Isolation of 3-amino-4-nitrobenzyl acetate: evidence of an undisclosed impurity in 5-amino-2-nitrobenzoic acid
Quillian, Brandon; Hendricks, Jordan; Trivitayakhun, Matthew; Padgett, Clifford W.; Acta Crystallographica Section E 71 (2015) 606–608; doi:10.1107/S2056989015008750

data_2240582
_publ_section_title
;
 Isolation of 3-amino-4-nitrobenzyl acetate: evidence of an undisclosed
 impurity in 5-amino-2-nitrobenzoic acid
;
_journal_coeditor_code           PK2548
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              606
_journal_page_last               608
_journal_paper_doi               10.1107/S2056989015008750
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H10 N2 O4'
_chemical_formula_moiety         'C9 H10 N2 O4'
_chemical_formula_sum            'C9 H10 N2 O4'
_chemical_formula_weight         210.19
_chemical_name_systematic
;
3-Amino-4-nitrobenzyl acetate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.341(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4803(15)
_cell_length_b                   11.4054(11)
_cell_length_c                   13.0936(13)
_cell_measurement_reflns_used    513
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      1.6
_cell_volume                     1937.9(4)
_computing_cell_refinement
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2014)
;
_computing_data_collection
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2014)
;
_computing_data_reduction
;
<i>CrystalClear-SM Expert</i> (Rigaku, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
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_computing_publication_material
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'XtaLABmini: Fixed Chi 2 circle'
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8409
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.291
_diffrn_reflns_theta_min         2.377
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         1759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0578P)^2^+0.2118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                1348
_reflns_number_total             1759
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2548sup1.cif
_cod_data_source_block           I
_cod_database_code               2240582
_cod_database_fobs_code          2240582
_shelxl_version_number           2.013