#------------------------------------------------------------------------------
#$Date: 2023-03-16 04:10:54 +0100 (Thu, 16 Mar 2023) $
#$Revision: 281907 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022704.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_2022704
loop_
_publ_author_name
'Aristov, Michael M.'
'Geng, Han'
'Harris, James W.'
'Berry, John F.'
_publ_section_title
;
Clarifying the structures of imidines: using crystallographic
characterization to identify tautomers and localized systems of
\p-bonding
;
_journal_coeditor_code EP3031
_journal_issue 4
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229623002036
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C5 H9 N3, C H4 O'
_chemical_formula_moiety 'C5 H9 N3, C H4 O'
_chemical_formula_sum 'C6 H13 N3 O'
_chemical_formula_weight 143.19
_chemical_name_systematic
;
6-Imino-3,4,5,6-tetrahydropyridin-2-amine methanol monosolvate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha 90
_cell_angle_beta 111.320(8)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 9.4887(9)
_cell_length_b 14.5341(11)
_cell_length_c 12.2828(10)
_cell_measurement_reflns_used 9930
_cell_measurement_temperature 100.00
_cell_measurement_theta_max 74.418
_cell_measurement_theta_min 4.919
_cell_volume 1578.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEXII Quazar'
_diffrn_measurement_method '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0368
_diffrn_reflns_av_unetI/netI 0.0211
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 26582
_diffrn_reflns_theta_full 67.500
_diffrn_reflns_theta_max 74.468
_diffrn_reflns_theta_min 4.919
_diffrn_source_current 1.1
_diffrn_source_power 0.55000000000000E-1
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.695
_exptl_absorpt_correction_T_max 0.7538
_exptl_absorpt_correction_T_min 0.6895
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.205
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 624
_exptl_crystal_size_max 0.03
_exptl_crystal_size_mid 0.02
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.350
_refine_diff_density_min -0.277
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.074
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 204
_refine_ls_number_reflns 3219
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.0432
_refine_ls_R_factor_gt 0.0400
_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^)+(0.0520P)^2^+0.8148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1050
_refine_ls_wR_factor_ref 0.1076
_reflns_number_gt 2938
_reflns_number_total 3219
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ep3031sup1.cif
_cod_data_source_block 2
_cod_database_code 2022704
_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 0.979
_shelx_estimated_absorpt_t_max 0.993
_shelx_hkl_file
;
-1 0 0 88.09 3.00
-2 0 0 8.60 1.10
-3 0 0 25.40 1.90
-4 0 0 19.20 2.00
-5 0 0 0.40 1.00
-6 0 0 213.98 10.20
-7 0 0 11.20 1.00
-7 0 0 8.30 0.90
-7 0 0 7.10 1.10
-7 0 0 8.90 0.80
-7 0 0 8.00 0.80
-7 0 0 6.90 2.30
-7 0 0 12.00 1.60
-7 0 0 10.20 1.10
7 0 0 9.20 2.60
-7 0 0 8.00 0.60
-7 0 0 8.00 1.20
-8 0 0 427.56 13.40
-8 0 0 472.55 13.20
-8 0 0 468.35 13.40
-8 0 0 470.15 13.40
-8 0 0 428.36 13.70
-8 0 0 454.85 13.40
-8 0 0 449.16 14.30
-8 0 0 459.35 14.10
-8 0 0 440.56 14.40
-9 0 0 96.29 4.00
-9 0 0 92.79 3.20
-9 0 0 98.49 3.20
-9 0 0 95.69 3.20
-9 0 0 98.49 3.00
-9 0 0 91.99 3.80
-9 0 0 89.19 4.10
-10 0 0 11.40 1.30
-10 0 0 12.00 0.80
-10 0 0 10.60 0.60
-10 0 0 10.20 0.80
-10 0 0 11.80 0.70
0 -1 0 0.00 0.20
0 -1 0 -0.10 0.20
1 -1 0 157.38 5.00
-1 -1 0 158.58 5.00
-1 -1 0 157.58 5.10
-1 -1 0 156.08 5.20
-2 -1 0 8.10 1.20
-2 1 0 8.50 1.10
-3 -1 0 522.55 24.70
3 1 0 544.45 18.70
-4 -1 0 62.49 3.70
4 1 0 68.29 3.50
-4 1 0 61.89 3.60
5 -1 0 15.20 2.40
-5 -1 0 15.00 2.70
5 1 0 16.10 1.90
-5 1 0 18.00 2.70
6 -1 0 27.80 3.10
6 -1 0 25.60 4.20
-6 -1 0 45.50 3.90
6 -1 0 30.30 3.10
-6 1 0 36.90 3.60
-7 -1 0 4.20 1.00
-7 -1 0 3.80 0.40
-7 -1 0 3.40 0.60
7 -1 0 2.40 1.60
-7 -1 0 3.50 0.50
-7 -1 0 2.80 1.00
-7 -1 0 6.00 1.30
-7 -1 0 3.40 0.50
-7 -1 0 9.20 2.80
-7 -1 0 3.20 0.90
-7 1 0 3.70 0.60
-7 1 0 3.50 0.40
-7 1 0 3.30 0.90
-7 1 0 7.90 2.50
-7 1 0 0.90 1.20
-7 1 0 2.50 0.50
-7 1 0 3.60 0.70
7 1 0 6.80 1.70
-7 1 0 3.80 0.80
-7 1 0 3.20 0.90
-7 1 0 5.20 1.00
-7 1 0 3.60 0.50
-7 1 0 3.40 0.80
-8 -1 0 244.08 8.70
-8 -1 0 251.87 8.70
-8 -1 0 267.77 7.90
-8 -1 0 264.27 7.60
-8 -1 0 268.57 7.90
-8 -1 0 261.37 7.90
-8 -1 0 241.68 8.10
-8 -1 0 256.67 8.50
-8 1 0 236.68 8.30
-8 1 0 253.47 7.80
-8 1 0 266.17 7.80
-8 1 0 265.97 7.60
-8 1 0 258.07 8.90
-8 1 0 249.68 8.60
-8 1 0 258.17 7.80
-8 1 0 243.48 8.10
-8 1 0 265.77 8.50
-8 1 0 249.88 7.90
-8 1 0 243.18 8.10
-9 -1 0 36.20 2.40
-9 -1 0 34.10 2.30
-9 -1 0 32.80 1.60
-9 -1 0 31.60 2.00
-9 -1 0 35.10 1.50
-9 -1 0 32.90 1.50
-9 -1 0 32.80 1.30
-9 1 0 29.80 2.10
-9 1 0 34.50 1.70
-9 1 0 28.60 2.00
-9 1 0 34.60 1.30
-9 1 0 32.60 1.40
-9 1 0 30.00 2.60
-9 1 0 35.70 1.50
-9 1 0 31.60 1.50
-10 -1 0 11.80 0.80
-10 -1 0 13.60 0.80
-10 -1 0 13.60 0.90
-10 -1 0 12.40 1.30
-10 -1 0 13.60 0.60
-10 1 0 12.20 1.00
-10 1 0 13.20 0.60
-10 1 0 13.50 1.50
-10 1 0 16.20 1.60
-10 1 0 13.70 0.80
-10 1 0 13.40 0.80
0 -2 0 314.87 19.50
0 -2 0 337.77 15.10
0 2 0 329.87 19.80
0 2 0 337.37 15.10
-1 -2 0 281.47 9.00
2 -2 0 20.00 1.40
-2 -2 0 20.80 1.50
-2 -2 0 18.90 1.50
-2 -2 0 22.80 1.60
-2 2 0 19.90 1.20
-3 -2 0 157.28 6.30
3 -2 0 161.28 6.10
-3 2 0 164.08 5.90
4 -2 0 174.48 7.20
-4 -2 0 178.58 7.60
-4 2 0 187.78 7.20
5 -2 0 288.07 11.70
5 -2 0 284.07 11.20
-5 -2 0 311.67 12.10
-5 2 0 288.57 11.20
6 -2 0 10.10 2.30
-6 -2 0 14.40 3.20
6 -2 0 11.30 2.20
-6 2 0 15.00 2.60
7 -2 0 71.39 6.30
-7 -2 0 73.39 2.60
-7 -2 0 72.49 3.40
-7 -2 0 76.59 2.40
-7 -2 0 73.99 2.60
-7 -2 0 84.09 6.80
-7 -2 0 68.49 3.10
-7 -2 0 85.39 3.40
-7 -2 0 71.69 3.10
-7 -2 0 73.59 2.70
-7 2 0 71.79 3.20
-7 2 0 73.69 5.90
7 2 0 72.39 4.50
-7 2 0 66.39 2.90
-7 2 0 67.79 3.60
-7 2 0 68.59 2.80
-7 2 0 69.79 3.10
-7 2 0 68.99 2.70
-7 2 0 74.39 3.20
-7 2 0 75.69 2.60
-7 2 0 73.19 2.60
-7 2 0 74.19 2.60
-7 2 0 72.99 2.40
-8 -2 0 150.98 5.50
-8 -2 0 158.18 5.70
-8 -2 0 161.78 5.10
-8 -2 0 152.68 5.90
-8 -2 0 161.78 5.10
-8 -2 0 164.78 6.10
-8 -2 0 165.88 4.90
-8 -2 0 163.88 5.10
-8 2 0 151.18 5.40
-8 2 0 154.88 5.20
-8 2 0 155.78 5.70
-8 2 0 148.89 5.40
-8 2 0 160.08 6.30
-8 2 0 155.18 5.00
-8 2 0 164.08 4.80
-8 2 0 161.58 5.80
-8 2 0 161.78 5.10
-8 2 0 153.68 5.70
-8 2 0 160.18 5.00
-9 -2 0 1.10 0.30
-9 -2 0 0.90 0.80
-9 -2 0 1.20 0.60
-9 -2 0 2.30 1.20
-9 -2 0 0.40 0.40
-9 -2 0 0.70 0.50
-9 2 0 1.00 0.50
-9 2 0 1.80 1.00
-9 2 0 2.50 1.00
-9 2 0 0.90 0.70
-9 2 0 0.80 0.30
-9 2 0 0.30 1.30
-9 2 0 1.70 0.50
-10 -2 0 21.80 1.00
-10 -2 0 22.30 0.90
-10 -2 0 21.60 1.10
-10 -2 0 21.80 1.40
-10 -2 0 19.90 1.10
-10 2 0 21.40 2.30
-10 2 0 19.20 1.80
-10 2 0 21.80 1.20
-10 2 0 21.50 0.80
-10 2 0 23.10 0.90
-10 2 0 21.40 1.10
0 -3 0 0.70 0.80
