#------------------------------------------------------------------------------
#$Date: 2024-07-02 05:17:34 +0300 (Tue, 02 Jul 2024) $
#$Revision: 292682 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572024.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_1572024
loop_
_publ_author_name
'Yamamoto, Ryo'
'Hashimoto, Shu'
'Okuno, Tsunehisa'
_publ_section_title
;
2-(Pyridin-4-yl)-2,3-dihydro-1H-naphtho[1,8-de][1,3,2]diazaborinine
;
_journal_coeditor_code BX4031
_journal_issue 6
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314624006151
_journal_volume 9
_journal_year 2024
_chemical_formula_iupac 'C15 H12 B N3'
_chemical_formula_moiety 'C15 H12 B N3'
_chemical_formula_sum 'C15 H12 B N3'
_chemical_formula_weight 245.09
_chemical_name_common
3-(Pyridin-4-yl)-2,4-diaza-3-boratricyclo[7.3.1.0^5,13^]trideca-1(13),5,7,9,11-pentaene
_chemical_name_systematic
2-(Pyridin-4-yl)-2,3-dihydro-1H-naphtho[1,8-de][1,3,2]diazaborinine
_space_group_crystal_system tetragonal
_space_group_IT_number 82
_space_group_name_Hall 'I -4'
_space_group_name_H-M_alt 'I -4'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 21.5659(3)
_cell_length_b 21.5659(3)
_cell_length_c 5.08630(10)
_cell_measurement_reflns_used 5132
_cell_measurement_temperature 100.00(10)
_cell_measurement_theta_max 74.9570
_cell_measurement_theta_min 2.9150
_cell_volume 2365.58(7)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)
;
_computing_data_collection
;
CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)
;
_computing_data_reduction
;
CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2013/2 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100.00(10)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix'
_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 0.0363
_diffrn_reflns_av_unetI/netI 0.0327
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_number 7772
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.980
_diffrn_reflns_theta_min 2.898
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 0.648
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.80731
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.376
_exptl_crystal_description block
_exptl_crystal_F_000 1024
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.05
_refine_diff_density_max 0.152
_refine_diff_density_min -0.155
_refine_ls_abs_structure_details
;
Flack x determined using 840 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack -0.2(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 180
_refine_ls_number_reflns 2268
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.056
_refine_ls_R_factor_all 0.0341
_refine_ls_R_factor_gt 0.0314
_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^)+(0.0502P)^2^+0.1789P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0803
_refine_ls_wR_factor_ref 0.0825
_reflns_number_gt 2125
_reflns_number_total 2268
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bx4031.cif
_cod_data_source_block I
_cod_original_cell_volume 2365.58(8)
_cod_database_code 1572024
_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 0.881
_shelx_estimated_absorpt_t_max 0.968
_shelx_hkl_file
;
0 0 -2 23.31 2.08
0 0 2 28.21 2.59
0 0 -4 104.18 6.34
0 0 4 102.94 7.03
0 0 4 113.17 7.23
0 0 6 861.06 26.01
0 1 -1 422.97 12.54
0 1 1 434.74 11.70
0 -1 -1 437.16 11.68
-1 0 -1 450.74 12.37
0 -1 1 434.26 11.68
0 1 -1 430.37 11.69
-1 0 1 425.38 12.84
0 -1 1 449.65 12.78
0 -1 3 320.71 12.30
1 0 -3 303.21 11.36
-1 0 3 297.47 12.08
0 1 -3 297.50 11.17
-1 0 -3 313.67 11.04
0 -1 -3 301.16 11.16
0 -1 5 46.22 4.78
-1 0 5 49.84 5.16
1 0 5 51.44 5.12
1 -1 0 7.58 0.53
-1 -1 2 244.94 9.06
-1 1 -2 241.84 8.41
-1 -1 -2 252.41 8.36
1 1 -2 253.92 8.75
1 -1 2 256.69 9.13
1 1 -4 16.24 3.11
-1 -1 4 16.48 3.49
-1 -1 4 23.01 3.60
1 -1 -4 14.79 2.65
1 -1 4 19.64 3.39
-1 1 -4 16.38 2.78
-1 -1 6 118.32 5.88
1 -1 6 120.17 5.85
-2 1 -1 49.72 2.28
1 2 -1 54.09 2.53
-1 -2 1 46.78 2.58
1 2 1 45.24 2.42
2 -1 1 49.38 1.92
2 -1 -1 51.54 1.91
-1 -2 3 30.98 3.43
-2 1 -3 37.28 3.13
1 2 -3 44.86 3.56
-1 -2 -3 40.68 3.11
2 -1 -3 41.78 3.52
1 2 5 103.75 7.08
2 -1 5 103.97 6.94
-1 -2 5 100.81 7.11
2 0 0 172.84 5.06
0 -2 0 164.38 4.98
-2 0 2 133.87 6.05
0 -2 2 129.32 5.85
-2 0 -2 136.15 5.14
0 2 2 120.52 5.74
2 0 -4 186.99 9.21
0 2 -4 175.62 9.03
0 -2 4 195.12 9.75
0 2 4 179.30 9.54
-2 0 4 200.48 10.05
2 0 -4 181.46 9.05
2 0 4 182.78 9.55
0 -2 4 172.64 9.44
-2 0 6 6.14 1.84
0 2 6 8.64 1.91
2 0 6 7.30 1.92
0 -2 6 8.62 1.96
-2 -1 -1 1277.93 33.96
1 -2 1 1243.83 34.61
1 -2 1 1283.97 33.93
-1 2 -1 1283.48 34.53
1 -2 -1 1251.81 33.90
-1 2 1 1258.69 34.70
2 1 -3 39.06 3.51
-1 2 3 42.10 3.92
-2 -1 -3 37.27 3.01
-2 -1 -3 42.70 3.09
-1 2 -3 40.72 3.49
