#------------------------------------------------------------------------------
#$Date: 2019-10-09 07:03:03 +0300 (Wed, 09 Oct 2019) $
#$Revision: 219178 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021794.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_2021794
loop_
_publ_author_name
'Shorunov, Sergey V.'
'Bermeshev, Maxim V.'
'Demchuk, Dmitry V.'
'Nelyubina, Yulia V.'
_publ_section_title
;
Synthesis and structure of 2,4,6-tricyclobutyl-1,3,5-trioxane
;
_journal_coeditor_code KQ2025
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1578
_journal_paper_doi 10.1107/S205698901900896X
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C15 H24 O3'
_chemical_formula_moiety 'C15 H24 O3'
_chemical_formula_sum 'C15 H24 O3'
_chemical_formula_weight 252.34
_chemical_name_systematic
;
2,4,6-Tricyclobutyl-1,3,5-trioxane
;
_space_group_crystal_system hexagonal
_space_group_IT_number 185
_space_group_name_Hall 'P 6c -2'
_space_group_name_H-M_alt 'P 63 c m'
_symmetry_space_group_name_Hall 'P 6c -2'
_symmetry_space_group_name_H-M 'P 63 c m'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2014/6
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 2
_cell_length_a 9.9966(12)
_cell_length_b 9.9966(12)
_cell_length_c 7.9461(10)
_cell_measurement_reflns_used 7859
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 30
_cell_measurement_theta_min 3
_cell_volume 687.68(15)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXL2014/6 (Sheldrick, 2015b)
;
_computing_publication_material
;
SHELXL2014/6 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker APEXII DUO CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0255
_diffrn_reflns_av_unetI/netI 0.0113
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 7859
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.961
_diffrn_reflns_theta_min 2.353
_exptl_absorpt_coefficient_mu 0.083
_exptl_absorpt_correction_T_max 0.7461
_exptl_absorpt_correction_T_min 0.7005
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.219
_exptl_crystal_description prism
_exptl_crystal_F_000 276
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.250
_exptl_crystal_size_min 0.200
_refine_diff_density_max 0.363
_refine_diff_density_min -0.223
_refine_ls_abs_structure_details 'Refined as an inversion twin'
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 35
_refine_ls_number_reflns 671
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.025
_refine_ls_R_factor_all 0.0417
_refine_ls_R_factor_gt 0.0406
_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^)+(0.0819P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1070
_refine_ls_wR_factor_ref 0.1083
_reflns_number_gt 645
_reflns_number_total 671
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file kq2025sup1.cif
_cod_data_source_block Trioxane
_cod_original_cell_volume 687.68(19)
_cod_database_code 2021794
_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 0.976
_shelx_estimated_absorpt_t_max 0.984
_shelx_hkl_file
;
0 1 0 717.83 10.50