0 -3 0 -0.40 0.60
1 -3 0 164.28 5.90
-1 -3 0 168.48 6.10
-1 -3 0 173.48 6.00
1 -3 0 164.68 6.10
-1 -3 0 168.58 5.70
-1 3 0 160.68 5.10
-2 -3 0 570.94 17.80
-2 -3 0 580.54 18.20
3 -3 0 685.03 42.40
-3 -3 0 680.03 30.40
-3 -3 0 693.63 43.00
3 -3 0 648.84 34.30
-3 3 0 697.33 26.50
-3 3 0 692.03 23.90
3 3 0 699.43 30.60
3 3 0 704.43 43.20
4 -3 0 0.80 0.80
4 -3 0 -1.20 0.70
-4 -3 0 0.60 1.10
-4 3 0 -0.40 0.60
5 -3 0 229.78 9.80
5 -3 0 246.48 10.60
-5 -3 0 247.98 10.70
-5 3 0 247.38 9.70
6 -3 0 71.09 5.00
6 -3 0 63.79 5.30
-6 -3 0 67.99 5.40
-6 3 0 69.49 4.80
7 -3 0 19.40 4.40
-7 -3 0 18.50 1.70
-7 -3 0 14.90 1.00
-7 -3 0 18.50 1.10
-7 -3 0 17.10 1.50
-7 -3 0 16.60 1.00
-7 -3 0 14.30 1.70
-7 -3 0 16.20 0.80
-7 3 0 16.70 0.80
-7 3 0 15.40 1.50
7 3 0 18.80 2.70
-7 3 0 18.60 1.70
-7 3 0 17.30 1.80
-7 3 0 17.20 0.90
-7 3 0 18.00 1.40
-7 3 0 17.30 1.30
-7 3 0 15.30 1.00
-7 3 0 20.40 2.20
-8 -3 0 85.39 3.00
-8 -3 0 80.29 3.90
-8 -3 0 87.89 2.70
-8 -3 0 86.19 2.90
-8 -3 0 84.09 3.00
-8 -3 0 75.29 3.30
-8 -3 0 81.79 3.50
-8 3 0 83.89 3.60
-8 3 0 82.39 3.60
-8 3 0 79.49 2.80
-8 3 0 82.09 2.90
-8 3 0 84.59 4.20
8 3 0 94.69 5.50
-8 3 0 77.59 3.20
-8 3 0 83.89 2.60
-8 3 0 76.69 3.30
-8 3 0 82.99 3.10
-9 -3 0 3.80 0.40
-9 -3 0 5.20 0.80
-9 -3 0 4.40 0.90
-9 -3 0 4.50 0.60
-9 -3 0 3.80 0.60
-9 -3 0 4.20 1.30
-9 3 0 4.90 0.90
-9 3 0 6.60 0.90
-9 3 0 4.70 1.20
-9 3 0 4.60 0.40
-9 3 0 7.00 1.20
-9 3 0 3.90 0.50
-9 3 0 4.20 1.50
-9 3 0 4.50 0.60
-10 -3 0 1.70 0.40
-10 -3 0 1.50 0.30
-10 -3 0 2.40 0.40
-10 -3 0 2.20 0.70
-10 -3 0 1.90 0.60
-10 3 0 0.80 1.40
-10 3 0 3.00 1.20
-10 3 0 2.20 0.50
-10 3 0 2.50 0.30
-10 3 0 1.50 0.60
0 -4 0 40.40 2.50
0 -4 0 42.00 2.60
1 -4 0 23.70 2.00
-1 -4 0 19.20 1.90
-1 -4 0 21.30 1.90
1 -4 0 18.90 1.70
-1 -4 0 22.40 1.50
-1 4 0 19.60 0.90
-2 -4 0 59.89 3.10
-2 -4 0 60.59 3.40
2 -4 0 56.69 3.40
2 -4 0 62.79 3.20
-2 -4 0 59.49 3.20
-2 4 0 54.39 2.20
-3 -4 0 48.90 3.20
-3 -4 0 44.30 2.80
3 -4 0 41.90 2.80
3 -4 0 42.50 3.20
-3 4 0 42.80 2.20
4 -4 0 229.28 9.20
-4 -4 0 237.38 9.70
4 -4 0 248.18 10.10
-4 4 0 221.68 8.40
5 -4 0 25.70 2.70
-5 -4 0 31.00 4.20
5 -4 0 29.00 4.00
-5 4 0 26.80 2.40
-6 -4 0 11.40 0.60
6 -4 0 11.70 2.70
-6 -4 0 11.90 3.00
-6 -4 0 13.00 0.90
-6 -4 0 11.30 0.90
-6 -4 0 10.10 1.90
6 -4 0 9.00 2.20
-6 4 0 9.30 2.20
-6 4 0 12.00 1.00
-7 -4 0 10.70 1.60
-7 -4 0 12.50 1.40
7 -4 0 10.50 3.60
-7 -4 0 11.90 1.10
-7 -4 0 10.20 0.70
-7 -4 0 11.10 1.40
-7 -4 0 11.30 0.90
7 -4 0 4.60 3.80
-7 -4 0 9.60 0.90
-7 4 0 10.40 0.60
-7 4 0 9.60 1.00
-7 4 0 7.90 1.00
-7 4 0 10.80 1.80
-7 4 0 11.10 1.20
-7 4 0 10.50 1.30
7 4 0 10.90 2.50
-7 4 0 14.60 1.60
-7 4 0 9.30 0.80
-8 -4 0 103.39 3.60
-8 -4 0 111.09 3.30
-8 -4 0 103.99 4.60
-8 -4 0 103.19 4.10
-8 -4 0 103.49 3.60
-8 -4 0 105.39 3.60
-8 -4 0 103.89 4.00
-8 4 0 102.09 3.50
-8 4 0 102.39 4.80
8 4 0 109.39 6.20
-8 4 0 104.59 3.70
-8 4 0 107.89 4.30
-8 4 0 103.09 3.20
-8 4 0 100.39 3.90
-8 4 0 107.39 4.30
-8 4 0 97.69 3.70
-9 -4 0 114.69 3.80
-9 -4 0 118.49 3.90
-9 -4 0 117.19 3.60
-9 -4 0 117.69 4.90
-9 -4 0 111.19 4.20
-9 -4 0 117.29 3.80
-9 4 0 116.09 4.00
-9 4 0 115.59 3.80
-9 4 0 117.59 4.50
-9 4 0 116.79 5.00
-9 4 0 109.39 4.10
-9 4 0 116.49 4.50
-9 4 0 112.49 3.50
-10 -4 0 2.50 0.40
-10 -4 0 3.70 0.60
-10 -4 0 2.80 0.40
-10 -4 0 2.60 0.30
-10 4 0 3.00 0.70
-10 4 0 1.60 1.30
-10 4 0 2.70 0.60
-10 4 0 3.50 0.90
-10 4 0 2.90 1.50
0 -5 0 0.00 0.80
0 -5 0 -0.10 0.90
-1 -5 0 1385.56 75.99
1 -5 0 1466.85 57.49
-1 -5 0 1482.55 58.99
-1 5 0 1511.75 58.49
1 5 0 1520.05 59.69
-1 5 0 1366.46 73.39
1 5 0 1493.95 77.39
2 -5 0 76.09 4.00
2 -5 0 70.69 4.20
-2 -5 0 69.89 4.00
-2 -5 0 70.09 3.90
-2 -5 0 68.39 3.60
-2 5 0 67.39 2.50
3 -5 0 12.30 2.20
-3 -5 0 9.90 1.90
-3 -5 0 7.70 1.80
-3 -5 0 9.90 1.90
3 -5 0 11.80 2.50
-3 5 0 11.10 0.90
4 -5 0 835.52 27.30
-4 -5 0 876.01 27.00
-4 -5 0 856.91 27.90
-4 5 0 799.62 25.60
5 -5 0 180.88 9.60
-5 -5 0 193.28 9.60
5 -5 0 179.88 8.70
-6 -5 0 0.30 0.50
-6 -5 0 0.20 0.40
-6 -5 0 0.90 0.70
-6 -5 0 0.90 1.00
-6 -5 0 0.80 0.40
6 -5 0 -0.70 1.60
-6 -5 0 0.20 0.90
6 -5 0 -0.80 1.40
-6 -5 0 0.20 0.30
-6 5 0 0.20 1.20
-6 5 0 0.50 0.60
-6 5 0 1.20 0.80
-6 5 0 1.60 0.40
-6 5 0 0.50 0.80
-6 5 0 0.90 0.90
-7 -5 0 19.20 1.20
-7 -5 0 22.00 1.00
-7 -5 0 20.10 2.10
-7 -5 0 22.30 1.20
7 -5 0 20.10 5.70
-7 -5 0 22.30 1.40
-7 -5 0 21.80 1.70
7 -5 0 19.00 4.70
-7 -5 0 21.50 2.00
-7 5 0 21.60 1.50
-7 5 0 23.90 1.50
-7 5 0 24.60 2.60
7 5 0 29.70 4.10
-7 5 0 22.50 2.00
-7 5 0 22.30 1.90
-7 5 0 24.20 1.20
-7 5 0 20.60 0.90
-7 5 0 21.50 1.80
-8 -5 0 15.30 1.10
-8 -5 0 17.10 1.10
-8 -5 0 16.80 2.20
-8 -5 0 18.40 1.60
-8 -5 0 15.90 1.30
-8 -5 0 16.10 0.80
-8 5 0 14.90 1.40
-8 5 0 16.40 1.90
-8 5 0 17.40 1.10
8 5 0 25.90 3.00
-8 5 0 15.70 0.80
-8 5 0 19.10 1.80
-8 5 0 17.20 2.20
-8 5 0 17.30 1.40
-9 -5 0 60.29 2.70
-9 -5 0 63.89 2.30
-9 -5 0 61.19 2.30
-9 -5 0 61.39 2.00
-9 -5 0 61.99 2.40
-9 -5 0 63.39 3.40
-9 5 0 60.49 3.00
-9 5 0 59.29 1.90
-9 5 0 60.49 3.70
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-9 -1 9 5.40 1.30
-9 1 9 6.60 0.80
-9 1 9 3.60 1.60
-9 1 9 6.90 1.30
-9 1 9 8.90 1.30
-9 1 9 5.90 0.60
-8 -1 9 271.97 8.80
8 -1 -9 257.77 8.30
-8 -1 9 268.47 9.00
-8 -1 9 264.97 8.10
-8 -1 9 272.77 8.60
-8 -1 9 263.07 8.10
-8 1 9 249.08 8.00
-8 1 9 270.77 9.10
8 1 -9 247.38 8.30
-8 1 9 264.57 8.60
-8 1 9 271.47 9.30
-8 1 9 267.17 8.80
-8 1 9 278.97 8.20
7 -1 -9 44.70 9.10
-7 -1 9 39.00 6.40
-7 -1 9 35.30 1.60
-7 -1 9 36.70 2.80
-7 -1 9 33.80 2.20
7 -1 -9 34.50 1.90
-7 -1 9 34.70 2.10
-7 -1 9 36.00 1.60
-7 -1 9 36.90 1.60
-7 1 9 36.50 2.20
7 1 -9 35.50 1.90
-7 1 9 50.09 7.40
-7 1 9 35.90 1.50
-7 1 9 32.70 2.00
-7 1 9 34.40 1.50
-7 1 9 35.60 1.60
-7 1 9 35.80 3.50
-7 1 9 32.80 2.60
7 1 -9 25.20 6.70
-6 -1 9 7.30 0.80
6 -1 -9 1.30 3.30
6 -1 -9 6.70 0.90
-6 -1 9 7.90 1.60
-6 -1 9 6.60 0.70
-6 -1 9 4.20 1.00
-6 -1 9 3.90 0.90
-6 -1 9 2.60 2.10
-6 1 9 4.20 0.90
-6 1 9 5.80 2.80
-6 1 9 4.60 0.90
6 1 -9 6.20 1.00
-6 1 9 2.10 1.90
-6 1 9 4.60 0.60
6 1 -9 0.20 2.80
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-5 -1 9 2.90 1.10
-5 -1 9 2.70 0.60
5 -1 -9 5.50 1.00
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-5 -1 9 5.40 0.80
5 -1 -9 7.00 4.40
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5 1 -9 0.70 2.70
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5 1 -9 3.50 0.80
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-4 -1 9 54.59 2.20
-4 -1 9 55.79 4.80
4 -1 -9 67.79 7.60
4 -1 -9 55.69 2.50
4 1 -9 54.09 2.50
-4 1 9 55.89 2.20
4 1 -9 60.19 7.20
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-3 -1 9 7.00 0.80
3 -1 -9 4.90 3.40
3 -1 -9 9.40 1.10
-3 -1 9 7.60 2.20
3 1 -9 8.20 3.40
3 1 -9 9.90 1.10
-3 1 9 7.10 0.80
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-2 -1 9 0.70 0.60
-2 -1 9 -0.50 0.90
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-2 -1 9 0.00 1.20
2 -1 -9 0.50 0.60
2 -1 -9 -1.70 2.00
2 1 -9 0.70 0.60
-2 1 9 1.70 1.10
