Reassessment of paracetamol orthorhombic Form III and determination of a novel low-temperature monoclinic Form III-m from powder diffraction data
Reiss, Céleste A.; van Mechelen, Jan B.; Goubitz, Kees; Peschar, René; Acta Crystallographica Section C 74 (2018) 392–399; doi:10.1107/S2053229618002619

data_2021811
_publ_section_title
;
 Reassessment of paracetamol orthorhombic Form III and determination of a
 novel low-temperature monoclinic Form III-m from powder diffraction data
;
_publ_section_keywords
;
powder diffraction, paracetamol; acetaminophen; polymorph; PXRD; reversible
phase transition; Rietveld refinement; crystal structure; reassessment; Monte
Carlo; structure prediction
;
_journal_coeditor_code           SK3670
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              392
_journal_page_last               399
_journal_paper_doi               10.1107/S2053229618002619
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C8 H9 N O2'
_chemical_formula_moiety         'C8 H9 N O2'
_chemical_formula_structural     'C8 H9 N O2'
_chemical_formula_sum            'C8 H9 N O2'
_chemical_formula_weight         151.16
_chemical_name_common            'paracetamol formIII-m'
_chemical_name_systematic
; 
<i>N</i>-(4-Hydroxyphenyl)acetamid
;
_space_group_IT_number           7
_space_group_name_Hall           'P -2xc'
_space_group_name_H-M_alt        'P c 1 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2xc'
_symmetry_space_group_name_H-M   'P c 1 1'
_audit_creation_date             2018-01-10T21:48
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
;
2018-01-10T21:48  Initial CIF as created by GSAS2CIF

2018-02-19 # Formatted by IUCr publCIF
;
_cell_angle_alpha                84.160(14)
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   11.75455(34)
_cell_length_b                   8.57201(31)
_cell_length_c                   14.5155(5)
_cell_measurement_temperature    100
_cell_volume                     1454.99(9)
_computing_structure_refinement
;
GSAS (Larson & Von Dreele, 1994)
;
_diffrn_ambient_temperature      100
_diffrn_detector_type            X'Celerator
_diffrn_measurement_device_type  'PANalytical X'Pert Pro MPD'
_diffrn_radiation_polarisn_ratio 0.95
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'PANalytical Cu LFF'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_density_diffrn    1.38
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  colourless
_pd_char_particle_morphology     powder
_pd_meas_2theta_range_inc        0.013
_pd_meas_2theta_range_max        59.984
_pd_meas_2theta_range_min        5.007
_pd_meas_number_of_points        4230
_pd_meas_scan_method             step
_pd_phase_name                   'form III Pc SML 100K'
_pd_proc_2theta_range_inc        0.013
_pd_proc_2theta_range_max        59.97477
_pd_proc_2theta_range_min        4.99777
_pd_proc_info_datetime           2018-01-10T21:48:04
_pd_proc_ls_background_function
;   GSAS Background function number 1 with  9 terms.
 Shifted Chebyshev function of 1st kind
      1:    5622.69     2:   -4042.75     3:    832.560     4:    171.284    
      5:    18.7131     6:   -408.715     7:    266.392     8:    55.8981    
      9:   -93.0254    
;
_pd_proc_ls_peak_cutoff          0.00500
_pd_proc_ls_pref_orient_corr
;
March-Dollase
AXIS  1 Ratio=     1.539 Frac     0.869  h= 0.000  k= 0.000  l= 1.000
AXIS  2 Ratio=     1.000 Frac     0.131  h= 0.000  k= 0.000  l= 1.000
Prefered orientation correction range: Min=   0.36881, Max=   1.79136

Dollase, W. A. (1986). J. Appl. Cryst. 19, 267--272.
;
_pd_proc_ls_profile_function
;
CW Profile function number 4 with  21 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl.
Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
Microstrain broadening by P.W. Stephens,  (1999). J. Appl.
Cryst.,32,281-289.
Peak tails are ignored  where the intensity is below 0.0050 times the peak
Aniso. broadening axis   0.0   1.0   0.0
;
_pd_proc_ls_prof_R_factor        0.0446
_pd_proc_ls_prof_wR_expected     0.0102
_pd_proc_ls_prof_wR_factor       0.0589
_pd_proc_number_of_points        4230
_pd_spec_mounting                ' glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              15
_pd_spec_size_equat              0.7
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   5.99
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_restraints     255
_refine_ls_R_Fsqd_factor         0.04111
_refine_ls_shift/su_max          0.40
_refine_ls_shift/su_mean         0.01
_reflns_d_resolution_high        1.545
_reflns_d_resolution_low         11.755
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              -5
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_total             422
_publcif_datablock.id            {a49eeb87-b11f-456d-a8e2-621b030d2203}
_cod_data_source_file            sk3670sup1.cif
_cod_data_source_block           FORMIII-100K-4MOL-TR_publ
_cod_database_code               2021811
_cod_database_fobs_code          2021811
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000
_geom_extra_table_head_e
;
Hydrogen-bridging scheme (\%A) for Form III-m
;
_geom_table_footnote_e
;
Symmetry codes: (i) <i>x</i>, <i>y</i>-1, <i>z</i>; 
(ii) <i>x</i>+1, <i>y</i>-1, <i>z</i>;
(iii) <i>x</i>, <i>y</i>+1, <i>z</i>;
(iv) <i>x</i>+1, <i>y</i>, <i>z</i>.
;
_geom_extra_table_head_d
;
Hydrogen-bridging scheme (\%A) for Form III-o
;
_geom_table_footnote_d
;
Symmetry codes: (i) <i>x</i>, <i>y</i>-1, <i>z</i>; 
(ii) <i>x</i>+1/2, -<i>y</i>, <i>z</i>;
(iii) <i>x</i>, <i>y</i>+1, <i>z</i>;
(iv) <i>x</i>-1/2, -<i>y</i>+1, <i>z</i>.
;