A structural and spectroscopic investigation of the hydrochlorination of 4-benzylaniline: the interaction of anhydrous hydrogen chloride with chlorobenzene
Gibson, Emma K.; Winfield, John M.; Muir, Kenneth W.; Carr, Robert H.; Eaglesham, Archie; Gavezzotti, Angelo; Parker, Stewart F.; Lennon, David; Physical Chemistry Chemical Physics 11 (2009) 288–297; doi:10.1039/b810027f

data_7200206
_publ_section_title
;
 A structural and spectroscopic investigation of the hydrochlorination
 of 4-benzylaniline: the interaction of anhydrous hydrogen chloride
 with chlorobenzene
;
_journal_issue                   2
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              288
_journal_page_last               297
_journal_paper_doi               10.1039/b810027f
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'Cl, C13 H14 N'
_chemical_formula_sum            'C13 H14 Cl N'
_chemical_formula_weight         219.7
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
4-benzylaniline hydrochloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2005-04-19T08:08:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.4360
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5504(2)
_cell_length_b                   22.0930(8)
_cell_length_c                   9.7906(4)
_cell_measurement_reflns_used    2750
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1
_cell_volume                     1151.51(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12278
_diffrn_reflns_theta_full        27.22
_diffrn_reflns_theta_max         27.22
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS as embodied in WINGX
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

calc w=1/[\s\^2\^(Fo\^2\^)+(0.0308P)\^2\^+0.5938P] where
P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                1964
_reflns_number_total             2504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B810027F.txt
_cod_data_source_block           BA.HCL
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7200206