(14) ?
O1B C1B C7B . . 108.22(12) ?
O1B C1B C6B . . 106.85(12) ?
O1B C1B C2B . . 110.61(13) ?
C7B C1B C6B . . 110.61(12) ?
C7B C1B C2B . . 110.33(13) ?
C6B C1B C2B . . 110.15(14) ?
C7A C8A C8A . 3_666 179.4(2) ?
C1B C6B H6BA . . 109.4 ?
C1B C6B H6BB . . 109.4 ?
C1B C6B C5B . . 111.36(15) ?
H6BA C6B H6BB . . 108.0 ?
C5B C6B H6BA . . 109.4 ?
C5B C6B H6BB . . 109.4 ?
C1A C2A H2AA . . 109.3 ?
C1A C2A H2AB . . 109.3 ?
C1A C2A C3A . . 111.56(16) ?
H2AA C2A H2AB . . 108.0 ?
C3A C2A H2AA . . 109.3 ?
C3A C2A H2AB . . 109.3 ?
C1A C6A H6AA . . 109.2 ?
C1A C6A H6AB . . 109.2 ?
H6AA C6A H6AB . . 107.9 ?
C5A C6A C1A . . 111.90(15) ?
C5A C6A H6AA . . 109.2 ?
C5A C6A H6AB . . 109.2 ?
C1B C2B H2BA . . 109.2 ?
C1B C2B H2BB . . 109.2 ?
H2BA C2B H2BB . . 107.9 ?
C3B C2B C1B . . 112.03(15) ?
C3B C2B H2BA . . 109.2 ?
C3B C2B H2BB . . 109.2 ?
C6B C5B H5BA . . 109.3 ?
C6B C5B H5BB . . 109.3 ?
H5BA C5B H5BB . . 107.9 ?
C4B C5B C6B . . 111.67(18) ?
C4B C5B H5BA . . 109.3 ?
C4B C5B H5BB . . 109.3 ?
C2B C3B H3BA . . 109.4 ?
C2B C3B H3BB . . 109.4 ?
C2B C3B C4B . . 111.26(19) ?
H3BA C3B H3BB . . 108.0 ?
C4B C3B H3BA . . 109.4 ?
C4B C3B H3BB . . 109.4 ?
C2A C3A H3AA . . 109.4 ?
C2A C3A H3AB . . 109.4 ?
C2A C3A C4A . . 111.19(18) ?
H3AA C3A H3AB . . 108.0 ?
C4A C3A H3AA . . 109.4 ?
C4A C3A H3AB . . 109.4 ?
C6A C5A H5AA . . 109.5 ?
C6A C5A H5AB . . 109.5 ?
H5AA C5A H5AB . . 108.1 ?
C4A C5A C6A . . 110.6(2) ?
C4A C5A H5AA . . 109.5 ?
C4A C5A H5AB . . 109.5 ?
C3A C4A H4AA . . 109.3 ?
C3A C4A H4AB . . 109.3 ?
C5A C4A C3A . . 111.62(18) ?
C5A C4A H4AA . . 109.3 ?
C5A C4A H4AB . . 109.3 ?
H4AA C4A H4AB . . 108.0 ?
C5B C4B H4BA . . 109.3 ?
C5B C4B H4BB . . 109.3 ?
C3B C4B C5B . . 111.81(18) ?
C3B C4B H4BA . . 109.3 ?
C3B C4B H4BB . . 109.3 ?
H4BA C4B H4BB . . 107.9 ?
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
O1A H1A . 0.8200 ?
O1A C1A . 1.4365(18) ?
O1B H1B . 0.8200 ?
O1B C1B . 1.4379(18) ?
C8B C8B 2_556 1.381(3) ?
C8B C7B . 1.195(2) ?
C7B C1B . 1.4764(19) ?
C7A C1A . 1.4709(19) ?
C7A C8A . 1.192(2) ?
C1A C2A . 1.521(2) ?
C1A C6A . 1.525(2) ?
C1B C6B . 1.520(2) ?
C1B C2B . 1.521(2) ?
C8A C8A 3_666 1.384(3) ?
C6B H6BA . 0.9700 ?
C6B H6BB . 0.9700 ?
C6B C5B . 1.522(3) ?
C2A H2AA . 0.9700 ?
C2A H2AB . 0.9700 ?
C2A C3A . 1.525(3) ?
C6A H6AA . 0.9700 ?
C6A H6AB . 0.9700 ?
C6A C5A . 1.517(3) ?
C2B H2BA . 0.9700 ?
C2B H2BB . 0.9700 ?
C2B C3B . 1.508(3) ?
C5B H5BA . 0.9700 ?
C5B H5BB . 0.9700 ?
C5B C4B . 1.512(4) ?
C3B H3BA . 0.9700 ?
C3B H3BB . 0.9700 ?
C3B C4B . 1.510(4) ?
C3A H3AA . 0.9700 ?
C3A H3AB . 0.9700 ?
C3A C4A . 1.526(4) ?
C5A H5AA . 0.9700 ?
C5A H5AB . 0.9700 ?
C5A C4A . 1.501(4) ?
C4A H4AA . 0.9700 ?
C4A H4AB . 0.9700 ?
C4B H4BA . 0.9700 ?
C4B H4BB . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_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
O1B H1B O1A . . 2_656 0.82 1.96 2.7709(15) 168 yes
O1A H1A O1B ? ? ? 0.82 1.94 2.7481(15) 168 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
O1A C1A C2A C3A . . . . -173.86(15) ?
O1A C1A C6A C5A . . . . 173.01(15) ?
O1B C1B C6B C5B . . . . 175.44(15) ?
O1B C1B C2B C3B . . . . -173.98(14) ?
C7B C1B C6B C5B . . . . -67.0(2) ?
C7B C1B C2B C3B . . . . 66.31(19) ?
C7A C1A C2A C3A . . . . 67.9(2) ?
C7A C1A C6A C5A . . . . -67.3(2) ?
C1A C2A C3A C4A . . . . 54.2(2) ?
C1A C6A C5A C4A . . . . -56.5(2) ?
C1B C6B C5B C4B . . . . -54.8(2) ?
C1B C2B C3B C4B . . . . 55.6(2) ?
C6B C1B C2B C3B . . . . -56.09(19) ?
C6B C5B C4B C3B . . . . 54.0(2) ?
C2A C1A C6A C5A . . . . 55.3(2) ?
C2A C3A C4A C5A . . . . -55.5(3) ?
C6A C1A C2A C3A . . . . -54.0(2) ?
C6A C5A C4A C3A . . . . 56.3(3) ?
C2B C1B C6B C5B . . . . 55.26(19) ?
C2B C3B C4B C5B . . . . -54.2(3) ?
_cod_database_fobs_code 2022778