1 -2 -3 42.62 3.41
-2 -1 3 40.02 3.86
1 -2 5 565.15 19.92
-1 2 5 523.34 19.69
-2 -1 5 499.65 19.66
2 -2 0 1661.68 44.42
2 2 -2 111.79 4.99
-2 -2 2 102.26 5.08
-2 2 -2 103.12 4.59
-2 2 2 96.52 5.05
-2 -2 -2 109.25 4.26
2 -2 4 19.25 3.33
2 -2 4 16.03 3.24
-2 2 4 12.73 3.05
-2 -2 4 18.74 3.18
2 2 -4 15.96 2.92
2 -2 -4 11.50 2.39
2 2 4 11.53 3.00
-2 2 -4 14.33 2.57
-2 -2 4 20.33 3.47
2 -2 6 146.13 6.51
-2 2 6 143.99 6.61
-2 -2 6 147.24 6.63
2 2 6 147.10 6.52
-3 2 -1 853.84 23.71
3 -2 1 845.01 23.50
3 -2 -1 864.42 23.51
2 3 -1 860.09 24.04
-2 -3 3 40.58 3.97
-3 2 3 41.18 3.98
2 3 -3 39.66 3.67
-3 2 -3 47.44 3.52
3 -2 -3 49.20 3.92
-3 2 5 187.14 9.95
3 -2 5 201.90 9.81
-2 -3 5 175.50 9.54
2 3 5 187.74 9.64
1 3 0 2023.49 53.17
1 3 0 1976.14 53.58
3 -1 0 2002.00 53.58
1 3 2 52.39 3.36
-1 -3 2 42.94 1.57
-1 -3 2 43.92 3.13
1 3 -2 49.53 3.12
-3 1 -2 41.18 2.72
3 -1 4 6.21 2.46
1 3 -4 1.78 1.95
3 -1 -4 4.78 2.09
-1 -3 4 5.72 2.62
3 -1 4 4.83 2.60
1 3 4 2.97 2.40
-1 -3 4 1.14 2.57
-1 -3 6 80.35 4.57
1 3 6 79.86 4.50
3 -1 6 78.61 4.50
-3 0 -1 228.59 6.90
0 3 1 232.99 7.31
0 -3 1 238.90 7.35
0 -3 1 240.66 6.92
0 -3 -1 230.14 6.88
3 0 -1 216.90 6.91
3 0 1 230.33 6.98
3 0 -3 36.35 3.50
-3 0 -3 38.82 3.13
0 3 -3 44.47 3.64
0 -3 -3 49.46 3.51
-3 0 3 40.11 3.92
0 -3 5 38.65 4.44
-3 0 5 43.93 4.71
0 3 5 40.24 4.57
3 0 5 48.65 4.71
3 1 0 1536.13 41.37
1 -3 0 1537.58 41.27
1 -3 2 166.09 5.01
1 -3 2 179.66 7.11
-3 -1 -2 183.81 6.21
-3 -1 2 163.54 7.25
-1 3 2 183.74 7.09
3 1 -2 184.51 7.02
-1 3 -2 180.62 6.81
-3 -1 -2 184.20 6.04
-1 3 -4 85.77 5.97
-3 -1 4 86.90 6.31
-1 3 4 82.83 6.27
3 1 -4 86.07 6.07
1 -3 4 85.71 6.25
-1 3 6 74.28 4.33
-3 -1 6 69.87 4.34
1 -3 6 70.26 4.23
-3 -2 -1 5028.92 135.12
-2 3 -1 5185.52 136.09
-3 -2 -1 5205.82 135.02
2 -3 1 5026.95 135.62
2 -3 -1 5185.01 135.65
-2 3 3 76.65 5.25
3 2 -3 74.72 4.97
-3 -2 -3 76.29 4.18
-2 3 -3 72.52 4.63
-3 -2 3 82.26 5.47
2 -3 5 107.46 6.97
-2 3 5 92.68 6.76
3 2 5 102.08 6.91
-3 -2 5 103.02 7.01
3 -3 0 1771.58 47.72
3 -3 2 1138.67 31.36
3 -3 -2 1112.78 31.31
-3 3 2 1201.40 33.50
3 3 -2 1114.53 33.00
-3 -3 2 1133.19 31.21
-3 3 -2 1212.44 32.74
-3 -3 -2 1169.43 31.64
-3 -3 2 1235.66 33.63
3 3 4 32.44 3.97
3 -3 -4 32.01 3.83
3 3 -4 29.16 3.90
-3 3 -4 32.79 3.56
-3 -3 4 40.10 4.40
3 -3 4 36.83 4.28
3 -3 4 33.79 4.25
3 -3 6 36.43 2.90
3 3 6 41.76 3.03
-3 -3 6 34.06 2.97
-3 3 6 36.48 3.02
4 -3 -1 405.16 12.38
-4 3 -1 417.80 12.49
4 -3 1 432.77 12.51
3 4 -3 27.68 3.14
-4 3 -3 26.91 2.78
-3 -4 3 26.30 3.27
-4 3 3 23.54 3.18
3 4 -5 109.37 6.93
-3 -4 5 130.29 7.71
3 4 5 112.75 7.09
4 -3 5 123.48 7.30
-4 3 5 124.29 7.69
2 4 0 1848.44 50.66
2 4 0 1947.94 51.38
4 -2 0 1987.91 51.38
4 -2 2 72.43 2.91
4 -2 -2 63.03 2.80
-2 -4 2 64.14 3.93
-4 2 2 77.31 4.58
2 4 -2 77.05 4.09
-2 -4 2 69.77 2.80
-2 -4 -2 70.65 2.79
-4 2 -2 67.72 3.59
4 -2 -4 13.28 2.81
2 4 -4 15.34 3.13
-2 -4 4 12.05 3.07
4 -2 4 8.46 2.66
-2 -4 4 12.83 3.00
-4 2 4 15.88 3.36
4 -2 4 13.86 2.98
2 4 4 13.42 2.96
-4 2 6 20.58 2.42
2 4 6 24.43 2.40
-2 -4 6 22.30 2.41
4 -2 6 29.51 2.61
-4 1 -1 1177.32 31.76
4 -1 1 1132.21 31.95
-1 -4 1 1122.94 32.02
1 4 1 1175.48 31.84
4 -1 -1 1203.48 32.03
1 4 -1 1184.74 31.84
1 4 -3 173.10 7.96
-1 -4 -3 162.22 7.03
4 -1 -3 159.65 7.93
-4 1 -3 171.85 7.29
4 -1 5 188.84 9.57
1 4 5 170.78 9.23
-1 -4 5 185.72 9.52
4 0 0 727.07 20.07
0 -4 0 725.18 19.95
0 4 0 700.47 19.55
0 4 2 353.05 11.47
0 -4 2 324.07 11.40
-4 0 -2 334.84 10.52
0 4 -2 331.93 11.24
0 -4 2 321.82 9.59
4 0 -4 143.01 8.17
4 0 4 149.44 8.46
-4 0 4 163.61 9.45
0 -4 4 169.39 9.01
0 4 -4 149.98 8.26
0 -4 4 154.44 8.57
0 4 4 136.88 8.21
4 0 6 15.73 2.17
0 4 6 13.62 1.99
0 -4 6 13.54 2.01
-4 0 6 19.63 2.44
-1 4 1 9636.07 258.57
1 -4 -1 9764.72 258.41
-4 -1 -1 9999.00 257.92
1 -4 1 9753.37 258.39
-1 4 -1 9611.70 258.83
-4 -1 -3 335.22 11.38
4 1 -3 346.79 12.85
-4 -1 3 328.97 13.20
-1 4 3 323.84 12.88
-1 4 -3 322.08 12.27
-4 -1 5 105.58 7.23
-1 4 5 113.38 7.17
1 -4 5 114.95 7.22
4 2 0 417.83 11.77
2 -4 0 434.49 12.39
2 -4 2 219.31 6.67
2 -4 -2 202.99 6.59
-2 4 2 207.68 8.09
-4 -2 2 215.99 8.65
-2 4 -2 210.37 7.95
4 2 -2 211.95 8.17
-4 -2 -2 221.33 7.01
-4 -2 4 39.65 4.75
-2 4 4 33.94 4.26
4 2 4 37.71 4.25
2 -4 4 29.70 3.98
2 -4 4 34.11 4.16
-4 -2 4 30.31 3.91
-2 4 4 30.46 3.60
-2 4 -4 26.82 3.41
2 -4 6 72.89 4.08
4 2 6 77.26 4.28
-4 -2 6 74.53 4.32
-2 4 6 71.78 4.13
3 -4 1 719.26 19.90
3 -4 -1 709.97 19.89
-3 4 -1 674.56 20.05
-4 -3 3 136.28 7.47
-3 4 -3 131.93 6.56
4 3 -3 135.58 7.03
-3 4 3 128.57 7.10
-3 4 5 11.82 2.76
-4 -3 5 11.43 2.73
4 3 -5 11.25 2.68
4 3 5 10.86 2.72
3 -4 5 13.88 2.89
4 -4 0 168.17 5.94
-4 4 2 238.38 9.44
-4 -4 2 245.81 9.62
4 4 -2 241.80 9.31
-4 4 -2 258.86 9.02
4 -4 2 255.13 8.04
4 -4 -2 242.31 7.99