-1 0 0 733.33 10.50
0 -1 0 729.33 10.80
0 1 0 774.62 10.60
1 -1 0 744.33 10.50
0 1 0 760.22 10.70
1 0 0 756.02 10.70
-1 1 0 749.13 10.00
-1 1 0 739.83 10.70
-1 0 0 707.73 10.50
1 -2 0 21.70 0.60
2 -1 0 21.90 0.60
-2 1 0 21.80 0.50
-1 2 0 22.60 0.50
1 1 0 22.50 0.70
-1 -1 0 23.00 0.60
-2 1 0 22.10 0.70
-1 -1 0 21.50 0.50
-1 2 0 22.40 0.60
-2 0 0 680.03 9.70
0 2 0 671.03 10.10
0 2 0 670.73 9.20
-2 0 0 665.03 9.10
2 -2 0 674.03 9.60
2 -2 0 678.93 9.90
2 -2 0 681.03 9.80
2 0 0 679.43 10.10
-2 2 0 676.13 9.30
0 -2 0 684.13 9.60
-2 3 0 0.60 0.10
-2 3 0 0.40 0.10
-1 -2 0 1.00 0.10
-3 1 0 0.40 0.20
3 -1 0 0.20 0.10
2 -3 0 0.40 0.20
-1 -2 0 0.50 0.10
1 2 0 0.30 0.20
-3 1 0 0.90 0.20
2 1 0 1.60 0.30
-2 -1 0 0.40 0.10
3 -2 0 0.40 0.10
-3 2 0 0.20 0.20
1 -3 0 0.50 0.10
-3 2 0 0.30 0.10
-1 3 0 0.50 0.10
-1 3 0 0.30 0.10
-2 -1 0 0.50 0.10
-3 3 0 58.89 1.30
3 0 0 59.99 1.60
0 3 0 59.69 1.50
3 -3 0 61.59 1.00
0 3 0 56.09 1.30
0 -3 0 58.39 1.20
-3 0 0 58.19 1.20
-3 0 0 58.69 1.40
3 -3 0 57.79 1.50
-4 1 0 357.16 5.80
-3 4 0 354.06 5.10
-4 1 0 350.36 5.20
3 -4 0 352.66 5.90
1 3 0 355.16 6.10
-1 -3 0 357.36 5.20
4 -1 0 344.97 5.90
-3 4 0 338.37 5.40
-1 -3 0 343.57 5.30
-2 4 0 236.98 3.90
2 2 0 241.08 4.60
-4 2 0 238.28 4.30
4 -2 0 234.48 4.00
-2 -2 0 240.48 3.70
-4 2 0 244.38 3.80
-2 4 0 237.08 3.90
-2 -2 0 242.08 3.70
2 -4 0 238.28 4.10
3 1 0 352.06 6.20
1 -4 0 349.87 5.50
-1 4 0 350.96 5.80
-1 4 0 343.67 5.40
-3 -1 0 354.76 5.20
4 -3 0 356.86 5.40
-4 3 0 358.26 5.40
-3 -1 0 357.16 5.50
-4 4 0 112.99 2.30
-4 0 0 115.79 2.10
0 4 0 113.09 2.60
4 -4 0 116.89 1.80
4 0 0 110.29 2.70
0 4 0 112.49 2.30
0 -4 0 113.09 2.10
4 -4 0 114.39 2.60
-4 0 0 116.69 2.40
1 4 0 -0.10 0.20
-4 5 0 0.30 0.10
-1 -4 0 -0.10 0.10
-4 5 0 0.10 0.20
-5 1 0 -0.10 0.10
4 -5 0 0.20 0.20
-1 -4 0 -0.30 0.10
5 -1 0 0.30 0.20
-5 1 0 0.30 0.20
5 -2 0 533.65 8.70
-3 5 0 528.65 8.20
-5 2 0 556.44 8.00
3 -5 0 539.95 8.60
2 3 0 539.15 9.20
-2 -3 0 549.74 8.00
-2 -3 0 555.74 8.00
-3 5 0 550.94 8.10
-5 2 0 546.65 8.80
-3 -2 0 550.24 8.10
-2 5 0 536.95 8.40
-2 5 0 553.94 8.20
3 2 0 532.75 9.20
-3 -2 0 547.85 7.90
5 -3 0 540.85 8.30
-5 3 0 533.95 8.80
2 -5 0 533.65 8.40
-5 3 0 549.15 8.00
-1 5 0 0.30 0.20
1 -5 0 0.30 0.20
5 -4 0 0.10 0.20
4 1 0 0.20 0.20
-4 -1 0 0.30 0.20
-5 4 0 0.00 0.20
-1 5 0 0.00 0.20
-4 -1 0 0.00 0.10
5 -4 0 0.20 0.10
-5 5 0 112.39 2.50
0 5 0 108.99 2.40
0 5 0 111.99 2.80
5 0 0 108.99 2.80
5 -5 0 107.09 2.80
-5 0 0 110.59 2.50
-5 0 0 116.39 2.20
5 -5 0 110.39 1.80
0 -5 0 109.19 2.10
5 -6 0 31.80 0.70
-1 -5 0 33.70 1.20
-6 1 0 32.40 1.10
-5 6 0 30.20 1.20
6 -1 0 31.50 1.40
-6 1 0 30.30 1.30
-1 -5 0 32.00 0.90
5 -6 0 32.50 1.40
1 5 0 29.00 1.40
2 4 0 41.60 1.70
6 -2 0 43.40 1.50
-2 -4 0 43.50 1.30
-4 6 0 42.90 1.50
-6 2 0 42.50 1.30
-6 2 0 45.50 1.60
-4 6 0 42.80 0.90
4 -6 0 43.30 1.60
-2 -4 0 44.60 1.10
-3 -3 0 482.35 7.20
6 -3 0 466.45 7.70
-3 -3 0 484.75 7.20
-6 3 0 468.45 8.20
-3 6 0 476.55 7.50
-6 3 0 494.35 7.40
3 -6 0 474.25 7.80
-3 6 0 478.25 7.40
3 3 0 467.25 8.50
2 -6 0 43.80 1.40
