Pressure-Controlled Neutral‒Ionic Transition and Disordering of NH···N Hydrogen Bonds in Pyrazole
Sikora, Magdalena; Katrusiak, Andrzej; The Journal of Physical Chemistry C 117 (2013) 10661–; doi:10.1021/jp401389v

data_1511986
_publ_section_title
;
 Pressure-Controlled Neutral--Ionic Transition and Disordering of
 NH&#x00B7;&#x00B7;&#x00B7;N Hydrogen Bonds in Pyrazole
;
_journal_issue                   20
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              10661
_journal_paper_doi               10.1021/jp401389v
_journal_volume                  117
_journal_year                    2013
_chemical_formula_moiety         'C3 H4 N2'
_chemical_formula_sum            'C3 H4 N2'
_chemical_formula_weight         68.08
_chemical_melting_point          341
_chemical_name_common            pyrazole
_chemical_name_systematic
; 
pyrazole 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2n'
_symmetry_space_group_name_H-M   'P n a b'
_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            8
_cell_length_a                   6.749(3)
_cell_length_b                   12.599(6)
_cell_length_c                   8.191(4)
_cell_measurement_reflns_used    177
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.97
_cell_volume                     696.5(6)
_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    'Mercury (Macrae et al., 2008))'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         480000
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.245
_diffrn_measured_fraction_theta_max 0.245
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2069
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   integration
_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    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       dipyramidal
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         177
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0521P)^2^+0.6577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                160
_reflns_number_total             177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp401389v_si_002.cif
_cod_data_source_block           pyrazole_0.48GPa
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
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_cod_database_code               1511986