4 4 -4 44.94 4.74
4 -4 4 55.99 5.18
4 -4 -4 50.30 4.74
4 4 4 46.07 4.49
-4 4 -4 48.24 4.33
4 -4 4 53.62 4.97
-4 -4 4 57.05 5.13
4 4 -4 43.38 4.49
4 -4 6 63.29 3.55
-4 -4 6 60.05 3.63
-4 4 6 55.14 3.44
5 -4 -1 1141.94 31.54
-5 4 -1 1156.56 31.49
5 -4 1 1115.07 31.52
4 5 -1 1089.52 31.61
-5 4 3 32.34 3.71
-4 -5 3 43.43 4.05
5 -4 3 39.16 3.71
-5 4 -3 35.67 3.23
5 -4 5 21.96 3.38
4 5 5 22.70 3.25
-4 -5 5 22.50 3.44
-5 4 5 15.98 3.11
4 5 -5 23.03 3.22
-5 4 5 18.30 2.74
3 5 0 118.32 4.67
3 5 0 119.13 3.84
5 -3 0 109.17 4.56
5 -3 -2 2187.51 61.21
-3 -5 -2 2250.72 61.04
-3 -5 2 2238.94 61.02
3 5 -2 2307.17 62.68
-3 -5 2 2356.15 62.70
5 -3 2 2299.48 61.23
-5 3 -2 2251.42 61.83
3 5 4 26.72 3.66
-3 -5 4 26.23 3.74
-3 -5 4 34.26 4.24
5 -3 -4 28.03 3.66
-5 3 4 41.45 4.75
3 5 -4 28.15 3.84
3 5 -4 35.03 3.93
5 -3 4 32.67 3.92
5 -3 4 30.24 3.89
-3 -5 6 11.65 1.73
-5 3 6 11.13 1.73
3 5 6 9.90 1.54
2 5 -1 994.55 27.39
2 5 -1 1017.71 27.54
2 5 1 962.85 27.34
5 -2 1 969.16 27.32
-2 -5 1 980.84 27.32
5 -2 -1 968.49 27.31
-5 2 -1 968.43 27.13
-2 -5 3 219.58 9.42
-5 2 -3 204.02 8.12
-5 2 3 178.35 9.19
2 5 -3 183.58 8.74
5 -2 5 40.96 4.26
2 5 -5 41.81 4.06
-2 -5 5 50.44 4.71
2 5 5 44.09 4.43
-5 2 5 50.93 5.02
5 -1 0 29.15 1.97
1 5 0 25.34 1.49
1 5 0 26.26 1.85
-1 -5 -2 502.07 14.76
1 5 -2 497.41 16.19
-5 1 -2 532.64 15.47
-1 -5 2 518.56 16.25
-1 -5 2 517.88 14.79
1 5 4 12.93 3.03
1 5 -4 16.95 3.02
1 5 4 14.40 2.52
-1 -5 4 8.14 2.96
-1 -5 4 18.34 3.32
5 -1 4 15.49 3.09
5 -1 -4 18.52 3.25
5 -1 6 9.39 1.78
1 5 6 6.67 1.50
-1 -5 6 11.05 1.81
5 0 -1 3349.37 88.48
0 -5 1 3391.24 88.20
0 -5 1 3262.09 88.33
5 0 1 3335.04 88.51
0 5 1 3203.31 88.08
0 -5 -1 3321.39 88.33
-5 0 -3 526.78 16.78
5 0 -3 534.42 18.47
-5 0 3 519.72 18.95
0 5 -3 555.57 18.32
0 -5 5 34.51 4.08
-5 0 5 34.52 4.26
5 0 5 33.29 3.85
0 5 5 33.70 3.88
5 1 0 2950.51 79.79
1 -5 0 2995.12 79.60
-1 5 2 145.53 4.88
-1 5 2 136.00 5.99
-5 -1 -2 133.08 4.95
-1 5 -2 125.93 5.89
-1 5 -2 135.09 4.81
1 -5 2 141.87 4.85
1 -5 -2 134.32 4.78
-1 5 -4 74.46 5.61
5 1 -4 75.95 5.86
1 -5 4 73.15 5.83
-5 -1 4 74.92 6.41
-1 5 4 69.78 5.25
-1 5 4 63.91 5.62
-1 5 6 59.83 3.42
1 -5 6 56.35 3.40
-5 -1 6 51.12 3.58
2 -5 -1 3037.69 78.06
2 -5 1 2978.92 78.02
-2 5 1 2811.88 77.87
-2 5 -1 2810.14 78.19
-5 -2 3 285.19 12.29
-2 5 -3 292.32 11.35
-2 5 3 307.48 12.07
5 2 -3 287.60 11.79
2 -5 5 16.23 3.00
5 2 -5 12.94 2.82
5 2 5 18.59 3.31
-2 5 5 12.29 2.85
-5 -2 5 11.62 2.92
3 -5 0 1.30 1.20
5 3 0 -0.05 0.68
-3 5 2 209.47 8.26
3 -5 2 215.06 7.12
-3 5 -2 219.46 8.19
5 3 -2 222.82 8.53
3 -5 -2 205.29 7.07
-5 -3 4 19.87 3.33
3 -5 4 14.70 3.05
5 3 -4 22.14 3.28
5 3 -4 16.39 3.18
-3 5 4 22.06 3.53
-3 5 4 21.18 3.20
3 -5 4 22.32 3.51
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21 6 -1 79.80 5.94
21 6 1 82.61 6.06
-6 21 1 90.73 6.74
-6 21 3 11.14 2.25
21 6 -3 10.62 1.86
21 6 -3 12.04 2.10
-21 -6 3 17.19 2.38
-6 21 -3 14.60 2.57
21 7 0 32.09 3.70
21 7 0 28.38 3.78
21 7 0 29.64 3.86
-7 21 2 183.94 8.86
-7 21 -2 170.68 8.19
7 -21 -2 157.22 7.91
7 -21 2 166.88 7.99
21 7 2 181.52 8.35
21 7 -2 184.03 8.68
21 7 -2 174.30 8.58
-7 21 2 180.33 9.07
-8 21 1 31.39 3.53
21 8 1 34.36 3.64
21 8 1 36.70 3.75
21 8 -1 39.56 4.18
21 8 1 44.14 4.17
-8 21 1 46.88 4.58
-8 21 3 43.27 3.44
21 8 -3 42.05 3.01
21 8 -3 42.07 3.25
-8 21 -3 46.60 3.72
21 9 0 31.80 3.34
21 9 0 28.74 3.59
21 9 0 23.46 3.32
-9 21 2 19.35 2.89
21 9 -2 22.04 2.87
9 -21 -2 17.32 2.59
21 9 -2 16.03 2.66
-10 21 1 38.18 3.58
10 -21 -1 38.50 4.16
10 -21 1 40.71 4.26
21 10 -1 37.78 3.81
-10 21 3 2.01 1.20
21 10 -3 0.32 1.01
-10 21 -3 0.55 1.24
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21 11 0 17.81 2.67
21 11 0 19.57 2.70
11 -21 0 15.67 3.09
-11 21 2 9.29 2.00
21 11 -2 14.81 2.34
21 11 -2 12.81 2.09
12 -21 -1 37.84 3.77
12 -21 1 31.73 3.49
21 12 -1 38.95 3.52
21 12 -1 32.00 3.25
-13 21 0 30.23 3.42
13 -21 0 29.46 3.42
-13 21 2 18.46 2.05
21 13 -2 13.48 1.83
21 14 -1 6.66 1.61
14 -21 -1 7.44 1.90
14 -21 1 3.65 1.64
15 -21 0 -0.65 1.62
16 -21 -1 23.13 2.07
16 -21 1 19.80 1.99
17 -21 0 8.22 1.42
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22 -13 -1 82.83 4.62
22 -13 1 83.73 4.63
22 -12 0 11.97 2.39
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22 -11 -1 8.35 2.14
22 -11 1 9.88 2.22
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22 -9 -1 51.32 4.58
22 -9 1 51.87 4.53
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22 -8 0 3.67 1.75
8 22 0 4.13 1.87
22 -8 0 1.81 2.27
8 22 -2 5.64 1.86
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8 22 -2 4.87 1.89
22 -8 2 6.74 1.62
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22 -7 1 72.77 5.06
7 22 -1 77.01 5.58
22 -7 1 68.42 4.97
22 -7 -1 73.83 5.61
