#------------------------------------------------------------------------------
#$Date: 2024-11-21 05:05:42 +0200 (Thu, 21 Nov 2024) $
#$Revision: 296044 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/26/2312694.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_2312694
loop_
_publ_author_name
'Al Mamari, Hamad H.'
'Al Sulaimi, Shamsaa'
'Mardiana, Lina'
'Waddell, Paul G.'
'Hall, Michael J.'
_publ_section_title
;
High-throughput crystallization and crystal structure of
N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-methylbenzamide:
a benzamide bearing the 4-aminoantipyrine moiety.
;
_journal_coeditor_code OV3177
_journal_issue 12
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi 10.1107/S2053229624010982
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C19 H19 N3 O2'
_chemical_formula_moiety 'C19 H19 N3 O2'
_chemical_formula_sum 'C19 H19 N3 O2'
_chemical_formula_weight 321.37
_chemical_name_systematic
N-(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-methylbenzamide
_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-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_cell_angle_alpha 90
_cell_angle_beta 104.295(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.0430(7)
_cell_length_b 6.0130(3)
_cell_length_c 20.3113(9)
_cell_measurement_reflns_used 8968
_cell_measurement_temperature 150.0(2)
_cell_measurement_theta_max 74.9300
_cell_measurement_theta_min 3.1950
_cell_volume 1661.99(14)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150.0(2)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0857
_diffrn_reflns_av_unetI/netI 0.0494
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 15556
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.315
_diffrn_reflns_theta_min 3.248
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.685
_exptl_absorpt_correction_T_max 0.978
_exptl_absorpt_correction_T_min 0.894
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2023), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.284
_exptl_crystal_description plate
_exptl_crystal_F_000 680
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.264
_refine_diff_density_min -0.290
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 223
_refine_ls_number_reflns 3320
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.049
_refine_ls_R_factor_all 0.0610
_refine_ls_R_factor_gt 0.0520
_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^)+(0.0936P)^2^+0.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1437
_refine_ls_wR_factor_ref 0.1555
_reflns_number_gt 2724
_reflns_number_total 3320
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ov3177sup1.cif
_cod_data_source_block 1a
_cod_database_code 2312694
_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 0.973
_shelx_hkl_file
;
0 0 -1 0.03 0.04
0 0 1 0.20 0.09
0 0 1 0.00 0.08
0 0 2 6.22 0.55
0 0 2 7.14 0.53
0 0 -2 6.45 0.53
0 0 2 5.71 0.56
0 0 -3 0.01 0.14
0 0 -3 0.11 0.07
0 0 3 0.16 0.26
0 0 3 0.07 0.14
0 0 4 16.94 1.31
0 0 4 17.70 1.27
0 0 4 20.16 1.23
0 0 -4 20.54 1.24
0 0 -5 0.15 0.25
0 0 5 -0.13 0.48
0 0 -5 -0.02 0.08
0 0 5 0.14 0.21
0 0 5 -0.02 0.41
0 0 6 571.79 32.59
0 0 6 527.18 32.60
0 0 6 556.75 32.69
0 0 -6 547.42 32.60
0 0 7 0.33 0.50
0 0 7 -0.06 0.24
0 0 -7 0.16 0.29
0 0 8 900.98 70.64
0 0 -8 961.82 70.57
0 0 -9 0.13 0.40
0 0 9 -0.40 0.61
0 0 10 0.46 0.73
0 0 -11 -0.14 0.44
0 0 11 0.20 0.64
0 0 11 -0.52 0.76
0 0 11 -0.09 0.74
0 0 11 0.37 0.62
0 0 -12 437.51 31.04
0 0 12 382.58 31.10
0 0 12 433.13 31.07
0 0 12 368.12 31.15
0 0 13 0.09 0.66
0 0 13 -0.84 0.82
0 0 -13 -0.13 0.52
0 0 13 -1.47 1.05
0 0 -14 24.31 2.11
0 0 14 21.11 2.24
0 0 14 17.89 2.21
0 0 14 21.00 2.25
0 0 14 21.30 2.26
0 0 15 -0.11 0.81
0 0 15 -1.39 1.23
0 0 15 -0.32 0.87
0 0 -15 -0.33 0.62
0 0 15 0.86 0.83
0 0 16 14.85 2.15
0 0 -16 21.69 2.04
0 0 16 16.45 2.16
0 0 16 17.66 2.12
0 0 16 20.95 2.19
0 0 17 0.12 0.83
0 0 -17 -0.10 0.66
0 0 17 -0.27 0.86
0 0 17 0.63 0.87
0 0 17 1.15 0.73
0 0 18 1.00 0.91
0 0 18 2.49 0.81
0 0 -18 1.83 0.71
0 0 19 -0.37 0.83
0 0 20 111.30 10.42
0 0 20 150.83 10.47
0 0 21 0.31 0.70
0 0 21 0.40 0.61
0 0 22 76.43 6.75
0 0 22 87.04 6.62
0 0 23 0.54 0.59
0 0 -24 45.64 3.82
0 1 0 0.28 0.22
0 1 0 0.15 0.24
0 1 -1 1919.15 135.55
0 1 -1 1818.00 135.53
0 -1 1 1687.73 135.48
0 1 1 1885.29 135.48