-6 4 0 43.80 1.40
6 -4 0 42.70 1.20
-2 6 0 43.70 1.40
-4 -2 0 45.00 1.30
-4 -2 0 45.60 1.20
-2 6 0 43.80 1.40
6 -4 0 43.60 1.70
4 2 0 44.90 1.80
5 1 0 32.20 1.50
-5 -1 0 28.60 1.10
-5 -1 0 31.60 1.00
1 -6 0 29.10 1.00
-6 5 0 29.70 1.20
6 -5 0 30.40 0.80
-1 6 0 30.00 1.20
-1 6 0 30.90 1.30
6 -5 0 30.90 1.40
6 -6 0 287.57 5.80
0 6 0 300.67 5.80
-6 0 0 300.57 4.90
6 0 0 287.77 5.90
0 6 0 295.97 5.10
0 -6 0 292.47 4.90
-6 0 0 301.47 5.40
-6 6 0 299.27 5.30
-1 -6 0 110.29 2.20
-7 1 0 102.99 2.80
-6 7 0 108.29 2.70
7 -1 0 100.19 3.00
1 6 0 102.49 3.10
-7 1 0 104.89 2.40
6 -7 0 103.29 2.90
-1 -6 0 106.69 2.50
-5 7 0 23.70 0.60
-5 7 0 23.90 1.20
5 -7 0 25.80 1.30
-2 -5 0 24.60 0.80
7 -2 0 26.30 1.30
-7 2 0 24.30 1.00
-7 2 0 24.40 1.30
2 5 0 22.80 1.40
-2 -5 0 27.30 1.10
4 -7 0 17.20 1.00
-7 3 0 17.60 1.10
-4 7 0 19.40 0.70
-7 3 0 18.30 0.90
-3 -4 0 19.10 0.90
3 4 0 19.00 1.30
-4 7 0 18.80 1.00
-3 -4 0 18.10 0.70
7 -3 0 17.30 1.00
-3 7 0 19.40 1.00
-7 4 0 19.00 1.00
3 -7 0 17.30 0.90
-3 7 0 18.90 0.80
-4 -3 0 18.40 0.80
7 -4 0 18.60 0.90
-4 -3 0 18.70 0.90
4 3 0 17.00 1.20
-5 -2 0 25.40 1.00
-2 7 0 27.10 1.10
7 -5 0 25.20 1.40
-5 -2 0 24.30 1.00
5 2 0 24.40 1.50
-7 5 0 22.50 1.10
7 -5 0 24.60 0.90
2 -7 0 23.70 1.00
-2 7 0 26.60 1.20
7 -6 0 106.49 3.10
1 -7 0 107.79 2.40
-7 6 0 107.59 2.70
-1 7 0 106.39 2.60
-6 -1 0 108.19 2.40
6 1 0 105.79 3.20
-1 7 0 105.29 2.80
-6 -1 0 104.79 2.60
7 0 0 962.60 16.00
0 7 0 944.21 15.60
0 7 0 971.30 14.20
-7 7 0 969.70 14.50
7 -7 0 948.61 15.50
-7 0 0 971.90 15.00
0 -7 0 959.70 14.20
-7 0 0 993.00 13.90
-1 -7 0 107.19 2.70
-1 -7 0 101.49 2.20
7 -8 0 102.49 3.10
-7 8 0 100.19 2.80
1 7 0 102.19 3.20
-8 1 0 102.39 2.50
8 -1 0 100.49 3.20
-8 1 0 103.29 2.90
-8 2 0 54.69 1.70
2 6 0 58.29 2.40
8 -2 0 53.49 2.10
-2 -6 0 55.19 1.80
-2 -6 0 53.29 1.40
-6 8 0 55.99 2.00
-8 2 0 54.19 2.10
6 -8 0 57.19 2.10
-8 3 0 2.60 0.50
3 5 0 2.80 0.70
-3 -5 0 3.20 0.50
-5 8 0 2.80 0.60
8 -3 0 2.70 0.50
-5 8 0 3.20 0.30
-3 -5 0 4.00 0.40
-8 3 0 2.60 0.60
5 -8 0 3.00 0.60
-4 -4 0 70.59 1.90
-4 8 0 69.69 1.70
4 -8 0 67.29 2.10
4 4 0 65.89 2.60
-4 -4 0 73.69 1.70
8 -4 0 69.59 2.00
-4 8 0 66.49 2.10
-8 4 0 69.79 2.00
3 -8 0 2.30 0.50
5 3 0 3.50 0.70
-8 5 0 2.30 0.50
-3 8 0 3.40 0.50
-5 -3 0 2.40 0.40
-3 8 0 3.10 0.60
-5 -3 0 2.50 0.40
8 -5 0 3.00 0.60
8 -5 0 2.70 0.40
-2 8 0 54.49 1.80
8 -6 0 54.39 2.20
-2 8 0 54.49 1.90
6 2 0 57.39 2.40
-6 -2 0 54.19 1.60
-8 6 0 55.19 1.90
8 -6 0 59.39 1.80
2 -8 0 55.49 1.70
-6 -2 0 53.99 1.70
-7 -1 0 98.99 2.70
-8 7 0 101.79 2.80
1 -8 0 99.39 2.30
-7 -1 0 102.99 2.40
7 1 0 103.79 3.40
-1 8 0 100.19 2.90
-1 8 0 102.09 2.70
8 -7 0 98.59 3.20
0 -8 0 286.37 5.00
8 -8 0 284.57 6.20
-8 8 0 288.67 5.70
-8 0 0 290.57 5.10
-8 0 0 285.17 5.70
8 0 0 285.07 6.40
0 8 0 288.67 6.10
-8 9 0 4.90 0.80
1 8 0 3.90 0.80
9 -1 0 4.00 0.90
8 -9 0 3.50 0.80
-9 1 0 4.70 0.80
-1 -8 0 4.90 0.70
-9 1 0 5.50 0.70
-2 -7 0 14.20 1.00
-9 2 0 16.60 1.20
2 7 0 14.00 1.30
-2 -7 0 14.30 1.10
-7 9 0 15.90 1.20
-9 2 0 14.20 1.00
7 -9 0 13.80 1.20
