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_2108515
_publ_section_title
;
 Structural, theoretic and spectroscopic analysis of
 2-methyl-5-nitroaniline salts with various inorganic acids
;
_journal_coeditor_code           AW5028
_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, Br'
_chemical_formula_sum            'C7 H9 Br N2 O2'
_chemical_formula_weight         233.07
_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                 110.200(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5689(3)
_cell_length_b                   6.4113(2)
_cell_length_c                   8.8248(4)
_cell_measurement_reflns_used    5231
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      30.2030
_cell_measurement_theta_min      2.6510
_cell_volume                     455.00(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_environment      air
_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 0.997
_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    -61.00  46.00   0.50    2.50    --   14.96 -57.00 -60.00  214
  2  \w    -16.00  91.00   0.50    2.50    --   14.96  57.00 120.00  214
  3  \w    -67.00  50.00   0.50    2.50    --   14.96 -77.00-150.00  234
  4  \w    -25.00  58.00   0.50    2.50    --   14.96 -99.00-120.00  166
  5  \w    -25.00  27.00   0.50    2.50    --  -16.06 -99.00  90.00  104
  6  \w    -16.00  91.00   0.50    2.50    --   14.96  57.00-150.00  214
  7  \w    -25.00  58.00   0.50    2.50    --   14.96 -99.00  90.00  166
  8  \w    -16.00  91.00   0.50    2.50    --   14.96  57.00 -30.00  214
  9  \w    -25.00  27.00   0.50    2.50    --  -16.06 -99.00 150.00  104
 10  \w   -106.00 -32.00   0.50    2.50    --  -16.06 178.00   0.00  148
 11  \w    -25.00  27.00   0.50    2.50    --  -16.06 -99.00 -30.00  104
 12  \w    -25.00  27.00   0.50    2.50    --  -16.06 -99.00 -90.00  104
 13  \w    -45.00  62.00   0.50    2.50    --  -16.06  37.00  90.00  214
 14  \w    -74.00   3.00   0.50    2.50    --  -16.06 125.00 -82.00  154
;
_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      0.0633977000
_diffrn_orient_matrix_UB_12      0.0701374000
_diffrn_orient_matrix_UB_13      0.0442379000
_diffrn_orient_matrix_UB_21      -0.0077970000
_diffrn_orient_matrix_UB_22      -0.0359700000
_diffrn_orient_matrix_UB_23      0.0730487000
_diffrn_orient_matrix_UB_31      0.0608401000
_diffrn_orient_matrix_UB_32      -0.0776404000
_diffrn_orient_matrix_UB_33      0.0060914000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            14243
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         4.019
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.479
_exptl_absorpt_correction_T_max  0.604
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.753
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0281P)^2^+0.1895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1187
_reflns_number_total             1279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5028sup1.cif
_cod_data_source_block           1
_cod_database_code               2108515
_cod_database_fobs_code          2108515
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C7 H9 N2 O2 Br1'
_shelx_estimated_absorpt_t_max   0.565
_shelx_estimated_absorpt_t_min   0.133
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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              74868
_shelx_hkl_checksum              95067
_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 1.581
_oxdiff_exptl_absorpt_empirical_full_min 0.639