Structural, theoretic and spectroscopic analysis of 2-methyl-5-nitroaniline salts with various inorganic acids
Medviediev, Volodymyr; Daszkiewicz, Marek; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619012472

data_2108517
_publ_section_title
;
 Structural, theoretic and spectroscopic analysis of
 2-methyl-5-nitroaniline salts with various inorganic acids
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619012472
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'C7 H9 N2 O2, N O3'
_chemical_formula_sum            'C7 H9 N3 O5'
_chemical_formula_weight         215.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.712(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1234(3)
_cell_length_b                   6.6252(2)
_cell_length_c                   8.5799(3)
_cell_measurement_reflns_used    6221
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      29.4240
_cell_measurement_theta_min      3.2150
_cell_volume                     456.44(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     35.00 104.75   0.75   15.00    --   14.80 178.00   0.00   93
  2  \w    -76.00 104.00   0.75   15.00    --   14.80   0.00-180.00  240
  3  \w   -107.00  73.75   0.75   15.00    --  -15.89   0.00 120.00  241
  4  \w    -25.00  56.75   0.75   15.00    --   14.80 -99.00 150.00  109
  5  \w    -25.00  26.00   0.75   15.00    --  -15.89 -99.00  90.00   68
  6  \w   -106.00 -33.25   0.75   15.00    --  -15.89 178.00 -90.00   97
  7  \w    -92.00  13.75   0.75   15.00    --  -15.89 -57.00 -30.00  141
  8  \w    -25.00  26.00   0.75   15.00    --  -15.89 -99.00-180.00   68
  9  \w    -25.00  26.00   0.75   15.00    --  -15.89 -99.00 -90.00   68
 10  \w    -25.00  56.75   0.75   15.00    --   14.80 -99.00-150.00  109
 11  \w    -25.00  26.00   0.75   15.00    --  -15.89 -99.00-150.00   68
 12  \w    -25.00  26.00   0.75   15.00    --  -15.89 -99.00  30.00   68
 13  \w    -25.00  26.00   0.75   15.00    --  -15.89 -99.00 120.00   68
 14  \w    -51.00  66.00   0.75   15.00    --  -15.89  77.00 -30.00  156
 15  \w   -106.00 -33.25   0.75   15.00    --  -15.89 178.00 150.00   97
 16  \w    -25.00  56.75   0.75   15.00    --   14.80 -99.00  90.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0772075000
_diffrn_orient_matrix_UB_12      -0.0186824000
_diffrn_orient_matrix_UB_13      0.0485705000
_diffrn_orient_matrix_UB_21      -0.0346751000
_diffrn_orient_matrix_UB_22      -0.0860973000
_diffrn_orient_matrix_UB_23      0.0318868000
_diffrn_orient_matrix_UB_31      0.0253405000
_diffrn_orient_matrix_UB_32      -0.0607680000
_diffrn_orient_matrix_UB_33      -0.0601764000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16584
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       plate
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.1128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1078
_reflns_number_total             1273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5028sup1.cif
_cod_data_source_block           3
_cod_database_code               2108517
_cod_database_fobs_code          2108517
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.952
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6)
;
_shelx_res_checksum              44429
_shelx_hkl_checksum              61216
_olex2_date_sample_data_collection 2017-04-15
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.936