9 -2 0 16.20 1.30
3 6 0 8.10 1.10
-6 9 0 8.80 1.00
-3 -6 0 7.50 0.60
-9 3 0 7.40 1.00
-3 -6 0 6.60 0.80
-9 3 0 6.90 0.80
6 -9 0 8.40 1.00
9 -3 0 8.50 1.00
-4 -5 0 146.59 3.20
-4 -5 0 142.59 2.80
9 -4 0 138.49 3.90
9 -4 0 139.59 3.40
4 5 0 134.99 4.20
-5 9 0 141.29 3.50
-9 4 0 142.89 3.30
5 -9 0 143.69 3.60
-5 9 0 143.09 2.60
-9 5 0 145.39 3.40
5 4 0 148.49 4.30
-4 9 0 140.09 3.50
-5 -4 0 145.49 3.10
9 -5 0 139.19 3.10
4 -9 0 136.39 3.40
9 -5 0 139.09 3.90
-5 -4 0 142.09 2.90
-4 9 0 141.39 2.90
-3 9 0 7.40 0.70
9 -6 0 5.30 0.90
-9 6 0 6.70 0.80
3 -9 0 7.80 0.70
-6 -3 0 8.50 0.80
6 3 0 6.70 1.00
-6 -3 0 6.80 0.60
-3 9 0 8.00 0.90
2 -9 0 14.40 0.90
-2 9 0 14.10 1.10
-2 9 0 14.90 1.00
-7 -2 0 15.70 1.00
7 2 0 13.60 1.40
-7 -2 0 16.00 1.00
-9 7 0 15.10 1.10
9 -7 0 15.40 1.40
-8 -1 0 5.90 0.80
9 -8 0 5.30 0.90
8 1 0 7.40 1.10
-8 -1 0 4.30 0.60
-9 8 0 3.00 0.60
1 -9 0 4.50 0.60
-1 9 0 4.10 0.70
-1 9 0 4.30 0.70
-9 0 0 88.59 2.80
0 9 0 95.19 3.10
-9 9 0 89.29 2.90
0 -9 0 87.59 2.70
-9 0 0 87.79 2.50
9 0 0 95.59 3.40
9 -9 0 85.39 3.20
-9 10 0 3.90 0.80
1 9 0 3.10 0.80
-10 1 0 3.80 0.70
10 -1 0 3.40 0.90
9 -10 0 4.90 0.90
-10 1 0 4.10 0.80
-1 -9 0 3.60 0.70
-2 -8 0 14.70 1.10
2 8 0 11.70 1.30
8 -10 0 10.70 1.20
10 -2 0 13.40 1.30
-8 10 0 13.10 1.20
-10 2 0 11.20 1.00
-10 2 0 10.40 1.20
3 7 0 0.10 0.50
-3 -7 0 0.70 0.40
-7 10 0 -0.30 0.40
10 -3 0 0.40 0.50
-10 3 0 1.10 0.50
7 -10 0 0.20 0.40
6 -10 0 15.50 1.20
-4 -6 0 16.10 1.10
10 -4 0 15.70 1.20
4 6 0 16.30 1.50
10 -4 0 14.80 1.30
-10 4 0 16.60 1.10
-6 10 0 16.40 1.20
-5 10 0 56.09 2.20
-5 -5 0 50.49 1.80
5 -10 0 54.29 2.10
-10 5 0 51.29 2.00
5 5 0 53.99 2.70
10 -5 0 51.59 2.40
4 -10 0 14.70 1.10
-4 10 0 17.50 1.30
-6 -4 0 17.20 1.10
6 4 0 16.00 1.50
-10 6 0 15.90 1.20
-4 10 0 17.50 1.00
10 -6 0 19.70 1.60
-10 7 0 0.70 0.50
10 -7 0 0.50 0.50
7 3 0 0.10 0.60
-3 10 0 0.40 0.40
-7 -3 0 0.10 0.30
3 -10 0 0.20 0.30
-3 10 0 0.20 0.40
-2 10 0 12.90 1.10
10 -8 0 11.60 1.40
8 2 0 10.50 1.40
-8 -2 0 15.10 1.60
-2 10 0 11.80 1.10
-8 -2 0 10.10 0.90
2 -10 0 12.00 0.90
-10 8 0 11.70 1.20
-1 10 0 3.70 0.80
-10 9 0 4.50 0.90
10 -9 0 4.90 1.00
9 1 0 3.30 0.90
-1 10 0 3.90 0.80
-9 -1 0 4.30 0.80
-9 -1 0 4.90 0.70
0 10 0 17.30 1.50
10 0 0 15.70 1.60
10 -10 0 16.40 1.60
-10 0 0 18.40 1.40
-10 10 0 16.10 1.40
0 -10 0 16.60 1.30
-10 0 0 16.10 1.20
1 10 0 16.20 1.60
11 -1 0 18.90 1.70
-1 -10 0 17.60 1.40
10 -11 0 17.30 1.60
-10 11 0 17.90 1.50
-11 1 0 18.20 1.30
-2 -9 0 49.30 2.10
11 -2 0 50.69 2.50
-11 2 0 52.09 2.00
-9 11 0 53.49 2.40
2 9 0 49.00 2.60
11 -2 0 51.49 2.40
9 -11 0 50.49 2.50
-11 3 0 0.80 0.50
11 -3 0 -0.60 0.50
11 -3 0 -0.30 0.50
-3 -8 0 -0.20 0.40
-8 11 0 0.40 0.50
8 -11 0 0.00 0.50
3 8 0 0.20 0.60
-7 11 0 9.10 1.20
-11 4 0 10.10 1.10
-4 -7 0 9.40 1.00
7 -11 0 11.30 1.30
4 7 0 9.60 1.40
11 -4 0 12.10 1.20
11 -4 0 9.00 1.20
11 -5 0 0.20 0.60
6 -11 0 0.70 0.50
-11 5 0 -0.20 0.40
5 6 0 0.20 0.60
-5 -6 0 -0.40 0.40
-6 11 0 0.30 0.50
-6 -5 0 0.60 0.40
11 -6 0 0.60 0.60
6 5 0 0.90 0.60
5 -11 0 -0.10 0.40
