#------------------------------------------------------------------------------
#$Date: 2022-08-24 04:30:33 +0300 (Wed, 24 Aug 2022) $
#$Revision: 277366 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244149.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_2244149
loop_
_publ_author_name
'Cheng, Dong'
'Meng, Xiang-Zhen'
'Tian, Fuyu'
'Yan, Dong'
'Wang, Xiaofei'
'Qian, Xueli'
'Wang, Junnan'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of
4-(3-methoxyphenyl)-2,6-diphenylpyridine
;
_journal_coeditor_code PK2666
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989022007812
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C24 H19 N O'
_chemical_formula_moiety 'C24 H19 N O'
_chemical_formula_sum 'C24 H19 N O'
_chemical_formula_weight 337.40
_chemical_name_systematic
;
4-(3-Methoxyphenyl)-2,6-diphenylpyridine
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha 90
_cell_angle_beta 100.7290(10)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 18.6588(2)
_cell_length_b 5.47390(10)
_cell_length_c 35.5689(5)
_cell_measurement_reflns_used 6287
_cell_measurement_temperature 200.00(10)
_cell_measurement_theta_max 71.3510
_cell_measurement_theta_min 2.5510
_cell_volume 3569.37(9)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2017/1 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 200.00(10)
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single'
_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 0.0156
_diffrn_reflns_av_unetI/netI 0.0181
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -4
_diffrn_reflns_limit_l_max 43
_diffrn_reflns_limit_l_min -42
_diffrn_reflns_number 8525
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 71.540
_diffrn_reflns_theta_min 2.529
_diffrn_source 'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu 0.593
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.74648
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2017)
;
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_density_diffrn 1.256
_exptl_crystal_description block
_exptl_crystal_F_000 1424
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.187
_refine_diff_density_min -0.151
_refine_ls_extinction_coef 0.00128(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2017/1 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 0.997
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 237
_refine_ls_number_reflns 3417
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.997
_refine_ls_R_factor_all 0.0363
_refine_ls_R_factor_gt 0.0343
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.7292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0971
_refine_ls_wR_factor_ref 0.0988
_reflns_number_gt 3189
_reflns_number_total 3417
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file pk2666sup1.cif
_cod_data_source_block I
_cod_database_code 2244149
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 -2 12.42 0.29
0 0 -4 3307.29 61.62
0 0 -6 3262.81 60.85
0 0 -8 736.70 13.94
0 0 -10 458.14 8.82
0 0 -12 1277.07 24.12
0 0 -14 368.38 7.30
0 0 -16 73.35 1.83
0 0 -18 0.07 0.14
0 0 -20 40.86 1.28
0 0 -22 288.56 6.08
0 0 -24 15.22 0.99
0 0 -24 16.31 0.79
0 0 24 15.73 1.07
0 0 -26 102.80 3.09
0 0 26 94.42 3.22
0 0 -28 285.65 6.86
0 0 28 295.63 7.14
0 0 -30 958.76 19.66
0 0 30 1001.35 20.21
0 0 -30 984.93 19.88
0 0 32 229.84 6.00
0 0 -32 222.47 5.62
0 0 34 991.58 20.43
0 0 36 37.34 1.82
0 0 38 25.90 1.41
0 0 40 36.90 1.56
0 0 42 134.72 3.35
0 1 1 1.74 0.16
0 1 -1 1.03 0.14
0 1 3 72.26 1.53
0 1 -3 65.66 1.50
0 -1 -3 66.61 1.50
0 -1 -3 70.19 1.42
0 -1 -5 315.51 5.94
0 1 -5 302.69 6.01
0 -1 -5 306.26 6.04
0 -1 -7 3828.21 71.32
0 1 -7 3811.86 71.39
0 -1 -9 8.16 0.37
0 1 -9 7.58 0.25
0 1 -9 7.28 0.38
0 1 -11 111.00 2.53
0 -1 -11 114.55 2.53
0 1 -11 113.44 2.30
0 -1 -11 115.71 2.58
0 1 -13 486.53 9.49
0 1 -13 479.41 9.19
0 -1 -13 474.27 9.52
0 -1 -13 486.86 9.48
0 1 -15 286.04 5.63
0 -1 -15 285.69 5.95
0 1 -15 288.05 5.96
0 -1 -15 289.92 5.98
0 -1 -17 27.55 1.07
0 -1 -17 28.20 1.06
0 -1 -19 215.36 4.75
0 1 -19 212.53 4.79
0 1 -21 27.78 1.17
0 -1 -21 26.56 1.12
0 -1 23 354.37 8.34
0 1 -23 367.24 7.76
0 1 23 359.16 8.27
0 -1 -23 384.92 7.92
0 1 -23 373.00 8.37
0 1 -23 378.50 8.05
0 1 -25 2.90 0.49
0 -1 25 2.16 0.50
0 1 25 1.38 0.43
0 1 -25 2.34 0.54
0 -1 -25 2.31 0.38
0 1 27 44.72 1.98
0 1 -27 43.93 1.83
0 -1 27 44.20 2.04
0 -1 -27 42.89 1.63
0 1 -27 45.66 2.02
0 1 29 1134.80 23.00
0 1 -29 1149.01 23.06
0 -1 -29 1129.74 22.30
0 1 -29 1121.24 22.74
0 -1 29 1153.85 23.18
0 1 31 57.87 2.38
0 -1 31 60.95 2.56
0 1 -31 60.18 2.46
0 -1 33 135.32 4.10
0 1 33 127.00 3.88
0 1 -33 130.18 3.90
0 1 -35 68.29 2.47
0 1 35 67.89 2.50
0 -1 35 70.69 2.67
0 -1 37 16.25 1.19
0 1 37 15.74 1.04
0 1 -37 15.43 1.02
0 -1 39 7.04 0.74
0 1 -39 7.36 0.61