0 1 -2 468.22 35.86
0 -1 2 445.40 35.82
0 1 2 511.04 35.82
0 1 -3 661.62 47.30
0 1 3 637.26 47.27
0 -1 3 593.11 47.27
0 1 4 946.16 69.90
0 -1 4 912.75 69.91
0 -1 4 914.74 69.90
0 1 -4 939.00 69.92
0 1 5 6303.54 460.49
0 -1 5 6409.11 460.51
0 -1 5 5965.98 460.46
0 -1 5 5958.75 460.46
0 -1 -5 5902.64 460.46
0 1 -5 6389.40 460.50
0 -1 6 684.50 26.79
0 1 6 662.39 26.72
0 -1 6 597.60 26.60
0 -1 6 640.76 26.66
0 1 -6 706.83 26.73
0 -1 -6 556.97 26.59
0 -1 7 32.02 2.57
0 1 7 34.85 2.54
0 -1 7 32.28 2.53
0 1 -7 31.00 2.50
0 -1 -7 27.33 2.40
0 -1 7 29.67 2.42
0 -1 8 6.52 0.91
0 -1 8 6.51 0.90
0 -1 8 4.42 0.61
0 1 8 6.05 0.81
0 -1 -8 5.64 0.60
0 1 -8 7.79 0.80
0 -1 -8 6.56 0.67
0 -1 9 482.44 34.23
0 -1 9 421.87 34.18
0 -1 -9 416.77 34.14
0 1 -9 448.87 34.27
0 1 9 424.77 34.28
0 -1 9 497.11 34.39
0 -1 -9 538.35 34.24
0 -1 10 29.01 2.23
0 1 10 21.68 2.07
0 -1 10 22.22 1.91
0 1 10 21.00 2.09
0 -1 10 22.60 2.17
0 1 11 144.44 13.10
0 -1 11 171.83 13.26
0 -1 11 153.80 12.93
0 1 11 166.23 13.04
0 -1 11 188.62 13.17
0 -1 11 177.03 13.21
0 1 11 150.02 13.07
0 -1 -11 192.20 13.04
0 -1 11 191.06 13.03
0 1 -11 172.96 13.07
0 1 12 30.98 2.48
0 -1 -12 29.89 2.36
0 1 12 22.87 2.44
0 -1 12 30.39 2.65
0 1 -12 29.87 2.43
0 -1 12 28.92 2.60
0 1 12 24.85 2.43
0 1 12 20.22 2.38
0 -1 12 23.66 2.52
0 -1 13 107.95 7.86
0 1 13 82.06 7.66
0 -1 13 92.67 7.87
0 1 13 88.58 7.84
0 -1 13 101.50 7.95
0 1 13 86.57 7.75
0 1 13 112.49 7.79
0 -1 -13 107.81 7.67
0 -1 13 101.29 7.92
0 1 13 85.53 7.72
0 1 -13 100.65 7.70
0 -1 14 3.78 1.36
0 1 14 1.20 1.10
0 1 14 8.86 1.13
0 1 14 5.87 1.04
0 -1 14 4.31 1.09
0 -1 14 6.23 1.23
0 1 14 4.98 1.02
0 1 -14 5.74 0.94
0 -1 -14 7.46 0.91
0 1 14 6.09 1.16
0 -1 14 6.48 1.14
0 -1 15 -1.89 1.29
0 1 15 -0.39 1.07
0 1 15 0.49 0.66
0 1 15 -0.32 0.74
0 -1 15 -0.78 0.91
0 -1 15 1.00 0.97
0 1 15 0.51 0.80
0 -1 15 0.77 0.83
0 1 -15 0.35 0.69
0 -1 -15 0.52 0.59
0 1 16 12.46 1.49
0 1 16 7.60 1.34
0 -1 16 10.63 1.59
0 1 16 9.04 1.40
0 -1 16 9.02 1.58
0 -1 16 8.17 1.50
0 -1 -16 8.47 1.22
0 1 -16 10.18 1.37
0 1 17 4.44 0.98
0 1 17 2.48 0.96
0 -1 17 -0.14 1.09
0 -1 17 1.45 0.88
0 1 17 2.00 0.79
0 -1 17 1.74 0.92
0 -1 -17 3.07 0.79
0 1 -17 1.11 0.80
0 1 -18 29.59 2.80
0 -1 -18 28.30 2.70
0 1 18 24.42 2.78
0 -1 18 28.47 3.03
0 1 18 31.64 2.87
0 1 19 83.57 7.35
0 -1 19 98.81 7.63
0 -1 20 2.84 1.03
0 1 20 2.69 0.89
0 -1 20 2.38 0.74
0 1 20 4.40 0.94
0 1 21 1.95 0.67
0 -1 21 2.65 0.70
0 1 21 1.72 0.74
0 -1 21 2.63 0.97
0 -1 22 0.30 0.51
0 -1 22 0.31 0.74
0 1 22 0.82 0.60
0 1 -23 12.92 1.45
0 -1 -23 11.74 1.44
0 -1 23 14.17 1.32
0 1 23 11.82 1.40
0 -1 23 12.77 1.53
0 2 0 4836.82 363.83
0 2 -1 24.05 1.83
0 2 -1 19.96 1.87
0 2 -2 426.31 28.29
0 -2 2 364.11 28.16
0 2 -2 361.57 28.31
0 2 -3 4.31 0.52
0 -2 3 3.36 0.40
0 2 3 3.49 0.41
0 2 -3 4.67 0.64
0 2 -4 190.48 14.50
0 2 -4 213.35 14.60
0 2 4 193.00 14.45
0 -2 4 179.86 14.44
0 -2 5 134.82 10.22
0 2 5 132.42 10.21
0 2 -5 139.63 10.26
0 -2 5 142.75 10.30
0 -2 5 117.14 10.20
0 2 -5 140.77 10.33
0 -2 -5 142.75 10.29
0 2 6 153.63 11.35
0 -2 6 150.75 11.37
0 -2 6 167.73 11.43
0 -2 -6 159.13 11.40
0 2 -6 159.55 11.47
0 -2 6 127.31 11.28
0 -2 7 643.96 48.15
0 2 7 619.74 48.11
0 2 -7 639.22 48.21
0 -2 -7 633.31 48.13
0 -2 7 652.53 48.13
0 -2 8 223.79 16.79
0 2 8 213.69 16.73
0 -2 8 211.63 16.66
0 -2 -8 230.59 16.72
0 -2 9 -0.04 0.77
0 -2 -9 0.23 0.33
0 2 -9 0.73 0.56
0 2 9 0.05 0.47
0 -2 9 0.26 0.30
0 -2 9 0.12 0.62
0 2 10 7.71 0.96
0 -2 10 7.09 1.08
0 2 10 4.31 0.93
0 -2 10 8.61 1.08
0 2 -10 7.42 0.99
0 -2 10 5.51 0.99
0 -2 10 6.86 1.08
0 -2 11 115.47 8.71
0 -2 11 119.21 8.93
0 2 11 106.35 8.78
0 -2 11 130.29 8.89
0 2 11 105.95 8.71
0 -2 -11 116.42 8.67
0 2 11 100.96 8.79
0 -2 11 120.72 8.96
0 2 11 108.25 8.73
0 2 11 122.65 8.86
0 -2 11 100.57 8.60
0 2 -11 112.16 8.82
0 -2 -12 6.69 0.83
0 2 12 5.69 0.85
0 2 12 5.43 0.96
0 -2 12 7.70 1.17
0 2 -12 8.49 1.11
0 2 -12 5.66 0.95
0 2 12 7.16 1.01
0 -2 12 3.66 1.28
0 2 12 4.30 1.06
0 -2 12 6.53 1.12
0 -2 12 9.05 1.29
0 2 12 6.04 1.00
0 -2 13 11.66 1.93
0 -2 13 13.16 1.72
0 -2 13 15.78 1.87
0 2 13 14.83 1.67
0 2 13 16.02 1.70
0 -2 13 15.66 1.87
0 2 13 11.68 1.60
0 2 -13 14.90 1.69
0 2 -13 16.09 1.66
0 -2 -13 16.28 1.50
0 -2 13 15.49 1.71
0 2 14 21.78 2.48
0 -2 14 28.82 2.80
0 2 14 27.20 2.60
0 2 -14 26.54 2.49
0 -2 14 25.68 2.71