-5 11 0 0.80 0.50
-11 6 0 -0.30 0.40
4 -11 0 10.60 1.00
11 -7 0 10.40 1.40
-11 7 0 9.20 1.10
-7 -4 0 9.80 1.00
7 4 0 10.50 1.40
-4 11 0 8.90 1.10
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7 -2 -9 2.70 0.90
2 5 -9 2.40 1.00
5 -7 9 0.30 0.70
7 -2 9 2.30 0.70
-5 7 9 1.80 0.80
-2 -5 9 1.90 0.90
-7 2 9 1.50 0.90
2 5 9 2.20 0.80
-7 3 -9 1.80 0.70
7 -3 -9 2.50 0.90
-3 -4 -9 2.00 0.70
3 4 -9 1.90 1.00
3 4 9 1.90 0.80
-7 3 9 1.10 0.90
4 -7 9 1.50 0.90
-3 -4 9 2.50 0.90
-4 7 9 1.60 0.80
4 3 -9 2.40 1.00
7 -4 -9 1.60 0.80
-7 4 -9 2.90 0.70
-4 -3 -9 0.80 0.50
7 -4 9 1.70 0.80
3 -7 9 2.40 1.00
-3 7 9 2.30 0.80
-7 4 9 1.50 0.90
4 3 9 2.40 0.80
-4 -3 9 3.00 1.00
-5 -2 -9 1.30 0.60
7 -5 -9 2.10 0.80
2 -7 -9 2.30 0.80
-2 7 -9 2.30 0.80
5 2 -9 1.60 0.90
-7 5 -9 2.60 0.70
2 -7 9 2.00 0.90
5 2 9 2.10 0.80
7 -5 9 3.50 0.90
-7 5 9 2.40 1.00
-5 -2 9 2.30 0.90
-2 7 9 3.40 0.90
-6 -1 -9 5.70 1.00
7 -6 -9 3.00 0.80
-1 7 -9 5.90 1.20
6 1 -9 6.90 1.50
1 -7 -9 5.40 0.90
-7 6 -9 6.10 1.00
6 1 9 5.10 1.00
-1 7 9 4.70 1.00
1 -7 9 4.70 1.10
-6 -1 9 4.10 1.10
7 -6 9 5.60 1.10
-7 6 9 5.20 1.30
0 7 -9 0.50 0.70
7 0 -9 0.60 0.80
0 -7 -9 -0.60 0.50
7 -7 -9 0.40 0.50
-7 0 -9 -0.40 0.50
-7 7 -9 0.00 0.50
-7 7 9 0.40 0.80
7 0 9 0.20 0.60
0 -7 9 -1.80 0.60
-7 0 9 -1.40 0.70
7 -7 9 -0.50 0.70
0 7 9 0.40 0.60
-8 2 -9 2.20 0.80
-2 -6 -9 2.50 0.80
2 6 -9 4.50 1.30
6 -8 -9 2.50 0.80
8 -2 -9 2.00 0.90
6 -8 9 3.00 1.00
-8 2 9 1.90 1.00
2 6 9 2.50 0.90
-2 -6 9 0.90 0.90
-3 -5 -9 1.90 0.60
8 -3 -9 1.50 0.80
3 5 -9 0.60 0.80
-8 3 -9 1.60 0.70
-8 3 9 0.50 0.90
5 -8 9 2.00 0.90
3 5 9 2.00 0.90
-3 -5 9 1.10 0.90
-8 4 -9 5.90 1.00
-4 -4 -9 6.60 1.00
8 -4 -9 6.20 1.30
4 4 -9 5.40 1.40
-4 8 9 6.10 1.20
4 -8 9 3.40 1.10
-8 4 9 7.70 1.50
-4 -4 9 5.00 1.20
4 4 9 5.10 1.10
-8 5 -9 1.50 0.70
8 -5 -9 0.90 0.70
-5 -3 -9 1.70 0.70
5 3 -9 0.70 0.90
-3 8 9 1.90 0.80
8 -5 9 0.50 0.80
-5 -3 9 1.90 1.00
3 -8 9 -0.30 0.80
-8 5 9 1.60 1.00
5 3 9 1.70 0.80
6 2 -9 2.50 1.10
2 -8 -9 1.60 0.70
8 -6 -9 3.00 0.90
-6 -2 -9 2.20 0.70
-8 6 -9 2.60 0.80
-2 8 9 2.30 0.90
2 -8 9 2.40 0.90
-8 6 9 2.00 1.00
8 -6 9 2.80 1.00
-6 -2 9 2.40 1.00
6 2 9 0.60 0.70
0 0 -10 28.60 1.80
0 0 10 29.70 1.90
0 1 -10 8.30 1.20
1 0 -10 10.30 1.30
-1 0 -10 9.50 1.20
1 -1 -10 9.80 1.30
0 -1 -10 9.20 1.20
-1 1 -10 12.60 1.20
1 -1 10 8.10 1.20
-1 1 10 11.50 1.40
1 0 10 10.00 1.20
0 -1 10 10.40 1.30
-1 0 10 10.10 1.30
0 1 10 8.60 1.20
-1 2 -10 0.80 0.50
1 1 -10 1.50 0.70
-2 1 -10 0.80 0.50
1 -2 -10 0.20 0.50
2 -1 -10 1.40 0.70
-2 1 10 2.00 0.80
-1 2 10 1.30 0.70
1 -2 10 0.80 0.70
1 1 10 0.80 0.70
-1 -1 10 2.40 0.90
2 -1 10 0.80 0.70
2 -2 -10 7.30 1.10
2 0 -10 6.10 1.20
-2 2 -10 4.90 0.90
0 2 -10 7.10 1.20
0 -2 10 6.10 1.10
-2 0 10 6.50 1.20
-2 2 10 7.90 1.20
0 2 10 7.50 1.10
2 -2 10 6.10 1.10
2 0 10 5.90 1.00
1 2 -10 3.00 0.90
2 -3 -10 1.20 0.60
3 -1 -10 2.20 0.80
-3 1 -10 1.40 0.60
-2 3 -10 1.50 0.60
2 -3 10 0.20 0.70
-2 3 10 1.80 0.80
-3 1 10 0.50 0.70
-1 -2 10 1.20 0.70
1 2 10 1.30 0.80
3 -1 10 1.90 0.70
-3 2 -10 1.70 0.60
-1 3 -10 2.40 0.70