0 1 39 6.86 0.63
0 -1 41 0.31 0.33
0 1 41 0.55 0.26
0 2 0 593.04 11.70
0 -2 0 612.72 11.58
0 -2 -2 12.72 0.51
0 -2 -2 13.65 0.44
0 2 -2 13.01 0.57
0 2 -4 10.58 0.52
0 2 4 10.86 0.51
0 -2 -4 11.35 0.40
0 -2 -4 10.37 0.48
0 2 -6 31.42 1.04
0 -2 -6 34.15 1.03
0 -2 -6 33.46 0.87
0 -2 -8 28.74 0.82
0 -2 -8 27.80 0.96
0 2 -8 27.49 0.97
0 -2 -10 56.52 1.46
0 -2 -10 57.12 1.63
0 2 -12 333.27 6.92
0 -2 -12 325.81 6.68
0 -2 -12 339.36 6.90
0 2 -14 189.43 4.31
0 -2 -14 188.53 4.12
0 -2 -14 191.91 4.31
0 2 -16 21.09 1.01
0 -2 -16 21.71 0.89
0 2 -18 30.14 1.30
0 -2 -18 33.23 1.21
0 -2 -20 31.88 1.27
0 -2 -20 31.47 1.33
0 2 -20 33.10 1.58
0 -2 20 30.91 1.45
0 2 20 31.84 1.46
0 2 -20 32.07 1.24
0 2 -22 7.93 0.72
0 2 -22 7.18 0.78
0 -2 22 6.38 0.68
0 2 -22 7.17 0.58
0 -2 -22 7.08 0.64
0 2 -24 543.95 11.75
0 2 -24 529.41 11.40
0 -2 24 518.61 11.55
0 2 -24 541.85 10.96
0 -2 -24 536.91 11.22
0 -2 26 25.81 1.49
0 2 -26 23.28 1.34
0 -2 -26 27.75 1.33
0 2 -26 26.10 1.21
0 -2 28 1.73 0.51
0 -2 30 0.77 0.45
0 2 -30 0.71 0.58
0 -2 32 84.05 2.98
0 2 -32 88.59 3.05
0 2 -34 6.78 0.79
0 -2 34 5.82 0.74
0 2 -36 1.32 0.46
0 -2 36 1.91 0.47
0 -2 38 23.28 1.18
0 2 -38 22.86 1.12
0 2 -40 0.11 0.25
0 -2 40 0.06 0.23
0 3 -1 24.11 0.97
0 3 1 25.12 0.97
0 -3 -3 475.46 9.61
0 3 3 505.72 9.73
0 3 -3 474.95 9.77
0 3 -5 5.34 0.47
0 -3 -5 5.19 0.41
0 -3 -7 65.39 1.85
0 3 -7 64.54 1.93
0 -3 -9 1350.92 26.28
0 3 -9 1383.46 26.38
0 -3 -11 117.65 3.04
0 3 -11 119.89 3.11
0 3 -13 153.14 3.91
0 3 13 147.21 4.13
0 -3 -13 159.64 3.82
0 3 -15 5.04 0.54
0 3 -15 5.01 0.56
0 3 15 4.54 0.62
0 -3 -15 4.74 0.51
0 3 -15 4.88 0.57
0 3 -17 8.53 0.75
0 3 17 7.48 0.79
0 -3 -17 7.69 0.66
0 3 -17 7.96 0.76
0 3 -17 9.56 0.71
0 3 19 39.66 1.88
0 3 -19 38.69 1.76
0 -3 -19 37.53 1.56
0 3 -19 39.61 1.51
0 3 -19 39.13 1.71
0 -3 -21 102.69 3.03
0 3 21 100.98 3.38
0 3 -21 103.43 2.86
0 3 -21 98.17 3.16
0 3 -21 103.74 3.30
0 -3 -23 117.99 3.43
0 3 23 123.43 3.81
0 3 -25 14.36 1.16
0 3 25 14.80 1.15
0 3 -25 14.44 0.91
0 3 27 11.29 0.98
0 3 -27 9.57 0.74
0 3 -27 11.17 1.03
0 3 -29 23.83 1.44
0 3 -31 0.16 0.44
0 3 -33 7.68 0.77
0 3 -35 12.86 0.86
0 3 -37 14.92 0.80
0 4 0 0.79 0.36
0 4 2 22.01 1.51
0 4 2 22.33 1.26
0 4 4 32.58 1.88
0 4 4 34.94 1.64
0 4 6 166.01 5.02
0 4 6 156.16 4.38
0 4 8 424.17 9.64
0 4 8 441.95 10.50
0 4 10 33.35 1.70
0 4 -10 34.61 1.60
0 4 10 38.06 2.18
0 4 12 422.72 10.39
0 4 -12 412.34 9.10
0 4 12 407.39 9.41
0 4 -14 0.20 0.31
0 4 14 -0.07 0.49
0 -4 -14 0.29 0.27
0 4 -16 48.21 1.80
0 4 16 46.96 2.13
0 -4 -16 45.90 1.77
0 4 -18 1.85 0.44
0 4 18 0.92 0.51
0 4 20 0.20 0.46
0 4 -20 0.73 0.46
0 4 22 49.54 2.23
0 4 -22 52.32 1.79
0 4 24 2.28 0.57
0 4 -24 1.34 0.43
0 4 -24 2.14 0.49
0 4 -26 50.74 1.68
0 4 26 51.00 2.11
0 4 -26 53.03 1.98
0 4 28 111.71 3.22
0 4 -28 103.27 3.03
0 4 30 25.67 1.19
0 4 30 26.88 1.60
0 4 -30 25.42 1.17
0 4 32 99.46 3.11
0 4 -32 99.37 2.60
0 5 -1 0.43 0.39
0 5 1 0.16 0.40
0 5 1 0.07 0.35
0 5 3 269.27 6.50
0 5 5 2.62 0.59
0 5 7 40.05 1.84
0 5 -7 36.47 1.70
0 5 -9 60.28 2.19
0 5 9 64.14 2.45
0 5 9 61.05 2.87
0 5 -11 6.61 0.67
0 5 11 5.56 0.78
0 5 11 6.75 0.97
0 5 13 3.10 0.64
0 5 -13 3.93 0.51
0 5 13 3.70 0.80
0 5 -15 15.52 0.88
0 5 15 13.28 1.31
0 5 15 14.72 1.13
0 5 -17 168.89 3.98
0 5 17 164.95 5.15
0 5 19 0.34 0.47
0 5 19 0.04 0.42
0 5 -19 0.52 0.36
0 5 -21 25.00 0.99
0 5 21 26.59 1.60
0 5 21 26.39 1.39
0 5 23 3.37 0.55
0 5 23 3.97 0.64
0 5 25 11.34 0.79
0 5 27 19.56 0.91
0 6 4 89.60 2.49
0 6 6 44.69 1.59
0 6 6 45.46 1.74
0 6 8 1.79 0.39
0 6 8 0.93 0.41
0 6 10 13.52 0.92
0 6 10 15.55 0.88
0 6 12 4.65 0.56
0 6 12 5.20 0.53
0 6 14 0.69 0.36
0 6 14 0.95 0.31
0 6 16 1.07 0.29
0 6 16 0.88 0.33
0 6 18 3.83 0.40
0 6 18 4.02 0.44
-1 0 43 0.02 0.22
-1 0 41 0.08 0.28
-1 0 39 -0.04 0.38
-1 0 37 -0.21 0.46
-1 0 35 0.27 0.42
-1 0 33 -0.10 0.45
1 0 -31 0.44 0.41
-1 0 31 0.05 0.48
1 0 -29 0.28 0.35
-1 0 29 0.09 0.40
1 0 -27 -0.11 0.34
-1 0 27 -0.25 0.37
1 0 -25 0.14 0.31
-1 0 25 0.90 0.39
1 0 -23 0.51 0.21
1 0 -21 0.67 0.20
1 0 -19 0.14 0.15
1 0 -17 0.01 0.14
1 0 -15 2.28 0.24
1 0 -13 0.06 0.12
1 0 -11 0.23 0.13
1 0 -9 0.25 0.11
1 0 -7 0.34 0.12
1 0 -7 0.16 0.09
1 0 -5 0.02 0.06
1 0 -5 8.64 0.25
-1 0 3 0.09 0.03
1 0 -3 0.13 0.04
-1 0 1 14.91 0.17
1 0 -1 0.07 0.02
-1 0 -1 0.48 0.04
-1 0 -3 0.70 0.07
-1 0 -5 0.29 0.09
-1 0 -7 0.52 0.13
-1 0 -9 1.12 0.16
-1 0 -11 2.55 0.22
-1 0 -13 1.91 0.22
-1 0 -15 0.88 0.19
-1 0 -17 -0.01 0.14
-1 0 -19 1.89 0.26
-1 0 -21 0.33 0.17
-1 0 -23 -0.02 0.16
1 0 23 -0.04 0.28
1 0 25 0.20 0.36
-1 0 -25 -0.17 0.33
-1 0 -27 0.29 0.38
1 0 27 0.39 0.47
-1 0 -29 -0.04 0.42
1 0 29 -0.14 0.43
-1 0 -31 0.19 0.44
1 0 31 0.65 0.53
1 0 33 0.41 0.55
1 0 35 -0.04 0.50
1 0 37 0.58 0.44
1 0 39 0.13 0.33
1 0 41 0.02 0.28
-1 -1 42 0.55 0.29
1 1 -40 31.34 1.22
-1 -1 40 32.07 1.45
-1 1 40 29.13 1.25