0 2 14 21.42 2.46
0 -2 14 26.91 2.71
0 2 -14 27.91 2.60
0 -2 -14 29.28 2.41
0 2 15 20.96 2.47
0 -2 15 30.22 2.86
0 2 15 28.92 2.65
0 2 -15 25.22 2.48
0 2 -15 27.03 2.60
0 2 15 19.98 2.49
0 -2 15 29.57 2.88
0 -2 15 26.18 2.75
0 -2 -15 27.23 2.40
0 2 16 77.10 5.80
0 2 -16 76.63 5.79
0 -2 16 70.48 5.94
0 2 16 55.54 5.60
0 -2 16 73.65 6.02
0 2 16 58.47 5.65
0 -2 16 74.29 5.97
0 -2 -16 63.24 5.50
0 2 17 -0.11 0.78
0 -2 17 -0.15 1.05
0 -2 -17 1.01 0.60
0 2 -17 -0.69 0.87
0 -2 17 1.15 0.86
0 2 18 20.21 2.30
0 -2 18 24.91 2.64
0 2 19 4.96 1.07
0 -2 19 7.73 1.41
0 2 -20 -0.11 0.86
0 -2 20 0.13 1.01
0 2 20 0.10 0.75
0 2 -21 47.44 3.75
0 -2 -21 37.72 3.50
0 -2 21 45.70 3.50
0 2 21 33.21 3.47
0 -2 21 42.90 3.78
0 2 -22 25.55 2.43
0 2 -22 25.74 2.37
0 -2 -22 22.22 2.28
0 -2 22 25.46 2.51
0 -2 22 29.53 2.32
0 -2 23 0.48 0.43
0 -2 -23 0.04 0.49
0 3 0 -0.23 0.50
0 3 1 0.29 0.48
0 3 -1 -0.06 0.53
0 -3 1 0.82 0.55
0 3 -2 2.53 0.64
0 3 -2 2.44 0.46
0 -3 2 2.10 0.60
0 3 -3 73.12 5.83
0 3 -3 72.40 5.66
0 -3 3 71.11 5.75
0 3 -4 74.99 6.10
0 -3 4 79.51 6.01
0 3 -4 69.53 6.00
0 3 -4 77.46 5.94
0 3 -5 5.32 0.88
0 3 5 6.37 0.89
0 -3 5 5.71 0.84
0 -3 -5 6.94 0.90
0 3 -5 7.81 0.99
0 3 -5 5.82 0.77
0 3 -6 -0.30 0.45
0 3 -6 -0.47 0.56
0 3 6 0.42 0.46
0 3 -6 1.62 0.68
0 -3 -6 0.33 0.49
0 -3 6 0.23 0.39
0 -3 6 0.16 0.93
0 3 -6 0.36 0.60
0 3 -6 0.05 0.38
0 3 -7 331.96 22.84
0 -3 7 365.93 22.76
0 3 -7 265.56 22.72
0 3 -7 278.04 22.68
0 -3 -7 284.86 22.66
0 3 -7 308.99 22.79
0 3 7 269.74 22.69
0 3 -8 3.94 0.78
0 3 -8 3.58 0.80
0 -3 -8 4.02 0.68
0 -3 8 4.52 1.13
0 3 -8 3.58 0.68
0 3 -8 3.10 0.80
0 3 8 3.16 0.70
0 3 9 27.19 2.62
0 3 -9 33.60 2.76
0 -3 9 27.37 2.46
0 -3 -9 28.69 2.54
0 3 -9 34.03 2.77
0 3 -9 23.10 2.59
0 3 -9 30.83 2.62
0 -3 9 39.70 2.80
0 3 -9 24.87 2.66
0 3 -10 72.64 5.76
0 3 -10 78.95 5.90
0 3 -10 68.05 5.89
0 3 -10 63.75 5.81
0 -3 -10 66.27 5.66
0 3 -10 75.84 5.92
0 3 10 69.88 5.80
0 -3 10 76.80 5.82
0 3 -11 165.31 14.01
0 3 -11 182.12 14.04
0 3 -11 179.98 13.99
0 3 11 173.39 13.90
0 -3 11 191.47 13.88
0 3 -12 149.68 12.78
0 3 12 157.29 12.65
0 3 -12 164.48 12.79
0 3 -12 153.16 12.71
0 -3 -12 170.01 12.51
0 -3 12 169.85 12.64
0 3 -13 190.45 15.87
0 3 13 186.91 15.67
0 3 -13 191.69 15.81
0 3 -13 211.69 15.85
0 -3 -13 210.14 15.57
0 -3 13 218.33 15.69
0 3 -14 4.60 1.15
0 -3 -14 2.90 0.65
0 3 -14 1.91 0.89
0 3 14 2.71 0.72
0 3 -14 2.51 0.93
0 3 -15 14.47 1.99
0 -3 -15 12.70 1.51
0 3 -15 17.45 1.91
0 3 -15 19.15 1.95
0 3 -16 0.62 0.79
0 3 -16 -0.26 0.89
0 3 -17 -0.19 0.68
0 3 -17 -0.25 1.10
0 3 -18 8.67 1.46
0 3 -19 0.31 0.78
0 3 -20 -0.80 0.76
0 -3 21 9.98 1.11
0 3 -21 8.10 1.16
0 -3 22 0.46 0.63
0 4 0 21.62 2.21
0 -4 0 24.55 2.27
0 4 0 25.61 2.29
0 4 -1 19.02 2.01
0 4 1 17.93 1.98
0 -4 1 23.81 2.16
0 -4 -1 20.39 2.03
0 -4 1 21.95 2.06
0 4 -1 22.78 2.07
0 4 1 20.92 2.06
0 4 -2 2.28 0.82
0 4 -2 1.06 0.53
0 4 2 0.71 0.52
0 -4 -2 1.02 0.62
0 -4 2 1.00 0.95
0 -4 2 0.23 0.73
0 4 2 0.63 0.62
0 4 -2 1.86 0.64
0 4 -3 18.53 1.92
0 4 3 19.11 1.97
0 -4 3 21.91 2.02
0 -4 -3 18.41 1.92
0 4 -3 21.93 2.10
0 -4 3 25.37 2.15
0 4 3 17.37 1.85
0 4 -3 16.98 1.91
0 4 -4 44.60 3.53
0 4 4 42.54 3.60
0 -4 4 45.74 3.59
0 -4 -4 37.49 3.49
0 4 -4 35.55 3.52
0 4 -4 43.00 3.69
0 4 -4 35.41 3.51
0 4 4 35.03 3.43
0 4 -5 11.83 1.43
0 4 -5 13.15 1.37
0 4 5 11.70 1.32
0 4 -5 12.28 1.43
0 -4 5 13.45 1.44
0 -4 -5 10.69 1.37
0 4 -5 9.93 1.40
0 4 -5 12.49 1.58
0 -4 5 15.72 1.74
0 4 5 12.82 1.49
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-15 1 3 88.16 8.81
-15 -1 3 113.46 9.11
-15 1 3 95.93 8.84
-15 -1 3 119.87 9.11
15 -1 -2 -0.41 1.15
15 1 -2 -0.57 1.02
-15 1 2 0.18 0.54
-15 1 2 -0.33 0.83
-15 -1 2 -0.92 1.13
-15 1 2 0.09 0.81
-15 -1 2 -0.11 1.03
15 -1 -1 9.33 1.43
15 1 -1 6.71 1.24
-15 1 1 5.59 0.80
-15 1 1 4.13 1.08
-15 -1 1 9.23 1.37
-15 1 1 5.23 1.08
-15 -1 1 7.69 1.33
-15 1 0 0.39 0.76
-15 -1 0 0.28 0.90
-15 1 0 0.25 0.73
-15 -1 0 -0.50 0.93
15 -1 0 0.08 1.07
15 1 0 0.60 0.91
-15 1 -1 20.23 2.32
-15 -1 -1 23.47 2.50
-15 1 -1 21.12 2.33
-15 -1 -1 25.84 2.53
15 -1 1 29.23 2.51
15 1 1 26.23 2.36
-15 -1 -2 6.22 1.14
-15 1 -2 4.42 0.99
-15 1 -2 4.29 0.98
-15 -1 -2 6.59 1.15
15 -1 2 7.62 1.23
15 1 2 4.15 0.95
-15 1 -3 0.77 0.66
-15 -1 -3 0.51 0.75
-15 1 -3 0.47 0.66
-15 -1 -3 0.47 0.77
15 -1 3 0.31 0.86
15 1 3 0.05 0.70