2 1 -10 2.20 0.80
3 -2 -10 2.10 0.70
-1 3 10 1.80 0.80
2 1 10 0.80 0.70
3 -2 10 -0.40 0.70
1 -3 10 2.20 0.90
-2 -1 10 0.70 0.80
-3 2 10 2.40 0.80
0 3 -10 4.70 1.00
3 0 -10 4.90 1.10
-3 3 -10 4.30 0.80
3 -3 -10 5.10 1.00
0 -3 10 2.70 0.90
0 3 10 5.70 1.10
-3 0 10 5.30 1.20
-3 3 10 6.40 1.10
3 0 10 4.70 0.90
3 -3 10 3.60 0.90
1 3 -10 3.00 0.90
-4 1 -10 2.10 0.80
3 -4 -10 4.00 0.90
4 -1 -10 3.40 1.00
-3 4 -10 1.80 0.70
3 -4 10 2.70 0.90
-4 1 10 2.60 0.90
4 -1 10 2.50 0.80
-3 4 10 3.00 0.90
1 3 10 1.90 0.80
-1 -3 10 4.30 1.10
2 -4 -10 4.90 1.00
4 -2 -10 4.80 1.00
-4 2 -10 4.90 0.90
-2 4 -10 3.70 0.90
2 2 -10 3.60 1.00
2 2 10 4.20 1.00
-4 2 10 4.10 1.10
2 -4 10 3.80 1.00
-2 -2 10 3.30 1.00
4 -2 10 3.30 0.90
4 -3 -10 1.30 0.70
-1 4 -10 2.70 0.80
-3 -1 -10 1.80 0.70
3 1 -10 3.90 1.10
-4 3 -10 2.10 0.60
1 -4 10 0.80 0.90
-1 4 10 3.10 0.90
-4 3 10 4.00 1.00
3 1 10 1.80 0.80
4 -3 10 1.10 0.70
-3 -1 10 3.50 1.00
0 4 -10 2.80 0.90
-4 4 -10 5.40 0.90
4 0 -10 3.40 1.00
4 -4 -10 4.60 1.00
-4 0 -10 4.30 0.80
4 0 10 1.80 0.80
0 -4 10 3.90 1.10
4 -4 10 3.70 1.00
0 4 10 3.80 0.90
-4 4 10 4.10 1.00
-4 0 10 3.10 1.00
4 -5 -10 2.80 0.90
-5 1 -10 2.80 0.70
5 -1 -10 4.70 1.30
1 4 -10 3.20 1.00
1 4 10 2.90 0.90
-1 -4 10 2.80 1.00
4 -5 10 3.30 1.00
-4 5 10 3.80 1.00
5 -1 10 2.80 0.80
-5 1 10 4.20 1.10
-2 -3 -10 2.40 0.70
2 3 -10 3.00 1.00
3 -5 -10 2.70 0.80
-5 2 -10 3.60 0.80
-3 5 -10 3.20 0.80
5 -2 -10 1.60 0.90
3 -5 10 3.20 1.00
2 3 10 3.90 1.00
-5 2 10 3.00 1.00
-2 -3 10 3.40 1.10
-3 -2 -10 2.50 0.70
-5 3 -10 2.00 0.60
3 2 -10 0.90 0.80
-2 5 -10 3.10 0.90
5 -3 -10 3.00 0.90
2 -5 10 3.90 1.10
-2 5 10 2.40 0.90
-5 3 10 2.60 0.90
-3 -2 10 3.10 1.00
5 -3 10 3.10 0.90
3 2 10 3.20 0.90
4 1 -10 4.10 1.20
-4 -1 -10 1.60 0.60
-1 5 -10 4.70 1.10
5 -4 -10 2.50 0.90
1 -5 10 2.20 1.00
-5 4 10 3.40 1.00
-4 -1 10 3.00 1.10
4 1 10 2.20 0.80
5 -4 10 3.00 0.90
-1 5 10 3.90 1.00
0 5 -10 2.00 0.90
5 -5 -10 2.60 0.80
5 0 -10 5.20 1.30
-5 0 -10 2.70 0.70
5 -5 10 3.10 1.00
-5 0 10 1.30 0.90
-5 5 10 3.10 1.10
0 -5 10 1.90 0.90
0 5 10 3.40 1.00
5 0 10 1.70 0.80
-6 1 -10 0.70 0.60
-1 -5 -10 1.10 0.60
5 -6 -10 1.50 0.70
1 5 -10 1.00 0.80
6 -1 -10 0.80 0.80
1 5 10 -0.40 0.70
-6 1 10 1.60 1.00
5 -6 10 0.70 0.90
-5 6 10 0.30 0.80
-1 -5 10 0.30 0.90
6 -1 10 0.60 0.70
4 -6 -10 13.60 1.60
2 4 -10 14.20 1.90
-6 2 -10 13.50 1.40
-2 -4 -10 12.80 1.20
6 -2 -10 16.80 2.10
-2 -4 10 12.50 1.70
-6 2 10 14.80 1.80
4 -6 10 13.70 1.60
2 4 10 11.40 1.40
6 -2 10 17.00 1.50
3 3 -10 4.70 1.30
6 -3 -10 3.80 1.10
-6 3 -10 5.70 1.00
-3 -3 -10 5.00 0.90
-3 -3 10 5.20 1.20
3 -6 10 4.10 1.10
-3 6 10 3.60 0.90
-6 3 10 2.60 1.00
3 3 10 4.50 1.00
-6 4 -10 14.00 1.50
4 2 -10 16.00 2.10
6 -4 -10 15.00 1.90
-2 6 -10 13.20 1.70
-4 -2 -10 11.50 1.20
2 -6 10 16.10 1.70
4 2 10 12.10 1.40
-2 6 10 11.20 1.40
-6 4 10 11.80 1.70
-4 -2 10 10.80 1.60
6 -4 10 13.00 1.50
5 1 -10 1.70 0.90
-5 -1 -10 1.20 0.60
6 -5 -10 0.60 0.70
-1 6 -10 1.10 0.80
-1 6 10 -0.30 0.60
1 -6 10 0.80 0.80
6 -5 10 0.90 0.80
-6 5 10 0.40 0.90
-5 -1 10 1.00 0.80
