#------------------------------------------------------------------------------
#$Date: 2023-08-24 04:43:32 +0300 (Thu, 24 Aug 2023) $
#$Revision: 285854 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022840.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_2022840
loop_
_publ_author_name
'Flores, Maritza J.'
'Mai, Brandon'
'Tanski, Joseph M.'
_publ_section_title
;
Spectroscopic, crystallographic, and Hirshfeld surface characterization
of nine-membered-ring-containing
9-methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione and its parent
tetrahydrocarbazole
;
_journal_coeditor_code DX2054
_journal_issue 9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023007259
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C13 H15 N O3'
_chemical_formula_moiety 'C13 H15 N O3'
_chemical_formula_sum 'C13 H15 N O3'
_chemical_formula_weight 233.26
_chemical_name_systematic
;
9-Methoxy-3,4,5,6-tetrahydro-1H-benzo[b]azonine-2,7-dione
;
_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
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 96.4840(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 16.0139(8)
_cell_length_b 8.2743(4)
_cell_length_c 8.5596(4)
_cell_measurement_reflns_used 9966
_cell_measurement_temperature 125.(2)
_cell_measurement_theta_max 30.5027
_cell_measurement_theta_min 2.5601
_cell_volume 1126.92(9)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2008), OLEX2 (Dolomanov et al.,
2009), and
Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 125.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0384
_diffrn_reflns_av_unetI/netI 0.0244
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 27192
_diffrn_reflns_theta_full 25.24
_diffrn_reflns_theta_max 30.53
_diffrn_reflns_theta_min 2.56
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 30.0
_diffrn_source_power 1.50
_diffrn_source_voltage 45
_exptl_absorpt_coefficient_mu 0.098
_exptl_absorpt_correction_T_max 1.00
_exptl_absorpt_correction_T_min 0.91
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.375
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 496
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.374
_refine_diff_density_min -0.190
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 158
_refine_ls_number_reflns 3432
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.044
_refine_ls_R_factor_all 0.0559
_refine_ls_R_factor_gt 0.0401
_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^)+(0.0545P)^2^+0.3033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0997
_refine_ls_wR_factor_ref 0.1099
_reflns_number_gt 2685
_reflns_number_total 3432
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dx2054sup1.cif
_cod_data_source_block I
_cod_database_code 2022840
_shelx_hkl_file
;
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-10 -2 -7 15.20 3.30
10 -2 7 21.00 4.20
10 -2 7 26.00 4.00
10 -2 7 23.00 3.70
-10 2 -8 6.20 3.00
10 2 8 3.80 2.40
10 2 8 9.20 3.10
10 2 8 -0.40 2.30
10 -2 8 4.90 2.60
-10 -2 -8 8.00 2.90
10 -2 8 10.40 3.80
-10 -2 -8 1.30 2.20
10 -2 8 6.20 2.90
10 2 9 1.20 2.30
10 2 9 0.50 3.00
-10 2 -9 -1.70 2.30
10 -2 9 1.20 2.90
10 -2 9 -1.90 2.10
10 -2 9 4.50 3.40
-10 -2 -9 0.30 2.50
-10 -2 -9 0.80 2.30
10 2 10 4.10 3.00
10 2 10 3.60 3.30
-10 -2 -10 3.50 3.00
10 -2 10 6.80 3.70
10 -2 10 0.10 3.50
10 -2 10 3.30 2.80
-10 -2 -10 3.70 3.00
-10 3 10 41.70 4.30
-10 3 10 33.10 5.40
10 -3 -10 38.10 5.30
10 3 -9 12.20 3.50
-10 3 9 6.50 3.00
-10 3 9 6.50 2.20
10 -3 -9 11.00 3.20
10 -3 -9 9.50 3.60
-10 -3 9 8.00 2.80
-10 3 8 58.59 5.50
-10 3 8 54.59 4.20
10 3 -8 50.99 4.60
10 3 -8 44.80 5.10
10 -3 -8 68.19 5.40
-10 -3 8 53.59 5.00
10 -3 -8 55.39 5.50
10 3 -7 11.30 2.70
-10 3 7 12.40 2.30
-10 3 7 13.20 3.20
-10 -3 7 17.70 1.40
10 -3 -7 15.50 3.10
-10 -3 7 11.80 3.10
10 -3 -7 16.50 3.70
-10 -3 7 14.60 2.90
10 3 -6 16.00 3.60
-10 3 6 11.60 2.20
-10 3 6 10.30 2.70
10 3 -6 22.00 3.40
-10 3 6 8.60 2.40
10 -3 -6 15.20 2.80
10 -3 -6 14.00 3.10
-10 -3 6 13.90 2.70
-10 -3 6 22.60 3.80
-10 -3 6 16.60 1.60
-10 3 5 74.79 4.30
-10 3 5 84.49 5.10
10 3 -5 88.49 5.10
10 3 -5 81.19 3.90
-10 3 5 75.89 4.90
-10 -3 5 85.59 4.90
10 -3 -5 74.19 5.50
-10 -3 5 80.79 5.60
-10 -3 5 83.19 3.30
-10 3 4 8.20 2.20
-10 3 4 5.80 1.70
10 3 -4 6.80 1.40
-10 3 4 7.10 2.00
10 3 -4 7.10 2.20
-10 -3 4 9.30 2.50
-10 -3 4 10.30 1.70
10 -3 -4 5.60 2.50
-10 -3 4 6.70 1.90
-10 3 3 7.30 2.10
10 3 -3 6.80 2.00