2 1 -9 -1.00 2.00
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1 -1 -9 7.80 1.00
1 -1 -9 8.30 0.90
-1 -1 9 5.00 1.50
1 -1 -9 5.40 3.70
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-1 -1 9 5.70 0.90
1 1 -9 6.90 0.90
-1 1 9 4.30 0.80
-1 1 9 8.50 1.90
-1 1 9 5.80 2.00
1 1 -9 6.70 0.80
1 1 -9 5.20 3.30
0 -1 -9 536.95 15.30
0 -1 -9 474.55 23.90
0 -1 9 478.35 15.50
0 -1 9 503.25 17.20
0 -1 -9 505.95 15.30
0 -1 9 544.55 21.10
0 -1 9 542.85 15.30
0 1 -9 483.55 15.20
0 1 9 469.65 20.00
0 1 9 500.35 15.20
0 1 9 533.95 15.30
0 1 -9 532.55 15.30
0 1 -9 525.65 25.30
0 1 9 506.15 17.50
-1 -1 -9 108.09 3.70
1 -1 9 121.29 8.60
-1 -1 -9 107.09 10.20
1 -1 9 100.39 3.80
1 -1 9 114.29 5.40
-1 1 -9 107.89 10.70
1 1 9 89.99 7.50
1 1 9 105.19 5.50
-1 1 -9 104.49 3.70
-1 1 -9 103.29 4.40
1 1 9 99.19 3.70
2 -1 9 56.39 6.40
2 -1 9 53.99 2.40
-2 -1 -9 54.29 2.60
-2 -1 -9 57.39 2.30
-2 1 -9 49.70 9.00
2 1 9 52.59 6.10
2 1 9 59.59 4.10
-2 1 -9 55.39 3.20
-2 1 -9 56.69 2.30
2 1 9 54.39 2.40
3 -1 9 0.60 0.70
-3 -1 -9 -0.10 1.10
-3 -1 -9 -0.60 0.70
-3 -1 -9 0.40 0.50
-3 1 -9 0.90 0.50
-3 1 -9 0.90 1.10
-3 1 -9 0.30 0.40
-3 1 -9 -0.40 0.70
3 1 9 0.50 0.60
-4 -1 -9 5.90 0.70
4 -1 9 6.30 0.90
-4 -1 -9 6.60 1.30
-4 -1 -9 5.40 0.80
-4 -1 -9 6.70 0.60
-4 -1 -9 4.40 1.00
-4 1 -9 6.10 0.70
-4 1 -9 5.20 1.00
-4 1 -9 5.50 0.80
4 1 9 7.90 0.90
-4 1 -9 5.70 0.60
-4 1 -9 5.10 1.30
-5 -1 -9 25.70 1.10
-5 -1 -9 26.00 1.30
-5 -1 -9 24.70 2.10
-5 -1 -9 27.20 1.60
5 -1 9 28.30 1.40
5 1 9 26.00 1.30
-5 1 -9 25.90 1.60
-5 1 -9 27.00 2.10
-5 1 -9 24.20 1.30
-5 1 -9 23.50 1.30
-6 -1 -9 0.90 0.50
-6 -1 -9 0.40 0.80
-6 1 -9 0.40 0.60
-6 1 -9 0.10 0.40
-6 1 -9 -0.20 0.80
-11 -2 9 6.30 0.90
-11 -2 9 4.70 0.50
-11 -2 9 4.80 1.00
-11 -2 9 4.90 0.40
-11 2 9 4.20 0.90
-11 2 9 5.90 0.50
-11 2 9 4.20 0.90
-11 2 9 5.60 0.90
-10 -2 9 0.20 0.50
-10 -2 9 0.30 0.40
-10 -2 9 0.10 0.90
-10 -2 9 -2.30 0.90
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-10 2 9 0.70 0.50
-10 2 9 0.50 1.20
-10 2 9 0.40 0.80
-9 -2 9 28.90 1.40
-9 -2 9 29.90 1.50
-9 -2 9 32.10 2.20
-9 -2 9 30.90 2.30
-9 -2 9 29.60 2.30
-9 2 9 32.30 2.50
-9 2 9 31.60 2.10
-9 2 9 30.80 3.20
-9 2 9 31.50 2.20
-9 2 9 28.80 1.50
-8 -2 9 56.69 3.00
8 -2 -9 60.59 2.50
-8 -2 9 61.39 2.30
-8 -2 9 58.49 2.30
-8 -2 9 60.89 3.20
-8 -2 9 55.89 3.00
-8 2 9 61.29 3.10
-8 2 9 59.19 3.20
-8 2 9 57.49 3.80
-8 2 9 59.89 2.80
-8 2 9 59.99 2.30
8 2 -9 56.49 2.60
7 -2 -9 0.40 0.70
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-7 -2 9 0.00 0.40
-7 -2 9 0.30 0.70
-7 -2 9 -0.20 0.50
7 -2 -9 -3.20 2.30
-7 -2 9 1.00 1.40
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7 2 -9 0.40 5.00
-7 2 9 -0.40 1.20
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7 2 -9 0.60 0.70
-7 2 9 -1.90 0.70
-7 2 9 -0.50 0.50
-7 2 9 -0.60 0.60
-7 2 9 0.00 1.90
-6 -2 9 15.00 1.50
-6 -2 9 12.60 1.30
-6 -2 9 12.00 1.60
-6 -2 9 14.60 1.10
-6 -2 9 16.60 3.90
-6 -2 9 12.00 0.90
6 -2 -9 20.50 5.20
6 -2 -9 14.50 1.40
-6 2 9 13.40 1.30
6 2 -9 13.10 1.30
-6 2 9 13.50 1.00
-6 2 9 15.50 3.80
-6 2 9 16.20 1.60
6 2 -9 17.20 5.40
-6 2 9 12.80 1.40
-6 2 9 13.60 2.30
-5 -2 9 4.80 1.10
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-5 -2 9 11.20 3.00
5 -2 -9 9.20 1.20
5 -2 -9 6.90 4.70
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-5 2 9 7.20 1.30
5 2 -9 8.60 1.10
-5 2 9 7.80 1.00
5 2 -9 11.50 4.20
-5 2 9 7.00 0.80
4 -2 -9 235.48 7.40
-4 -2 9 236.38 7.20
4 -2 -9 211.68 15.30
-4 -2 9 211.78 10.90
4 2 -9 237.58 7.40
-4 2 9 235.68 9.50
4 2 -9 213.08 14.60
-4 2 9 230.58 7.20
-4 2 9 230.28 11.60
3 -2 -9 93.59 9.20
3 -2 -9 76.19 3.10
-3 -2 9 78.49 5.60
-3 -2 9 76.29 2.90
-3 2 9 78.39 5.90
3 2 -9 76.99 3.10
3 2 -9 92.99 9.10
-3 2 9 76.49 4.50
-3 2 9 76.89 2.80
2 -2 -9 17.80 1.40
2 -2 -9 25.60 6.00
-2 -2 9 19.60 3.20
-2 -2 9 16.90 3.20
-2 -2 9 19.80 1.30
-2 -2 9 20.30 1.50
2 2 -9 19.30 1.40
-2 2 9 19.50 2.80
2 2 -9 26.20 6.10
-2 2 9 17.70 1.20
-2 2 9 17.60 1.20
1 -2 -9 113.49 9.90
1 -2 -9 104.19 3.60
1 -2 -9 101.89 3.80
-1 -2 9 101.69 4.00
-1 -2 9 104.09 3.70
-1 -2 9 96.49 6.30
-1 -2 9 106.09 7.30
1 2 -9 97.99 9.50
1 2 -9 106.99 3.70
-1 2 9 100.39 5.40
-1 2 9 96.89 6.40
-1 2 9 105.19 3.60
-1 2 9 108.49 3.70
1 2 -9 102.99 3.80
0 -2 -9 151.28 11.60
0 -2 9 134.09 8.90
0 -2 -9 143.29 4.70
0 -2 9 141.19 4.70
0 -2 9 131.99 6.20
0 -2 -9 134.69 4.70
0 2 -9 136.49 4.70
0 2 -9 140.99 4.70
0 2 -9 142.99 5.20
0 2 9 139.69 6.70
0 2 9 144.79 4.70
0 2 9 133.79 4.70
0 2 9 129.69 8.30
1 -2 9 12.20 3.60
-1 -2 -9 1.70 3.20
1 -2 9 4.40 0.90
-1 -2 -9 4.10 0.70
1 2 9 4.00 0.80
-1 2 -9 4.40 4.20
-1 2 -9 4.50 0.80
1 2 9 4.50 2.70
1 2 9 5.40 1.90
-1 2 -9 3.60 1.20
2 -2 9 24.30 1.60
-2 -2 -9 21.60 1.30
-2 -2 -9 23.90 1.70
2 2 9 27.30 2.90
-2 2 -9 20.80 2.20
2 2 9 22.10 1.50
-2 2 -9 23.30 1.40
-3 -2 -9 46.70 1.90
-3 -2 -9 45.70 2.40
-3 -2 -9 44.40 2.90
3 -2 9 46.20 2.20
-3 2 -9 44.30 2.90
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3 2 9 49.30 3.70
3 2 9 47.50 2.20
-3 2 -9 48.30 2.00
-3 2 -9 55.69 2.30
-3 2 -9 43.80 1.90
-3 2 -9 46.90 2.10
4 -2 9 74.99 2.90
-4 -2 -9 74.19 3.10
-4 -2 -9 74.09 3.60
-4 -2 -9 76.59 2.60
-4 -2 -9 75.09 2.80
-4 -2 -9 79.09 2.60
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-4 2 -9 74.49 3.10
-4 2 -9 71.59 2.50
4 2 9 75.69 2.90
-4 2 -9 79.69 3.60
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5 -2 9 -0.10 0.60
-5 -2 -9 0.90 0.40
-5 -2 -9 -0.30 0.60
-5 -2 -9 -0.30 0.40
-5 2 -9 1.00 1.00
-5 2 -9 0.30 0.50
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-11 -3 9 7.80 0.50
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-10 -3 9 14.30 0.90
-10 -3 9 13.70 1.40
-10 -3 9 15.00 1.70
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-10 3 9 13.90 1.60
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-9 -3 9 7.10 1.20
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-8 -3 9 46.30 2.00
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8 -3 -9 54.19 2.10
-8 -3 9 44.00 2.00
-8 -3 9 52.09 2.80
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7 -3 -9 -0.20 0.70
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6 -3 -9 1.00 0.70
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6 -3 -9 -0.90 3.90
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6 3 -9 0.60 2.70
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6 3 -9 0.20 0.70
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-6 3 9 0.10 0.70
5 -3 -9 43.90 2.20
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5 -3 -9 59.89 10.60
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5 3 -9 45.00 2.20
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-5 3 9 43.20 3.40
-5 3 9 45.30 2.50
5 3 -9 38.30 7.10
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4 -3 -9 119.89 11.20
-4 -3 9 121.19 4.50
4 -3 -9 125.19 4.50
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-4 3 9 130.79 4.20
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4 3 -9 129.09 4.50