-15 1 -4 0.86 0.64
-15 -1 -4 2.31 0.79
-15 1 -4 1.52 0.70
-15 -1 -4 0.48 0.77
15 -1 4 1.55 0.85
15 1 4 1.23 0.70
-15 1 -5 9.47 1.21
-15 -1 -5 11.85 1.41
-15 1 -5 6.57 1.14
-15 -1 -5 8.48 1.32
15 -1 5 12.79 1.26
15 1 5 11.94 1.15
-15 -1 -6 3.80 0.93
-15 1 -6 3.69 0.89
-15 -1 -6 3.19 0.97
-15 1 -7 1.03 0.69
-15 -1 -7 1.00 0.75
-15 -2 16 10.55 1.20
15 2 -16 4.78 0.90
-15 -2 15 0.78 0.76
15 2 -15 -0.08 0.66
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15 2 -14 2.28 0.71
-15 -2 13 -0.17 0.69
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15 -2 -12 -0.04 0.63
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-15 2 12 1.39 0.55
-15 -2 12 -0.83 0.79
-15 2 12 -0.30 0.57
15 2 -11 1.29 0.70
15 -2 -11 0.58 0.65
-15 -2 11 1.30 0.75
-15 2 11 0.24 0.57
-15 -2 11 1.40 0.80
-15 2 11 0.08 0.55
15 2 -10 26.60 2.25
15 -2 -10 19.46 2.21
-15 -2 10 32.23 2.48
-15 -2 10 27.86 2.56
-15 2 10 19.61 2.30
-15 -2 10 30.47 2.60
-15 2 10 21.76 2.32
-15 2 9 0.06 0.62
-15 -2 9 -1.15 0.91
-15 2 9 0.84 0.62
-15 -2 9 -0.55 0.80
-15 2 9 0.87 0.65
-15 -2 9 1.33 0.84
-15 2 9 0.09 0.66
15 2 -9 0.05 0.73
15 -2 -9 0.05 0.74
-15 -2 8 -0.23 0.80
-15 2 8 0.09 0.63
-15 2 8 -0.69 0.66
-15 -2 8 -0.76 0.93
-15 -2 8 -0.23 0.76
-15 2 8 0.23 0.61
-15 2 8 1.26 0.67
-15 2 8 -0.31 0.67
-15 -2 8 -1.67 1.03
15 -2 -8 -1.85 0.95
15 2 -8 -1.42 0.92
-15 -2 7 -0.94 1.06
-15 2 7 -0.19 0.83
-15 2 7 -1.17 0.85
-15 -2 7 -1.38 1.14
-15 -2 7 2.63 0.90
-15 2 7 1.46 0.70
-15 2 7 0.13 0.76
-15 -2 7 -0.85 1.14
15 2 -7 -2.22 1.09
-15 2 6 15.27 1.74
-15 -2 6 15.28 2.02
-15 2 6 13.15 1.83
-15 2 6 13.70 1.72
-15 -2 6 21.37 2.00
-15 2 6 20.20 1.72
-15 -2 6 15.44 1.91
15 -2 -6 17.86 1.90
15 2 -6 18.64 1.81
-15 -2 5 6.65 1.41
-15 2 5 4.49 1.14
-15 2 5 7.70 1.13
-15 -2 5 8.86 1.34
-15 2 5 10.10 1.09
-15 2 5 5.95 1.09
-15 -2 5 9.14 1.37
15 -2 -5 6.90 1.35
15 2 -5 9.11 1.24
-15 -2 4 22.98 2.68
-15 2 4 20.10 2.50
-15 2 4 29.10 2.35
-15 2 4 22.36 2.40
-15 -2 4 34.37 2.71
15 -2 -4 33.51 2.64
15 2 -4 29.89 2.49
-15 2 4 19.62 2.37
-15 -2 4 30.55 2.67
-15 -2 3 6.06 1.22
-15 2 3 5.80 1.09
-15 2 3 6.88 1.04
-15 -2 3 7.65 1.20
15 -2 -3 9.06 1.30
15 2 -3 8.64 1.14
-15 2 3 8.48 0.98
-15 2 3 5.10 0.98
-15 -2 3 7.81 1.24
15 -2 -2 22.93 2.10
15 2 -2 20.87 1.92
-15 2 2 16.02 1.86
-15 -2 2 26.30 2.17
-15 2 2 18.61 1.78
-15 2 2 24.60 2.09
-15 2 2 14.29 1.84
-15 -2 2 21.11 2.07
-15 2 1 0.59 0.55
-15 -2 1 1.46 0.72
-15 2 1 1.25 0.50
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-15 -2 1 0.98 0.70
-15 2 1 0.98 0.61
15 -2 -1 1.19 0.83
15 2 -1 0.05 0.64
-15 2 0 0.33 0.53
-15 -2 0 1.00 0.70
-15 2 0 0.95 0.47
-15 2 0 0.96 0.56
-15 -2 0 0.90 0.71
-15 2 0 1.70 0.71
15 -2 0 0.73 0.77
15 2 0 1.49 0.63
-15 -2 -1 -0.24 0.56
-15 2 -1 0.56 0.40
-15 -2 -1 0.25 0.60
-15 2 -1 0.16 0.57
15 -2 1 0.15 0.70
-15 -2 -2 5.41 0.83
-15 2 -2 2.93 0.53
-15 -2 -2 4.31 0.81
15 -2 2 6.11 0.90
-15 2 -2 7.84 0.98
-15 -2 -3 3.82 0.70
-15 2 -3 4.38 0.80
-15 -2 -4 -0.40 0.46
-15 -3 14 1.20 0.78
15 3 -13 0.65 0.58
15 3 -12 0.82 0.50
15 3 -11 -0.13 0.37
-15 3 9 -0.18 0.46
-15 3 8 2.79 0.58
-15 3 7 7.41 0.87
-15 3 6 4.92 0.73
-15 3 5 31.83 2.64
-15 3 4 13.44 1.30
-15 3 3 8.25 0.92
-15 3 2 0.12 0.48
-15 3 1 1.49 0.55
-15 3 0 2.05 0.57
-16 0 16 0.49 0.81
-16 0 15 0.49 0.87
-16 0 14 -0.07 0.85
16 0 -14 0.39 0.61
-16 0 14 0.35 0.89
-16 0 13 -0.46 0.80
16 0 -13 -0.77 0.73
-16 0 13 -0.84 0.81
-16 0 12 0.17 0.68
16 0 -12 0.16 0.74
-16 0 12 -0.25 0.69
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16 0 -11 -0.06 0.78
-16 0 11 0.13 0.59
-16 0 11 -0.09 0.69
-16 0 10 5.65 1.12
16 0 -10 7.45 1.15
-16 0 10 6.46 1.01
-16 0 10 6.30 1.10
-16 0 9 0.10 0.70
-16 0 9 -0.30 0.73
16 0 -9 -0.74 0.88
-16 0 9 -0.83 0.77
-16 0 9 -0.21 0.66
-16 0 8 0.81 0.88
16 0 -8 2.23 0.97
-16 0 8 1.71 0.78
-16 0 8 1.08 0.71
-16 0 7 0.83 0.84
16 0 -7 -0.46 0.96
-16 0 7 -0.59 0.78
-16 0 7 -0.59 0.74
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16 0 -6 0.66 0.94
-16 0 6 0.30 0.76
-16 0 6 1.13 0.76
-16 0 5 -0.32 0.79
-16 0 5 -0.53 0.76
-16 0 5 0.15 0.76
16 0 -5 0.13 0.96
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16 0 -4 0.79 0.96
-16 0 3 0.15 0.70
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16 0 -3 0.45 0.92
-16 0 2 6.06 1.17
-16 0 2 6.89 1.20
-16 0 1 -0.14 0.68
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16 0 -1 -0.84 0.87