-10 3 3 6.80 1.70
10 3 -3 6.30 1.30
-10 3 3 6.30 1.90
-10 -3 3 9.50 2.10
10 -3 -3 4.90 2.40
-10 -3 3 6.00 1.40
10 -3 -3 9.00 1.70
-10 -3 3 5.80 1.90
-10 3 2 201.28 7.10
-10 3 2 206.08 6.50
-10 3 2 215.18 7.00
10 3 -2 211.58 5.40
10 3 -2 216.28 7.50
-10 -3 2 210.28 7.00
-10 -3 2 207.08 7.80
10 -3 -2 202.48 6.20
-10 -3 2 196.08 6.30
10 -3 -2 194.78 7.50
10 3 -1 2.80 1.50
10 3 -1 4.60 1.20
-10 3 1 5.10 1.70
-10 3 1 7.00 1.60
-10 3 1 1.70 1.20
-10 3 1 3.10 0.80
10 -3 -1 4.00 1.60
10 -3 -1 4.30 1.90
-10 -3 1 3.10 1.70
-10 -3 1 0.70 1.20
-10 -3 1 1.60 1.20
10 3 0 3.60 1.50
10 3 0 7.90 1.50
-10 3 0 10.10 2.00
-10 3 0 10.50 1.90
-10 3 0 10.60 1.50
-10 3 0 7.30 1.50
-10 -3 0 7.80 2.10
-10 -3 0 6.80 1.70
-10 -3 0 7.90 1.80
10 -3 0 10.50 2.20
10 -3 0 10.90 2.40
10 -3 0 10.20 1.90
-10 -3 0 11.00 1.80
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10 3 1 52.59 4.00
-10 3 -1 59.59 3.20
-10 3 -1 54.09 4.00
-10 3 -1 57.69 2.80
10 3 1 51.99 3.10
-10 -3 -1 55.29 3.90
10 -3 1 51.89 3.80
10 -3 1 56.49 4.20
10 -3 1 56.09 3.50
-10 -3 -1 61.09 3.90
-10 -3 -1 49.40 2.30
-10 -3 -1 54.09 3.80
-10 3 -2 3.90 1.90
10 3 2 5.00 1.60
10 3 2 3.70 2.00
-10 3 -2 4.50 1.30
-10 3 -2 6.10 1.50
10 -3 2 5.30 1.70
10 -3 2 3.10 1.50
-10 -3 -2 5.30 1.60
-10 -3 -2 3.70 1.10
10 -3 2 4.00 2.20
-10 -3 -2 6.10 1.90
-10 -3 -2 4.90 1.80
10 3 3 90.19 4.50
10 3 3 87.39 5.20
-10 3 -3 79.49 4.90
-10 3 -3 85.79 3.70
10 -3 3 98.69 4.50
-10 -3 -3 91.39 5.10
10 -3 3 88.39 4.70
10 -3 3 84.49 4.10
10 -3 3 84.09 5.40
-10 -3 -3 96.59 4.40
-10 -3 -3 87.69 5.10
-10 -3 -3 93.49 4.00
-10 3 -4 4.60 1.80
10 3 4 7.00 2.20
10 3 4 5.70 1.90
-10 -3 -4 8.10 1.80
10 -3 4 7.30 2.10
10 -3 4 5.60 1.80
10 -3 4 8.50 2.70
-10 -3 -4 7.10 2.20
10 3 5 9.90 2.40
-10 3 -5 12.30 2.80
10 3 5 16.10 3.10
10 3 5 12.30 2.60
10 -3 5 12.60 3.40
10 -3 5 15.10 2.80
-10 -3 -5 13.80 2.90
-10 -3 -5 18.00 2.80
10 -3 5 9.60 2.40
10 3 6 15.60 2.90
10 3 6 19.50 3.40
10 3 6 20.10 3.60
-10 3 -6 21.90 3.80
-10 -3 -6 19.00 3.20
-10 -3 -6 21.80 3.60
10 -3 6 17.10 3.20
10 -3 6 20.90 3.20
10 -3 6 18.30 3.90
10 3 7 31.80 4.20
10 3 7 32.90 4.50
-10 3 -7 32.90 4.50
10 3 7 33.20 4.30
-10 -3 -7 25.00 3.90
-10 -3 -7 31.70 4.10
10 -3 7 30.40 4.20
10 -3 7 27.70 4.00
10 -3 7 30.30 5.00
-10 3 -8 10.70 3.20
10 3 8 9.90 3.60
10 -3 8 9.70 3.80
10 -3 8 4.10 2.50
-10 -3 -8 3.70 2.50
-10 -3 -8 10.90 3.10
10 -3 8 5.60 3.00
10 3 9 -0.30 3.10
-10 3 -9 -2.00 2.20
10 -3 9 -0.90 2.40
10 -3 9 -0.10 2.90
-10 -3 -9 -2.00 2.40
10 -3 9 7.30 4.10
-10 -3 -9 -0.90 2.30
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-10 4 10 21.60 4.70
10 -4 -10 16.00 4.30
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10 4 -9 1.40 2.70
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-10 4 9 3.50 2.80
10 -4 -9 1.80 2.60
10 -4 -9 5.20 3.30
-10 -4 9 1.30 2.70
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-10 4 8 2.90 2.30
10 4 -8 1.00 2.30
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10 -4 -8 1.60 2.80
-10 -4 8 4.60 1.00
10 -4 -8 4.70 2.70
-10 -4 8 7.70 3.50
10 4 -7 -0.20 2.00
-10 4 7 -0.50 1.50
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10 -4 -7 -0.20 2.00
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-10 -4 7 -0.50 1.70
10 -4 -7 -2.10 2.20
-10 -4 7 0.90 0.80
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10 4 -6 -0.40 1.80
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10 4 -6 2.60 1.50
-10 -4 6 1.10 0.90
-10 -4 6 0.90 1.70
-10 -4 6 2.70 2.10
10 -4 -6 -0.70 2.20
10 -4 -6 1.50 1.90
-10 4 5 85.59 5.30
-10 4 5 78.79 4.70
10 4 -5 76.99 4.10
-10 4 5 76.69 5.20
10 4 -5 76.89 5.30
10 -4 -5 77.49 5.80
-10 -4 5 82.59 4.70
-10 -4 5 68.69 5.30
-10 -4 5 70.79 3.40
10 -4 -5 79.59 5.00
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10 4 -4 9.50 2.50
10 4 -4 12.90 2.10
-10 4 4 9.40 2.20
-10 4 4 9.30 2.40
-10 -4 4 12.30 2.30
-10 -4 4 6.90 1.50
-10 -4 4 14.10 3.20
10 -4 -4 9.50 3.00
-10 4 3 17.00 2.60
10 4 -3 16.20 2.20
10 4 -3 21.40 3.30
-10 4 3 20.20 2.80
-10 4 3 16.10 2.60
-10 -4 3 14.70 2.20
10 -4 -3 11.60 2.80
-10 -4 3 22.40 2.70
-10 -4 3 20.60 3.20
-10 4 2 1.40 1.60
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-10 -4 2 -0.60 1.00
-10 -4 2 1.50 1.40
10 -4 -2 -0.10 1.70
10 -4 -2 -0.30 1.30
-10 -4 2 -0.60 1.40
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10 4 -1 -1.00 1.00
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-10 4 1 -0.20 0.80
10 -4 -1 -0.90 1.40
