The structure of N-aminopyrazole in the solid state and in solution: an experimental and computational study
Antonio Jime´nez, Jose´; María Claramunt, Rosa; Mó, Otilia; Yáñez, Manuel; Wehrmann, Frank; Buntkowsky, Gerd; Limbach, Hans-Heinrich; Goddard, Richard; Elguero, Jose´; Physical Chemistry Chemical Physics 1 (1999) 5113–; doi:10.1039/a906187h

data_7217109
_publ_section_title
;
 The structure of N-aminopyrazole in the solid state and in solution: an
 experimental and computational study
;
_journal_issue                   22
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              5113
_journal_paper_doi               10.1039/a906187h
_journal_volume                  1
_journal_year                    1999
_chemical_formula_sum            'C3 H5 N3'
_chemical_formula_weight         83.10
_chemical_name_common            N-aminopyrazole
_chemical_name_systematic
; 
 1-aminopyrazole 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.468(7)
_cell_length_b                   13.484(3)
_cell_length_c                   5.7549(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      23.17
_cell_volume                     812.3(6)
_computing_cell_refinement       'EXPRESS / CAD4 software (Enraf-Nonius, 1995)'
_computing_data_collection       'EXPRESS / CAD4 software (Enraf-Nonius, 1995)'
_computing_data_reduction
'DATAP (Coppens,Leiserowitz & Rabinovich, 1965)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.836
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1166
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3420
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        13.04
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       rod
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.069(11)
_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   1.144
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.1663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1327
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                797
_reflns_number_total             935
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            906187h.txt
_cod_data_source_block           2949
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.1663P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.1663P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7217109