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4 3 -9 138.89 11.30
3 -3 -9 54.49 2.50
-3 -3 9 57.29 2.40
-3 -3 9 55.29 4.60
-3 -3 9 56.29 2.30
3 -3 -9 66.29 8.10
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3 3 -9 63.99 7.50
3 3 -9 56.59 2.50
2 -3 -9 81.69 8.50
2 -3 -9 75.99 2.90
-2 -3 9 76.29 2.90
-2 -3 9 75.09 5.40
2 -3 -9 73.59 3.00
-2 -3 9 83.89 6.10
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2 3 -9 80.19 8.70
-2 3 9 78.69 2.90
2 3 -9 78.49 2.90
-2 3 9 75.59 2.90
-2 3 9 74.69 4.60
2 3 -9 77.29 3.10
-1 -3 9 8.50 1.00
-1 -3 9 6.70 2.10
1 -3 -9 8.50 0.90
-1 -3 9 10.90 1.00
1 -3 -9 15.20 4.60
1 -3 -9 9.90 1.10
-1 -3 9 6.20 2.60
1 3 -9 8.70 1.00
1 3 -9 11.10 1.20
-1 3 9 8.50 0.90
1 3 -9 12.70 4.50
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0 -3 9 119.09 8.50
0 -3 -9 111.89 4.00
0 -3 -9 108.89 10.00
0 -3 9 118.19 4.10
0 -3 -9 113.19 4.00
0 3 9 116.79 4.00
0 3 -9 114.59 4.00
0 3 9 111.69 6.00
0 3 9 109.59 7.50
0 3 9 112.39 4.00
0 3 -9 124.49 4.80
0 3 -9 107.19 10.70
0 3 -9 114.49 4.00
1 -3 9 60.79 2.60
1 -3 9 69.29 6.70
-1 -3 -9 65.19 2.80
-1 -3 -9 62.59 2.50
1 3 9 60.39 6.00
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1 3 9 65.69 4.50
1 3 9 64.19 2.60
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2 -3 9 33.30 1.90
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3 -3 9 26.90 1.70
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3 3 9 34.40 3.20
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3 3 9 23.00 1.50
-3 3 -9 29.10 1.70
-3 3 -9 22.40 1.50
-3 3 -9 26.30 1.60
4 -3 9 15.90 1.30
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-4 -3 -9 18.30 1.20
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4 3 9 16.40 1.20
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5 -3 9 10.80 1.00
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-11 -4 9 33.60 1.30
-11 -4 9 33.20 1.80
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-10 -4 9 -0.30 0.30
-10 4 9 -0.20 0.80
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8 -4 -9 2.30 0.70
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7 -4 -9 7.50 1.00
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6 -4 -9 49.10 2.40
6 -4 -9 94.29 14.60
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6 4 -9 51.69 2.50
-6 4 9 52.19 2.70
-6 4 9 50.79 2.30
-6 4 9 54.79 5.70
-6 4 9 50.69 2.00
6 4 -9 42.30 8.10
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5 -4 -9 17.90 1.50
-5 -4 9 14.50 1.20
5 -4 -9 6.10 5.20
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5 4 -9 17.70 1.50
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-5 4 9 16.70 1.40
-5 4 9 15.60 1.40
5 4 -9 19.90 5.50
-5 4 9 19.50 4.10
-4 -4 9 264.57 12.70
-4 -4 9 281.47 8.60
-4 -4 9 269.17 8.80
4 -4 -9 285.77 9.10
4 -4 -9 287.47 18.40
-4 -4 9 288.37 8.90
4 4 -9 305.37 18.00
-4 4 9 297.97 8.80
4 4 -9 298.87 9.10
-4 4 9 292.47 14.10
-4 4 9 289.87 11.30
-3 -4 9 13.00 2.70
3 -4 -9 15.70 1.30
-3 -4 9 15.30 1.30
3 -4 -9 20.50 5.90
-3 -4 9 14.20 1.20
3 -4 -9 15.30 1.10
-3 4 9 12.80 1.10
3 4 -9 23.40 6.10
3 4 -9 13.00 1.30
-3 4 9 19.70 4.00
3 4 -9 17.40 1.20
-3 4 9 13.50 1.10
-3 4 9 12.10 2.20
-2 -4 9 57.19 2.50
-2 -4 9 62.09 2.60
2 -4 -9 65.39 8.00
2 -4 -9 60.89 2.40
-2 -4 9 60.59 5.50
2 -4 -9 62.39 2.60
-2 4 9 61.59 2.40
-2 4 9 65.79 4.30
2 4 -9 64.09 9.90
2 4 -9 59.99 2.60
2 4 -9 55.59 2.50
-2 4 9 61.69 2.40
1 -4 -9 104.99 9.80
-1 -4 9 95.19 3.60
-1 -4 9 96.99 3.50
-1 -4 9 96.49 7.50
1 -4 -9 94.29 3.60
-1 -4 9 88.89 6.80
1 -4 -9 99.29 3.50
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1 4 -9 93.69 3.60
1 4 -9 104.79 10.30
1 4 -9 100.99 3.50
-1 4 9 97.89 3.50
-1 4 9 89.49 5.30
0 -4 -9 8.90 1.00
0 -4 9 9.50 1.20
0 -4 -9 8.50 1.00
0 -4 9 6.50 3.40
0 -4 -9 8.60 4.60
0 -4 9 5.90 3.00
0 4 9 9.90 2.80
0 4 9 7.90 1.00
0 4 -9 9.80 1.10
0 4 9 8.70 2.20
0 4 9 6.70 0.90
0 4 -9 7.40 0.90
0 4 -9 11.40 4.20
1 -4 9 51.89 8.00
-1 -4 -9 44.80 2.00
-1 -4 -9 48.90 2.30
1 -4 9 39.50 6.50
1 -4 9 42.90 2.20
-1 4 -9 56.99 2.70
1 4 9 43.80 2.10
1 4 9 46.90 5.40
-1 4 -9 47.00 2.10
-1 4 -9 41.50 8.10
1 4 9 39.80 3.80
-2 -4 -9 3.40 0.70
2 -4 9 3.30 0.90
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2 4 9 2.20 1.80
2 4 9 3.30 0.80
-2 4 -9 3.70 0.70
-2 4 -9 3.30 0.90
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3 -4 9 1.90 0.80
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3 4 9 0.90 1.70
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3 4 9 1.40 0.70
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4 -4 9 5.60 0.90
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-4 4 -9 6.30 0.90
4 4 9 5.20 0.80
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5 -4 9 9.20 0.90
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5 4 9 10.10 0.90
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-9 -5 9 19.20 1.90
-9 -5 9 19.30 1.10
-9 5 9 20.70 1.10
9 5 -9 22.20 1.50
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-8 -5 9 72.69 2.60
8 -5 -9 69.69 2.80
-8 -5 9 67.69 3.20
-8 -5 9 72.09 3.40
-8 -5 9 71.49 2.60
-8 -5 9 67.79 2.30
-8 -5 9 67.29 2.30
-8 5 9 75.69 3.50
-8 5 9 71.29 3.90
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8 5 -9 65.99 2.90
7 -5 -9 52.19 2.40
-7 -5 9 50.29 2.70
-7 -5 9 53.29 2.00
-7 -5 9 52.49 2.00
-7 -5 9 53.59 2.10
-7 -5 9 49.50 1.80
-7 -5 9 51.29 2.70
-7 5 9 51.79 2.80
-7 5 9 48.90 2.40
-7 5 9 50.69 1.90
7 5 -9 49.99 2.50
-7 5 9 51.79 2.70
-7 5 9 50.89 2.00
-7 5 9 50.49 3.60
-6 -5 9 90.49 12.30
-6 -5 9 80.39 2.80
6 -5 -9 79.49 3.20
-6 -5 9 75.79 3.40
-6 -5 9 81.09 3.00
-6 5 9 77.29 3.20
-6 5 9 80.59 3.30
-6 5 9 91.69 13.30
-6 5 9 82.39 2.90
-6 5 9 81.59 3.60
6 5 -9 82.19 3.30
-6 5 9 83.49 4.20
-5 -5 9 38.80 1.60
5 -5 -9 46.70 10.20
-5 -5 9 38.60 5.90
-5 -5 9 42.10 2.00
5 -5 -9 40.20 2.20
-5 5 9 52.29 5.40
5 5 -9 40.00 2.20
-5 5 9 39.50 2.00
-5 5 9 39.60 2.30
5 5 -9 37.00 7.70
-5 5 9 38.60 3.30
-5 5 9 40.30 1.80
-4 -5 9 46.20 2.10
-4 -5 9 44.40 4.50
4 -5 -9 37.90 8.10
4 -5 -9 47.40 2.30
-4 -5 9 46.30 2.20
-4 5 9 45.30 3.70
4 5 -9 38.60 7.00
-4 5 9 46.90 2.00
-4 5 9 50.09 5.20
4 5 -9 44.80 2.30
3 -5 -9 9.60 5.10
-3 -5 9 9.40 1.10
3 -5 -9 7.20 1.00
-3 -5 9 9.70 1.00
3 -5 -9 12.90 1.00
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3 5 -9 8.50 1.10
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3 5 -9 6.80 4.40
-3 5 9 10.00 1.00
3 5 -9 10.40 1.10
-3 5 9 7.00 1.80
-2 -5 9 3.90 0.90
-2 -5 9 1.00 2.10
2 -5 -9 4.80 0.70
2 -5 -9 3.40 3.40
2 -5 -9 3.50 0.80
-2 -5 9 3.50 0.80
2 5 -9 5.00 0.80
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2 5 -9 -1.00 2.80
2 5 -9 4.60 0.90
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1 -5 -9 162.88 5.50
1 -5 -9 164.68 5.40
1 -5 -9 151.08 12.30
-1 -5 9 156.18 5.50
-1 -5 9 168.28 5.50
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-1 5 9 164.58 5.40
1 5 -9 159.18 5.50
1 5 -9 164.58 13.60
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1 5 -9 168.88 5.50
0 -5 -9 62.19 2.50