22 -7 1 77.69 5.61
7 22 1 74.58 5.60
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22 -6 0 30.47 3.54
22 -6 0 26.33 3.93
6 22 2 14.02 2.70
22 -6 -2 9.61 2.25
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22 -6 2 16.66 2.58
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22 -5 1 79.84 5.64
5 22 -1 82.39 6.06
22 -5 -1 76.78 5.90
22 -5 1 68.54 5.63
5 22 1 80.17 6.15
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22 -4 0 12.82 3.02
22 -4 2 60.18 4.62
22 -4 -2 49.17 4.18
22 -4 2 52.98 4.35
4 22 2 59.15 5.07
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3 22 1 9.61 3.04
22 -3 1 13.26 2.92
22 -3 -1 11.99 3.04
22 -3 1 14.95 3.10
3 22 -1 12.75 3.11
22 -3 -1 12.22 2.53
3 22 -1 8.95 2.27
3 22 -3 21.16 2.58
-22 3 3 19.62 2.73
3 22 -3 16.19 2.48
2 22 0 -0.42 2.24
22 -2 0 -1.28 2.38
22 -2 0 -1.79 1.85
2 22 -2 69.64 5.36
22 -2 2 60.44 4.98
2 22 -2 60.55 5.05
2 22 2 65.34 5.53
22 -1 1 12.46 2.92
1 22 1 16.61 2.98
22 -1 -1 13.13 3.11
22 -1 1 12.28 3.28
22 -1 -1 15.98 2.80
1 22 -1 15.81 2.90
1 22 -3 10.92 2.10
22 -1 3 9.78 2.01
22 0 0 24.76 3.90
0 22 0 17.82 3.56
22 0 0 18.30 3.21
0 22 2 2.02 2.41
0 22 2 1.96 1.77
22 0 2 2.67 1.99
0 22 -2 1.40 2.06
22 0 2 2.02 2.08
22 0 -2 2.92 1.62
0 22 -2 3.44 2.15
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22 1 -1 179.37 9.01
22 1 -1 161.37 9.17
22 1 1 164.17 9.17
-1 22 -1 162.01 8.67
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-1 22 -3 34.29 3.08
-22 -1 3 32.07 3.41
22 2 0 -0.43 2.32
22 2 0 1.89 2.01
-2 22 2 17.49 3.32
-2 22 2 14.38 2.71
-2 22 -2 8.07 2.43
22 2 2 14.13 2.75
22 2 -2 11.20 2.26
22 2 -2 12.88 2.49
-2 22 -2 7.95 2.39
-3 22 1 122.62 7.13
22 3 1 135.81 7.86
-3 22 -1 143.16 8.43
22 3 -1 118.58 7.27
22 3 -1 134.89 7.82
-3 22 1 147.13 8.87
-3 22 3 28.85 2.91
-3 22 -3 25.80 2.47
22 3 -3 19.60 2.17
-22 -3 3 23.54 2.91
-4 22 0 11.31 3.25
22 4 0 13.03 2.91
-4 22 2 6.64 2.53
-4 22 2 5.77 2.15
-4 22 -2 4.30 2.01
22 4 2 5.41 2.13
22 4 -2 6.71 2.03
22 4 -2 5.22 1.96
-4 22 -2 4.69 2.05
-5 22 1 2.85 2.30
-5 22 1 4.36 1.88
22 5 1 4.01 2.23
-5 22 -1 6.03 2.56
22 5 -1 7.07 2.42
22 5 -1 3.46 1.96
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22 5 -3 16.28 1.96
-22 -5 3 13.79 2.07
22 6 0 22.24 3.18
-6 22 2 54.22 4.43
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6 -22 -2 55.41 4.13
6 -22 2 52.81 4.11
22 6 2 62.47 4.44
22 6 -2 66.82 4.64
22 6 -2 65.30 4.75
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-7 22 1 11.47 2.30
22 7 1 11.08 2.36
22 7 1 14.40 2.55
22 7 -1 17.13 2.86
-7 22 3 15.79 2.07
22 7 -3 20.01 2.07
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22 8 0 126.18 6.76
22 8 0 126.28 7.15
-8 22 2 5.65 1.87
22 8 -2 6.78 1.84
22 8 -2 3.04 1.62
-22 -8 2 3.45 1.59
-9 22 1 3.30 1.71
22 9 -1 2.86 1.73
9 -22 -1 0.30 1.89
9 -22 1 1.21 2.08
22 10 0 1.06 1.54
10 -22 0 -1.27 2.20
-10 22 2 8.61 1.74
22 10 -2 5.61 1.72
22 11 -1 3.79 1.50
11 -22 -1 3.81 1.84
11 -22 1 6.88 2.23
22 11 -1 2.78 1.53
12 -22 0 0.26 1.62
22 12 0 2.90 1.40
22 12 -2 9.80 1.59
22 12 -2 6.69 1.44
22 13 -1 19.97 2.19
13 -22 -1 18.55 2.33
13 -22 1 18.05 2.42
22 13 -1 15.63 1.93
14 -22 0 27.85 2.76
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23 -13 0 0.54 1.22
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23 -12 -1 8.30 1.65
23 -12 1 8.22 1.61
23 -11 0 6.73 2.08
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23 -10 -1 17.81 2.43
23 -10 1 13.54 2.27
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9 23 -2 28.54 2.59
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8 23 -1 12.34 2.34
23 -8 1 13.43 2.14
23 -8 -1 11.43 2.40
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23 -7 0 65.23 4.66
23 -7 0 69.39 5.42
7 23 0 75.03 5.31
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23 -7 2 36.19 2.91
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6 23 1 10.70 2.60
23 -6 1 8.08 2.16
6 23 -1 11.85 2.76
23 -6 -1 9.27 2.52
23 -6 1 7.64 2.46
23 -6 1 11.17 2.34
6 23 -3 24.19 2.11
23 -5 0 4.51 1.86
5 23 0 6.04 2.19
23 -5 0 7.96 2.62
23 -5 2 45.16 3.68
-23 5 2 49.16 4.07
5 23 2 47.97 4.10
5 23 -2 46.85 3.73
4 23 1 20.89 3.36
23 -4 1 16.63 2.73
23 -4 -1 21.41 3.22
23 -4 1 15.53 2.98
4 23 -1 17.24 3.07
4 23 -3 8.20 1.65
-23 4 3 10.50 1.67
3 23 0 37.47 4.20
23 -3 0 30.97 3.72
23 -3 0 35.45 4.29
3 23 2 16.37 2.83
3 23 -2 20.73 2.98
23 -3 2 17.99 2.64
3 23 -2 19.44 2.70
2 23 1 21.06 3.65
23 -2 1 25.05 3.31
23 -2 -1 13.65 3.10
23 -2 1 19.76 3.42
23 -2 -1 20.35 2.83
2 23 -3 41.27 3.04
-23 2 3 40.89 3.18
2 23 -3 40.29 3.09
23 -1 0 5.28 2.28
23 -1 0 6.29 2.60
1 23 0 4.62 2.44
23 -1 0 5.29 2.18
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23 -1 2 25.58 3.05
23 -1 -2 20.83 2.43
1 23 -2 29.40 3.28
0 23 1 33.30 4.29