-16 0 0 1.37 0.74
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16 0 0 2.41 0.89
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16 0 1 -0.31 0.76
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16 0 2 4.13 0.81
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16 1 -15 -0.15 0.64
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16 1 -12 1.25 0.67
16 -1 -12 0.41 0.68
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16 1 -11 3.10 0.88
16 -1 -11 1.30 0.85
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-16 -1 10 8.37 1.30
-16 1 10 6.37 1.15
16 1 -10 9.65 1.27
16 -1 -10 9.14 1.23
-16 1 10 8.41 1.08
-16 -1 10 9.97 1.23
-16 -1 10 11.78 1.42
-16 1 10 9.34 1.21
-16 -1 9 3.37 0.92
-16 1 9 3.03 0.79
-16 -1 9 2.42 0.89
-16 1 9 2.67 0.80
16 -1 -9 2.08 0.87
16 1 -9 3.76 0.90
-16 1 9 1.57 0.69
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16 -1 -8 -0.65 0.91
16 1 -8 -0.80 0.89
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16 -1 -7 0.36 0.93
16 1 -7 0.23 0.90
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16 -1 -6 -2.34 0.98
16 1 -6 -1.33 0.96
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16 -1 -5 6.40 1.16
16 1 -5 6.45 1.10
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16 -1 -4 10.10 1.27
16 1 -4 9.29 1.17
-16 1 4 5.12 0.98
-16 -1 4 6.00 1.09
-16 1 4 7.09 1.00
-16 -1 4 6.47 1.14
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-16 -1 3 3.93 1.00
16 -1 -3 4.08 0.99
16 1 -3 5.28 0.96
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-16 -1 3 3.88 0.96
-16 1 3 4.58 0.84
-16 -1 3 4.27 0.91
16 -1 -2 1.31 0.87
16 1 -2 0.69 0.75
-16 1 2 1.08 0.62
-16 -1 2 1.29 0.76
-16 1 2 1.11 0.59
-16 -1 2 1.12 0.73
16 -1 -1 12.02 1.33
16 1 -1 11.82 1.28
-16 1 1 8.26 1.15
-16 1 1 8.55 1.13
-16 -1 1 9.56 1.26
-16 -1 1 7.96 1.24
-16 1 0 7.68 1.02
-16 -1 0 8.09 1.15
16 -1 0 9.28 1.19
16 1 0 9.37 1.06
-16 1 0 5.61 0.99
-16 -1 0 8.20 1.14
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16 -1 1 -1.23 0.75
16 1 1 -1.36 0.66
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-16 1 -2 2.19 0.69
-16 -1 -2 2.86 0.88
-16 1 -3 6.51 0.96
-16 -1 -3 7.15 1.08
-16 1 -4 0.50 0.59
-16 -1 -4 -0.21 0.65
16 2 -14 3.58 0.62
16 2 -13 2.18 0.68
16 2 -12 0.66 0.63
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16 2 -11 0.55 0.53
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-16 -2 8 2.01 0.65
-16 -2 7 21.62 2.04
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-17 -1 7 0.05 0.78
-17 -1 6 6.55 1.10
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-17 -1 4 1.07 0.75
-17 1 4 1.12 0.63
-17 -1 4 0.91 0.75
-17 1 3 -0.41 0.62
-17 -1 3 -0.37 0.75
-17 1 2 0.81 0.64
-17 -1 2 1.07 0.78
-17 1 1 6.17 0.85
-17 -1 1 7.12 0.96
0 0 0 0.00 0.00
TITL mjh230060_fa in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 14.042981 6.013011 20.311256 90.0000 104.2945 90.0000
ZERR 4.00 0.000670 0.000281 0.000934 0.0000 0.0047 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 76.00 76.00 12.00 8.00
REM CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.04 0.10 0.19
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 4495
_shelx_res_file
;
TITL mjh230060_fa_a.res in P2(1)/c
mjh230060_fa.res
created by SHELXL-2019/1 at 11:29:36 on 30-Aug-2023
REM Old TITL mjh230060_fa in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.182, Rweak 0.051, Alpha 0.014
REM 0.253 for 338 systematic absences, Orientation as input
REM Formula found by SHELXT: C19 N3 O2
CELL 1.54184 14.043 6.013 20.3113 90 104.295 90
ZERR 4 0.0007 0.0003 0.0009 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 76 76 12 8
EQIV $1 1-X,1-Y,1-Z
L.S. 4
PLAN 20
SIZE 0.04 0.1 0.19
TEMP -123
HTAB N1 O1_$1
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.093600 0.297700
FVAR 0.54470
O1 4 0.381788 0.600419 0.427179 11.00000 0.04278 0.03081 =
0.02867 -0.00270 0.00242 0.00127
O2 4 0.640904 0.522852 0.340692 11.00000 0.05680 0.04762 =
0.02991 -0.00151 0.00783 0.00124
N1 3 0.581446 0.422743 0.430454 11.00000 0.03919 0.03656 =
0.02555 -0.00171 0.00036 0.00149
H1 2 0.586833 0.422516 0.473619 11.00000 -1.20000
N2 3 0.374732 0.169779 0.312198 11.00000 0.04499 0.02542 =
0.03033 -0.00208 0.00206 0.00007
N3 3 0.328303 0.321833 0.346633 11.00000 0.03884 0.02822 =
0.02909 -0.00140 0.00129 -0.00018