0 -5 9 62.69 2.70
0 -5 9 75.29 7.10
0 -5 9 55.79 6.20
0 -5 -9 62.39 2.60
0 -5 -9 62.99 2.80
0 5 9 62.99 2.60
0 5 9 63.19 2.60
0 5 9 66.39 4.70
0 5 -9 66.19 2.70
0 5 -9 63.59 2.60
0 5 -9 80.69 9.70
1 -5 9 1.40 0.90
-1 -5 -9 1.30 0.60
-1 -5 -9 2.50 0.80
1 -5 9 1.10 3.60
1 5 9 1.90 1.90
-1 5 -9 1.90 0.70
1 5 9 1.50 2.60
1 5 9 1.50 0.70
-2 -5 -9 6.90 0.80
-2 -5 -9 7.50 1.10
2 -5 9 8.40 1.10
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2 5 9 7.70 1.00
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2 5 9 1.70 2.00
-3 -5 -9 37.90 1.60
3 -5 9 38.50 2.00
-3 -5 -9 29.60 1.50
-3 -5 -9 37.20 2.10
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3 5 9 45.80 3.70
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3 5 9 38.80 1.90
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-4 -5 -9 0.40 0.40
4 -5 9 0.00 0.70
-4 -5 -9 -0.10 0.70
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-4 5 -9 -0.30 0.60
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4 5 9 0.40 0.50
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-5 -5 -9 11.50 1.10
5 -5 9 13.50 1.00
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5 5 9 11.60 0.90
-10 -6 9 41.30 2.10
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-10 6 9 40.10 2.20
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-9 -6 9 161.58 4.80
-9 -6 9 163.38 5.10
-9 -6 9 160.08 5.00
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-9 6 9 161.48 5.00
9 6 -9 163.18 5.30
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-8 -6 9 9.40 0.90
-8 -6 9 8.20 0.80
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-8 -6 9 7.20 0.60
8 -6 -9 9.70 1.00
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8 6 -9 7.40 1.00
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7 -6 -9 16.50 1.40
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-7 -6 9 16.90 1.10
-7 -6 9 16.70 1.00
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7 6 -9 17.00 1.60
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6 -6 -9 6.30 1.10
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6 6 -9 5.10 1.00
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-6 6 9 5.30 1.90
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5 -6 -9 39.00 8.10
5 -6 -9 44.60 2.20
5 6 -9 31.70 7.20
-5 6 9 43.00 3.20
-5 6 9 40.10 2.40
-5 6 9 40.50 2.00
-5 6 9 41.00 1.80
5 6 -9 42.40 2.30
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4 -6 -9 7.50 5.90
-4 -6 9 16.50 1.40
-4 -6 9 16.30 1.30
4 -6 -9 14.40 1.40
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4 6 -9 12.50 1.30
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4 6 -9 14.70 5.10
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3 -6 -9 3.90 0.70
3 -6 -9 3.40 0.90
3 -6 -9 -0.60 3.20
3 6 -9 2.80 0.80
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3 6 -9 3.10 3.80
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2 -6 -9 82.79 3.30
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2 -6 -9 69.39 8.70
2 -6 -9 82.89 3.10
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2 6 -9 93.99 10.40
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1 -6 -9 1.70 3.50
1 -6 -9 2.50 0.80
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1 -6 -9 0.80 0.50
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1 6 -9 1.10 3.60
1 6 -9 2.60 0.80
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1 6 -9 3.60 0.90
0 -6 9 173.98 11.70
0 -6 -9 170.58 5.70
0 -6 9 168.38 11.40
0 -6 -9 177.28 5.80
0 -6 9 169.98 5.90
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1 -6 9 -0.70 0.80
-1 -6 -9 -0.60 0.70
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3 -6 9 1.50 0.80
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3 6 9 -0.80 1.60
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3 6 9 1.10 0.60
4 -6 9 3.00 0.80
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8 -7 -9 32.50 1.70
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5 -7 -9 112.49 4.30
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4 -7 -9 3.70 4.70
4 -7 -9 5.10 1.00
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4 7 -9 7.10 4.80
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3 -7 -9 -0.20 0.50
3 -7 -9 1.60 4.10
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3 -7 -9 -0.40 0.70
3 7 -9 0.30 0.80
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2 -7 -9 -0.70 2.90
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2 -7 -9 2.10 0.60
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2 -7 -9 1.50 0.80
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1 -7 -9 15.90 1.40
1 -7 -9 15.40 1.20
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0 -7 -9 17.30 1.20
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0 -7 9 21.30 1.40
0 -7 -9 17.40 1.40
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1 -7 9 52.19 2.60
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3 -7 9 0.70 0.80
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4 -8 -9 468.55 13.80
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3 -8 -9 45.70 2.10
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3 -8 -9 45.40 2.40
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2 -8 -9 1.10 0.80
2 -8 -9 3.50 0.70
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2 8 -9 2.60 0.90
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1 -8 -9 46.90 2.30
1 -8 -9 48.80 2.10
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1 8 -9 45.90 1.90
1 8 -9 47.60 2.30
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0 -8 9 4.50 0.80
0 -8 9 0.80 1.00
0 -8 -9 1.50 0.70
0 -8 -9 1.10 0.60
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3 -3 -14 28.00 1.40
3 3 -14 27.70 1.40
-3 3 14 29.70 1.40
3 3 -14 29.10 1.50
2 -3 -14 21.70 1.20
-2 -3 14 24.60 1.30
-2 3 14 23.40 1.20
-2 3 14 22.40 1.10
2 3 -14 21.50 1.20
1 -3 -14 27.10 1.30
-1 -3 14 30.10 1.40
-1 3 14 26.60 1.20
-1 3 14 27.70 1.20
1 3 -14 28.30 1.20
1 3 -14 28.30 1.30
0 -3 -14 23.20 1.00
0 -3 14 23.30 1.20
0 -3 -14 23.70 1.00
0 3 -14 23.90 1.00
0 3 -14 26.30 1.10
0 3 14 22.70 1.10
-7 -4 14 0.40 0.30
7 -4 -14 0.80 0.50
-7 -4 14 0.90 0.30
7 4 -14 0.20 0.50
-7 4 14 0.50 0.30
-6 -4 14 23.50 1.00
-6 -4 14 22.60 1.10
6 -4 -14 24.30 1.30
-6 4 14 23.80 1.10
-6 4 14 23.60 1.00
6 4 -14 25.30 1.40
5 -4 -14 19.20 1.20
-5 -4 14 18.70 1.00
5 4 -14 17.20 1.20
-5 4 14 18.00 0.90
-5 4 14 19.20 1.00
-4 -4 14 2.00 0.50
4 -4 -14 4.20 0.60
4 -4 -14 2.00 0.60
4 4 -14 1.40 0.60
4 4 -14 1.90 0.70
-4 4 14 2.00 0.50
3 -4 -14 1.60 0.50
3 -4 -14 1.20 0.50
-3 -4 14 1.60 0.50
-3 4 14 0.90 0.50
3 4 -14 1.30 0.60
2 -4 -14 13.30 0.90
-2 -4 14 14.30 0.90
-2 -4 14 14.70 1.10
2 4 -14 13.70 0.80
-2 4 14 13.00 0.90
2 4 -14 14.70 1.00
1 -4 -14 22.30 1.10
-1 -4 14 21.70 1.20
1 4 -14 20.60 1.00
1 4 -14 20.10 1.10
-1 4 14 20.20 1.00
-1 4 14 19.70 1.00
-7 -5 14 0.60 0.30
7 -5 -14 1.10 0.50
7 5 -14 1.20 0.50
-7 5 14 1.10 0.30
-6 -5 14 2.00 0.30