0 23 -1 43.73 4.65
23 0 1 33.78 3.90
23 0 -1 35.26 4.01
23 0 1 30.82 3.96
23 0 -1 35.05 3.70
0 23 -3 53.78 3.38
-23 0 3 49.14 3.67
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23 1 0 0.79 2.14
23 1 0 -0.68 1.92
-1 23 2 1.38 2.09
-1 23 2 3.50 1.87
-1 23 -2 2.09 2.03
23 1 -2 2.73 1.55
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23 2 -1 87.14 5.72
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-23 -2 3 88.69 4.91
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23 3 0 228.46 10.45
23 3 0 213.55 10.14
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23 3 2 9.61 2.19
23 3 -2 6.48 1.76
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-4 23 1 14.31 2.36
23 4 1 18.52 2.97
-4 23 -1 19.64 3.18
23 4 -1 17.28 2.75
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-4 23 3 22.32 2.22
-23 -4 3 24.00 2.32
23 5 0 69.34 5.09
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23 5 2 35.51 3.28
23 5 -2 39.70 3.28
23 5 -2 40.89 3.50
-23 -5 2 34.14 3.53
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23 6 1 57.48 4.32
23 6 1 57.11 4.36
23 6 -1 61.34 4.55
23 6 -1 49.85 4.33
-6 23 1 55.81 4.78
-7 23 0 24.25 3.33
23 7 0 24.61 2.95
23 7 0 19.97 2.87
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23 7 -2 2.22 1.50
23 7 -2 1.09 1.36
-23 -7 2 1.11 1.26
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23 8 -1 7.90 2.02
8 -23 -1 8.38 2.35
8 -23 1 4.57 1.89
9 -23 0 84.45 5.56
23 9 0 84.28 5.14
-9 23 2 52.13 3.37
23 9 -2 56.02 3.49
23 9 -2 47.56 3.41
10 -23 -1 8.11 2.01
10 -23 1 6.52 1.88
23 10 -1 6.98 1.76
11 -23 0 169.69 7.62
23 11 0 152.29 6.71
12 -23 -1 6.52 1.56
12 -23 1 8.36 1.58
13 -23 0 23.58 2.45
24 -12 0 19.63 2.08
24 -11 -1 18.10 1.92
24 -11 1 23.01 2.05
24 -10 0 25.11 2.81
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24 -9 -1 0.38 1.47
24 -9 1 1.91 1.51
24 -8 0 22.44 2.33
24 -8 0 27.96 3.12
8 24 -2 1.40 1.08
7 24 1 3.22 1.70
24 -7 -1 2.94 1.38
24 -7 -1 2.58 1.78
24 -7 1 3.26 1.79
7 24 -1 2.62 1.58
24 -7 1 4.59 1.49
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24 -6 0 48.83 3.73
24 -6 0 42.95 4.09
6 24 0 48.90 4.17
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6 24 -2 6.98 1.73
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5 24 1 10.13 2.32
24 -5 -1 10.64 2.09
24 -5 1 8.14 1.87
24 -5 -1 6.96 2.09
24 -5 1 6.62 2.10
5 24 -1 6.51 2.16
24 -5 1 4.27 1.73
24 -4 0 25.12 3.06
4 24 0 27.60 3.31
24 -4 0 25.68 3.44
24 -4 2 24.49 2.55
-24 4 2 23.10 2.74
4 24 2 25.93 2.91
3 24 1 26.13 3.51
24 -3 1 19.78 2.76
24 -3 -1 29.48 3.38
24 -3 1 27.98 3.29
24 -3 1 29.86 3.28
3 24 -1 32.16 3.52
24 -2 0 9.77 2.58
2 24 0 8.88 2.49
2 24 -2 65.53 4.54
24 -2 2 74.74 4.51
2 24 2 63.49 4.68
2 24 -2 59.46 3.99
24 -1 1 4.30 1.79
24 -1 -1 1.92 1.47
0 24 0 41.33 4.40
24 0 0 49.29 4.30
24 0 0 46.25 4.66
0 24 -2 58.24 4.36
24 0 2 54.57 4.09
24 0 -2 53.21 3.38
-24 0 2 67.66 4.66
0 24 2 59.32 4.63
0 24 -2 55.99 3.86
-1 24 1 30.20 3.91
-1 24 -1 35.38 3.86
24 1 -1 32.14 3.29
24 2 0 1.47 1.61
-2 24 2 17.26 2.75
-2 24 -2 17.15 2.47
24 2 2 15.38 2.30
24 2 -2 15.99 2.07
-24 -2 2 17.92 2.64
-2 24 -2 13.47 2.09
-3 24 1 24.31 3.34
24 3 1 19.02 2.73
-3 24 -1 21.16 3.13
24 3 1 18.49 2.71
24 3 -1 23.61 2.90
24 4 0 3.55 1.73
24 4 0 5.39 1.97
-4 24 2 4.84 1.89
-4 24 2 3.51 1.48
24 4 2 3.88 1.55
24 4 -2 5.54 1.49
-24 -4 2 5.97 1.81
-4 24 -2 2.40 1.30
-5 24 1 18.03 2.83
24 5 1 13.21 2.28
24 5 1 13.60 2.28
24 5 -1 21.11 2.65
-6 24 0 11.80 2.48
24 6 0 14.14 2.30
24 6 -2 3.81 1.25
-24 -6 2 4.00 1.43
-6 24 -2 2.83 1.37
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24 7 -1 0.74 1.14
24 7 -1 2.94 1.68
7 -24 -1 0.92 1.60
7 -24 1 2.05 1.62
8 -24 0 103.74 5.81
24 8 0 94.38 5.19
9 -24 -1 8.91 1.90
9 -24 1 5.26 1.62
24 9 -1 6.85 1.61
10 -24 0 0.62 1.53
11 -24 -1 46.78 2.98
11 -24 1 50.29 3.02
12 -24 0 7.85 1.52
25 -9 0 0.34 1.23
25 -8 -1 48.29 3.15
25 -8 1 50.85 3.19
25 -7 0 84.28 4.94
6 25 -1 27.92 2.60
25 -6 1 23.78 2.30
25 -6 -1 26.11 2.60
25 -6 1 25.29 2.65
6 25 1 29.60 2.66
6 25 -1 30.17 2.59
5 25 0 17.54 2.56
25 -5 0 15.63 2.19
25 -5 0 14.39 2.44
5 25 -2 13.59 1.77
4 25 1 3.55 1.72
25 -4 -1 2.71 1.39
25 -4 1 2.74 1.33
25 -4 -1 4.53 1.75
25 -4 1 5.13 1.71
4 25 -1 3.39 1.68
25 -4 1 3.78 1.56
3 25 0 5.02 2.06
25 -3 0 2.76 1.58
25 -3 0 3.24 1.87
3 25 -2 21.08 2.31
-25 3 2 20.76 2.19
2 25 1 2.95 1.86
25 -2 -1 1.32 1.39
25 -2 1 3.78 1.61
2 25 -1 1.27 1.74
25 -2 1 2.93 1.77
25 -1 0 54.78 4.12
1 25 -2 85.60 4.54
25 -1 2 76.86 4.26
0 25 -1 32.38 3.39
25 0 -1 33.09 3.13
25 0 1 36.10 3.25
25 0 1 38.77 3.41
0 25 1 35.55 3.63
-1 25 0 114.38 6.70
-1 25 -2 2.24 1.26
-25 -1 2 4.22 1.59
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25 2 1 45.98 3.63
25 2 -1 38.62 3.25
-2 25 1 41.00 3.76