5 1 10 0.70 0.70
0 0 -11 -0.40 0.50
0 0 11 -0.20 0.70
0 1 -11 -0.10 0.50
-1 1 -11 -0.10 0.50
1 0 -11 0.50 0.60
0 -1 -11 0.20 0.50
-1 0 -11 -0.20 0.50
1 -1 -11 -0.30 0.50
1 0 11 -0.90 0.60
0 -1 11 0.00 0.80
0 1 11 0.30 0.70
1 -1 11 0.30 0.80
-1 1 11 0.40 0.70
-1 0 11 -0.40 0.70
1 -2 -11 8.80 1.30
2 -1 -11 9.40 1.50
1 1 -11 9.80 1.50
-1 2 -11 8.60 1.30
-1 -1 -11 8.30 1.30
-2 1 -11 9.30 1.30
-1 2 11 5.90 1.20
-1 -1 11 9.60 1.40
-2 1 11 10.10 1.40
2 -1 11 8.60 1.30
1 -2 11 8.50 1.40
2 -2 -11 0.10 0.60
-2 0 -11 0.20 0.50
2 0 -11 -0.50 0.50
0 2 -11 0.00 0.60
-2 2 -11 0.10 0.50
0 -2 -11 -0.30 0.50
0 -2 11 -0.40 0.70
2 -2 11 0.00 0.80
-2 2 11 -0.30 0.70
-2 0 11 0.50 0.80
2 -3 -11 2.80 0.90
-2 3 -11 3.60 0.90
3 -1 -11 2.80 1.00
1 2 -11 2.80 1.00
-3 1 11 2.00 1.00
2 -3 11 2.30 1.00
-2 3 11 2.60 1.00
-1 -2 11 0.30 0.90
2 1 -11 2.30 0.90
-3 2 -11 1.90 0.70
-1 3 -11 3.90 1.00
1 -3 -11 2.70 0.90
3 -2 -11 2.80 1.00
-3 2 11 1.90 0.90
3 -2 11 1.60 0.90
1 -3 11 1.20 0.90
-2 -1 11 3.60 1.10
;
_shelx_hkl_checksum 89775
_shelx_res_file
;
TITL a_a.res in P6(3)cm
CELL 0.71073 9.9966 9.9966 7.9461 90.000 90.000 120.000
ZERR 2.000 0.0012 0.0012 0.0010 0.000 0.000 0.000
LATT -1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, 1/2+Z
SYMM Y, -X+Y, 1/2+Z
SYMM X-Y, X, 1/2+Z
SYMM -Y, -X, 1/2+Z
SYMM -X+Y, Y, 1/2+Z
SYMM X, X-Y, 1/2+Z
SYMM Y, X, Z
SYMM X-Y, -Y, Z
SYMM -X, -X+Y, Z
SFAC C H O
UNIT 30 48 6
TEMP -153.000
size 0.20 0.25 0.30
L.S. 10
acta
BOND $H
htab
conf
omit -4 58
FMAP 2
PLAN 20
WGHT 0.081900 0.114800
FVAR 0.63200
O1 3 0.000000 0.134667 0.477370 10.50000 0.01007 0.01218 =
0.01699 0.00171 0.00000 0.00503
C1 1 0.134824 0.134824 0.535092 10.50000 0.01126 0.01126 =
0.01353 -0.00162 -0.00162 0.00566
AFIX 13
H1A 2 0.138407 0.138407 0.660859 10.50000 -1.20000
AFIX 0
C2 1 0.274517 0.274517 0.464533 10.50000 0.01232 0.01232 =
0.01928 0.00024 0.00024 0.00557
AFIX 13
H2A 2 0.271606 0.271605 0.338739 10.50000 -1.20000
AFIX 0
C3 1 0.435218 0.310602 0.528115 11.00000 0.01184 0.01416 =
0.03387 -0.00080 -0.00216 0.00684
AFIX 23
H3A 2 0.493819 0.285175 0.446226 11.00000 -1.20000
H3B 2 0.433425 0.266688 0.640319 11.00000 -1.20000
AFIX 0
C4 1 0.483872 0.483872 0.531863 10.50000 0.01236 0.01236 =
0.03035 -0.00143 -0.00143 0.00437
AFIX 23
H4A 2 0.542047 0.542046 0.431036 10.50000 -1.20000
H4B 2 0.537662 0.537662 0.636473 10.50000 -1.20000
AFIX 0
HKLF 4
REM a_a.res in P6(3)cm
REM R1 = 0.0406 for 645 Fo > 4sig(Fo) and 0.0417 for all 671 data
REM 34 parameters refined using 0 restraints
END
WGHT 0.0749 0.0983
REM Instructions for potential hydrogen bonds
EQIV $1 y, -x+y, z+1/2
HTAB C1 O1_$1
REM Highest difference peak 0.363, deepest hole -0.223, 1-sigma level 0.054
Q1 1 0.0000 0.1401 0.5893 10.50000 0.05 0.36
Q2 1 0.0000 0.1289 0.3552 10.50000 0.05 0.21
Q3 1 0.2735 0.2735 0.6018 10.50000 0.05 0.21
Q4 1 0.2124 0.2124 0.5036 10.50000 0.05 0.20
Q5 1 0.4772 0.4317 0.5280 11.00000 0.05 0.19
Q6 1 0.3577 0.2774 0.5026 11.00000 0.05 0.17
Q7 1 0.1552 0.1552 0.4121 10.50000 0.05 0.16
