Low-temperature phase transition and high-pressure phase stability of 1<i>H</i>-pyrazole-1-carboxamidine nitrate
Rejnhardt, Piotr; Drozd, Marek; Daszkiewicz, Marek; Acta Crystallographica Section B 77 (2021) 996–1002; doi:10.1107/S2052520621010970

data_2108921
_publ_section_title
;
 Low-temperature phase transition and high-pressure phase stability of
 1<i>H</i>-pyrazole-1-carboxamidine nitrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              996
_journal_page_last               1002
_journal_paper_doi               10.1107/S2052520621010970
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C4 H7 N4, N O3'
_chemical_formula_sum            'C4 H7 N5 O3'
_chemical_formula_weight         173.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.028(6)
_cell_length_b                   10.152(6)
_cell_length_c                   13.36(5)
_cell_measurement_reflns_used    163
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.9140
_cell_measurement_theta_min      3.9980
_cell_volume                     675(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2214
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.349
_diffrn_measured_fraction_theta_max 0.350
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -20.00  31.60   0.60   30.00    --   25.00   0.00   0.00   86
  2  \w    -20.00  35.80   0.60   30.00    --   25.00   0.00 180.00   93
  3  \w     -3.00  46.80   0.60   30.00    --   25.00 -40.00-170.00   83
  4  \w     -3.00  46.80   0.60   30.00    --   25.00 -40.00  10.00   83
  5  \w      8.00  65.00   0.60   30.00    --   25.00 -82.00  30.00   95
  6  \w      8.00  65.00   0.60   30.00    --   25.00 -82.00-150.00   95
  7  \w     32.50  88.90   0.60   30.00    --   25.00-135.00-122.00   94
  8  \w     32.00  89.00   0.60   30.00    --   25.00-135.00  58.00   95
  9  \w     25.00  46.60   0.60   30.00    --  -25.00-135.00  58.00   36
 10  \w     25.00  46.60   0.60   30.00    --  -25.00-135.00-122.00   36
 11  \w      0.00  22.80   0.60   30.00    --  -25.00 -82.00-150.00   38
 12  \w      0.00  22.80   0.60   30.00    --  -25.00 -82.00  30.00   38
 13  \w    -19.00  17.00   0.60   30.00    --  -25.00 -40.00  10.00   60
 14  \w    -19.00  17.00   0.60   30.00    --  -25.00 -40.00-170.00   60
 15  \w    -33.00  21.60   0.60   30.00    --  -25.00   0.00 180.00   91
 16  \w    -33.00  21.60   0.60   30.00    --  -25.00   0.00   0.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0582101000
_diffrn_orient_matrix_UB_12      -0.0137089000
_diffrn_orient_matrix_UB_13      -0.0439652000
_diffrn_orient_matrix_UB_21      0.1311441000
_diffrn_orient_matrix_UB_22      0.0038063000
_diffrn_orient_matrix_UB_23      0.0281493000
_diffrn_orient_matrix_UB_31      -0.0046111000
_diffrn_orient_matrix_UB_32      -0.0683337000
_diffrn_orient_matrix_UB_33      0.0105371000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1281
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.349
_diffrn_reflns_Laue_measured_fraction_max 0.350
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3550
_diffrn_reflns_point_group_measured_fraction_full 0.349
_diffrn_reflns_point_group_measured_fraction_max 0.350
_diffrn_reflns_theta_full        24.779
_diffrn_reflns_theta_max         24.779
_diffrn_reflns_theta_min         4.015
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_refine_diff_density_max         0.135
_refine_diff_density_min         -0.121
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.03(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0966P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                221
_reflns_number_total             403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5086sup1.cif
_cod_data_source_block           1.15GPa
_cod_original_cell_volume        676(3)
_cod_database_code               2108921
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4N4NO3H7
_reflns_odcompleteness_completeness 34.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.73
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
2.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
;
_shelx_res_checksum              88414
_shelx_hkl_checksum              90943
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.023
_oxdiff_exptl_absorpt_empirical_full_min 0.542