-1 1 38 29.63 1.42
1 1 -38 31.72 1.44
1 1 -36 93.08 2.99
-1 1 36 91.23 2.97
-1 -1 36 98.36 3.22
-1 1 34 96.14 3.19
-1 -1 34 103.31 3.44
-1 -1 32 400.15 9.42
-1 1 32 408.21 9.23
1 1 -32 392.39 9.23
1 1 -30 342.27 8.04
-1 1 30 349.35 8.27
1 1 -30 355.69 8.34
-1 -1 30 360.50 8.48
-1 -1 28 102.47 3.40
1 1 -28 97.46 3.08
1 -1 -28 101.36 2.87
1 1 -28 105.23 3.39
-1 1 28 102.32 3.32
-1 1 26 19.32 1.23
-1 -1 26 19.97 1.31
1 1 -26 19.33 1.26
1 -1 -26 19.40 1.01
1 1 -26 18.72 1.10
1 1 -24 0.28 0.27
-1 1 24 0.14 0.31
-1 -1 24 0.64 0.39
1 1 -24 0.08 0.28
1 1 -24 0.20 0.37
1 -1 -24 0.05 0.21
1 1 -22 82.25 2.29
1 -1 -22 88.38 2.43
1 1 -22 86.19 2.79
1 -1 -20 772.98 15.09
1 1 -20 756.57 15.02
1 -1 -20 749.05 14.96
1 -1 -18 82.76 2.22
1 -1 -18 81.68 2.20
1 -1 -16 20.87 0.86
1 -1 -16 20.58 0.86
1 -1 -14 680.88 13.39
1 -1 -14 693.91 13.37
1 1 -12 50.04 1.10
1 -1 -12 50.97 1.40
1 -1 -12 52.70 1.36
1 -1 -10 34.12 0.97
1 1 -10 35.33 0.98
1 1 -10 35.39 0.77
1 -1 -10 35.48 1.04
1 -1 -8 1698.65 30.42
1 1 -8 1710.22 30.44
1 1 -6 2951.26 55.31
1 -1 -6 2968.41 55.29
-1 1 4 4935.83 92.35
1 -1 -4 4909.99 92.25
1 1 -4 4996.79 92.24
-1 -1 2 0.12 0.04
1 -1 -2 0.19 0.09
-1 1 2 0.15 0.12
1 1 -2 0.07 0.10
-1 1 0 1007.37 18.75
1 1 0 1000.70 18.65
-1 -1 0 980.55 18.62
-1 1 -2 3239.29 59.95
-1 -1 -2 3299.49 59.86
-1 -1 -2 3131.97 59.73
1 1 2 3274.69 59.84
-1 -1 -4 5024.26 90.93
-1 -1 -4 4752.19 91.05
-1 1 -4 4749.22 91.08
-1 -1 -6 74.25 1.58
-1 1 -6 72.37 1.68
-1 -1 -6 73.56 1.68
-1 -1 -8 38.51 0.99
-1 1 -8 39.43 1.08
-1 1 -8 40.21 0.91
-1 -1 -10 120.78 2.64
-1 1 -10 122.38 2.72
-1 1 -10 123.28 2.49
-1 1 -12 9.15 0.50
-1 1 -12 9.99 0.37
-1 -1 -12 9.96 0.48
-1 -1 -12 9.94 0.52
-1 1 -14 4.82 0.27
-1 -1 -14 3.83 0.36
-1 1 -14 4.41 0.40
-1 -1 -14 4.26 0.36
-1 1 -16 300.94 5.96
-1 1 -16 304.85 6.32
-1 -1 -16 296.64 6.27
-1 1 -18 114.04 2.89
-1 -1 -18 115.55 2.85
-1 -1 -20 0.88 0.27
-1 1 -20 0.60 0.27
1 -1 22 0.11 0.30
-1 -1 -22 0.21 0.22
-1 1 -22 0.08 0.25
-1 1 -22 0.04 0.31
-1 1 -22 0.60 0.27
1 1 22 0.06 0.27
-1 1 -24 75.86 2.64
-1 1 -24 78.90 2.48
1 -1 24 72.14 2.66
1 1 24 75.34 2.60
-1 -1 -24 79.33 2.30
1 -1 26 259.99 6.57
-1 1 -26 272.81 6.53
1 1 26 254.74 6.43
-1 -1 -26 265.00 5.95
-1 1 -26 263.61 6.28
1 1 28 9.37 0.93
-1 1 -28 8.39 0.80
-1 -1 -28 7.85 0.67
1 -1 28 9.11 0.95
-1 1 -28 7.62 0.87
-1 1 -30 478.04 10.56
1 1 30 471.66 10.56
1 -1 30 465.85 10.72
-1 1 -32 4.53 0.76
1 -1 32 4.48 0.74
1 1 32 3.14 0.63
-1 1 -34 101.46 3.20
1 -1 34 103.98 3.38
1 1 34 97.46 3.18
1 -1 36 29.86 1.59
1 1 36 29.37 1.48
-1 1 -36 29.24 1.42
1 -1 38 34.11 1.59
-1 1 -38 32.76 1.37
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17 1 16 60.94 2.55
17 -1 16 62.98 2.42
17 1 16 69.23 2.42
17 -1 16 65.28 2.39
17 -1 18 77.27 2.57
17 1 18 80.46 2.51
17 -1 18 75.91 2.50
17 -1 20 111.69 3.14
17 1 20 116.28 3.10
17 -1 20 114.24 3.10
17 1 22 0.61 0.30
17 2 -31 8.69 0.62
-17 2 31 9.81 0.63
17 2 -29 4.39 0.48
-17 2 29 4.00 0.47
17 2 -27 1.55 0.41
-17 2 27 1.50 0.38
17 2 -25 1.90 0.46
-17 2 25 2.46 0.46
17 2 -23 1.31 0.46
-17 2 23 0.82 0.36
17 2 -21 5.96 0.73
-17 2 21 6.34 0.69
17 2 -19 30.23 1.37
-17 2 19 32.08 1.52
17 2 -19 30.04 1.61
17 2 -17 19.18 1.11
-17 2 17 18.06 1.11
17 2 -17 17.28 1.25
17 2 -15 17.72 1.11
17 2 -15 16.13 1.21
17 2 -15 17.07 1.22
17 2 -13 31.67 1.60
17 2 -13 36.52 1.85
17 2 -13 31.98 1.70
17 2 -11 23.53 1.41
17 2 -11 22.97 1.52
17 2 -11 24.35 1.46
17 2 -9 0.27 0.42
17 2 -9 0.42 0.46
17 2 -9 -0.05 0.47
17 2 -7 20.20 1.39
17 2 -7 20.78 1.51
17 2 -7 19.39 1.31
17 2 -5 1.18 0.53
17 2 -5 0.89 0.51
17 2 -5 1.08 0.58
17 2 -3 29.79 1.77
17 2 -3 30.49 1.64
17 2 -1 39.42 2.09
17 2 -1 42.25 1.96
17 2 1 61.90 2.68
17 2 1 61.92 2.43
17 2 3 19.06 1.45
17 2 3 21.15 1.33
17 2 5 85.46 3.24
17 2 5 83.66 2.87
17 2 7 6.47 0.77
17 2 7 8.11 0.96
17 2 9 2.10 0.51
17 2 9 1.94 0.64
17 2 11 8.19 0.92
-17 2 -11 6.83 0.66
17 2 11 8.65 0.78
17 2 13 41.89 1.96
-17 2 -13 42.22 1.58
17 2 13 44.09 1.68
17 2 15 74.53 2.60
-17 2 -15 73.56 2.18
17 2 17 0.19 0.32
17 3 -24 28.38 1.13
17 3 -24 29.79 1.10
17 3 -22 3.80 0.44
-17 3 22 4.16 0.45
17 3 -20 34.04 1.36
17 3 -18 6.34 0.63
17 3 -18 5.73 0.42
17 3 -16 14.62 0.98
17 3 -14 26.40 1.41
17 3 -12 0.87 0.45
17 3 -12 1.37 0.49
17 3 -10 -0.13 0.42
17 3 -10 -0.18 0.45
17 3 -8 62.36 2.48
17 3 -8 58.88 2.45
17 3 -6 4.46 0.77
17 3 -6 3.99 0.73
17 3 -4 2.30 0.62
17 3 -2 23.80 1.53
17 3 0 3.41 0.71
17 3 0 4.47 0.75
17 3 2 22.31 1.49
17 3 2 21.98 1.39
17 3 4 5.11 0.76
17 3 4 4.95 0.73
17 3 6 23.76 1.45
17 3 6 18.13 1.21
17 3 8 53.83 2.23
17 3 10 8.61 0.85
17 3 12 25.58 1.34
17 3 12 24.05 1.18
17 3 14 -0.03 0.30
17 3 14 0.07 0.25
17 4 -19 2.43 0.30
17 4 -17 34.90 1.24
17 4 -15 0.70 0.28
17 4 -13 8.10 0.64
17 4 -11 25.13 1.17
17 4 -9 3.27 0.50
17 4 -7 0.93 0.36
17 4 -5 0.31 0.33