-10 -4 1 -1.40 1.00
-10 -4 1 -1.20 1.40
10 -4 -1 0.60 1.90
-10 -4 1 -1.00 1.20
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10 4 0 371.26 8.80
-10 4 0 371.96 8.60
-10 4 0 365.36 8.20
-10 4 0 369.66 10.40
10 4 0 356.76 10.40
10 -4 0 352.46 9.50
-10 -4 0 367.86 10.10
-10 -4 0 375.26 10.80
10 -4 0 362.86 10.60
-10 -4 0 384.36 10.20
10 -4 0 360.06 9.90
-10 4 -1 373.96 10.80
-10 4 -1 388.16 8.90
10 4 1 361.56 10.70
-10 4 -1 402.86 10.30
10 4 1 373.86 9.20
-10 4 -1 386.96 8.60
-10 -4 -1 398.46 10.80
10 -4 1 398.76 10.10
10 -4 1 388.06 10.80
-10 -4 -1 392.96 10.90
-10 -4 -1 387.76 10.60
10 -4 1 387.36 10.80
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10 4 2 642.14 15.20
10 4 2 640.04 13.60
-10 4 -2 639.34 15.30
-10 -4 -2 660.93 15.10
-10 -4 -2 644.84 14.60
10 -4 2 635.04 15.50
10 -4 2 643.94 14.20
10 -4 2 659.93 14.60
-10 -4 -2 655.03 15.20
-10 4 -3 142.39 5.70
10 4 3 149.09 6.80
10 4 3 147.09 6.10
-10 4 -3 151.18 6.70
-10 -4 -3 153.18 6.10
10 -4 3 152.48 6.10
-10 -4 -3 145.89 6.60
-10 -4 -3 146.09 6.80
10 -4 3 151.78 7.40
10 -4 3 149.19 6.30
-10 4 -4 33.00 3.30
-10 4 -4 21.80 3.50
10 4 4 28.70 3.50
10 4 4 28.30 3.80
10 -4 4 28.90 3.50
-10 -4 -4 30.00 3.70
10 -4 4 42.50 4.80
10 4 5 3.80 2.30
-10 4 -5 -0.10 2.00
10 4 5 1.30 2.10
10 -4 5 2.70 1.90
10 -4 5 2.30 2.30
-10 -4 -5 2.40 2.10
10 -4 5 3.90 2.00
10 4 6 76.19 5.60
10 4 6 85.59 5.90
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10 -4 6 84.79 5.60
-10 -4 -6 82.39 5.90
10 -4 6 80.89 5.50
10 -4 6 85.99 7.00
10 4 7 99.79 6.80
-10 4 -7 87.39 6.60
-10 -4 -7 103.19 6.90
10 -4 7 93.89 6.40
10 -4 7 96.39 7.60
10 -4 7 93.69 6.10
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10 -4 8 4.10 2.60
-10 -4 -8 0.10 2.40
10 -4 8 -0.90 2.90
10 -4 8 1.30 2.60
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10 -4 9 -4.00 2.70
-10 -4 -9 1.40 3.00
10 -4 9 0.60 3.30
10 -4 9 3.80 2.80
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10 -5 -9 -4.10 2.30
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10 -5 -9 -2.10 3.30
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-10 -5 8 3.40 2.70
-10 -5 8 1.10 1.00
10 -5 -8 -0.70 2.30
10 -5 -8 -1.70 2.70
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-10 -5 7 7.30 1.40
10 -5 -7 8.00 2.80
10 -5 -7 9.20 3.40
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10 -5 -6 -0.30 2.10
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10 -5 -6 -1.50 1.90
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-10 -5 5 8.40 2.80
10 -5 -5 11.30 2.70
10 -5 -5 10.40 3.40
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-10 -5 5 10.10 1.80
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-10 -5 4 5.60 1.50
10 -5 -4 8.30 2.90
10 -5 -4 6.90 2.10
-10 -5 4 5.90 2.60
-10 -5 4 8.30 2.10
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-10 5 3 48.00 4.20
10 5 -3 43.50 3.40
10 5 -3 40.70 4.30
-10 5 3 45.10 3.80
-10 -5 3 45.60 3.40
10 -5 -3 45.90 4.70
-10 -5 3 50.69 3.70
-10 -5 3 38.00 4.40
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10 -5 -2 66.09 4.00
-10 -5 2 56.69 4.80
-10 -5 2 69.49 4.40
-10 -5 2 69.39 4.20
10 -5 -2 65.29 5.20
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10 -5 -1 -0.60 1.50
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10 -5 0 8.80 2.40
-10 -5 0 6.50 2.30
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10 -5 0 8.90 2.50
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-10 -5 -1 43.30 4.10
10 -5 1 39.70 4.10
10 -5 1 42.10 4.10
-10 -5 -1 45.70 4.10
10 -5 1 45.00 3.90
-10 -5 -1 39.70 3.80
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10 -5 2 3.80 2.10
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10 -5 2 -1.70 1.70
10 -5 2 6.30 2.10
-10 -5 -2 3.50 1.80
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-10 -5 -3 14.90 2.80
10 -5 3 14.60 2.70
10 -5 3 13.80 2.80
10 -5 3 13.30 3.40
-10 -5 -3 10.40 2.60
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10 -5 4 -3.20 2.10
-10 -5 -4 2.50 2.00
10 -5 4 -1.00 1.60
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10 5 5 45.70 4.70
10 5 5 37.60 4.50
-10 5 -5 39.80 4.40
-10 -5 -5 44.90 4.70
10 -5 5 44.30 4.30
10 -5 5 47.10 5.50
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10 -5 6 -0.10 2.00
10 -5 6 -2.50 2.50
-10 -5 -6 2.10 2.30
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-10 -5 -7 12.80 3.70
10 -5 7 10.40 3.90
10 -5 7 11.80 3.20
