#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/58/2105867.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2105867
loop_
_publ_author_name
'Patyk, Ewa'
'Marciniak, Jedrzej'
'Tomkowiak, Hanna'
'Katrusiak, Andrzej'
'Merz, Klaus'
_publ_section_title
;
 Isothermal and isochoric crystallization of highly hygroscopic pyridine
 N-oxide of aqueous solution
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              487
_journal_page_last               491
_journal_paper_doi               10.1107/S2052520614011226
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C5 H5 N O'
_chemical_formula_sum            'C5 H5 N O'
_chemical_formula_weight         95.10
_chemical_melting_point          338
_chemical_name_common            Pyridine-N-oxide
_chemical_name_systematic        Pyridine-N-oxide
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_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                   5.5890(8)
_cell_length_b                   5.5890(8)
_cell_length_c                   13.550(3)
_cell_measurement_reflns_used    1100
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      3.94
_cell_volume                     423.26(13)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A.  2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.402
_diffrn_measured_fraction_theta_max 0.402
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1100
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         3.94
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Correction for absorption of the diamond-anvil cell and the sample
 were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
 Mickiewicz University Poznań; Katrusiak, A. (2004) Z. Kristallogr.
 219, 461-467).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal trapezohedron'
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.075
_refine_diff_density_min         -0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0346P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                159
_reflns_number_total             181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5041sup1.cif
_cod_data_source_block           5PNO_1.05GPa
_cod_original_cell_volume        423.26(12)
_cod_original_sg_symbol_H-M      P4(1)2(1)2
_cod_database_code               2105867
_cod_database_fobs_code          2105867
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
O O1 0.1786(4) 0.1786(4) 0.0000 0.0469(11) Uani d S 1 2
N N1 0.0135(6) 0.0135(6) 0.0000 0.0323(11) Uani d S 1 2
C C1 0.0392(7) -0.1868(7) 0.05564(16) 0.0288(9) Uani d . 1 1
C C2 -0.1305(8) -0.3604(7) 0.05531(18) 0.0334(9) Uani d . 1 1
C C3 -0.3351(6) -0.3351(6) 0.0000 0.0321(13) Uani d S 1 2
H H1 0.188(4) -0.171(5) 0.0982(19) 0.039 Uiso d . 1 1
H H2 -0.102(6) -0.495(6) 0.093(2) 0.039 Uiso d . 1 1
H H3 -0.439(6) -0.439(6) 0.0000 0.039 Uiso d S 1 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0428(16) 0.0428(16) 0.0552(17) -0.016(4) 0.0029(10) -0.0029(10)
N1 0.0340(17) 0.0340(17) 0.0290(16) 0.008(5) 0.0038(11) -0.0038(11)
C1 0.0261(18) 0.033(2) 0.0272(12) 0.003(3) 0.0020(16) 0.0025(15)
C2 0.043(2) 0.030(2) 0.0263(13) 0.011(4) 0.0077(19) 0.0028(14)
C3 0.033(2) 0.033(2) 0.0296(16) -0.006(4) 0.0077(16) -0.0077(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 N1 C1 . 7 120.6(3)
O1 N1 C1 . . 120.6(3)
C1 N1 C1 7 . 118.9(6)
C2 C1 N1 . . 120.9(4)
C2 C1 H1 . . 129.4(16)
N1 C1 H1 . . 109.4(17)
C1 C2 C3 . . 120.7(3)
C1 C2 H2 . . 117(2)
C3 C2 H2 . . 122(2)
C2 C3 C2 . 7 117.9(5)
C2 C3 H3 . . 121.0(3)
C2 C3 H3 7 . 121.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O1 N1 . 1.305(4)
N1 C1 7 1.357(4)
N1 C1 . 1.357(4)
C1 C2 . 1.357(4)
C1 H1 . 1.01(2)
C2 C3 . 1.374(4)
C2 H2 . 0.92(4)
C3 C2 7 1.374(4)
C3 H3 . 0.82(5)
