Isothermal and isochoric crystallization of highly hygroscopic pyridine <i>N</i>-oxide of aqueous solution
Patyk, Ewa; Marciniak, Jedrzej; Tomkowiak, Hanna; Katrusiak, Andrzej; Merz, Klaus; Acta Crystallographica Section B 70 (2014) 487–491; doi:10.1107/S2052520614011226

data_2105866
_publ_section_title
;
 Isothermal and isochoric crystallization of highly hygroscopic pyridine
 <i>N</i>-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                   5.6608(8)
_cell_length_b                   5.6608(8)
_cell_length_c                   13.625(3)
_cell_measurement_reflns_used    1450
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      3.90
_cell_volume                     436.61(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 0.544
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       '\f- and \w-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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1450
_diffrn_reflns_theta_full        26.85
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         3.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.47
_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 Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
 219, 461-467).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal trapezohedron'
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   5(5)
_refine_ls_extinction_coef       0.55(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0425
_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/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                233
_reflns_number_total             262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zb5041sup1.cif
_cod_data_source_block           3PNO_0.78GPa
_cod_original_cell_volume        436.61(12)
_cod_original_sg_symbol_H-M      P4(1)2(1)2
_cod_database_code               2105866
_cod_database_fobs_code          2105866