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-10 -5 -8 -0.40 2.70
10 -5 8 1.90 3.40
10 -5 8 0.00 2.30
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10 -6 -9 8.60 3.40
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10 -6 -8 2.40 3.40
-10 -6 8 2.40 2.90
10 -6 -8 4.20 3.20
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10 -6 -7 4.00 2.80
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-10 -6 7 2.40 2.60
10 -6 -7 12.00 3.70
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-10 -6 6 2.30 2.40
10 -6 -6 5.60 3.20
10 -6 -6 5.40 2.60
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10 6 -5 8.90 2.40
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10 -6 -5 11.80 3.40
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-10 -6 5 6.50 2.70
10 -6 -5 9.60 2.70
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-10 -6 4 8.30 2.20
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10 -6 -4 9.90 2.60
10 -6 -4 12.90 3.70
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10 6 -3 50.69 4.90
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10 -6 -3 44.70 3.70
10 -6 -3 43.90 5.00
-10 -6 3 40.10 3.60
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10 -6 -2 14.70 2.40
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10 -6 -2 13.40 3.30
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10 6 -1 62.19 5.20
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-10 -6 1 65.39 4.50
10 -6 -1 55.29 5.20
10 -6 -1 59.19 4.30
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10 6 0 85.39 4.90
10 6 0 83.69 5.70
-10 -6 0 85.89 5.90
10 -6 0 88.79 5.40
-10 -6 0 88.49 5.50
-10 -6 0 75.09 4.80
10 -6 0 91.39 6.10
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10 6 1 15.50 2.60
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-10 -6 -1 27.90 3.80
-10 -6 -1 17.90 3.30
10 -6 1 15.10 3.10
10 -6 1 20.30 3.80
-10 -6 -1 21.50 3.50
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10 6 2 12.50 3.00
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10 -6 2 12.20 3.10
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-10 -6 -2 14.90 3.00
-10 -6 -2 13.20 2.90
10 -6 2 7.50 2.50
10 -6 2 6.10 2.70
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10 6 3 13.80 3.10
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10 -6 3 11.50 3.00
10 -6 3 12.60 2.90
10 -6 3 11.60 3.30
-10 -6 -3 11.60 2.80
-10 -6 -3 13.70 3.20
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-10 -6 -4 1.80 2.20
10 -6 4 1.00 1.90
10 -6 4 -0.80 2.40
10 6 5 2.40 2.60
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20 -3 0 0.20 3.20
-20 -3 0 1.10 2.40
20 -3 0 2.80 3.50
-20 3 -1 3.20 2.90
20 3 1 2.10 3.60
-20 -3 -1 7.70 3.50
20 -3 1 1.30 3.60
20 3 2 20.60 5.10
-20 3 -2 25.50 4.80
-20 -3 -2 20.50 4.40
20 -3 2 19.70 4.90
-20 3 -3 2.40 3.10
20 3 3 -0.60 3.50
-20 -3 -3 -0.20 3.10
20 -3 3 1.90 4.10
-20 4 5 0.40 2.70
-20 4 5 6.40 3.60
-20 4 5 4.50 3.30
20 4 -5 2.00 3.70
-20 -4 5 5.50 3.70
-20 4 4 5.30 3.60
-20 4 4 13.30 3.80
-20 4 4 8.90 3.70
20 4 -4 8.40 4.50
20 4 -4 -0.60 3.60
-20 -4 4 7.30 3.60
20 -4 -4 9.00 4.70
-20 -4 4 5.40 2.90
-20 4 3 3.70 3.20
-20 4 3 5.50 3.20
20 4 -3 7.20 4.30
20 4 -3 -1.00 3.60
-20 -4 3 4.00 3.20
-20 -4 3 3.70 2.80
20 -4 -3 2.20 4.30
-20 4 2 3.10 2.90
20 4 -2 0.80 3.40
20 4 -2 4.10 3.70
-20 4 2 0.20 2.60
-20 -4 2 2.40 3.10
20 -4 -2 2.40 3.80
-20 -4 2 2.90 2.50
20 4 -1 -3.00 3.10
20 4 -1 0.60 3.50
-20 4 1 -2.90 2.60
-20 -4 1 0.10 2.20
20 -4 -1 1.00 3.50
-20 -4 1 -1.50 2.40
-20 4 0 -4.70 2.20
20 4 0 -2.60 3.30
20 4 0 -4.50 3.10
20 -4 0 1.80 3.40
-20 -4 0 1.10 2.60
20 -4 0 -0.20 3.30
-20 -4 0 0.40 2.70
-20 4 -1 30.00 5.20
20 4 1 22.20 5.30
-20 -4 -1 38.80 5.80
20 -4 1 28.60 5.50
-20 4 -2 17.40 4.30
20 4 2 13.40 4.90
20 -4 2 11.10 4.90
-20 -4 -2 8.70 3.90
-20 5 4 3.50 3.10
-20 -5 4 8.20 6.70
20 5 -3 3.40 4.40
20 5 -3 -0.10 3.90
-20 5 3 5.40 3.40
-20 -5 3 3.60 3.20
-20 -5 3 1.10 2.50
-20 -5 3 4.50 4.10
20 -5 -3 -0.90 3.90
20 5 -2 5.20 4.30
-20 5 2 6.20 3.60
20 5 -2 6.80 4.30
20 -5 -2 10.10 4.60
-20 -5 2 14.50 4.80
-20 -5 2 7.60 3.30
-20 -5 2 7.30 3.10
20 5 -1 70.89 7.80
20 5 -1 75.19 8.00
-20 5 1 79.09 7.30
-20 -5 1 85.79 7.70
20 -5 -1 84.19 8.10
-20 -5 1 73.69 7.90
-20 -5 1 76.09 6.80
20 5 0 10.90 4.70
-20 5 0 4.50 3.60
20 5 0 6.30 4.10
-20 -5 0 0.20 2.40
-20 -5 0 1.00 3.20
20 -5 0 8.60 4.40
-20 5 -1 -1.50 3.30
20 -5 1 0.90 3.90
21 0 -5 3.90 4.20
-21 0 5 -0.30 2.20
-21 0 5 -0.40 3.00
21 0 -4 8.30 4.70