C1 1 0.490733 0.339353 0.391547 11.00000 0.03932 0.03098 =
0.02792 0.00098 0.00044 0.00335
C2 1 0.473504 0.176573 0.343497 11.00000 0.04524 0.02943 =
0.02871 0.00208 0.00158 0.00512
C3 1 0.399275 0.439754 0.393765 11.00000 0.04024 0.02623 =
0.02415 0.00072 0.00127 -0.00162
C4 1 0.236530 0.412543 0.310763 11.00000 0.03721 0.02417 =
0.03560 0.00186 0.00007 -0.00396
C5 1 0.211248 0.412578 0.239905 11.00000 0.04419 0.03197 =
0.03606 0.00398 0.00019 -0.00612
AFIX 43
H5 2 0.253987 0.349381 0.215301 11.00000 -1.20000
AFIX 0
C6 1 0.122324 0.506858 0.206012 11.00000 0.05291 0.03626 =
0.04259 0.00605 -0.00783 -0.00756
AFIX 43
H6 2 0.103769 0.506162 0.157755 11.00000 -1.20000
AFIX 0
C7 1 0.060644 0.601432 0.241497 11.00000 0.04562 0.03540 =
0.06209 0.00144 -0.01105 0.00072
AFIX 43
H7 2 0.000435 0.667327 0.217807 11.00000 -1.20000
AFIX 0
C8 1 0.087006 0.599844 0.312064 11.00000 0.04189 0.03661 =
0.06178 -0.00513 0.00415 0.00074
AFIX 43
H8 2 0.044716 0.665848 0.336515 11.00000 -1.20000
AFIX 0
C9 1 0.174308 0.503029 0.347147 11.00000 0.04397 0.03052 =
0.04111 -0.00188 0.00397 -0.00430
AFIX 43
H9 2 0.191323 0.498654 0.395395 11.00000 -1.20000
AFIX 0
C10 1 0.323279 -0.045354 0.296686 11.00000 0.06111 0.02609 =
0.03432 -0.00032 0.00631 -0.00703
AFIX 137
H10A 2 0.326081 -0.125786 0.339086 11.00000 -1.50000
H10B 2 0.355110 -0.134114 0.267729 11.00000 -1.50000
H10C 2 0.254513 -0.018877 0.272952 11.00000 -1.50000
AFIX 0
C11 1 0.542025 0.020404 0.322495 11.00000 0.05627 0.04053 =
0.04269 -0.00792 0.00041 0.01392
AFIX 137
H11A 2 0.528618 -0.131411 0.335284 11.00000 -1.50000
H11B 2 0.609824 0.060621 0.345154 11.00000 -1.50000
H11C 2 0.532985 0.028639 0.273147 11.00000 -1.50000
AFIX 0
C12 1 0.646310 0.527003 0.401764 11.00000 0.04020 0.03031 =
0.03100 0.00200 0.00384 0.00794
C13 1 0.723978 0.661429 0.449401 11.00000 0.03979 0.03383 =
0.02972 0.00659 0.00312 0.00210
C14 1 0.823454 0.638021 0.449462 11.00000 0.04216 0.04851 =
0.03798 0.01196 0.00675 0.00622
C15 1 0.890320 0.782468 0.491322 11.00000 0.04191 0.06717 =
0.04984 0.01573 0.00411 -0.00653
AFIX 43
H15 2 0.958279 0.768532 0.493049 11.00000 -1.20000
AFIX 0
C16 1 0.860651 0.943804 0.529990 11.00000 0.06300 0.05706 =
0.04530 0.00193 0.00279 -0.02205
AFIX 43
H16 2 0.907959 1.038829 0.557856 11.00000 -1.20000
AFIX 0
C17 1 0.762663 0.967966 0.528432 11.00000 0.06669 0.03933 =
0.03988 -0.00163 0.00895 -0.00982
AFIX 43
H17 2 0.741807 1.081099 0.554378 11.00000 -1.20000
AFIX 0
C18 1 0.694926 0.825459 0.488611 11.00000 0.04782 0.03530 =
0.03325 0.00128 0.00709 0.00035
AFIX 43
H18 2 0.627359 0.839894 0.488038 11.00000 -1.20000
AFIX 0
C19 1 0.857458 0.464872 0.407505 11.00000 0.04880 0.06571 =
0.05451 0.00948 0.01177 0.01892
AFIX 137
H19A 2 0.831736 0.319332 0.416327 11.00000 -1.50000
H19B 2 0.929442 0.460215 0.419470 11.00000 -1.50000
H19C 2 0.833464 0.501673 0.359240 11.00000 -1.50000
AFIX 0
HKLF 4
REM mjh230060_fa_a.res in P2(1)/c
REM wR2 = 0.1555, GooF = S = 1.049, Restrained GooF = 1.049 for all data
REM R1 = 0.0520 for 2724 Fo > 4sig(Fo) and 0.0610 for all 3320 data
REM 223 parameters refined using 0 restraints
END
WGHT 0.0936 0.2977
REM Highest difference peak 0.264, deepest hole -0.290, 1-sigma level 0.052
Q1 1 0.3719 0.6025 0.4667 11.00000 0.05 0.26
Q2 1 0.3914 0.5851 0.3826 11.00000 0.05 0.26
Q3 1 0.3197 0.2964 0.3891 11.00000 0.05 0.26
Q4 1 0.8729 0.8074 0.5283 11.00000 0.05 0.25
Q5 1 0.6549 0.5108 0.2994 11.00000 0.05 0.23
Q6 1 0.3840 0.4573 0.4366 11.00000 0.05 0.23
Q7 1 0.7088 0.6665 0.4929 11.00000 0.05 0.21
Q8 1 0.3517 0.3159 0.3019 11.00000 0.05 0.20
Q9 1 0.5552 0.0489 0.2783 11.00000 0.05 0.20
Q10 1 0.8299 0.5117 0.4472 11.00000 0.05 0.20
Q11 1 0.4216 0.4504 0.3534 11.00000 0.05 0.19
Q12 1 0.7016 0.8235 0.4433 11.00000 0.05 0.19
Q13 1 0.3997 0.1921 0.2712 11.00000 0.05 0.19
Q14 1 0.8735 0.5286 0.3646 11.00000 0.05 0.18
Q15 1 0.1667 0.4694 0.3914 11.00000 0.05 0.18
Q16 1 0.4723 0.1894 0.3898 11.00000 0.05 0.17
Q17 1 0.7581 0.9945 0.5429 11.00000 0.05 0.17
Q18 1 0.3330 -0.0742 0.2509 11.00000 0.05 0.17
Q19 1 0.3489 0.1746 0.3539 11.00000 0.05 0.17
Q20 1 0.6495 0.4326 0.3683 11.00000 0.05 0.17
;
_shelx_res_checksum 5062
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 0.38179(7) 0.60042(17) 0.42718(5) 0.0352(3) Uani d 1 . .