25 3 0 356.42 13.00
-3 25 0 365.64 13.75
-25 -3 2 6.50 1.53
-4 25 1 12.52 2.28
25 4 -1 13.68 1.98
25 4 1 12.88 1.95
25 4 1 10.03 1.95
25 4 -1 15.22 2.12
25 5 0 32.64 2.94
-5 25 0 31.53 3.17
-6 25 1 10.66 1.87
-6 25 -1 14.41 1.96
25 6 -1 14.20 1.77
25 6 -1 16.81 2.07
6 -25 -1 11.58 1.97
6 -25 1 10.47 1.92
-7 25 0 2.19 1.39
7 -25 0 2.51 1.57
8 -25 -1 47.72 3.04
8 -25 1 43.27 2.98
9 -25 0 -0.34 1.23
26 -6 0 1.97 1.28
4 26 0 3.84 1.48
26 -4 0 8.44 1.49
26 -4 0 6.82 1.48
26 -3 1 39.24 2.83
3 26 1 40.75 3.10
3 26 -1 36.33 2.98
26 -2 0 24.70 2.47
2 26 0 29.03 2.88
26 -1 -1 5.67 1.56
26 -1 1 6.30 1.56
0 26 0 3.24 1.69
26 0 0 2.87 1.35
-1 26 1 3.29 1.61
26 2 0 74.25 4.23
-2 26 0 73.00 4.62
-3 26 1 4.81 1.55
-3 26 -1 4.46 1.50
26 3 -1 5.17 1.32
26 3 1 5.69 1.38
26 4 0 360.13 11.72
26 4 0 350.89 11.63
-4 26 0 334.79 12.07
5 -26 1 8.50 1.50
6 -26 0 0.16 1.22
-1 27 0 13.92 1.81
0 0 0 0.00 0.00
TITL 4PYBdan1_auto in I4/m
REM I4/m (#87 in standard setting)
CELL 1.54184 21.565903 21.565903 5.086325 90.0000 90.0000 90.0000
ZERR 7.00 0.000329 0.000329 0.000119 0.0000 0.0000 0.0000
LATT 2
SYMM -x,-y, z
SYMM -y, x, z
SYMM y,-x, z
SFAC C H B N
UNIT 105.00 84.00 7.00 21.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 33436
_shelx_res_file
;
TITL 4PYBdan1_auto in I-4 #82
CELL 1.54184 21.5659 21.5659 5.0863 90 90 90
ZERR 8 0.0003 0.0003 0.0001 0 0 0
LATT -2
SYMM +Y,-X,-Z
SYMM -X,-Y,+Z
SYMM -Y,+X,-Z
SFAC C H N B
UNIT 120 96 24 8
L.S. 10 0 0
PLAN 2
SIZE 0.2 0.05 0.05
TEMP -173
CONF
BOND
fmap 2 53
MORE -1
BOND $H
ACTA
REM
REM
REM
WGHT 0.050200 0.178900
FVAR 0.42071
N3 3 0.200411 0.031499 -0.004094 11.00000 0.02358 0.02382 =
0.02254 -0.00032 -0.00041 0.00170
C7 1 0.288675 0.154970 0.513201 11.00000 0.02725 0.02523 =
0.02326 0.00251 -0.00006 0.00159
AFIX 43
H7 2 0.332368 0.160393 0.507136 11.00000 -1.20000
AFIX 0
C1 1 0.392646 -0.017772 -0.506260 11.00000 0.02292 0.02633 =
0.03174 0.00040 0.00164 0.00038
AFIX 43
H1 2 0.431493 -0.003178 -0.568928 11.00000 -1.20000
AFIX 0
N2 3 0.293945 0.079336 0.158717 11.00000 0.02028 0.02249 =
0.02229 0.00085 0.00121 0.00122
C13 1 0.100218 0.058949 0.182047 11.00000 0.02537 0.02604 =
0.02865 0.00416 0.00023 -0.00007
AFIX 43
H13 2 0.079731 0.032355 0.061113 11.00000 -1.20000
AFIX 0
C10 1 0.158947 0.140424 0.537559 11.00000 0.03125 0.02351 =
0.02164 0.00677 0.00423 0.00579
C15 1 0.194549 0.106415 0.349052 11.00000 0.02620 0.02017 =
0.01927 0.00530 0.00217 0.00455
C5 1 0.315733 -0.089471 -0.512920 11.00000 0.02724 0.02450 =
0.03010 -0.00433 -0.00204 -0.00080
AFIX 43
H5 2 0.298892 -0.127018 -0.579573 11.00000 -1.20000
AFIX 0
C6 1 0.260121 0.114207 0.341449 11.00000 0.02698 0.02005 =
0.01827 0.00504 0.00162 0.00269
C14 1 0.163867 0.065134 0.172825 11.00000 0.02705 0.02095 =
0.02138 0.00569 0.00181 0.00255
C11 1 0.093634 0.131340 0.545188 11.00000 0.03013 0.02834 =
0.02782 0.00679 0.00938 0.00881
AFIX 43
H11 2 0.069325 0.152653 0.672058 11.00000 -1.20000
AFIX 0
B1 4 0.265790 0.037531 -0.018090 11.00000 0.02545 0.01940 =
0.02120 0.00408 0.00008 0.00270
C3 1 0.304108 -0.001456 -0.224245 11.00000 0.02272 0.02282 =
0.02037 0.00173 -0.00335 0.00298
C4 1 0.281474 -0.057011 -0.327137 11.00000 0.02229 0.02740 =
0.02899 -0.00001 -0.00025 -0.00081
AFIX 43
H4 2 0.242561 -0.072653 -0.269997 11.00000 -1.20000
AFIX 0
C12 1 0.065637 0.091913 0.369982 11.00000 0.02477 0.02904 =
0.03191 0.00917 0.00505 0.00437
AFIX 43
H12 2 0.021908 0.086776 0.375805 11.00000 -1.20000
AFIX 0
N1 3 0.370869 -0.071176 -0.603641 11.00000 0.02723 0.02630 =
0.02699 -0.00345 -0.00151 0.00383
C2 1 0.361836 0.017557 -0.319118 11.00000 0.02528 0.02103 =
0.02760 -0.00122 -0.00090 -0.00092
AFIX 43
H2A 2 0.380061 0.054745 -0.255464 11.00000 -1.20000
AFIX 0
C9 1 0.190056 0.181270 0.710940 11.00000 0.03828 0.02426 =
0.02051 0.00138 0.00423 0.00916
AFIX 43
H9 2 0.167044 0.203905 0.838041 11.00000 -1.20000
AFIX 0
C8 1 0.253101 0.188413 0.696871 11.00000 0.03870 0.02233 =
0.02261 0.00097 -0.00193 0.00352
AFIX 43
H8 2 0.273166 0.216442 0.813167 11.00000 -1.20000
AFIX 0
H3 2 0.180397 0.005833 -0.124768 11.00000 0.04157
H2 2 0.336380 0.087018 0.166713 11.00000 0.02821
HKLF 4
REM 4PYBdan1_auto in I-4 #82
REM R1 = 0.0314 for 2125 Fo > 4sig(Fo) and 0.0341 for all 2268 data
REM 180 parameters refined using 0 restraints
END
WGHT 0.0489 0.2065
REM Highest difference peak 0.152, deepest hole -0.155, 1-sigma level 0.035
Q1 1 0.2863 0.0197 -0.1386 11.00000 0.05 0.15
Q2 1 0.1767 0.1166 0.4714 11.00000 0.05 0.13
;
_shelx_res_checksum 65534
_shelxl_version_number 20.13
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+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
N N3 0.20041(7) 0.03150(8) -0.0041(4) 0.0233(4) Uani d 1 . .