-6 -5 14 3.00 0.50
6 -5 -14 1.80 0.60
-6 5 14 1.90 0.40
-6 5 14 1.70 0.40
6 5 -14 1.60 0.60
-5 -5 14 34.90 1.40
5 -5 -14 33.50 1.60
-5 5 14 34.80 1.30
-5 5 14 35.80 1.40
5 5 -14 33.10 1.60
-4 -5 14 -0.10 0.40
4 -5 -14 0.20 0.60
4 -5 -14 -0.10 0.40
-4 5 14 0.20 0.40
4 5 -14 0.40 0.60
4 5 -14 0.20 0.50
-3 -5 14 3.50 0.60
3 -5 -14 3.90 0.60
3 -5 -14 4.00 0.50
-3 5 14 3.50 0.60
3 5 -14 3.30 0.60
-2 -5 14 13.90 0.90
2 -5 -14 11.80 0.80
-2 -5 14 11.20 0.80
2 5 -14 10.70 0.90
-2 5 14 11.30 0.80
2 5 -14 11.60 0.70
1 -5 -14 5.80 0.60
-1 -5 14 7.90 0.80
1 5 -14 5.20 0.60
1 5 -14 7.00 0.60
-6 -6 14 11.80 0.70
6 -6 -14 11.20 0.90
-6 -6 14 11.40 0.70
-6 6 14 12.30 0.60
-6 6 14 11.90 0.70
6 6 -14 13.20 0.90
-5 -6 14 -0.10 0.30
5 -6 -14 0.80 0.50
-5 -6 14 0.70 0.40
-5 6 14 0.10 0.30
5 6 -14 0.10 0.50
-5 6 14 -0.10 0.30
-4 -6 14 69.29 2.30
4 -6 -14 67.79 2.30
-4 6 14 67.69 2.30
4 6 -14 66.29 2.40
4 6 -14 65.19 2.20
3 -6 -14 3.60 0.50
-3 -6 14 3.50 0.50
-3 6 14 3.60 0.50
3 6 -14 4.30 0.60
2 -6 -14 27.80 1.20
2 -6 -14 33.20 2.00
-2 -6 14 28.70 1.60
2 6 -14 26.60 1.20
-2 6 14 26.70 1.20
5 -7 -14 100.89 3.20
-5 -7 14 100.59 3.10
-5 -7 14 99.09 3.10
-5 7 14 97.69 3.10
5 7 -14 99.79 3.40
-5 7 14 96.99 3.00
-4 -7 14 16.20 0.90
4 -7 -14 17.60 0.90
-4 7 14 16.70 0.80
-4 7 14 16.40 0.80
-3 -7 14 1.70 0.40
3 7 -14 2.80 0.50
-3 7 14 2.30 0.40
-6 0 15 0.00 0.30
6 0 -15 0.10 0.50
-5 0 15 0.00 0.40
5 0 -15 -0.60 0.50
4 0 -15 1.90 0.40
4 0 -15 1.10 0.40
-4 0 15 0.20 0.40
3 0 -15 -0.20 0.40
-3 0 15 0.00 0.40
2 0 -15 0.10 0.30
6 -1 -15 0.50 0.50
-6 -1 15 0.80 0.30
6 1 -15 -0.20 0.40
-6 1 15 0.50 0.30
5 -1 -15 16.70 1.00
-5 -1 15 15.90 0.70
-5 1 15 17.70 0.70
5 1 -15 16.90 1.00
-5 1 15 16.90 0.90
4 -1 -15 1.00 0.40
4 -1 -15 1.10 0.50
-4 1 15 0.50 0.40
3 -1 -15 6.30 0.60
-3 1 15 6.10 0.70
3 1 -15 6.20 0.60
2 -1 -15 4.80 0.50
2 1 -15 4.20 0.50
2 1 -15 3.00 0.50
-6 -2 15 6.00 0.50
6 -2 -15 6.30 0.60
6 2 -15 5.60 0.60
-6 2 15 5.70 0.40
-5 -2 15 9.70 0.50
5 -2 -15 11.00 0.80
-5 -2 15 9.50 0.70
-5 2 15 9.70 0.60
-5 2 15 10.40 0.70
5 2 -15 11.60 0.80
4 -2 -15 8.80 1.00
-4 -2 15 5.50 0.60
-4 2 15 5.80 0.60
-4 2 15 5.00 0.50
4 2 -15 7.90 0.80
-3 -2 15 45.50 1.60
3 -2 -15 42.90 1.60
3 2 -15 43.40 1.70
-3 2 15 44.80 1.60
5 -3 -15 1.40 0.50
-5 -3 15 0.90 0.40
-5 -3 15 0.70 0.30
5 3 -15 1.10 0.40
-5 3 15 0.60 0.30
-5 3 15 0.60 0.30
-4 -3 15 17.60 0.90
-4 3 15 17.20 0.90
-4 3 15 16.40 0.70
-3 -3 15 2.90 0.40
3 3 -15 2.50 0.40
-3 3 15 2.50 0.40
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 96515
_shelx_res_file
;
TITL berry1122_a.res in P2(1)/c
berry1122.res
created by SHELXL-2018/1 at 10:55:40 on 26-Jan-2023
REM Old TITL
REM SHELXT solution in P2(1)/c: R1 0.127, Rweak 0.004, Alpha 0.021
REM 0.487 for 142 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 N8
CELL 1.54178 9.4887 14.5341 12.2828 90 111.32 90
ZERR 8 0.0009 0.0011 0.001 0 0.008 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 48 104 24 8
EQIV $1 -1+X,+Y,+Z
EQIV $2 1+X,+Y,+Z
EQIV $3 1-X,-0.5+Y,0.5-Z
L.S. 24
PLAN 22
SIZE 0.01 0.02 0.03
TEMP -173.15
CONF
HTAB O1 N3
HTAB O2 N6
HTAB N1 N5
HTAB N1 O1_$1
HTAB N4 N2
HTAB N4 O2_$2
HTAB C9 O1_$3
BOND $H
list 4
MORE -1
fmap 2 53
acta 135
REM
REM
REM
WGHT 0.052000 0.814800
FVAR 0.47529 0.85363
O1 4 0.918092 0.530596 0.322278 11.00000 0.01002 0.01824 =
0.02108 -0.00381 0.00931 -0.00205
AFIX 147
H1 2 0.843291 0.500710 0.324261 11.00000 -1.50000
AFIX 0
C11 1 0.950210 0.604119 0.404310 11.00000 0.01312 0.01918 =
0.02278 -0.00412 0.00922 -0.00307
AFIX 137
H11A 2 0.914773 0.662174 0.362792 11.00000 -1.50000
H11B 2 1.059570 0.607547 0.447497 11.00000 -1.50000
H11C 2 0.898395 0.593247 0.459110 11.00000 -1.50000
AFIX 0
O2 4 -0.238497 0.180157 0.499861 11.00000 0.00916 0.03406 =
0.01293 0.00376 0.00441 -0.00006
AFIX 147
H2 2 -0.177175 0.196182 0.468403 11.00000 -1.50000
AFIX 0
C12 1 -0.160482 0.168880 0.621373 11.00000 0.02090 0.01983 =
0.01294 0.00136 0.00610 0.00103
AFIX 127
H12A 2 -0.075415 0.126555 0.634784 21.00000 -1.20000
H12B 2 -0.229589 0.143625 0.656730 21.00000 -1.20000
H12C 2 -0.122367 0.228643 0.656828 21.00000 -1.20000
H12D 2 -0.209499 0.205994 0.664111 -21.00000 -1.20000
H12E 2 -0.055325 0.188924 0.642165 -21.00000 -1.20000
H12F 2 -0.162546 0.103905 0.642067 -21.00000 -1.20000
AFIX 0
N1 3 0.189810 0.440822 0.341028 11.00000 0.00804 0.00949 =
0.01990 0.00232 0.00717 0.00063
AFIX 93
H1A 2 0.193322 0.380372 0.345176 11.00000 -1.20000
H1B 2 0.107360 0.470129 0.338113 11.00000 -1.20000
AFIX 0
N2 3 0.430776 0.441594 0.343671 11.00000 0.00819 0.01020 =
0.01298 0.00111 0.00508 -0.00043
N3 3 0.670784 0.445582 0.334716 11.00000 0.01216 0.01391 =
0.03132 -0.00299 0.01217 -0.00106
H3 2 0.658003 0.384235 0.337343 11.00000 -1.20000
N4 3 0.455503 0.244913 0.414959 11.00000 0.01252 0.01084 =
0.02441 0.00265 0.00946 0.00438
AFIX 93
H4A 2 0.441875 0.301552 0.387785 11.00000 -1.20000
H4B 2 0.544157 0.218156 0.432102 11.00000 -1.20000
AFIX 0
N5 3 0.210700 0.241243 0.403853 11.00000 0.01270 0.00776 =
0.01386 0.00043 0.00673 -0.00001
N6 3 -0.034801 0.235021 0.402990 11.00000 0.01403 0.01502 =
0.01511 -0.00028 0.00606 -0.00425
H6 2 -0.030166 0.294098 0.379898 11.00000 -1.20000
C1 1 0.308619 0.487697 0.339171 11.00000 0.00825 0.01047 =
0.00706 0.00110 0.00271 0.00046
C2 1 0.294193 0.591287 0.333686 11.00000 0.00996 0.00934 =
0.01739 0.00271 0.00538 0.00156
AFIX 23
H2A 2 0.314806 0.615714 0.413238 11.00000 -1.20000
H2B 2 0.189341 0.608325 0.284329 11.00000 -1.20000
AFIX 0
C3 1 0.403314 0.634413 0.283875 11.00000 0.01404 0.01127 =
0.01850 0.00361 0.00745 -0.00034
AFIX 23
H3A 2 0.407300 0.701797 0.296414 11.00000 -1.20000
H3B 2 0.368326 0.622714 0.198743 11.00000 -1.20000
AFIX 0
C4 1 0.559681 0.593173 0.344056 11.00000 0.01127 0.01235 =
0.01731 0.00127 0.00593 -0.00142
AFIX 23
H4C 2 0.628254 0.615835 0.305505 11.00000 -1.20000
H4D 2 0.600702 0.613484 0.426622 11.00000 -1.20000
AFIX 0
C5 1 0.554773 0.489075 0.339474 11.00000 0.00859 0.01360 =
0.01137 0.00104 0.00363 -0.00072
SAME 0.01 0.02 C6 C7A C8A C9A C10
C6 1 0.342200 0.199784 0.430108 11.00000 0.01709 0.00916 =
0.01498 0.00050 0.00787 0.00251
PART 1
C7 1 0.371824 0.101283 0.472490 21.00000 0.01589 0.00732 =
0.02134 0.00230 0.00103 0.00263
AFIX 23
H7A 2 0.477899 0.095201 0.527129 21.00000 -1.20000
H7B 2 0.357403 0.060030 0.405148 21.00000 -1.20000
AFIX 0
C8 1 0.265306 0.072546 0.534048 21.00000 0.03110 0.00873 =
0.01666 0.00629 0.00830 0.00200
AFIX 23
H8A 2 0.275274 0.005791 0.551184 21.00000 -1.20000
H8B 2 0.290335 0.106319 0.608716 21.00000 -1.20000
AFIX 0
C9 1 0.104446 0.095041 0.453005 21.00000 0.02279 0.00728 =
0.02047 -0.00035 0.01284 -0.00365
AFIX 23
H9A 2 0.077210 0.056923 0.381497 21.00000 -1.20000
H9B 2 0.032970 0.080500 0.492550 21.00000 -1.20000
AFIX 0
PART 2
C9A 1 0.141886 0.104704 0.503284 -21.00000 0.03955
AFIX 23
H9AA 2 0.166713 0.124120 0.585420 -21.00000 -1.20000
H9AB 2 0.053918 0.062706 0.482943 -21.00000 -1.20000