17 4 -5 0.50 0.35
17 4 -3 1.52 0.41
17 4 -3 1.45 0.39
17 4 -1 2.37 0.45
17 4 -1 1.74 0.38
17 4 1 30.60 1.38
17 4 1 29.44 1.26
17 4 3 25.67 1.23
17 4 3 25.34 1.10
17 4 5 22.58 1.10
17 4 5 21.49 0.95
17 4 7 85.83 2.42
-18 0 32 39.67 1.41
18 0 -32 42.74 1.41
18 0 -30 144.22 3.63
18 0 -28 54.43 1.94
18 0 -26 2.49 0.53
18 0 -24 21.55 1.30
18 0 -22 3.99 0.68
18 0 -20 358.78 8.41
18 0 -18 142.64 4.22
18 0 -16 22.87 1.47
18 0 -14 291.09 7.24
18 0 -12 541.75 12.01
18 0 -10 16.75 1.31
18 0 -8 70.36 2.80
18 0 -6 329.54 8.09
18 0 -4 867.71 18.28
18 0 -2 83.98 3.15
18 0 0 255.68 6.66
18 0 2 59.36 2.55
18 0 4 21.78 1.46
18 0 4 21.81 1.49
18 0 6 5.33 0.83
18 0 6 5.86 0.84
18 0 8 18.98 1.38
18 0 8 17.37 1.31
18 0 10 8.58 0.96
18 0 12 51.87 2.28
18 0 14 89.00 3.05
18 0 16 137.62 3.91
18 0 18 210.71 5.14
-18 1 31 3.90 0.43
-18 1 29 0.23 0.24
18 -1 -27 18.60 0.96
18 1 -27 17.50 1.08
18 -1 -25 0.50 0.32
18 1 -25 0.61 0.42
18 -1 -23 14.20 0.97
18 1 -23 14.46 1.08
18 -1 -21 15.50 1.06
18 1 -21 15.16 1.13
18 -1 -19 157.84 4.31
18 1 -19 152.23 4.42
18 -1 -17 28.62 1.53
18 1 -17 29.61 1.65
18 -1 -15 90.45 3.04
18 1 -15 88.98 3.16
18 -1 -13 11.03 1.00
18 1 -13 11.68 1.09
18 -1 -11 363.74 8.63
18 1 -11 383.63 8.89
18 1 -9 32.64 1.74
18 -1 -9 32.93 1.73
18 1 -9 34.53 1.86
18 1 -7 217.59 5.91
18 1 -7 237.32 6.11
18 -1 -7 220.33 5.84
18 1 -5 189.03 5.33
18 -1 -5 185.37 5.15
18 1 -3 48.89 2.31
18 -1 -3 51.32 2.23
18 1 -1 0.57 0.58
18 -1 -1 0.42 0.45
18 1 1 180.75 5.07
18 -1 1 167.26 4.85
18 1 3 12.31 1.15
18 -1 3 13.08 1.11
18 1 5 44.20 2.07
18 -1 5 40.68 1.94
18 1 7 0.74 0.53
18 -1 7 0.79 0.50
18 1 7 1.20 0.63
18 1 9 96.57 3.47
18 1 9 102.95 3.34
18 -1 9 105.59 3.31
18 1 11 1.45 0.54
18 -1 11 2.23 0.54
18 1 11 1.33 0.54
18 1 13 21.45 1.40
18 1 13 24.94 1.36
18 -1 13 24.95 1.36
18 1 15 10.92 0.97
18 1 15 11.11 0.86
18 -1 15 11.61 0.88
18 1 17 0.32 0.35
18 -1 17 0.71 0.35
18 1 17 0.95 0.40
-18 2 28 14.42 0.79
18 2 -28 15.79 0.81
-18 2 26 26.12 1.16
18 2 -26 28.65 1.24
-18 2 24 11.56 0.78
18 2 -24 11.74 0.84
-18 2 22 13.87 0.90
18 2 -22 15.51 1.01
18 2 -20 1.88 0.50
-18 2 20 1.96 0.40
18 2 -18 3.49 0.62
-18 2 18 3.84 0.50
18 2 -16 6.35 0.76
18 2 -14 15.47 1.13
18 2 -14 15.64 1.14
18 2 -12 22.00 1.38
18 2 -12 21.39 1.33
18 2 -10 22.37 1.45
18 2 -10 22.12 1.36
18 2 -8 0.30 0.43
18 2 -8 0.56 0.40
18 2 -8 0.45 0.48
18 2 -6 35.96 1.74
18 2 -6 34.86 1.90
18 2 -6 34.11 1.70
18 2 -4 4.60 0.70
18 2 -4 4.62 0.68
18 2 -4 3.93 0.74
18 2 -2 22.69 1.41
18 2 -2 21.94 1.50
18 2 -2 21.42 1.32
18 2 0 14.81 1.16
18 2 0 13.50 1.04
18 2 2 17.83 1.27
18 2 2 18.76 1.20
18 2 4 3.87 0.61
18 2 4 3.22 0.64
18 2 6 1.24 0.44
18 2 6 1.43 0.52
18 2 8 64.37 2.44
18 2 8 64.39 2.20
18 2 10 24.21 1.36
18 2 10 25.32 1.21
18 2 12 13.07 0.93
18 2 12 12.23 0.78
18 2 14 1.35 0.36
18 3 -21 4.37 0.40
18 3 -19 5.13 0.48
18 3 -17 6.46 0.57
18 3 -15 19.52 1.03
18 3 -13 37.22 1.54
18 3 -11 26.55 1.34
18 3 -11 29.98 1.52
18 3 -9 15.89 1.06
18 3 -9 16.35 1.16
18 3 -7 13.50 1.01
18 3 -7 13.77 1.06
18 3 -5 43.30 1.89
18 3 -5 47.66 2.01
18 3 -3 34.78 1.69
18 3 -1 1.47 0.52
18 3 1 0.64 0.44
18 3 1 0.85 0.44
18 3 3 69.06 2.48
18 3 3 69.62 2.44
18 3 5 8.28 0.79
18 3 5 7.21 0.74
18 3 7 4.50 0.60
18 3 7 2.95 0.49
18 3 9 16.02 0.98
18 3 9 15.53 0.92
18 3 11 45.43 1.62
18 3 11 45.27 1.57
18 4 -12 7.32 0.52
18 4 -10 5.45 0.47
18 4 -8 5.71 0.51
18 4 -6 17.29 0.89
18 4 -4 16.46 0.87
18 4 -2 41.16 1.45
18 4 -2 40.71 1.41
18 4 0 4.92 0.48
18 4 0 4.38 0.42
19 0 -29 -0.09 0.25
19 0 -27 0.19 0.30
19 0 -25 -0.16 0.33
19 0 -23 0.21 0.36
19 0 -21 0.08 0.40
19 0 -19 0.12 0.41
19 0 -17 -0.04 0.41
19 0 -15 -0.17 0.49
19 0 -13 -0.04 0.49
19 0 -11 0.68 0.49
19 0 -9 -0.05 0.47
19 0 -7 0.19 0.50
19 0 -5 -0.19 0.52
19 0 -3 0.10 0.51
19 0 -1 0.67 0.56
19 0 1 0.14 0.50
19 0 3 -0.18 0.52
19 0 5 0.04 0.51
19 0 7 0.34 0.46
19 0 9 -0.08 0.44
19 0 9 0.44 0.42
19 0 11 0.07 0.45
19 0 11 -0.11 0.38
19 0 13 0.20 0.35
19 0 15 0.23 0.30
-19 1 30 0.02 0.18
-19 1 28 -0.04 0.21
19 1 -26 4.59 0.57
-19 1 26 4.54 0.50
19 -1 -24 8.08 0.65
19 1 -24 6.84 0.72
19 -1 -22 57.65 2.03
19 1 -22 63.19 2.25
19 -1 -20 19.62 1.14
19 1 -20 20.97 1.27
19 -1 -18 40.99 1.74
19 1 -18 42.04 1.90
19 -1 -16 85.35 2.83
19 1 -16 91.72 3.04
19 -1 -14 2.13 0.55
19 1 -14 1.33 0.56
19 -1 -12 5.11 0.68
19 1 -12 6.34 0.85
19 -1 -10 213.87 5.58
19 1 -10 228.13 5.83
19 1 -8 274.84 6.76
19 -1 -8 275.68 6.77
19 1 -8 288.97 7.02
19 1 -6 11.77 1.03
19 -1 -6 11.69 1.01
19 1 -6 9.71 1.04
19 1 -4 69.48 2.67
19 1 -4 74.74 2.78
19 -1 -4 70.64 2.64
19 1 -2 30.36 1.70
19 -1 -2 28.02 1.55
19 1 0 39.30 1.91
19 -1 0 35.95 1.78
19 1 2 36.95 1.85
19 -1 2 36.27 1.77
19 1 4 2.59 0.66
19 -1 4 3.41 0.63
19 1 6 29.64 1.58
19 -1 6 32.58 1.58
19 1 8 0.84 0.46
19 -1 8 0.79 0.45
19 1 10 4.45 0.64
19 -1 10 5.15 0.66
19 1 12 7.04 0.70