-21 0 4 4.90 3.50
-21 0 4 2.90 2.70
-21 0 3 2.60 2.90
21 0 -3 -1.10 3.60
-21 0 3 -1.00 2.30
21 0 -3 2.90 3.50
21 0 -2 138.19 8.90
21 0 -2 124.29 8.90
-21 0 2 139.19 8.40
-21 0 2 139.89 8.40
21 0 -1 -0.50 3.10
-21 0 1 -3.30 2.30
-21 0 1 -0.90 2.30
21 0 -1 -4.70 2.90
21 0 0 6.90 4.00
-21 0 0 5.00 2.80
21 0 0 4.40 4.60
21 0 1 -1.70 3.20
-21 0 -1 3.70 3.00
-21 0 -2 14.70 3.70
21 0 2 10.50 4.90
-21 0 -3 0.30 2.50
-21 1 5 7.00 3.60
-21 1 5 14.00 3.60
21 1 -5 11.50 4.90
21 -1 -5 2.70 4.40
-21 -1 5 8.00 3.10
-21 -1 5 15.40 4.50
-21 1 4 38.40 5.80
-21 1 4 36.70 5.40
21 1 -4 40.10 6.80
21 1 -4 38.80 6.10
-21 -1 4 30.50 5.40
21 -1 -4 34.70 6.10
-21 -1 4 49.40 5.60
21 1 -3 25.30 5.50
-21 1 3 34.70 5.30
21 1 -3 21.30 4.90
-21 1 3 20.20 4.20
-21 -1 3 12.80 3.30
21 -1 -3 21.60 5.40
-21 -1 3 18.50 4.40
21 1 -2 0.00 3.50
-21 1 2 2.70 2.40
21 1 -2 -7.00 2.80
-21 1 2 -1.00 2.30
21 -1 -2 -2.10 3.20
21 -1 -2 -1.70 3.20
-21 -1 2 2.60 2.40
-21 -1 2 -1.90 2.40
-21 1 1 0.90 2.70
21 1 -1 2.60 3.50
21 1 -1 2.40 3.40
-21 -1 1 2.20 3.00
-21 -1 1 0.70 2.50
21 -1 -1 1.50 3.00
21 -1 -1 2.70 3.30
-21 1 0 45.60 5.70
21 1 0 46.80 6.80
-21 -1 0 53.19 5.90
21 -1 0 41.10 6.50
21 -1 0 41.60 7.30
-21 1 -1 -0.80 2.40
21 1 1 -1.20 3.60
21 -1 1 -3.20 3.40
-21 -1 -1 0.10 2.50
-21 1 -2 8.70 3.40
21 1 2 11.80 4.40
21 -1 2 8.80 4.40
-21 -1 -2 4.50 3.20
-21 -1 -3 34.60 5.50
21 -1 3 34.70 9.80
21 2 -5 -1.10 3.30
-21 2 5 0.50 3.10
-21 2 5 2.70 2.60
-21 2 5 1.20 2.80
21 2 -5 0.50 5.40
21 -2 -5 -4.00 6.10
-21 -2 5 0.40 4.30
-21 -2 5 2.00 2.70
21 2 -4 5.30 3.90
-21 2 4 3.70 2.90
21 2 -4 1.00 3.50
-21 2 4 3.00 2.70
-21 2 4 1.60 3.00
-21 -2 4 3.60 3.00
-21 -2 4 2.50 2.60
21 -2 -4 1.10 3.40
21 2 -3 11.50 4.90
-21 2 3 9.50 3.40
-21 2 3 16.00 4.10
21 2 -3 19.40 4.70
-21 2 3 13.70 3.70
-21 -2 3 14.30 3.50
21 -2 -3 16.90 4.70
-21 -2 3 15.80 4.30
21 2 -2 -0.30 3.40
-21 2 2 1.40 2.40
21 2 -2 -1.80 3.40
-21 2 2 0.60 2.50
-21 2 2 -2.60 2.20
21 -2 -2 -5.40 3.30
-21 -2 2 2.00 2.40
-21 -2 2 5.00 3.10
21 -2 -2 1.90 3.60
21 2 -1 15.30 4.60
-21 2 1 8.00 3.20
21 2 -1 17.00 5.00
-21 2 1 14.80 3.80
21 -2 -1 10.60 4.00
21 -2 -1 9.60 4.30
-21 -2 1 8.00 3.50
-21 -2 1 12.30 3.40
-21 2 0 11.00 3.40
21 2 0 1.40 3.90
-21 2 0 5.50 3.00
21 -2 0 2.40 5.00
21 -2 0 4.50 3.70
-21 -2 0 1.10 2.80
21 2 1 26.20 5.90
-21 2 -1 17.50 4.20
-21 2 -1 17.60 4.00
21 -2 1 28.90 5.60
-21 -2 -1 21.00 4.70
21 2 2 41.60 7.00
-21 2 -2 37.20 5.70
21 -2 2 41.60 6.90
-21 -2 -2 41.70 6.00
-21 2 -3 8.10 3.50
-21 -2 -3 1.90 4.00
21 3 -4 7.10 4.70
21 3 -4 5.70 3.90
-21 3 4 0.70 3.00
-21 3 4 9.40 3.60
-21 3 4 0.80 2.60
-21 -3 4 9.20 3.20
21 -3 -4 4.50 4.10
-21 -3 4 2.70 3.20
-21 3 3 4.20 2.80
21 3 -3 1.80 3.50
21 3 -3 4.50 4.40
-21 3 3 8.70 3.50
-21 3 3 6.00 3.20
-21 -3 3 2.50 2.60
21 -3 -3 2.70 4.10
-21 -3 3 4.20 3.20
21 3 -2 6.30 4.20
-21 3 2 18.10 4.20
21 3 -2 11.50 4.50
-21 3 2 8.60 3.30
-21 -3 2 9.90 3.40
-21 -3 2 21.60 4.80
21 -3 -2 19.10 5.30
21 3 -1 2.30 3.70
-21 3 1 2.20 2.80
21 3 -1 -1.00 3.80
-21 3 1 -0.10 2.40
21 -3 -1 2.20 3.80
-21 -3 1 1.30 2.90
-21 -3 1 4.70 3.10
21 -3 -1 7.00 4.00
-21 3 0 -1.40 2.60
21 3 0 -1.10 3.60
-21 -3 0 1.20 3.20
21 -3 0 3.50 3.60
-21 3 -1 40.00 5.70
21 3 1 24.90 5.70
21 -3 1 25.00 5.50
-21 -3 -1 40.80 6.20
-21 3 -2 6.40 3.50
21 -3 2 -1.70 3.90
-21 4 3 7.40 3.60
21 4 -3 9.60 4.50
21 4 -3 3.20 4.20
-21 4 3 9.90 3.60
-21 -4 3 7.80 3.20
21 -4 -3 11.80 5.10
21 4 -2 5.40 4.10
21 4 -2 2.80 3.90
-21 4 2 1.00 3.00
-21 -4 2 0.30 3.70
-21 -4 2 -0.30 2.60
21 -4 -2 8.40 4.40
21 4 -1 40.20 6.60
-21 4 1 44.30 6.20
21 4 -1 31.40 6.20
21 -4 -1 32.20 6.10
-21 -4 1 34.70 6.10
-21 -4 1 37.80 5.70
-21 4 0 43.00 6.00
21 -4 0 47.50 7.30
-21 4 -1 1.90 3.20
21 -4 1 -2.40 3.40
-22 0 4 26.50 4.70
22 0 -4 28.00 7.20
22 0 -3 -2.60 3.40
-22 0 3 -2.70 2.10
22 0 -3 2.60 3.80
-22 0 3 -1.20 2.90
22 0 -2 16.40 5.10
-22 0 2 12.80 3.90
-22 0 2 12.90 3.50
22 0 -2 17.10 4.90
22 0 -1 -1.40 3.60
-22 0 1 -1.90 2.80
22 0 -1 4.90 3.80
22 0 0 2.00 3.70
-22 0 0 1.20 2.80
-22 0 -1 -2.80 2.50
22 0 1 -4.80 3.60
-22 0 -2 11.10 3.80
-22 1 4 57.79 10.10
-22 1 4 44.60 6.00
22 1 -4 45.40 7.30
22 1 -4 45.60 10.90
22 -1 -4 47.30 11.70
-22 -1 4 44.10 5.90
22 1 -3 3.00 3.90
22 1 -3 -0.20 3.80
-22 1 3 -1.30 2.60
-22 1 3 2.40 2.80
-22 -1 3 -0.80 2.40
22 -1 -3 0.80 3.90
-22 -1 3 1.00 3.10
22 1 -2 6.90 4.30
-22 1 2 2.90 3.10
-22 1 2 2.50 2.90
22 1 -2 4.30 4.20
-22 -1 2 0.10 2.60
-22 -1 2 5.00 3.30
22 -1 -2 9.30 4.30