C C7 0.28868(9) 0.15497(9) 0.5132(4) 0.0252(4) Uani d 1 . .
H H7 0.3324 0.1604 0.5071 0.030 Uiso calc 1 . .
C C1 0.39265(9) -0.01777(9) -0.5063(4) 0.0270(4) Uani d 1 . .
H H1 0.4315 -0.0032 -0.5689 0.032 Uiso calc 1 . .
N N2 0.29394(8) 0.07934(7) 0.1587(3) 0.0217(3) Uani d 1 . .
C C13 0.10022(9) 0.05895(9) 0.1820(4) 0.0267(4) Uani d 1 . .
H H13 0.0797 0.0324 0.0611 0.032 Uiso calc 1 . .
C C10 0.15895(9) 0.14042(9) 0.5376(4) 0.0255(4) Uani d 1 . .
C C15 0.19455(9) 0.10642(8) 0.3491(4) 0.0219(4) Uani d 1 . .
C C5 0.31573(9) -0.08947(9) -0.5129(4) 0.0273(4) Uani d 1 . .
H H5 0.2989 -0.1270 -0.5796 0.033 Uiso calc 1 . .
C C6 0.26012(9) 0.11421(8) 0.3414(4) 0.0218(4) Uani d 1 . .
C C14 0.16387(9) 0.06513(9) 0.1728(4) 0.0231(4) Uani d 1 . .
C C11 0.09363(10) 0.13134(9) 0.5452(4) 0.0288(5) Uani d 1 . .
H H11 0.0693 0.1527 0.6721 0.035 Uiso calc 1 . .
B B1 0.26579(10) 0.03753(10) -0.0181(4) 0.0220(4) Uani d 1 . .
C C3 0.30411(9) -0.00146(9) -0.2242(4) 0.0220(4) Uani d 1 . .
C C4 0.28147(9) -0.05701(9) -0.3271(4) 0.0262(4) Uani d 1 . .
H H4 0.2426 -0.0727 -0.2700 0.031 Uiso calc 1 . .
C C12 0.06564(9) 0.09191(9) 0.3700(4) 0.0286(5) Uani d 1 . .
H H12 0.0219 0.0868 0.3758 0.034 Uiso calc 1 . .
N N1 0.37087(8) -0.07118(8) -0.6036(3) 0.0268(4) Uani d 1 . .
C C2 0.36184(9) 0.01756(9) -0.3191(4) 0.0246(4) Uani d 1 . .
H H2A 0.3801 0.0547 -0.2555 0.030 Uiso calc 1 . .
C C9 0.19006(10) 0.18127(9) 0.7109(4) 0.0277(5) Uani d 1 . .
H H9 0.1670 0.2039 0.8380 0.033 Uiso calc 1 . .
C C8 0.25310(10) 0.18841(9) 0.6969(4) 0.0279(4) Uani d 1 . .
H H8 0.2732 0.2164 0.8132 0.033 Uiso calc 1 . .
H H3 0.1804(12) 0.0058(12) -0.125(6) 0.042(7) Uiso d 1 . .
H H2 0.3364(11) 0.0870(10) 0.167(5) 0.028(6) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N3 0.0236(8) 0.0238(8) 0.0225(8) 0.0017(6) -0.0004(7) -0.0003(7)
C7 0.0272(9) 0.0252(9) 0.0233(10) 0.0016(8) -0.0001(8) 0.0025(8)
C1 0.0229(9) 0.0263(9) 0.0317(10) 0.0004(8) 0.0016(9) 0.0004(9)
N2 0.0203(8) 0.0225(7) 0.0223(8) 0.0012(6) 0.0012(7) 0.0008(7)
C13 0.0254(10) 0.0260(9) 0.0287(10) -0.0001(8) 0.0002(9) 0.0042(9)
C10 0.0313(10) 0.0235(9) 0.0216(10) 0.0058(8) 0.0042(8) 0.0068(8)
C15 0.0262(9) 0.0202(8) 0.0193(9) 0.0045(7) 0.0022(8) 0.0053(7)
C5 0.0272(10) 0.0245(9) 0.0301(10) -0.0008(8) -0.0020(9) -0.0043(8)
C6 0.0270(9) 0.0200(8) 0.0183(9) 0.0027(7) 0.0016(8) 0.0050(8)
C14 0.0271(9) 0.0209(9) 0.0214(9) 0.0025(7) 0.0018(8) 0.0057(8)
C11 0.0301(10) 0.0283(10) 0.0278(11) 0.0088(8) 0.0094(9) 0.0068(8)
B1 0.0254(10) 0.0194(9) 0.0212(10) 0.0027(8) 0.0001(9) 0.0041(9)
C3 0.0227(9) 0.0228(9) 0.0204(9) 0.0030(7) -0.0033(7) 0.0017(7)
C4 0.0223(9) 0.0274(9) 0.0290(10) -0.0008(8) -0.0003(8) 0.0000(9)
C12 0.0248(9) 0.0290(10) 0.0319(11) 0.0044(8) 0.0051(9) 0.0092(9)
N1 0.0272(9) 0.0263(8) 0.0270(9) 0.0038(7) -0.0015(7) -0.0034(7)
C2 0.0253(9) 0.0210(9) 0.0276(10) -0.0009(8) -0.0009(8) -0.0012(8)
C9 0.0383(11) 0.0243(10) 0.0205(10) 0.0092(8) 0.0042(9) 0.0014(8)
C8 0.0387(11) 0.0223(9) 0.0226(10) 0.0035(8) -0.0019(9) 0.0010(8)
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'
B B 0.0090 0.0039 '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
C14 N3 B1 . . 123.02(17) ?