19 -1 12 6.78 0.67
19 1 14 0.03 0.28
19 -1 14 0.08 0.30
19 1 16 49.27 1.60
19 2 -25 0.22 0.25
-19 2 25 0.08 0.17
-19 2 23 26.71 1.10
19 2 -23 32.21 1.29
-19 2 21 17.44 0.89
19 2 -21 21.99 1.12
19 2 -19 1.79 0.45
19 2 -17 25.84 1.35
19 2 -15 9.91 0.85
19 2 -13 194.06 5.00
19 2 -13 196.66 5.00
19 2 -11 38.93 1.78
19 2 -11 39.55 1.75
19 2 -9 55.59 2.25
19 2 -9 54.06 2.12
19 2 -7 12.11 1.05
19 2 -7 12.70 0.98
19 2 -5 49.86 2.18
19 2 -5 52.47 2.04
19 2 -3 0.21 0.40
19 2 -3 0.27 0.44
19 2 -1 8.76 0.93
19 2 -1 9.11 0.80
19 2 1 6.02 0.66
19 2 1 5.90 0.78
19 2 3 12.19 0.87
19 2 5 3.75 0.51
19 2 7 3.02 0.44
19 2 9 1.96 0.36
19 3 -16 0.57 0.23
19 3 -14 10.87 0.66
19 3 -12 4.54 0.46
19 3 -10 5.16 0.53
19 3 -10 5.33 0.63
19 3 -8 5.35 0.56
19 3 -8 5.68 0.65
19 3 -6 14.00 0.88
19 3 -6 13.06 0.94
19 3 -4 85.18 2.58
19 3 -4 84.18 2.68
19 3 -2 10.21 0.78
19 3 -2 9.75 0.83
19 3 0 51.85 1.85
19 3 2 31.83 1.36
19 3 4 21.84 1.05
19 3 4 19.31 1.04
19 3 6 67.11 2.07
20 0 -26 143.98 3.53
20 0 -24 164.74 4.08
20 0 -22 0.12 0.32
20 0 -20 16.49 1.05
20 0 -18 56.92 2.14
20 0 -16 17.35 1.15
20 0 -14 43.22 1.92
20 0 -12 89.77 2.98
20 0 -10 147.42 4.21
20 0 -8 424.55 9.54
20 0 -6 65.67 2.48
20 0 -4 10.84 1.00
20 0 -2 581.32 12.52
20 0 0 23.86 1.41
20 0 2 122.31 3.68
20 0 4 67.09 2.42
20 0 6 0.43 0.44
20 0 8 11.57 0.91
20 0 10 221.21 5.28
20 0 12 0.05 0.30
20 0 14 43.55 1.48
20 1 -25 1.28 0.35
-20 1 25 0.90 0.24
-20 1 23 21.82 1.00
20 -1 -23 23.84 1.01
20 -1 -21 3.06 0.43
20 1 -21 2.08 0.47
-20 1 21 2.36 0.37
20 -1 -19 53.45 1.89
20 1 -19 56.48 2.09
20 -1 -17 47.94 1.83
20 1 -17 53.13 2.05
20 -1 -15 11.83 0.87
20 1 -15 13.62 1.04
20 -1 -13 40.88 1.74
20 1 -13 44.76 1.91
20 -1 -11 16.83 1.10
20 1 -11 17.27 1.21
20 -1 -9 32.27 1.54
20 1 -9 33.34 1.66
20 -1 -7 40.06 1.75
20 1 -7 39.68 1.84
20 1 -5 56.71 2.15
20 -1 -5 57.69 2.17
20 1 -5 58.48 2.29
20 1 -3 11.95 0.96
20 -1 -3 12.52 0.96
20 1 -3 12.68 1.05
20 1 -1 21.80 1.30
20 1 -1 22.26 1.34
20 -1 -1 23.08 1.27
20 1 1 1.49 0.55
20 -1 1 1.70 0.48
20 1 3 98.08 3.03
20 -1 3 94.08 2.91
20 1 5 36.42 1.63
20 -1 5 36.20 1.56
20 1 7 18.68 1.09
20 -1 7 18.56 1.05
20 1 9 10.40 0.78
20 -1 9 11.32 0.78
20 1 11 20.02 0.99
20 -1 11 18.87 0.95
20 2 -22 22.58 0.98
20 2 -20 12.23 0.76
20 2 -18 27.89 1.24
20 2 -16 119.27 3.26
20 2 -14 70.13 2.28
20 2 -12 152.72 3.93
20 2 -12 150.79 3.96
20 2 -10 250.90 5.87
20 2 -10 244.87 5.81
20 2 -8 95.70 2.92
20 2 -8 92.27 2.80
20 2 -6 136.13 3.84
20 2 -6 140.81 3.71
20 2 -4 42.60 1.79
20 2 -4 38.57 1.60
20 2 -2 66.96 2.34
20 2 -2 61.59 2.09
20 2 0 40.97 1.75
20 2 0 38.46 1.52
20 2 2 3.37 0.47
20 2 2 3.48 0.56
20 2 4 11.63 0.87
20 2 4 12.08 0.74
20 2 6 12.66 0.87
20 2 6 12.15 0.68
20 2 8 0.76 0.32
20 3 -7 18.14 0.96
20 3 -5 14.15 0.84
20 3 -3 16.12 0.89
20 3 -1 5.04 0.50
21 0 -23 -0.06 0.25
21 0 -21 -0.12 0.28
21 0 -19 -0.22 0.29
21 0 -17 0.09 0.34
21 0 -15 0.48 0.37
21 0 -13 0.56 0.42
21 0 -11 -0.07 0.35
21 0 -9 0.10 0.38
21 0 -7 -0.17 0.39
21 0 -5 0.14 0.40
21 0 -3 0.07 0.41
21 0 -1 -0.10 0.37
21 0 1 -0.06 0.37
21 0 3 0.06 0.35
21 0 5 0.11 0.33
21 0 7 -0.13 0.31
21 0 9 0.29 0.29
21 1 -22 2.95 0.40
21 1 -20 55.21 1.87
21 -1 -18 32.15 1.25
21 1 -18 34.97 1.45
21 1 -16 5.48 0.64
21 -1 -16 4.73 0.52
21 -1 -14 16.27 0.93
21 1 -14 18.54 1.09
21 -1 -12 41.06 1.59
21 1 -12 44.73 1.77
21 -1 -10 1.33 0.41
21 1 -10 1.05 0.47
21 -1 -8 96.89 2.83
21 1 -8 99.70 3.01
21 -1 -6 13.43 0.89
21 1 -6 13.71 0.98
21 -1 -4 11.82 0.84
21 1 -4 13.01 0.95
21 -1 -2 161.07 4.11
21 1 -2 169.40 4.30
21 -1 0 2.62 0.45
21 1 0 2.34 0.47
21 1 0 2.45 0.42
21 -1 2 2.80 0.45
21 1 2 2.41 0.45
21 1 2 2.10 0.40
21 1 4 0.11 0.29
21 -1 4 0.33 0.28
21 1 4 0.03 0.25
21 1 6 16.47 0.87
21 1 6 16.28 0.90
21 -1 6 17.12 0.87
21 1 8 30.46 1.18
21 2 -17 1.08 0.29
21 2 -15 0.75 0.29
21 2 -13 107.39 2.83
21 2 -11 35.99 1.38
21 2 -9 16.18 0.86
21 2 -9 16.73 0.90
21 2 -7 27.69 1.19
21 2 -7 26.93 1.16
21 2 -5 32.00 1.32
21 2 -5 31.41 1.25
21 2 -3 36.09 1.42
21 2 -3 34.03 1.29
21 2 -1 40.98 1.54
21 2 -1 41.48 1.40
21 2 1 3.36 0.44
21 2 3 0.09 0.25
22 0 -18 4.01 0.43
22 0 -16 0.02 0.26
22 0 -14 15.62 0.90
22 0 -12 68.28 2.14
22 0 -10 23.35 1.14
22 0 -8 1.62 0.41
22 0 -6 13.73 0.86
22 0 -4 1.29 0.38
22 0 -2 27.63 1.22
22 0 0 61.70 1.96
22 0 2 120.96 3.09
22 0 4 94.69 2.50
22 1 -17 4.18 0.44
22 1 -15 0.47 0.29
22 1 -13 26.32 1.18
22 -1 -11 0.35 0.24
22 1 -11 -0.05 0.27
22 -1 -9 159.52 3.91
22 1 -9 184.22 4.22
22 -1 -7 2.14 0.36
22 1 -7 2.42 0.44
22 -1 -5 5.24 0.48
22 1 -5 4.63 0.53
22 -1 -3 9.20 0.61
22 1 -3 9.03 0.68
22 1 -1 3.03 0.43
22 1 1 42.57 1.47
0 0 0 0.00 0.00
TITL 9 in I2/a
REM I2/a (#15 in standard setting)
CELL 1.54184 18.658770 5.473899 35.568919 90.0000 100.7292 90.0000
ZERR 50.00 0.000244 0.000072 0.000490 0.0000 0.0013 0.0000
LATT 2
SYMM -x+1/2, y,-z
SFAC C H N O S