22 -1 -2 2.60 3.80
22 1 -1 -2.00 3.60
-22 1 1 -3.10 2.30
22 1 -1 5.70 4.00
-22 -1 1 2.30 2.80
22 -1 -1 3.20 3.40
-22 -1 1 -0.70 2.80
22 -1 -1 -5.70 3.20
22 1 0 8.80 4.30
-22 1 0 5.60 3.40
-22 -1 0 7.80 3.70
22 -1 0 3.00 4.20
-22 1 -1 10.80 3.80
22 1 1 12.80 5.10
-22 -1 -1 20.80 4.50
22 -1 1 20.60 5.20
22 2 -3 10.90 4.40
22 2 -3 3.70 4.30
-22 2 3 3.50 3.20
-22 2 3 6.10 3.20
22 -2 -3 5.00 4.40
-22 -2 3 4.40 2.80
-22 2 2 0.20 2.60
22 2 -2 -3.60 3.50
22 2 -2 2.20 4.10
22 -2 -2 4.60 4.20
-22 -2 2 -0.50 2.40
-22 -2 2 5.90 3.80
22 2 -1 -2.30 3.90
22 2 -1 -4.60 3.20
-22 2 1 3.00 3.00
22 -2 -1 -2.70 3.70
-22 -2 1 -2.40 2.80
22 -2 -1 0.20 3.40
-22 -2 1 0.40 2.30
22 2 0 57.19 7.70
-22 2 0 66.59 7.10
-22 2 0 47.60 5.60
22 -2 0 48.90 7.40
-22 -2 0 49.60 7.10
-22 2 -1 24.80 4.70
22 -2 1 21.00 5.10
-22 3 2 11.60 4.00
-22 3 2 13.00 3.90
22 3 -2 13.20 5.00
-22 -3 2 8.60 3.40
22 -3 -2 8.90 4.80
-22 3 1 10.10 4.00
22 3 -1 11.30 4.60
-22 -3 1 16.30 4.10
22 -3 -1 15.50 5.10
-22 3 0 0.80 2.80
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 33670
_shelx_res_file
;
TITL MF2923C_a.res in P2(1)/c
MF2923C_a.res
created by SHELXL-2017/1 at 11:07:58 on 19-Jun-2023
CELL 0.71073 16.0139 8.2743 8.5596 90.000 96.484 90.000
ZERR 4.000 0.0008 0.0004 0.0004 0.000 0.001 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H N O
UNIT 52 60 4 12
REM Old TITL MF2923C in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.118, Rweak 0.003, Alpha 0.020
REM 0.306 for 169 systematic absences, Orientation as input
REM Formula found by SHELXT: C13 N O3
L.S. 16
ACTA
BOND
BOND $H
CONF
DFIX 0.88 N1 H1
HTAB
EQIV $1 x, -y+1/2, z-1/2
HTAB N1 O1_$1
EQIV $2 x, -y+3/2, z-1/2
HTAB C5 O2_$2
EQIV $3 -x+1, y-1/2, -z+3/2
HTAB C13 O2_$3
LIST 4
TEMP -148
SIZE 0.4 0.1 0.03
REM faint yellow needle
FMAP 2
PLAN 20
REM EXTI 0.000000
WGHT 0.054500 0.303300
FVAR 0.61194
O1 4 0.112422 0.382916 0.518398 11.00000 0.02013 0.03147 =
0.01490 0.00142 0.00160 0.00400
O2 4 0.278554 0.621499 0.562008 11.00000 0.03169 0.02230 =
0.02744 -0.00773 -0.00732 0.00510
O3 4 0.478747 0.125903 0.650222 11.00000 0.01789 0.02273 =
0.03323 -0.00219 -0.00608 0.00530
N1 3 0.166381 0.256187 0.316400 11.00000 0.01712 0.02111 =
0.01431 -0.00251 -0.00232 -0.00068
H1 2 0.156357 0.222870 0.219874 11.00000 -1.20000
C1 1 0.107726 0.348002 0.377266 11.00000 0.01473 0.02052 =
0.01743 0.00224 -0.00004 -0.00311
C2 1 0.040816 0.419647 0.259995 11.00000 0.01546 0.02871 =
0.01876 0.00166 -0.00273 0.00017
AFIX 23
H2A 2 -0.005196 0.463892 0.315330 11.00000 -1.20000
H2B 2 0.017052 0.334840 0.186381 11.00000 -1.20000
AFIX 0
C3 1 0.079629 0.555807 0.167663 11.00000 0.02091 0.02489 =
0.01793 0.00264 -0.00316 0.00180
AFIX 23
H3A 2 0.106874 0.506150 0.081181 11.00000 -1.20000
H3B 2 0.033617 0.625756 0.119347 11.00000 -1.20000
AFIX 0
C4 1 0.144607 0.662758 0.265194 11.00000 0.02089 0.02047 =
0.02281 0.00176 -0.00359 0.00266
AFIX 23
H4A 2 0.125394 0.681824 0.369587 11.00000 -1.20000
H4B 2 0.147046 0.768829 0.212390 11.00000 -1.20000
AFIX 0
C5 1 0.234450 0.589707 0.289014 11.00000 0.01936 0.02026 =
0.02116 0.00320 0.00059 0.00084
AFIX 23
H5A 2 0.236483 0.499036 0.214073 11.00000 -1.20000
H5B 2 0.274181 0.673160 0.259799 11.00000 -1.20000
AFIX 0
C6 1 0.266343 0.527907 0.452013 11.00000 0.01398 0.01858 =
0.02118 -0.00121 -0.00083 0.00021
C7 1 0.293624 0.354275 0.471295 11.00000 0.01623 0.01706 =
0.01559 -0.00115 0.00129 0.00132
C8 1 0.371052 0.323666 0.559887 11.00000 0.01675 0.01837 =
0.01872 -0.00227 0.00007 0.00090
AFIX 43
H8 2 0.401666 0.409546 0.613125 11.00000 -1.20000
AFIX 0
C9 1 0.402923 0.167266 0.569629 11.00000 0.01493 0.02145 =
0.01928 0.00044 0.00075 0.00334
C10 1 0.357323 0.040988 0.492786 11.00000 0.02109 0.01772 =
0.02366 -0.00109 0.00278 0.00324
AFIX 43
H10 2 0.379971 -0.065242 0.496916 11.00000 -1.20000
AFIX 0
C11 1 0.279309 0.069858 0.410658 11.00000 0.02074 0.01784 =
0.02017 -0.00294 0.00168 -0.00101
AFIX 43
H11 2 0.247791 -0.017201 0.361538 11.00000 -1.20000
AFIX 0
C12 1 0.246796 0.226108 0.399718 11.00000 0.01569 0.01939 =
0.01324 -0.00046 0.00130 0.00049
C13 1 0.527499 0.252862 0.727461 11.00000 0.01963 0.02814 =
0.03088 -0.00288 -0.00528 0.00204
AFIX 137
H13A 2 0.540945 0.332863 0.649661 11.00000 -1.50000
H13B 2 0.579679 0.208190 0.781320 11.00000 -1.50000
H13C 2 0.495377 0.304782 0.804483 11.00000 -1.50000
AFIX 0
HKLF 4
REM MF2923C_a.res in P2(1)/c