AFIX 0
C7A 1 0.404217 0.116319 0.509479 -21.00000 0.02213
AFIX 23
H7AA 2 0.482399 0.084901 0.487294 -21.00000 -1.20000
H7AB 2 0.450947 0.136391 0.591897 -21.00000 -1.20000
AFIX 0
C8A 1 0.274617 0.051498 0.495666 -21.00000 0.04320
AFIX 23
H8AA 2 0.306708 0.004182 0.557862 -21.00000 -1.20000
H8AB 2 0.244586 0.019944 0.419149 -21.00000 -1.20000
AFIX 0
PART 0
C10 1 0.091962 0.195342 0.420367 11.00000 0.01837 0.00961 =
0.01345 -0.00166 0.00924 -0.00343
HKLF 4
REM berry1122_a.res in P2(1)/c
REM R1 = 0.0400 for 2938 Fo > 4sig(Fo) and 0.0432 for all 3219 data
REM 204 parameters refined using 5 restraints
END
WGHT 0.0520 0.8148
REM Highest difference peak 0.350, deepest hole -0.277, 1-sigma level 0.048
Q1 1 0.5261 0.5680 0.2616 11.00000 0.05 0.35
Q2 1 0.1017 0.1444 0.4370 11.00000 0.05 0.29
Q3 1 0.4790 0.6207 0.3316 11.00000 0.05 0.27
Q4 1 0.3035 0.5389 0.3306 11.00000 0.05 0.26
Q5 1 0.3463 0.1466 0.4459 11.00000 0.05 0.22
Q6 1 0.5524 0.5391 0.3424 11.00000 0.05 0.21
Q7 1 0.1638 0.2172 0.4149 11.00000 0.05 0.20
Q8 1 0.3561 0.6070 0.3153 11.00000 0.05 0.18
Q9 1 0.2741 0.2224 0.4280 11.00000 0.05 0.17
Q10 1 0.4217 0.3981 0.3251 11.00000 0.05 0.17
Q11 1 0.3753 0.4629 0.3397 11.00000 0.05 0.17
Q12 1 0.4838 0.4640 0.3375 11.00000 0.05 0.15
Q13 1 0.2000 0.2793 0.3728 11.00000 0.05 0.15
Q14 1 0.1812 0.0839 0.4856 11.00000 0.05 0.14
Q15 1 -0.2788 0.1009 0.4461 11.00000 0.05 0.14
Q16 1 0.2194 0.3663 0.3933 11.00000 0.05 0.13
Q17 1 -0.1148 0.2159 0.3976 11.00000 0.05 0.13
Q18 1 -0.2702 0.2451 0.5004 11.00000 0.05 0.13
Q19 1 0.8749 0.5617 0.2380 11.00000 0.05 0.13
Q20 1 0.3968 0.2201 0.4270 11.00000 0.05 0.12
Q21 1 0.0399 0.2233 0.4359 11.00000 0.05 0.12
Q22 1 0.5487 0.4989 0.2125 11.00000 0.05 0.12
;
_shelx_res_checksum 69061
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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 O1 0.91809(9) 0.53060(6) 0.32228(8) 0.0154(2) Uani d 1 . .
H H1 0.843291 0.500710 0.324261 0.023 Uiso calc 1 . .
C C11 0.95021(14) 0.60412(9) 0.40431(12) 0.0176(3) Uani d 1 . .
H H11A 0.914773 0.662174 0.362792 0.026 Uiso calc 1 . .
H H11B 1.059570 0.607547 0.447497 0.026 Uiso calc 1 . .
H H11C 0.898395 0.593247 0.459110 0.026 Uiso calc 1 . .
O O2 -0.23850(10) 0.18016(7) 0.49986(8) 0.0186(2) Uani d 1 . .
H H2 -0.177175 0.196182 0.468403 0.028 Uiso calc 1 . .
C C12 -0.16048(15) 0.16888(9) 0.62137(11) 0.0179(3) Uani d 1 . .
H H12A -0.075415 0.126555 0.634784 0.021 Uiso calc 0.854(6) . .
H H12B -0.229589 0.143625 0.656730 0.021 Uiso calc 0.854(6) . .
H H12C -0.122367 0.228643 0.656828 0.021 Uiso calc 0.854(6) . .
H H12D -0.209499 0.205994 0.664111 0.021 Uiso calc 0.146(6) . .
H H12E -0.055325 0.188924 0.642165 0.021 Uiso calc 0.146(6) . .
H H12F -0.162546 0.103905 0.642067 0.021 Uiso calc 0.146(6) . .
N N1 0.18981(11) 0.44082(7) 0.34103(9) 0.0119(2) Uani d 1 . .
H H1A 0.193322 0.380372 0.345176 0.014 Uiso calc 1 . .
H H1B 0.107360 0.470129 0.338113 0.014 Uiso calc 1 . .
N N2 0.43078(10) 0.44159(7) 0.34367(8) 0.0101(2) Uani d 1 . .
N N3 0.67078(12) 0.44558(8) 0.33472(10) 0.0179(2) Uani d 1 . .
H H3 0.6580(19) 0.3842(13) 0.3373(15) 0.022 Uiso d 1 . .
N N4 0.45550(12) 0.24491(7) 0.41496(10) 0.0152(2) Uani d 1 . .
H H4A 0.441875 0.301552 0.387785 0.018 Uiso calc 1 . .
H H4B 0.544157 0.218156 0.432102 0.018 Uiso calc 1 . .
N N5 0.21070(11) 0.24124(7) 0.40385(9) 0.0109(2) Uani d 1 . .
N N6 -0.03480(12) 0.23502(7) 0.40299(9) 0.0145(2) Uani d 1 . .
H H6 -0.0302(19) 0.2941(12) 0.3799(15) 0.017 Uiso d 1 . .
C C1 0.30862(12) 0.48770(8) 0.33917(9) 0.0086(2) Uani d 1 . .
C C2 0.29419(13) 0.59129(8) 0.33369(11) 0.0121(2) Uani d 1 . .
H H2A 0.314806 0.615714 0.413238 0.015 Uiso calc 1 . .
H H2B 0.189341 0.608325 0.284329 0.015 Uiso calc 1 . .
C C3 0.40331(13) 0.63441(8) 0.28387(11) 0.0142(2) Uani d 1 . .
H H3A 0.407300 0.701797 0.296414 0.017 Uiso calc 1 . .
H H3B 0.368326 0.622714 0.198743 0.017 Uiso calc 1 . .
C C4 0.55968(13) 0.59317(8) 0.34406(11) 0.0134(2) Uani d 1 . .
H H4C 0.628254 0.615835 0.305505 0.016 Uiso calc 1 . .
H H4D 0.600702 0.613484 0.426622 0.016 Uiso calc 1 . .
C C5 0.55477(13) 0.48907(8) 0.33947(10) 0.0112(2) Uani d 1 . .
C C6 0.34220(14) 0.19978(8) 0.43011(11) 0.0132(2) Uani d 1 . .
C C7 0.3718(2) 0.10128(11) 0.4725(2) 0.0165(4) Uani d 0.854(6) A 1
H H7A 0.477899 0.095201 0.527129 0.020 Uiso calc 0.854(6) A 1
H H7B 0.357403 0.060030 0.405148 0.020 Uiso calc 0.854(6) A 1
C C8 0.26531(19) 0.07255(12) 0.53405(16) 0.0189(5) Uani d 0.854(6) A 1
H H8A 0.275274 0.005791 0.551184 0.023 Uiso calc 0.854(6) A 1
H H8B 0.290335 0.106319 0.608716 0.023 Uiso calc 0.854(6) A 1
C C9 0.1044(2) 0.09504(10) 0.4530(2) 0.0155(4) Uani d 0.854(6) A 1
H H9A 0.077210 0.056923 0.381497 0.019 Uiso calc 0.854(6) A 1
H H9B 0.032970 0.080500 0.492550 0.019 Uiso calc 0.854(6) A 1
C C9A 0.1419(16) 0.1047(10) 0.5033(18) 0.040(4) Uiso d 0.146(6) A 2
H H9AA 0.166713 0.124120 0.585420 0.047 Uiso calc 0.146(6) A 2
H H9AB 0.053918 0.062706 0.482943 0.047 Uiso calc 0.146(6) A 2
C C7A 0.4042(12) 0.1163(7) 0.5095(12) 0.022(4) Uiso d 0.146(6) A 2
H H7AA 0.482399 0.084901 0.487294 0.027 Uiso calc 0.146(6) A 2
H H7AB 0.450947 0.136391 0.591897 0.027 Uiso calc 0.146(6) A 2
C C8A 0.2746(14) 0.0515(8) 0.4957(16) 0.043(4) Uiso d 0.146(6) A 2
H H8AA 0.306708 0.004182 0.557862 0.052 Uiso calc 0.146(6) A 2
H H8AB 0.244586 0.019944 0.419149 0.052 Uiso calc 0.146(6) A 2
C C10 0.09196(14) 0.19534(8) 0.42037(10) 0.0128(2) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0100(4) 0.0182(4) 0.0211(5) -0.0020(3) 0.0093(3) -0.0038(3)
C11 0.0131(6) 0.0192(6) 0.0228(6) -0.0031(5) 0.0092(5) -0.0041(5)
O2 0.0092(4) 0.0341(5) 0.0129(4) -0.0001(4) 0.0044(3) 0.0038(4)
C12 0.0209(6) 0.0198(6) 0.0129(6) 0.0010(5) 0.0061(5) 0.0014(5)
N1 0.0080(4) 0.0095(5) 0.0199(5) 0.0006(3) 0.0072(4) 0.0023(4)
N2 0.0082(5) 0.0102(5) 0.0130(5) -0.0004(3) 0.0051(4) 0.0011(4)
N3 0.0122(5) 0.0139(5) 0.0313(6) -0.0011(4) 0.0122(4) -0.0030(4)
N4 0.0125(5) 0.0108(5) 0.0244(5) 0.0044(4) 0.0095(4) 0.0026(4)
N5 0.0127(5) 0.0078(4) 0.0139(5) 0.0000(4) 0.0067(4) 0.0004(4)
N6 0.0140(5) 0.0150(5) 0.0151(5) -0.0043(4) 0.0061(4) -0.0003(4)
C1 0.0083(5) 0.0105(5) 0.0071(5) 0.0005(4) 0.0027(4) 0.0011(4)
C2 0.0100(5) 0.0093(5) 0.0174(6) 0.0016(4) 0.0054(4) 0.0027(4)
C3 0.0140(6) 0.0113(5) 0.0185(6) -0.0003(4) 0.0074(5) 0.0036(4)
C4 0.0113(5) 0.0123(6) 0.0173(6) -0.0014(4) 0.0059(5) 0.0013(4)
C5 0.0086(5) 0.0136(6) 0.0114(5) -0.0007(4) 0.0036(4) 0.0010(4)
C6 0.0171(6) 0.0092(5) 0.0150(6) 0.0025(4) 0.0079(5) 0.0005(4)
C7 0.0159(8) 0.0073(7) 0.0213(10) 0.0026(6) 0.0010(8) 0.0023(7)
C8 0.0311(9) 0.0087(7) 0.0167(8) 0.0020(6) 0.0083(7) 0.0063(6)
C9 0.0228(8) 0.0073(7) 0.0205(10) -0.0037(6) 0.0128(8) -0.0004(6)
C10 0.0184(6) 0.0096(5) 0.0134(6) -0.0034(4) 0.0092(5) -0.0017(4)
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'
N N 0.0311 0.0180 '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
C11 O1 H1 . . 109.5 ?