UNIT 50.00 50.00 50.00 50.00 50.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 70507
_shelx_res_file
;
TITL 9_a.res in I2/a
9.res
created by SHELXL-2017/1 at 15:57:42 on 02-May-2022
REM Old TITL 9 in I2/a
REM SHELXT solution in I2/a
REM R1 0.132, Rweak 0.059, Alpha 0.024, Orientation as input
REM Formula found by SHELXT: C21 N O
CELL 1.54184 18.6588 5.4739 35.5689 90 100.729 90
ZERR 8 0.0002 0.0001 0.0005 0 0.001 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H N O
UNIT 192 152 8 8
L.S. 20
PLAN 1
CONF
BOND $H
LIST 4
MORE -1
fmap 2
ACTA
REM
REM
REM
WGHT 0.055700 1.729200
EXTI 0.001283
FVAR 0.40207
O1 4 0.318763 0.101787 0.434099 11.00000 0.04054 0.04152 =
0.04869 0.00732 0.00895 -0.01142
N1 3 0.560386 0.989615 0.365108 11.00000 0.02512 0.02879 =
0.03006 0.00040 0.00501 -0.00057
C1 1 0.527941 1.006340 0.395763 11.00000 0.02437 0.02792 =
0.03011 0.00050 0.00453 0.00099
C2 1 0.466134 0.870642 0.398952 11.00000 0.02626 0.03247 =
0.03053 -0.00122 0.00757 -0.00095
AFIX 43
H2 2 0.445343 0.884525 0.420676 11.00000 -1.20000
AFIX 0
C3 1 0.435872 0.714848 0.369518 11.00000 0.02267 0.02938 =
0.03201 0.00088 0.00407 0.00055
C4 1 0.469014 0.700618 0.337658 11.00000 0.02610 0.03284 =
0.02916 -0.00217 0.00319 -0.00192
AFIX 43
H4 2 0.449647 0.600015 0.317211 11.00000 -1.20000
AFIX 0
C5 1 0.531473 0.838196 0.336577 11.00000 0.02463 0.02860 =
0.02869 0.00242 0.00295 0.00188
C6 1 0.570272 0.824654 0.303625 11.00000 0.02390 0.03258 =
0.02743 0.00381 0.00253 0.00281
C7 1 0.620059 1.005870 0.298437 11.00000 0.03598 0.03386 =
0.03554 0.00191 0.00867 -0.00190
AFIX 43
H7 2 0.628023 1.137188 0.315289 11.00000 -1.20000
AFIX 0
C8 1 0.657771 0.992256 0.268437 11.00000 0.03993 0.04493 =
0.04310 0.00889 0.01558 -0.00373
AFIX 43
H8 2 0.690790 1.114477 0.265319 11.00000 -1.20000
AFIX 0
C9 1 0.646727 0.798521 0.243101 11.00000 0.03857 0.05463 =
0.03201 0.00724 0.01339 0.00768
AFIX 43
H9 2 0.672523 0.789083 0.223154 11.00000 -1.20000
AFIX 0
C10 1 0.597085 0.619253 0.247671 11.00000 0.03691 0.04947 =
0.03332 -0.00696 0.00718 0.00339
AFIX 43
H10 2 0.589029 0.489378 0.230547 11.00000 -1.20000
AFIX 0
C11 1 0.559061 0.631482 0.277681 11.00000 0.03010 0.04008 =
0.03473 -0.00318 0.00622 -0.00274
AFIX 43
H11 2 0.525773 0.509472 0.280488 11.00000 -1.20000
AFIX 0
C12 1 0.370157 0.565471 0.371709 11.00000 0.02346 0.03093 =
0.03303 -0.00632 0.00802 -0.00115
C13 1 0.308598 0.577216 0.342615 11.00000 0.02937 0.04390 =
0.03282 -0.00077 0.00490 -0.00319
AFIX 43
H13 2 0.307468 0.684207 0.322203 11.00000 -1.20000
AFIX 0
C14 1 0.249430 0.428894 0.344368 11.00000 0.02597 0.05165 =
0.03834 -0.00560 0.00094 -0.00486
AFIX 43
H14 2 0.208289 0.439001 0.325132 11.00000 -1.20000
AFIX 0
C15 1 0.250028 0.265215 0.374186 11.00000 0.02541 0.04014 =
0.04420 -0.00974 0.01010 -0.00845
AFIX 43
H15 2 0.210233 0.163835 0.374717 11.00000 -1.20000
AFIX 0
C16 1 0.311146 0.255182 0.403291 11.00000 0.02998 0.03102 =
0.03695 -0.00453 0.01142 -0.00164
C17 1 0.370491 0.407755 0.402150 11.00000 0.02351 0.03243 =
0.03399 -0.00453 0.00418 -0.00117
AFIX 43
H17 2 0.410674 0.403553 0.422021 11.00000 -1.20000
AFIX 0
C18 1 0.561093 1.179599 0.426200 11.00000 0.02439 0.02909 =
0.03301 -0.00204 0.00507 0.00107
C19 1 0.602559 1.375313 0.417682 11.00000 0.03936 0.03174 =
0.03741 -0.00092 0.00971 -0.00382
AFIX 43
H19 2 0.609761 1.397731 0.392735 11.00000 -1.20000
AFIX 0
C20 1 0.633230 1.537122 0.445936 11.00000 0.05251 0.03336 =
0.05216 -0.00509 0.01105 -0.01360
AFIX 43
H20 2 0.661015 1.666984 0.439753 11.00000 -1.20000
AFIX 0
C21 1 0.623334 1.509287 0.483127 11.00000 0.05068 0.04245 =
0.04533 -0.01446 0.00473 -0.01001
AFIX 43
H21 2 0.643968 1.619274 0.501995 11.00000 -1.20000
AFIX 0
C22 1 0.582412 1.315984 0.491787 11.00000 0.06419 0.06564 =
0.03415 -0.01143 0.01269 -0.02359
AFIX 43
H22 2 0.574972 1.295836 0.516738 11.00000 -1.20000
AFIX 0
C23 1 0.552079 1.150668 0.463856 11.00000 0.05075 0.05116 =
0.03632 -0.00576 0.01181 -0.02267
AFIX 43
H23 2 0.525391 1.018874 0.470363 11.00000 -1.20000
AFIX 0
C24 1 0.264810 -0.084191 0.433856 11.00000 0.03940 0.03263 =
0.07032 0.00338 0.02239 -0.00405
AFIX 137
H24A 2 0.261990 -0.182605 0.411288 11.00000 -1.50000
H24B 2 0.218282 -0.009630 0.433972 11.00000 -1.50000
H24C 2 0.277951 -0.185138 0.456145 11.00000 -1.50000
AFIX 0
HKLF 4
REM 9_a.res in I2/a
REM R1 = 0.0343 for 3189 Fo > 4sig(Fo) and 0.0363 for all 3417 data
REM 237 parameters refined using 0 restraints
END
WGHT 0.0476 1.7299
REM Highest difference peak 0.187, deepest hole -0.151, 1-sigma level 0.031
Q1 1 0.3987 0.6464 0.3703 11.00000 0.05 0.19
;
_shelx_res_checksum 96752
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.31876(5) 0.10179(16) 0.43410(2) 0.0435(2) Uani d 1 . .
N N1 0.56039(4) 0.98962(16) 0.36511(2) 0.0280(2) Uani d 1 . .