REM R1 = 0.0401 for 2685 Fo > 4sig(Fo) and 0.0559 for all 3432 data
REM 158 parameters refined using 1 restraints
END
WGHT 0.0545 0.3034
REM Instructions for potential hydrogen bonds
HTAB N1 O1_$1
HTAB C5 O2_$2
HTAB C13 O2_$3
REM Highest difference peak 0.374, deepest hole -0.190, 1-sigma level 0.049
Q1 1 0.3958 0.2495 0.5395 11.00000 0.05 0.37
Q2 1 0.2481 0.5586 0.3676 11.00000 0.05 0.37
Q3 1 0.2719 0.3009 0.4211 11.00000 0.05 0.35
Q4 1 0.2785 0.4327 0.4670 11.00000 0.05 0.35
Q5 1 0.2616 0.1494 0.4147 11.00000 0.05 0.34
Q6 1 0.0753 0.3861 0.3151 11.00000 0.05 0.34
Q7 1 0.3836 0.1098 0.5249 11.00000 0.05 0.33
Q8 1 0.1147 0.5962 0.2250 11.00000 0.05 0.31
Q9 1 0.0609 0.4935 0.2183 11.00000 0.05 0.31
Q10 1 0.3327 0.3336 0.5126 11.00000 0.05 0.30
Q11 1 0.2091 0.2466 0.3595 11.00000 0.05 0.29
Q12 1 0.3260 0.0725 0.4354 11.00000 0.05 0.28
Q13 1 0.3133 0.0456 0.4833 11.00000 0.05 0.25
Q14 1 0.1878 0.6193 0.2773 11.00000 0.05 0.25
Q15 1 0.1524 0.3410 0.3356 11.00000 0.05 0.24
Q16 1 0.4400 0.1527 0.6054 11.00000 0.05 0.22
Q17 1 0.1224 0.3998 0.4416 11.00000 0.05 0.21
Q18 1 0.1376 0.2956 0.3541 11.00000 0.05 0.20
Q19 1 0.2724 0.6780 0.3129 11.00000 0.05 0.20
Q20 1 0.1281 0.7277 0.3477 11.00000 0.05 0.19
;
_shelx_res_checksum 37894
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 0.11242(5) 0.38292(11) 0.51840(9) 0.02220(19) Uani d 1 . .
O O2 0.27855(6) 0.62150(11) 0.56201(10) 0.0280(2) Uani d 1 . .
O O3 0.47875(5) 0.12590(10) 0.65022(10) 0.0253(2) Uani d 1 . .
N N1 0.16638(6) 0.25619(12) 0.31640(10) 0.01783(19) Uani d 1 . .
H H1 0.1564(9) 0.2229(17) 0.2199(14) 0.021 Uiso d 1 . .
C C1 0.10773(7) 0.34800(14) 0.37727(12) 0.0177(2) Uani d 1 . .
C C2 0.04082(7) 0.41965(15) 0.26000(13) 0.0213(2) Uani d 1 . .
H H2A -0.005196 0.463892 0.31533 0.026 Uiso calc 1 . .
H H2B 0.017052 0.33484 0.186381 0.026 Uiso calc 1 . .
C C3 0.07963(7) 0.55581(15) 0.16766(13) 0.0217(2) Uani d 1 . .
H H3A 0.106874 0.50615 0.081181 0.026 Uiso calc 1 . .
H H3B 0.033617 0.625756 0.119347 0.026 Uiso calc 1 . .
C C4 0.14461(7) 0.66276(14) 0.26519(13) 0.0218(2) Uani d 1 . .
H H4A 0.125394 0.681824 0.369587 0.026 Uiso calc 1 . .
H H4B 0.147046 0.768829 0.21239 0.026 Uiso calc 1 . .
C C5 0.23445(7) 0.58971(14) 0.28901(13) 0.0204(2) Uani d 1 . .
H H5A 0.236483 0.499036 0.214073 0.024 Uiso calc 1 . .
H H5B 0.274181 0.67316 0.259799 0.024 Uiso calc 1 . .
C C6 0.26634(7) 0.52791(14) 0.45201(13) 0.0181(2) Uani d 1 . .
C C7 0.29362(7) 0.35427(13) 0.47129(12) 0.0163(2) Uani d 1 . .
C C8 0.37105(7) 0.32367(13) 0.55989(12) 0.0181(2) Uani d 1 . .
H H8 0.401666 0.409546 0.613125 0.022 Uiso calc 1 . .
C C9 0.40292(7) 0.16727(14) 0.56963(12) 0.0186(2) Uani d 1 . .
C C10 0.35732(7) 0.04099(14) 0.49279(13) 0.0208(2) Uani d 1 . .
H H10 0.379971 -0.065242 0.496916 0.025 Uiso calc 1 . .
C C11 0.27931(7) 0.06986(14) 0.41066(13) 0.0196(2) Uani d 1 . .
H H11 0.247791 -0.017201 0.361538 0.024 Uiso calc 1 . .
C C12 0.24680(6) 0.22611(13) 0.39972(12) 0.0161(2) Uani d 1 . .
C C13 0.52750(8) 0.25286(16) 0.72746(15) 0.0268(3) Uani d 1 . .
H H13A 0.540945 0.332863 0.649661 0.04 Uiso calc 1 . .
H H13B 0.579679 0.20819 0.78132 0.04 Uiso calc 1 . .
H H13C 0.495377 0.304782 0.804483 0.04 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 0.0201(4) 0.0315(5) 0.0149(3) 0.0040(3) 0.0016(3) 0.0014(3)
O2 0.0317(5) 0.0223(4) 0.0274(4) 0.0051(3) -0.0073(4) -0.0077(3)
O3 0.0179(4) 0.0227(4) 0.0332(5) 0.0053(3) -0.0061(3) -0.0022(3)
N1 0.0171(4) 0.0211(5) 0.0143(4) -0.0007(3) -0.0023(3) -0.0025(3)
C1 0.0147(5) 0.0205(5) 0.0174(5) -0.0031(4) 0.0000(4) 0.0022(4)
C2 0.0155(5) 0.0287(6) 0.0188(5) 0.0002(4) -0.0027(4) 0.0017(4)
C3 0.0209(5) 0.0249(6) 0.0179(5) 0.0018(4) -0.0032(4) 0.0026(4)
C4 0.0209(5) 0.0205(5) 0.0228(5) 0.0027(4) -0.0036(4) 0.0018(4)
C5 0.0194(5) 0.0203(5) 0.0212(5) 0.0008(4) 0.0006(4) 0.0032(4)
C6 0.0140(5) 0.0186(5) 0.0212(5) 0.0002(4) -0.0008(4) -0.0012(4)
C7 0.0162(5) 0.0171(5) 0.0156(4) 0.0013(4) 0.0013(4) -0.0011(4)
C8 0.0167(5) 0.0184(5) 0.0187(5) 0.0009(4) 0.0001(4) -0.0023(4)
C9 0.0149(5) 0.0214(5) 0.0193(5) 0.0033(4) 0.0007(4) 0.0004(4)
C10 0.0211(5) 0.0177(5) 0.0237(5) 0.0032(4) 0.0028(4) -0.0011(4)
C11 0.0207(5) 0.0178(5) 0.0202(5) -0.0010(4) 0.0017(4) -0.0029(4)
C12 0.0157(5) 0.0194(5) 0.0132(4) 0.0005(4) 0.0013(3) -0.0005(4)
C13 0.0196(5) 0.0281(6) 0.0309(6) 0.0020(5) -0.0053(5) -0.0029(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C9 O3 C13 . . 117.19(9) ?
