Hydrogen Bonding in Nitroanilines: Neutron Diffraction Study of m-Nitroaniline at 100 K
Goeta, Andrés E.; Wilson, Chick C.; Autino, Juan C.; Ellena, Javier; Punte, Graciela; Chemistry of Materials 12 (2000) 3342–3346; doi:10.1021/cm001092u

data_4000019
_publ_section_title
;
 Hydrogen Bonding in Nitroanilines: Neutron Diffraction Study of
 m-Nitroaniline at 100 K
;
_journal_coden_ASTM              CMATEX
_journal_issue                   11
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3342
_journal_page_last               3346
_journal_paper_doi               10.1021/cm001092u
_journal_volume                  12
_journal_year                    2000
_chemical_formula_sum            'C6 H6 N2 O2'
_chemical_formula_weight         138.00
_chemical_name_common            m-nitroaniline
_chemical_name_systematic        m-nitroaniline
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.905(4)
_cell_length_b                   6.484(1)
_cell_length_c                   5.016(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     614.9(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  SXD
_diffrn_measurement_method       'Time of flight LAUE diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.5-5.0
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11625
_diffrn_reflns_theta_max         ?
_diffrn_reflns_theta_min         ?
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.61
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
The linear absorption coefficient is wavelength dependent
 and it is calculated as:
          mu = 0.82 + 0.79 * lambda  [cm^-1]
The value of 1.61 given in _exptl_absorpt_coefficient_mu
is the value at 1 \%A
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'prismatic needle'
_exptl_crystal_F_000             19.07
_exptl_crystal_size_max          10
_exptl_crystal_size_mid          2
_exptl_crystal_size_min          2
_refine_diff_density_max         1.410
_refine_diff_density_min         -2.238
_refine_diff_density_rms         0.347
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       0.127
_refine_ls_extinction_method     'Becker-Coppens Lorentzian model'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+6.3506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                1664
_reflns_number_total             1664
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            cm001092u.cif
_cod_data_source_block           mna
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4000019