C C1 0.52794(5) 1.00634(19) 0.39576(3) 0.0275(2) Uani d 1 . .
C C2 0.46613(5) 0.87064(19) 0.39895(3) 0.0295(2) Uani d 1 . .
H H2 0.445343 0.884525 0.420676 0.035 Uiso calc 1 . .
C C3 0.43587(5) 0.71485(19) 0.36952(3) 0.0282(2) Uani d 1 . .
C C4 0.46901(5) 0.7006(2) 0.33766(3) 0.0296(2) Uani d 1 . .
H H4 0.449647 0.600015 0.317211 0.036 Uiso calc 1 . .
C C5 0.53147(5) 0.83820(19) 0.33658(3) 0.0276(2) Uani d 1 . .
C C6 0.57027(5) 0.8247(2) 0.30363(3) 0.0283(2) Uani d 1 . .
C C7 0.62006(6) 1.0059(2) 0.29844(3) 0.0349(3) Uani d 1 . .
H H7 0.628023 1.137188 0.315289 0.042 Uiso calc 1 . .
C C8 0.65777(7) 0.9923(2) 0.26844(3) 0.0416(3) Uani d 1 . .
H H8 0.690790 1.114477 0.265319 0.050 Uiso calc 1 . .
C C9 0.64673(6) 0.7985(2) 0.24310(3) 0.0409(3) Uani d 1 . .
H H9 0.672523 0.789083 0.223154 0.049 Uiso calc 1 . .
C C10 0.59708(6) 0.6193(2) 0.24767(3) 0.0398(3) Uani d 1 . .
H H10 0.589029 0.489378 0.230547 0.048 Uiso calc 1 . .
C C11 0.55906(6) 0.6315(2) 0.27768(3) 0.0349(3) Uani d 1 . .
H H11 0.525773 0.509472 0.280488 0.042 Uiso calc 1 . .
C C12 0.37016(5) 0.5655(2) 0.37171(3) 0.0288(2) Uani d 1 . .
C C13 0.30860(6) 0.5772(2) 0.34262(3) 0.0355(3) Uani d 1 . .
H H13 0.307468 0.684207 0.322203 0.043 Uiso calc 1 . .
C C14 0.24943(6) 0.4289(2) 0.34437(3) 0.0393(3) Uani d 1 . .
H H14 0.208289 0.439001 0.325132 0.047 Uiso calc 1 . .
C C15 0.25003(6) 0.2652(2) 0.37419(3) 0.0361(3) Uani d 1 . .
H H15 0.210233 0.163835 0.374717 0.043 Uiso calc 1 . .
C C16 0.31115(6) 0.2552(2) 0.40329(3) 0.0320(2) Uani d 1 . .
C C17 0.37049(5) 0.4078(2) 0.40215(3) 0.0301(2) Uani d 1 . .
H H17 0.410674 0.403553 0.422021 0.036 Uiso calc 1 . .
C C18 0.56109(5) 1.17960(19) 0.42620(3) 0.0289(2) Uani d 1 . .
C C19 0.60256(6) 1.3753(2) 0.41768(3) 0.0358(3) Uani d 1 . .
H H19 0.609761 1.397731 0.392735 0.043 Uiso calc 1 . .
C C20 0.63323(7) 1.5371(2) 0.44594(4) 0.0458(3) Uani d 1 . .
H H20 0.661015 1.666984 0.439753 0.055 Uiso calc 1 . .
C C21 0.62333(7) 1.5093(2) 0.48313(4) 0.0467(3) Uani d 1 . .
H H21 0.643968 1.619274 0.501995 0.056 Uiso calc 1 . .
C C22 0.58241(8) 1.3160(3) 0.49179(4) 0.0542(4) Uani d 1 . .
H H22 0.574972 1.295836 0.516738 0.065 Uiso calc 1 . .
C C23 0.55208(7) 1.1507(3) 0.46386(3) 0.0456(3) Uani d 1 . .
H H23 0.525391 1.018874 0.470363 0.055 Uiso calc 1 . .
C C24 0.26481(7) -0.0842(2) 0.43386(4) 0.0459(3) Uani d 1 . .
H H24A 0.261990 -0.182605 0.411288 0.069 Uiso calc 1 . .
H H24B 0.218282 -0.009630 0.433972 0.069 Uiso calc 1 . .
H H24C 0.277951 -0.185138 0.456145 0.069 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0405(5) 0.0415(5) 0.0487(5) -0.0114(4) 0.0090(4) 0.0073(4)
N1 0.0251(4) 0.0288(4) 0.0301(4) -0.0006(3) 0.0050(3) 0.0004(3)
C1 0.0244(5) 0.0279(5) 0.0301(5) 0.0010(4) 0.0045(4) 0.0005(4)
C2 0.0263(5) 0.0325(5) 0.0305(5) -0.0010(4) 0.0076(4) -0.0012(4)
C3 0.0227(5) 0.0294(5) 0.0320(5) 0.0006(4) 0.0041(4) 0.0009(4)
C4 0.0261(5) 0.0328(5) 0.0292(5) -0.0019(4) 0.0032(4) -0.0022(4)
C5 0.0246(5) 0.0286(5) 0.0287(5) 0.0019(4) 0.0029(4) 0.0024(4)
C6 0.0239(5) 0.0326(5) 0.0274(5) 0.0028(4) 0.0025(4) 0.0038(4)
C7 0.0360(6) 0.0339(6) 0.0355(6) -0.0019(5) 0.0087(4) 0.0019(5)
C8 0.0399(6) 0.0449(7) 0.0431(6) -0.0037(5) 0.0156(5) 0.0089(5)
C9 0.0386(6) 0.0546(7) 0.0320(6) 0.0077(5) 0.0134(5) 0.0072(5)
C10 0.0369(6) 0.0495(7) 0.0333(6) 0.0034(5) 0.0072(5) -0.0070(5)
C11 0.0301(5) 0.0401(6) 0.0347(6) -0.0027(5) 0.0062(4) -0.0032(5)
C12 0.0235(5) 0.0309(5) 0.0330(5) -0.0011(4) 0.0080(4) -0.0063(4)
C13 0.0294(5) 0.0439(6) 0.0328(5) -0.0032(5) 0.0049(4) -0.0008(5)
C14 0.0260(5) 0.0517(7) 0.0383(6) -0.0049(5) 0.0009(4) -0.0056(5)
C15 0.0254(5) 0.0401(6) 0.0442(6) -0.0085(4) 0.0101(4) -0.0097(5)
C16 0.0300(5) 0.0310(5) 0.0369(5) -0.0016(4) 0.0114(4) -0.0045(4)
C17 0.0235(5) 0.0324(5) 0.0340(5) -0.0012(4) 0.0042(4) -0.0045(4)
C18 0.0244(5) 0.0291(5) 0.0330(5) 0.0011(4) 0.0051(4) -0.0020(4)
C19 0.0394(6) 0.0317(6) 0.0374(6) -0.0038(5) 0.0097(5) -0.0009(5)
C20 0.0525(7) 0.0334(6) 0.0522(7) -0.0136(5) 0.0111(6) -0.0051(5)
C21 0.0507(7) 0.0425(7) 0.0453(7) -0.0100(6) 0.0047(5) -0.0145(6)
C22 0.0642(9) 0.0656(9) 0.0341(6) -0.0236(7) 0.0127(6) -0.0114(6)
C23 0.0508(7) 0.0512(7) 0.0363(6) -0.0227(6) 0.0118(5) -0.0058(5)
C24 0.0394(6) 0.0326(6) 0.0703(9) -0.0040(5) 0.0224(6) 0.0034(6)
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
C16 O1 C24 . . 117.66(9) ?
C5 N1 C1 . . 118.45(9) ?
N1 C1 C2 . . 122.25(9) ?
N1 C1 C18 . . 116.44(9) ?
C2 C1 C18 . . 121.31(9) ?
C1 C2 H2 . . 120.2 ?
C3 C2 C1 . . 119.54(9) ?
C3 C2 H2 . . 120.2 ?
C2 C3 C4 . . 118.00(9) ?
C2 C3 C12 . . 121.48(9) ?
C4 C3 C12 . . 120.51(9) ?
C3 C4 H4 . . 120.2 ?
C3 C4 C5 . . 119.54(9) ?
C5 C4 H4 . . 120.2 ?
N1 C5 C4 . . 122.19(9) ?
N1 C5 C6 . . 116.07(9) ?