O O2 0.64090(9) 0.5229(2) 0.34069(5) 0.0453(3) Uani d 1 . .
N N1 0.58145(9) 0.4227(2) 0.43045(7) 0.0351(3) Uani d 1 . .
H H1 0.5868(13) 0.423(3) 0.4736(10) 0.042 Uiso d 1 . .
N N2 0.37473(10) 0.1698(2) 0.31220(6) 0.0349(3) Uani d 1 . .
N N3 0.32830(9) 0.3218(2) 0.34663(6) 0.0333(3) Uani d 1 . .
C C1 0.49073(11) 0.3394(3) 0.39155(7) 0.0341(4) Uani d 1 . .
C C2 0.47350(12) 0.1766(2) 0.34350(7) 0.0358(4) Uani d 1 . .
C C3 0.39927(11) 0.4398(2) 0.39377(7) 0.0314(3) Uani d 1 . .
C C4 0.23653(11) 0.4125(2) 0.31076(8) 0.0339(4) Uani d 1 . .
C C5 0.21125(12) 0.4126(3) 0.23990(8) 0.0391(4) Uani d 1 . .
H H5 0.253987 0.349381 0.215301 0.047 Uiso calc 1 . .
C C6 0.12232(13) 0.5069(3) 0.20601(9) 0.0474(4) Uani d 1 . .
H H6 0.103769 0.506162 0.157755 0.057 Uiso calc 1 . .
C C7 0.06064(13) 0.6014(3) 0.24150(10) 0.0520(5) Uani d 1 . .
H H7 0.000435 0.667327 0.217807 0.062 Uiso calc 1 . .
C C8 0.08701(13) 0.5998(3) 0.31206(10) 0.0483(4) Uani d 1 . .
H H8 0.044716 0.665848 0.336515 0.058 Uiso calc 1 . .
C C9 0.17431(12) 0.5030(3) 0.34715(9) 0.0397(4) Uani d 1 . .
H H9 0.191323 0.498654 0.395395 0.048 Uiso calc 1 . .
C C10 0.32328(14) -0.0454(3) 0.29669(8) 0.0415(4) Uani d 1 . .
H H10A 0.326081 -0.125786 0.339086 0.062 Uiso calc 1 . .
H H10B 0.355110 -0.134114 0.267729 0.062 Uiso calc 1 . .
H H10C 0.254513 -0.018877 0.272952 0.062 Uiso calc 1 . .
C C11 0.54203(14) 0.0204(3) 0.32250(9) 0.0486(5) Uani d 1 . .
H H11A 0.528618 -0.131411 0.335284 0.073 Uiso calc 1 . .
H H11B 0.609824 0.060621 0.345154 0.073 Uiso calc 1 . .
H H11C 0.532985 0.028639 0.273147 0.073 Uiso calc 1 . .
C C12 0.64631(11) 0.5270(3) 0.40176(8) 0.0347(4) Uani d 1 . .
C C13 0.72398(11) 0.6614(3) 0.44940(7) 0.0354(4) Uani d 1 . .
C C14 0.82345(12) 0.6380(3) 0.44946(8) 0.0434(4) Uani d 1 . .
C C15 0.89032(13) 0.7825(4) 0.49132(9) 0.0542(5) Uani d 1 . .
H H15 0.958279 0.768532 0.493049 0.065 Uiso calc 1 . .
C C16 0.86065(15) 0.9438(4) 0.52999(10) 0.0570(5) Uani d 1 . .
H H16 0.907959 1.038829 0.557856 0.068 Uiso calc 1 . .
C C17 0.76266(14) 0.9680(3) 0.52843(9) 0.0494(5) Uani d 1 . .
H H17 0.741807 1.081099 0.554378 0.059 Uiso calc 1 . .
C C18 0.69493(13) 0.8255(3) 0.48861(8) 0.0393(4) Uani d 1 . .
H H18 0.627359 0.839894 0.488038 0.047 Uiso calc 1 . .
C C19 0.85746(14) 0.4649(4) 0.40751(10) 0.0565(5) Uani d 1 . .
H H19A 0.831736 0.319332 0.416327 0.085 Uiso calc 1 . .
H H19B 0.929442 0.460215 0.419470 0.085 Uiso calc 1 . .