C14 N3 H3 . . 118.1(17) ?
B1 N3 H3 . . 118.8(17) ?
C6 C7 H7 . . 119.9 ?
C6 C7 C8 . . 120.13(18) ?
C8 C7 H7 . . 119.9 ?
N1 C1 H1 . . 118.0 ?
N1 C1 C2 . . 123.90(18) ?
C2 C1 H1 . . 118.0 ?
C6 N2 B1 . . 122.82(16) ?
C6 N2 H2 . . 112.8(15) ?
B1 N2 H2 . . 124.4(15) ?
C14 C13 H13 . . 119.9 ?
C14 C13 C12 . . 120.1(2) ?
C12 C13 H13 . . 119.9 ?
C11 C10 C15 . . 118.62(19) ?
C9 C10 C15 . . 118.83(18) ?
C9 C10 C11 . . 122.54(18) ?
C6 C15 C10 . . 119.37(18) ?
C6 C15 C14 . . 121.14(17) ?
C14 C15 C10 . . 119.49(17) ?
C4 C5 H5 . . 118.0 ?
N1 C5 H5 . . 118.0 ?
N1 C5 C4 . . 124.06(18) ?
C7 C6 N2 . . 121.89(17) ?
C7 C6 C15 . . 119.97(17) ?
N2 C6 C15 . . 118.14(16) ?
N3 C14 C15 . . 117.81(16) ?
C13 C14 N3 . . 122.15(18) ?
C13 C14 C15 . . 120.03(18) ?
C10 C11 H11 . . 119.9 ?
C12 C11 C10 . . 120.23(18) ?
C12 C11 H11 . . 119.9 ?
N3 B1 C3 . . 120.36(18) ?
N2 B1 N3 . . 117.04(18) ?
N2 B1 C3 . . 122.60(17) ?
C4 C3 B1 . . 121.57(17) ?
C4 C3 C2 . . 115.74(18) ?
C2 C3 B1 . . 122.68(17) ?
C5 C4 C3 . . 120.12(18) ?
C5 C4 H4 . . 119.9 ?
C3 C4 H4 . . 119.9 ?
C13 C12 H12 . . 119.3 ?
C11 C12 C13 . . 121.46(18) ?
C11 C12 H12 . . 119.3 ?
C5 N1 C1 . . 116.03(17) ?
C1 C2 C3 . . 120.15(17) ?
C1 C2 H2A . . 119.9 ?
C3 C2 H2A . . 119.9 ?
C10 C9 H9 . . 119.7 ?
C8 C9 C10 . . 120.51(19) ?
C8 C9 H9 . . 119.7 ?
C7 C8 H8 . . 119.4 ?
C9 C8 C7 . . 121.19(19) ?
C9 C8 H8 . . 119.4 ?
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
N3 C14 . 1.399(3) ?
N3 B1 . 1.418(3) ?
N3 H3 . 0.93(3) ?
C7 H7 . 0.9500 ?
C7 C6 . 1.384(3) ?
C7 C8 . 1.408(3) ?
C1 H1 . 0.9500 ?
C1 N1 . 1.339(3) ?
C1 C2 . 1.389(3) ?
N2 C6 . 1.401(2) ?
N2 B1 . 1.411(3) ?
N2 H2 . 0.93(2) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.380(3) ?
C13 C12 . 1.405(3) ?
C10 C15 . 1.431(3) ?
C10 C11 . 1.423(3) ?
C10 C9 . 1.416(3) ?
C15 C6 . 1.425(3) ?
C15 C14 . 1.426(3) ?
C5 H5 . 0.9500 ?
C5 C4 . 1.389(3) ?
C5 N1 . 1.335(3) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.372(3) ?
B1 C3 . 1.578(3) ?
C3 C4 . 1.396(3) ?
C3 C2 . 1.397(3) ?
C4 H4 . 0.9500 ?
C12 H12 . 0.9500 ?
C2 H2A . 0.9500 ?
C9 H9 . 0.9500 ?
C9 C8 . 1.370(3) ?
C8 H8 . 0.9500 ?
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
N2 H2 N1 6_554 0.93(2) 2.21(2) 3.113(2) 162(2) 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
N3 B1 C3 C4 . . . . -23.9(3) ?
N3 B1 C3 C2 . . . . 154.92(19) ?
N2 B1 C3 C4 . . . . 156.09(19) ?
N2 B1 C3 C2 . . . . -25.1(3) ?
C10 C15 C6 C7 . . . . -0.8(3) ?
C10 C15 C6 N2 . . . . 178.65(16) ?
C10 C15 C14 N3 . . . . -178.38(17) ?
C10 C15 C14 C13 . . . . 1.0(3) ?
C10 C11 C12 C13 . . . . 0.9(3) ?
C10 C9 C8 C7 . . . . -0.8(3) ?
C15 C10 C11 C12 . . . . -1.7(3) ?
C15 C10 C9 C8 . . . . 0.5(3) ?
C6 C7 C8 C9 . . . . 0.3(3) ?
C6 N2 B1 N3 . . . . -0.3(3) ?
C6 N2 B1 C3 . . . . 179.77(16) ?
C6 C15 C14 N3 . . . . 1.4(3) ?
C6 C15 C14 C13 . . . . -179.24(18) ?
C14 N3 B1 N2 . . . . 0.6(3) ?
C14 N3 B1 C3 . . . . -179.47(17) ?
C14 C13 C12 C11 . . . . 0.9(3) ?
C14 C15 C6 C7 . . . . 179.45(17) ?
C14 C15 C6 N2 . . . . -1.1(3) ?
C11 C10 C15 C6 . . . . -179.01(17) ?
C11 C10 C15 C14 . . . . 0.7(3) ?
C11 C10 C9 C8 . . . . 179.81(19) ?
B1 N3 C14 C13 . . . . 179.50(19) ?
B1 N3 C14 C15 . . . . -1.1(3) ?
B1 N2 C6 C7 . . . . 179.99(18) ?
B1 N2 C6 C15 . . . . 0.5(3) ?
B1 C3 C4 C5 . . . . 178.49(18) ?
B1 C3 C2 C1 . . . . -178.13(18) ?
C4 C5 N1 C1 . . . . -0.6(3) ?
C4 C3 C2 C1 . . . . 0.7(3) ?
C12 C13 C14 N3 . . . . 177.53(17) ?
C12 C13 C14 C15 . . . . -1.8(3) ?
N1 C1 C2 C3 . . . . -1.1(3) ?
N1 C5 C4 C3 . . . . 0.3(3) ?
C2 C1 N1 C5 . . . . 0.9(3) ?
C2 C3 C4 C5 . . . . -0.4(3) ?
C9 C10 C15 C6 . . . . 0.3(3) ?
C9 C10 C15 C14 . . . . -179.93(16) ?
C9 C10 C11 C12 . . . . 179.00(18) ?
C8 C7 C6 N2 . . . . -178.96(17) ?
C8 C7 C6 C15 . . . . 0.5(3) ?