C1 N1 C12 . . 122.17(9) ?
C1 N1 H1 . . 118.8(9) ?
C12 N1 H1 . . 118.8(9) ?
O1 C1 N1 . . 122.53(10) ?
O1 C1 C2 . . 121.33(10) ?
N1 C1 C2 . . 115.85(9) ?
C1 C2 C3 . . 109.33(9) ?
C1 C2 H2A . . 109.8 ?
C3 C2 H2A . . 109.8 ?
C1 C2 H2B . . 109.8 ?
C3 C2 H2B . . 109.8 ?
H2A C2 H2B . . 108.3 ?
C4 C3 C2 . . 115.34(9) ?
C4 C3 H3A . . 108.4 ?
C2 C3 H3A . . 108.4 ?
C4 C3 H3B . . 108.4 ?
C2 C3 H3B . . 108.4 ?
H3A C3 H3B . . 107.5 ?
C3 C4 C5 . . 114.03(10) ?
C3 C4 H4A . . 108.7 ?
C5 C4 H4A . . 108.7 ?
C3 C4 H4B . . 108.7 ?
C5 C4 H4B . . 108.7 ?
H4A C4 H4B . . 107.6 ?
C6 C5 C4 . . 117.52(9) ?
C6 C5 H5A . . 107.9 ?
C4 C5 H5A . . 107.9 ?
C6 C5 H5B . . 107.9 ?
C4 C5 H5B . . 107.9 ?
H5A C5 H5B . . 107.2 ?
O2 C6 C7 . . 120.19(10) ?
O2 C6 C5 . . 120.27(10) ?
C7 C6 C5 . . 119.03(9) ?
C12 C7 C8 . . 119.84(10) ?
C12 C7 C6 . . 122.73(9) ?
C8 C7 C6 . . 117.38(9) ?
C9 C8 C7 . . 119.81(10) ?
C9 C8 H8 . . 120.1 ?
C7 C8 H8 . . 120.1 ?
O3 C9 C8 . . 124.13(10) ?
O3 C9 C10 . . 115.90(10) ?
C8 C9 C10 . . 119.97(10) ?
C11 C10 C9 . . 120.30(10) ?
C11 C10 H10 . . 119.9 ?
C9 C10 H10 . . 119.9 ?
C10 C11 C12 . . 120.24(10) ?
C10 C11 H11 . . 119.9 ?
C12 C11 H11 . . 119.9 ?
C11 C12 C7 . . 119.74(10) ?
C11 C12 N1 . . 120.44(10) ?
C7 C12 N1 . . 119.81(10) ?
O3 C13 H13A . . 109.5 ?
O3 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
O3 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 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 C1 . 1.2361(13) ?
O2 C6 . 1.2177(13) ?
O3 C9 . 1.3705(13) ?
O3 C13 . 1.4260(15) ?
N1 C1 . 1.3570(14) ?
N1 C12 . 1.4218(14) ?
N1 H1 . 0.869(12) ?
C1 C2 . 1.5047(15) ?
C2 C3 . 1.5463(17) ?
C2 H2A . 0.99 ?
C2 H2B . 0.99 ?
C3 C4 . 1.5384(16) ?
C3 H3A . 0.99 ?
C3 H3B . 0.99 ?
C4 C5 . 1.5526(16) ?
C4 H4A . 0.99 ?
C4 H4B . 0.99 ?
C5 C6 . 1.5192(15) ?
C5 H5A . 0.99 ?
C5 H5B . 0.99 ?
C6 C7 . 1.5053(15) ?
C7 C12 . 1.3995(15) ?
C7 C8 . 1.4015(15) ?
C8 C9 . 1.3901(16) ?
C8 H8 . 0.95 ?
C9 C10 . 1.3961(16) ?
C10 C11 . 1.3834(16) ?
C10 H10 . 0.95 ?
C11 C12 . 1.3930(15) ?
C11 H11 . 0.95 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
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 4_565 0.869(12) 1.990(12) 2.8426(12) 166.7(14) y
C5 H5B O2 4_575 0.99 2.41 3.2085(14) 138 y
C13 H13B O2 2_646 0.98 2.60 3.5793(15) 174 y
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
C12 N1 C1 O1 . . . . -15.63(16) ?
C12 N1 C1 C2 . . . . 158.31(10) ?
O1 C1 C2 C3 . . . . 102.43(12) ?
N1 C1 C2 C3 . . . . -71.59(13) ?
C1 C2 C3 C4 . . . . -38.86(13) ?
C2 C3 C4 C5 . . . . 82.68(12) ?
C3 C4 C5 C6 . . . . -108.22(11) ?
C4 C5 C6 O2 . . . . -65.85(14) ?
C4 C5 C6 C7 . . . . 122.35(11) ?
O2 C6 C7 C12 . . . . 142.88(11) ?
C5 C6 C7 C12 . . . . -45.31(14) ?
O2 C6 C7 C8 . . . . -39.79(15) ?
C5 C6 C7 C8 . . . . 132.02(10) ?
C12 C7 C8 C9 . . . . 3.25(16) ?
C6 C7 C8 C9 . . . . -174.16(10) ?
C13 O3 C9 C8 . . . . -0.42(16) ?
C13 O3 C9 C10 . . . . 178.85(10) ?
C7 C8 C9 O3 . . . . 178.48(10) ?
C7 C8 C9 C10 . . . . -0.76(16) ?
O3 C9 C10 C11 . . . . 178.79(10) ?
C8 C9 C10 C11 . . . . -1.91(16) ?
C9 C10 C11 C12 . . . . 2.07(17) ?
C10 C11 C12 C7 . . . . 0.44(16) ?
C10 C11 C12 N1 . . . . -179.54(10) ?
C8 C7 C12 C11 . . . . -3.09(15) ?
C6 C7 C12 C11 . . . . 174.17(10) ?
C8 C7 C12 N1 . . . . 176.89(9) ?
C6 C7 C12 N1 . . . . -5.85(15) ?
C1 N1 C12 C11 . . . . 132.57(11) ?
C1 N1 C12 C7 . . . . -47.40(14) ?
_cod_database_fobs_code 2022840