Q8 1 0.0699 0.1332 0.5075 11.00000 0.05 0.14
Q9 1 0.7034 0.7034 0.4147 10.50000 0.05 0.13
Q10 1 0.4175 0.2845 0.3918 11.00000 0.05 0.13
Q11 1 0.2341 0.2341 0.8119 10.50000 0.05 0.10
Q12 1 0.4803 0.2696 0.5195 11.00000 0.05 0.10
Q13 1 0.5382 0.5382 0.5035 10.50000 0.05 0.10
Q14 1 0.5577 0.5577 0.3520 10.50000 0.05 0.10
Q15 1 0.4011 0.2980 0.6947 11.00000 0.05 0.09
Q16 1 0.1381 0.0000 0.7107 10.50000 0.05 0.09
Q17 1 0.2494 0.1939 0.2712 11.00000 0.05 0.09
Q18 1 0.5425 0.2990 0.2993 11.00000 0.05 0.09
Q19 1 0.1090 0.1801 0.7627 11.00000 0.05 0.08
Q20 1 0.3168 0.2544 0.7035 11.00000 0.05 0.08
;
_shelx_res_checksum 95057
_shelxl_version_number 2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
O O1 0.0000 0.13467(13) 0.4774(2) 0.0133(4) Uani d 1
C C1 0.13482(17) 0.13482(17) 0.5351(3) 0.0120(5) Uani d 1
H H1A 0.1384 0.1384 0.6609 0.014 Uiso calc 1
C C2 0.2745(2) 0.2745(2) 0.4645(3) 0.0149(4) Uani d 1
H H2A 0.2716 0.2716 0.3387 0.018 Uiso calc 1
C C3 0.43522(17) 0.31060(18) 0.5281(3) 0.0198(4) Uani d 1
H H3A 0.4938 0.2852 0.4462 0.024 Uiso calc 1
H H3B 0.4334 0.2667 0.6403 0.024 Uiso calc 1
C C4 0.4839(2) 0.4839(2) 0.5319(4) 0.0192(5) Uani d 1
H H4A 0.5420 0.5420 0.4310 0.023 Uiso calc 1
H H4B 0.5377 0.5377 0.6365 0.023 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
O1 0.0101(7) 0.0122(6) 0.0170(7) 0.0050(3) 0.000 0.0017(5)
C1 0.0113(7) 0.0113(7) 0.0135(9) 0.0057(6) -0.0016(7) -0.0016(7)
C2 0.0123(7) 0.0123(7) 0.0193(8) 0.0056(7) 0.0002(7) 0.0002(7)
C3 0.0118(6) 0.0142(7) 0.0339(8) 0.0068(6) -0.0022(7) -0.0008(8)
C4 0.0124(7) 0.0124(7) 0.0304(9) 0.0044(7) -0.0014(10) -0.0014(10)
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
C1 O1 C1 . 2 110.23(18) y
O1 C1 O1 3 . 110.03(17) y
O1 C1 C2 3 . 108.66(11) ?
O1 C1 C2 . . 108.66(11) ?
O1 C1 H1A 3 . 109.8 ?
O1 C1 H1A . . 109.8 ?
C2 C1 H1A . . 109.8 ?
C1 C2 C3 . . 117.97(13) ?
C1 C2 C3 . 10 117.97(13) ?
C3 C2 C3 . 10 88.59(16) y
C1 C2 H2A . . 110.2 ?
C3 C2 H2A . . 110.2 ?
C3 C2 H2A 10 . 110.2 ?
C2 C3 C4 . . 88.62(11) y
C2 C3 H3A . . 113.9 ?
C4 C3 H3A . . 113.9 ?
C2 C3 H3B . . 113.9 ?
C4 C3 H3B . . 113.9 ?
H3A C3 H3B . . 111.1 ?
C3 C4 C3 . 10 88.39(15) ?
C3 C4 H4A . . 113.9 ?
C3 C4 H4A 10 . 113.9 ?
C3 C4 H4B . . 113.9 ?
C3 C4 H4B 10 . 113.9 ?
H4A C4 H4B . . 111.1 ?
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 C1 . 1.4229(13) y
O1 C1 2 1.4230(13) ?
C1 O1 3 1.4229(13) n
C1 C2 . 1.505(3) y
C1 H1A . 1.0000 ?
C2 C3 . 1.545(2) y
C2 C3 10 1.545(2) ?
C2 H2A . 1.0000 ?
C3 C4 . 1.548(2) y
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C3 10 1.548(2) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
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
C1 H1A O1 5 1.00 2.52 3.514(3) 177.1
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_4
_geom_torsion
C1 O1 C1 O1 2 3 58.4(3)
C1 O1 C1 C2 2 . 177.20(10)
O1 C1 C2 C3 3 . -67.9(2)
O1 C1 C2 C3 . . 172.39(15)
O1 C1 C2 C3 3 10 -172.39(15)
O1 C1 C2 C3 . 10 67.9(2)
C1 C2 C3 C4 . . -139.29(18)
C3 C2 C3 C4 10 . -18.09(19)
C2 C3 C4 C3 . 10 18.05(19)