O1 C11 H11A . . 109.5 ?
O1 C11 H11B . . 109.5 ?
O1 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C12 O2 H2 . . 109.5 ?
O2 C12 H12A . . 109.5 ?
O2 C12 H12B . . 109.5 ?
O2 C12 H12C . . 109.5 ?
O2 C12 H12D . . 109.5 ?
O2 C12 H12E . . 109.5 ?
O2 C12 H12F . . 109.5 ?
H12A C12 H12B . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12A C12 H12D . . 141.1 ?
H12A C12 H12E . . 56.3 ?
H12A C12 H12F . . 56.3 ?
H12B C12 H12C . . 109.5 ?
H12B C12 H12D . . 56.3 ?
H12B C12 H12E . . 141.1 ?
H12B C12 H12F . . 56.3 ?
H12C C12 H12D . . 56.3 ?
H12C C12 H12E . . 56.3 ?
H12C C12 H12F . . 141.1 ?
H12D C12 H12E . . 109.5 ?
H12D C12 H12F . . 109.5 ?
H12E C12 H12F . . 109.5 ?
H1A N1 H1B . . 120.0 ?
C1 N1 H1A . . 120.0 ?
C1 N1 H1B . . 120.0 ?
C1 N2 C5 . . 119.40(10) ?
C5 N3 H3 . . 110.8(11) ?
H4A N4 H4B . . 120.0 ?
C6 N4 H4A . . 120.0 ?
C6 N4 H4B . . 120.0 ?
C6 N5 C10 . . 119.50(10) ?
C10 N6 H6 . . 109.1(10) ?
N1 C1 C2 . . 116.70(10) ?
N2 C1 N1 . . 118.50(10) ?
N2 C1 C2 . . 124.79(10) ?
C1 C2 H2A . . 109.3 ?
C1 C2 H2B . . 109.3 ?
C1 C2 C3 . . 111.45(10) ?
H2A C2 H2B . . 108.0 ?
C3 C2 H2A . . 109.3 ?
C3 C2 H2B . . 109.3 ?
C2 C3 H3A . . 109.8 ?
C2 C3 H3B . . 109.8 ?
C2 C3 C4 . . 109.26(10) ?
H3A C3 H3B . . 108.3 ?
C4 C3 H3A . . 109.8 ?
C4 C3 H3B . . 109.8 ?
C3 C4 H4C . . 109.4 ?
C3 C4 H4D . . 109.4 ?
H4C C4 H4D . . 108.0 ?
C5 C4 C3 . . 111.38(10) ?
C5 C4 H4C . . 109.4 ?
C5 C4 H4D . . 109.4 ?
N2 C5 C4 . . 120.87(10) ?
N3 C5 N2 . . 120.65(11) ?
N3 C5 C4 . . 118.46(10) ?
N4 C6 C7 . . 117.14(11) ?
N4 C6 C7A . . 109.7(4) ?
N5 C6 N4 . . 118.88(11) ?
N5 C6 C7 . . 123.93(12) ?
N5 C6 C7A . . 128.9(4) ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
C6 C7 C8 . . 110.85(12) ?
H7A C7 H7B . . 108.1 ?
C8 C7 H7A . . 109.5 ?
C8 C7 H7B . . 109.5 ?
C7 C8 H8A . . 110.2 ?
C7 C8 H8B . . 110.2 ?
H8A C8 H8B . . 108.5 ?
C9 C8 C7 . . 107.73(15) ?
C9 C8 H8A . . 110.2 ?
C9 C8 H8B . . 110.2 ?
C8 C9 H9A . . 109.6 ?
C8 C9 H9B . . 109.6 ?
H9A C9 H9B . . 108.1 ?
C10 C9 C8 . . 110.18(14) ?
C10 C9 H9A . . 109.6 ?
C10 C9 H9B . . 109.6 ?
H9AA C9A H9AB . . 107.4 ?
C8A C9A H9AA . . 108.3 ?
C8A C9A H9AB . . 108.3 ?
C8A C9A C10 . . 115.8(11) ?
C10 C9A H9AA . . 108.3 ?
C10 C9A H9AB . . 108.3 ?
C6 C7A H7AA . . 110.0 ?
C6 C7A H7AB . . 110.0 ?
H7AA C7A H7AB . . 108.4 ?
C8A C7A C6 . . 108.3(8) ?
C8A C7A H7AA . . 110.0 ?
C8A C7A H7AB . . 110.0 ?
C9A C8A H8AA . . 109.7 ?
C9A C8A H8AB . . 109.7 ?
C7A C8A C9A . . 109.7(10) ?
C7A C8A H8AA . . 109.7 ?
C7A C8A H8AB . . 109.7 ?
H8AA C8A H8AB . . 108.2 ?
N5 C10 C9 . . 121.04(11) ?
N5 C10 C9A . . 114.5(5) ?
N6 C10 N5 . . 121.55(11) ?
N6 C10 C9 . . 117.32(11) ?
N6 C10 C9A . . 120.8(4) ?
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 H1 . 0.8400 ?
O1 C11 . 1.4236(15) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
O2 H2 . 0.8400 ?
O2 C12 . 1.4139(15) ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C12 H12D . 0.9800 ?
C12 H12E . 0.9800 ?
C12 H12F . 0.9800 ?
N1 H1A . 0.8800 ?
N1 H1B . 0.8800 ?
N1 C1 . 1.3245(15) ?
N2 C1 . 1.3225(15) ?
N2 C5 . 1.3810(14) ?
N3 H3 . 0.902(19) ?
N3 C5 . 1.2890(16) ?
N4 H4A . 0.8800 ?
N4 H4B . 0.8800 ?
N4 C6 . 1.3290(16) ?
N5 C6 . 1.3158(16) ?
N5 C10 . 1.3863(15) ?
N6 H6 . 0.910(18) ?
N6 C10 . 1.2799(17) ?
C1 C2 . 1.5111(15) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C2 C3 . 1.5165(16) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 C4 . 1.5197(16) ?
C4 H4C . 0.9900 ?
C4 H4D . 0.9900 ?
C4 C5 . 1.5141(16) ?
C6 C7 . 1.5143(18) ?
C6 C7A . 1.533(8) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C7 C8 . 1.524(2) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C8 C9 . 1.524(2) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 C10 . 1.5051(17) ?
C9A H9AA . 0.9900 ?
C9A H9AB . 0.9900 ?
C9A C8A . 1.510(9) ?
C9A C10 . 1.627(16) ?
C7A H7AA . 0.9900 ?
C7A H7AB . 0.9900 ?
C7A C8A . 1.509(9) ?
C8A H8AA . 0.9900 ?
C8A H8AB . 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
_geom_hbond_publ_flag
O1 H1 N3 . 0.84 1.87 2.7051(14) 173.9 yes
O2 H2 N6 . 0.84 1.89 2.7312(14) 177.7 yes
N1 H1A N5 . 0.88 2.13 2.9896(14) 164.3 yes
N1 H1B O1 1_455 0.88 1.94 2.8233(13) 176.3 yes
N4 H4A N2 . 0.88 2.10 2.9739(14) 172.6 yes
N4 H4B O2 1_655 0.88 2.00 2.8639(14) 166.6 yes
C9 H9A O1 2_645 0.99 2.55 3.439(2) 149.7 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
N1 C1 C2 C3 . . . . -157.01(10) ?
N2 C1 C2 C3 . . . . 23.88(16) ?
N4 C6 C7 C8 . . . . 155.78(15) ?
N4 C6 C7A C8A . . . . -162.9(9) ?
N5 C6 C7 C8 . . . . -26.8(3) ?
N5 C6 C7A C8A . . . . 35.6(14) ?
C1 N2 C5 N3 . . . . -174.68(11) ?
C1 N2 C5 C4 . . . . 7.19(16) ?
C1 C2 C3 C4 . . . . -47.65(13) ?
C2 C3 C4 C5 . . . . 52.55(13) ?
C3 C4 C5 N2 . . . . -33.54(15) ?
C3 C4 C5 N3 . . . . 148.29(11) ?
C5 N2 C1 N1 . . . . 178.71(10) ?
C5 N2 C1 C2 . . . . -2.20(17) ?
C6 N5 C10 N6 . . . . 175.54(11) ?
C6 N5 C10 C9 . . . . -7.94(19) ?
C6 N5 C10 C9A . . . . 15.7(7) ?
C6 C7 C8 C9 . . . . 51.6(2) ?
C6 C7A C8A C9A . . . . -47.2(19) ?
C7 C8 C9 C10 . . . . -56.0(2) ?
C8 C9 C10 N5 . . . . 35.7(2) ?
C8 C9 C10 N6 . . . . -147.66(14) ?
C8A C9A C10 N5 . . . . -33.4(16) ?
C8A C9A C10 N6 . . . . 166.6(10) ?
C10 N5 C6 N4 . . . . -179.33(11) ?
C10 N5 C6 C7 . . . . 3.3(2) ?
C10 N5 C6 C7A . . . . -19.3(7) ?
C10 C9A C8A C7A . . . . 50(2) ?
_cod_database_fobs_code 2022704