H H19C 0.833464 0.501673 0.359240 0.085 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 0.0428(6) 0.0308(6) 0.0287(5) 0.0013(4) 0.0024(4) -0.0027(4)
O2 0.0568(7) 0.0476(7) 0.0299(6) 0.0012(6) 0.0078(5) -0.0015(5)
N1 0.0392(7) 0.0366(7) 0.0255(6) 0.0015(5) 0.0004(5) -0.0017(6)
N2 0.0450(7) 0.0254(6) 0.0303(6) 0.0001(5) 0.0021(5) -0.0021(5)
N3 0.0388(7) 0.0282(6) 0.0291(6) -0.0002(5) 0.0013(5) -0.0014(5)
C1 0.0393(8) 0.0310(8) 0.0279(7) 0.0033(6) 0.0004(6) 0.0010(6)
C2 0.0452(8) 0.0294(8) 0.0287(7) 0.0051(6) 0.0016(6) 0.0021(6)
C3 0.0402(8) 0.0262(7) 0.0242(7) -0.0016(6) 0.0013(6) 0.0007(6)
C4 0.0372(8) 0.0242(7) 0.0356(8) -0.0040(6) 0.0001(6) 0.0019(6)
C5 0.0442(8) 0.0320(8) 0.0361(8) -0.0061(7) 0.0002(7) 0.0040(7)
C6 0.0529(10) 0.0363(9) 0.0426(9) -0.0076(7) -0.0078(8) 0.0060(7)
C7 0.0456(9) 0.0354(9) 0.0621(12) 0.0007(7) -0.0110(8) 0.0014(8)
C8 0.0419(9) 0.0366(9) 0.0618(11) 0.0007(7) 0.0041(8) -0.0051(8)
C9 0.0440(9) 0.0305(8) 0.0411(9) -0.0043(6) 0.0040(7) -0.0019(7)
C10 0.0611(10) 0.0261(8) 0.0343(8) -0.0070(7) 0.0063(7) -0.0003(6)
C11 0.0563(10) 0.0405(9) 0.0427(9) 0.0139(8) 0.0004(8) -0.0079(8)
C12 0.0402(8) 0.0303(8) 0.0310(8) 0.0079(6) 0.0038(6) 0.0020(6)
C13 0.0398(8) 0.0338(8) 0.0297(7) 0.0021(6) 0.0031(6) 0.0066(6)
C14 0.0422(8) 0.0485(10) 0.0380(9) 0.0062(7) 0.0067(7) 0.0120(8)
C15 0.0419(9) 0.0672(13) 0.0498(10) -0.0065(9) 0.0041(8) 0.0157(10)
C16 0.0630(12) 0.0571(12) 0.0453(10) -0.0220(10) 0.0028(9) 0.0019(9)
C17 0.0667(12) 0.0393(9) 0.0399(9) -0.0098(8) 0.0089(8) -0.0016(8)
C18 0.0478(9) 0.0353(9) 0.0333(8) 0.0004(7) 0.0071(7) 0.0013(6)
C19 0.0488(10) 0.0657(13) 0.0545(11) 0.0189(9) 0.0118(9) 0.0095(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0210
1 0 0 0.0140
0 1 0 0.0871
0 -1 0 0.1011
1 0 -2 0.0377
-1 0 2 0.0367
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 N1 H1 . . 114.1(12) ?
C12 N1 H1 . . 122.7(12) ?
C12 N1 C1 . . 122.25(13) ?
N3 N2 C10 . . 114.41(13) ?
C2 N2 N3 . . 106.81(11) ?
C2 N2 C10 . . 120.57(13) ?
N2 N3 C4 . . 117.86(11) ?
C3 N3 N2 . . 109.39(12) ?
C3 N3 C4 . . 124.08(12) ?
N1 C1 C3 . . 121.64(13) ?
C2 C1 N1 . . 129.16(14) ?
C2 C1 C3 . . 108.92(13) ?
N2 C2 C11 . . 120.04(14) ?
C1 C2 N2 . . 109.45(14) ?
C1 C2 C11 . . 130.51(15) ?
O1 C3 N3 . . 124.61(14) ?
O1 C3 C1 . . 130.33(14) ?
N3 C3 C1 . . 105.02(12) ?
C5 C4 N3 . . 119.73(14) ?
C9 C4 N3 . . 119.17(13) ?
C9 C4 C5 . . 121.09(15) ?
C4 C5 H5 . . 120.7 ?
C6 C5 C4 . . 118.69(17) ?
C6 C5 H5 . . 120.7 ?
C5 C6 H6 . . 119.6 ?
C7 C6 C5 . . 120.87(17) ?
C7 C6 H6 . . 119.6 ?
C6 C7 H7 . . 120.2 ?
C6 C7 C8 . . 119.65(16) ?
C8 C7 H7 . . 120.2 ?
C7 C8 H8 . . 119.7 ?
C9 C8 C7 . . 120.68(18) ?
C9 C8 H8 . . 119.7 ?
C4 C9 H9 . . 120.5 ?
C8 C9 C4 . . 118.99(16) ?
C8 C9 H9 . . 120.5 ?
N2 C10 H10A . . 109.5 ?
N2 C10 H10B . . 109.5 ?
N2 C10 H10C . . 109.5 ?
H10A C10 H10B . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C2 C11 H11A . . 109.5 ?
C2 C11 H11B . . 109.5 ?
C2 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O2 C12 N1 . . 123.23(15) ?
O2 C12 C13 . . 121.13(14) ?
N1 C12 C13 . . 115.56(13) ?
C14 C13 C12 . . 120.70(15) ?
C18 C13 C12 . . 118.77(14) ?
C18 C13 C14 . . 120.21(15) ?
C13 C14 C19 . . 121.78(17) ?
C15 C14 C13 . . 117.12(17) ?
C15 C14 C19 . . 121.09(17) ?
C14 C15 H15 . . 119.0 ?
C16 C15 C14 . . 122.09(17) ?
C16 C15 H15 . . 119.0 ?
C15 C16 H16 . . 119.9 ?
C15 C16 C17 . . 120.22(17) ?
C17 C16 H16 . . 119.9 ?
C16 C17 H17 . . 120.4 ?
C16 C17 C18 . . 119.17(18) ?
C18 C17 H17 . . 120.4 ?
C13 C18 H18 . . 119.4 ?
C17 C18 C13 . . 121.17(17) ?
C17 C18 H18 . . 119.4 ?
C14 C19 H19A . . 109.5 ?
C14 C19 H19B . . 109.5 ?
C14 C19 H19C . . 109.5 ?
H19A C19 H19B . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 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 C3 . 1.2396(18) ?
O2 C12 . 1.2242(19) ?
N1 H1 . 0.86(2) ?
N1 C1 . 1.4148(19) ?
N1 C12 . 1.351(2) ?
N2 N3 . 1.4055(18) ?
N2 C2 . 1.376(2) ?
N2 C10 . 1.4773(19) ?
N3 C3 . 1.3933(18) ?
N3 C4 . 1.4232(19) ?
C1 C2 . 1.361(2) ?
C1 C3 . 1.430(2) ?
C2 C11 . 1.481(2) ?
C4 C5 . 1.395(2) ?
C4 C9 . 1.387(2) ?
C5 H5 . 0.9500 ?
C5 C6 . 1.389(2) ?
C6 H6 . 0.9500 ?
C6 C7 . 1.379(3) ?
C7 H7 . 0.9500 ?
C7 C8 . 1.389(3) ?
C8 H8 . 0.9500 ?
C8 C9 . 1.385(2) ?
C9 H9 . 0.9500 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 C13 . 1.503(2) ?
C13 C14 . 1.404(2) ?
C13 C18 . 1.391(2) ?
C14 C15 . 1.402(3) ?
C14 C19 . 1.496(3) ?
C15 H15 . 0.9500 ?
C15 C16 . 1.376(3) ?
C16 H16 . 0.9500 ?
C16 C17 . 1.376(3) ?
C17 H17 . 0.9500 ?
C17 C18 . 1.383(2) ?
C18 H18 . 0.9500 ?
C19 H19A . 0.9800 ?
C19 H19B . 0.9800 ?
C19 H19C . 0.9800 ?
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
N1 H1 O1 3_666 0.86(2) 1.96(2) 2.8125(17) 171.3(18) yes
_cod_database_fobs_code 2312694