C4 C5 C6 . . 121.73(9) ?
C7 C6 C5 . . 120.13(10) ?
C11 C6 C5 . . 121.59(10) ?
C11 C6 C7 . . 118.28(10) ?
C6 C7 H7 . . 119.7 ?
C8 C7 C6 . . 120.67(11) ?
C8 C7 H7 . . 119.7 ?
C7 C8 H8 . . 119.7 ?
C9 C8 C7 . . 120.54(11) ?
C9 C8 H8 . . 119.7 ?
C8 C9 H9 . . 120.3 ?
C10 C9 C8 . . 119.40(10) ?
C10 C9 H9 . . 120.3 ?
C9 C10 H10 . . 119.8 ?
C9 C10 C11 . . 120.43(11) ?
C11 C10 H10 . . 119.8 ?
C6 C11 H11 . . 119.7 ?
C10 C11 C6 . . 120.69(11) ?
C10 C11 H11 . . 119.7 ?
C13 C12 C3 . . 120.52(10) ?
C17 C12 C3 . . 120.01(9) ?
C17 C12 C13 . . 119.44(10) ?
C12 C13 H13 . . 120.2 ?
C14 C13 C12 . . 119.56(11) ?
C14 C13 H13 . . 120.2 ?
C13 C14 H14 . . 119.3 ?
C13 C14 C15 . . 121.44(10) ?
C15 C14 H14 . . 119.3 ?
C14 C15 H15 . . 120.5 ?
C14 C15 C16 . . 118.90(10) ?
C16 C15 H15 . . 120.5 ?
O1 C16 C15 . . 124.70(10) ?
O1 C16 C17 . . 115.27(9) ?
C15 C16 C17 . . 120.02(10) ?
C12 C17 C16 . . 120.58(10) ?
C12 C17 H17 . . 119.7 ?
C16 C17 H17 . . 119.7 ?
C19 C18 C1 . . 120.49(10) ?
C19 C18 C23 . . 118.09(10) ?
C23 C18 C1 . . 121.41(10) ?
C18 C19 H19 . . 119.7 ?
C20 C19 C18 . . 120.57(11) ?
C20 C19 H19 . . 119.7 ?
C19 C20 H20 . . 119.5 ?
C21 C20 C19 . . 121.08(12) ?
C21 C20 H20 . . 119.5 ?
C20 C21 H21 . . 120.7 ?
C22 C21 C20 . . 118.70(11) ?
C22 C21 H21 . . 120.7 ?
C21 C22 H22 . . 119.6 ?
C21 C22 C23 . . 120.85(12) ?
C23 C22 H22 . . 119.6 ?
C18 C23 H23 . . 119.7 ?
C22 C23 C18 . . 120.69(12) ?
C22 C23 H23 . . 119.7 ?
O1 C24 H24A . . 109.5 ?
O1 C24 H24B . . 109.5 ?
O1 C24 H24C . . 109.5 ?
H24A C24 H24B . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C16 . 1.3668(14) ?
O1 C24 . 1.4306(14) ?
N1 C1 . 1.3452(13) ?
N1 C5 . 1.3432(13) ?
C1 C2 . 1.3940(14) ?
C1 C18 . 1.4849(14) ?
C2 H2 . 0.9300 ?
C2 C3 . 1.3864(14) ?
C3 C4 . 1.3905(14) ?
C3 C12 . 1.4879(14) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.3941(14) ?
C5 C6 . 1.4897(14) ?
C6 C7 . 1.3946(15) ?
C6 C11 . 1.3934(15) ?
C7 H7 . 0.9300 ?
C7 C8 . 1.3852(16) ?
C8 H8 . 0.9300 ?
C8 C9 . 1.3820(18) ?
C9 H9 . 0.9300 ?
C9 C10 . 1.3796(18) ?
C10 H10 . 0.9300 ?
C10 C11 . 1.3890(15) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.3970(14) ?
C12 C17 . 1.3839(15) ?
C13 H13 . 0.9300 ?
C13 C14 . 1.3811(16) ?
C14 H14 . 0.9300 ?
C14 C15 . 1.3868(17) ?
C15 H15 . 0.9300 ?
C15 C16 . 1.3913(16) ?
C16 C17 . 1.3936(15) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.3876(15) ?
C18 C23 . 1.3897(15) ?
C19 H19 . 0.9300 ?
C19 C20 . 1.3812(17) ?
C20 H20 . 0.9300 ?
C20 C21 . 1.3778(19) ?
C21 H21 . 0.9300 ?
C21 C22 . 1.3730(19) ?
C22 H22 . 0.9300 ?
C22 C23 . 1.3845(18) ?
C23 H23 . 0.9300 ?
C24 H24A . 0.9600 ?
C24 H24B . 0.9600 ?
C24 H24C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C7 H7 N1 . 0.93 2.49 2.8025(13) 100 yes
C14 H14 Cg2 6_565 0.93 2.74 3.5482(12) 146 yes
C24 H24A Cg3 1_545 0.93 2.81 3.6787(13) 150 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
O1 C16 C17 C12 . . . . 177.88(9) ?
N1 C1 C2 C3 . . . . -0.90(15) ?
N1 C1 C18 C19 . . . . 24.21(14) ?
N1 C1 C18 C23 . . . . -155.42(11) ?
N1 C5 C6 C7 . . . . -16.90(14) ?
N1 C5 C6 C11 . . . . 162.10(10) ?
C1 N1 C5 C4 . . . . 0.54(15) ?
C1 N1 C5 C6 . . . . -179.20(9) ?
C1 C2 C3 C4 . . . . 0.02(15) ?
C1 C2 C3 C12 . . . . 179.70(9) ?
C1 C18 C19 C20 . . . . 179.78(11) ?
C1 C18 C23 C22 . . . . -179.00(12) ?
C2 C1 C18 C19 . . . . -155.29(10) ?
C2 C1 C18 C23 . . . . 25.08(16) ?
C2 C3 C4 C5 . . . . 1.09(15) ?
C2 C3 C12 C13 . . . . 125.72(11) ?
C2 C3 C12 C17 . . . . -56.26(14) ?
C3 C4 C5 N1 . . . . -1.42(15) ?
C3 C4 C5 C6 . . . . 178.32(9) ?
C3 C12 C13 C14 . . . . 177.10(10) ?
C3 C12 C17 C16 . . . . -175.78(9) ?
C4 C3 C12 C13 . . . . -54.60(14) ?
C4 C3 C12 C17 . . . . 123.41(11) ?
C4 C5 C6 C7 . . . . 163.35(10) ?
C4 C5 C6 C11 . . . . -17.65(15) ?
C5 N1 C1 C2 . . . . 0.62(15) ?
C5 N1 C1 C18 . . . . -178.87(9) ?
C5 C6 C7 C8 . . . . 178.44(10) ?
C5 C6 C11 C10 . . . . -178.45(10) ?
C6 C7 C8 C9 . . . . -0.03(18) ?
C7 C6 C11 C10 . . . . 0.57(16) ?
C7 C8 C9 C10 . . . . 0.69(18) ?
C8 C9 C10 C11 . . . . -0.70(18) ?
C9 C10 C11 C6 . . . . 0.07(17) ?
C11 C6 C7 C8 . . . . -0.59(16) ?
C12 C3 C4 C5 . . . . -178.60(9) ?
C12 C13 C14 C15 . . . . -0.93(18) ?
C13 C12 C17 C16 . . . . 2.26(16) ?
C13 C14 C15 C16 . . . . 1.44(18) ?
C14 C15 C16 O1 . . . . -179.69(10) ?
C14 C15 C16 C17 . . . . -0.10(16) ?
C15 C16 C17 C12 . . . . -1.75(16) ?
C17 C12 C13 C14 . . . . -0.93(16) ?
C18 C1 C2 C3 . . . . 178.57(9) ?
C18 C19 C20 C21 . . . . -0.2(2) ?
C19 C18 C23 C22 . . . . 1.37(19) ?
C19 C20 C21 C22 . . . . 0.3(2) ?
C20 C21 C22 C23 . . . . 0.5(2) ?
C21 C22 C23 C18 . . . . -1.4(2) ?
C23 C18 C19 C20 . . . . -0.59(17) ?
C24 O1 C16 C15 . . . . 9.02(16) ?
C24 O1 C16 C17 . . . . -170.59(10) ?
_cod_database_fobs_code 2244149