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_2108911
_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             2021-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.11(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0993(14)
_cell_length_b                   10.252(8)
_cell_length_c                   13.845(3)
_cell_measurement_reflns_used    457
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.2600
_cell_measurement_theta_min      2.9780
_cell_volume                     714.7(6)
_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 0.410
_diffrn_measured_fraction_theta_max 0.410
_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  32.00   0.50   40.00    --   25.00   0.00   0.00  104
  2  \w    -20.00  36.00   0.50   40.00    --   25.00   0.00 180.00  112
  3  \w     -3.00  47.00   0.50   40.00    --   25.00 -40.00-170.00  100
  4  \w     -3.00  47.00   0.50   40.00    --   25.00 -40.00  10.00  100
  5  \w      8.00  65.00   0.50   40.00    --   25.00 -82.00  30.00  114
  6  \w      8.00  65.00   0.50   40.00    --   25.00 -82.00-150.00  114
  7  \w     32.50  89.00   0.50   40.00    --   25.00-135.00-122.00  113
  8  \w     32.00  89.00   0.50   40.00    --   25.00-135.00  58.00  114
  9  \w     25.00  47.00   0.50   40.00    --  -25.00-135.00  58.00   44
 10  \w     25.00  47.00   0.50   40.00    --  -25.00-135.00-122.00   44
 11  \w      0.00  23.00   0.50   40.00    --  -25.00 -82.00-150.00   46
 12  \w      0.00  23.00   0.50   40.00    --  -25.00 -82.00  30.00   46
 13  \w    -19.00  17.00   0.50   40.00    --  -25.00 -40.00  10.00   72
 14  \w    -19.00  17.00   0.50   40.00    --  -25.00 -40.00-170.00   72
 15  \w    -33.00  22.00   0.50   40.00    --  -25.00   0.00 180.00  110
 16  \w    -33.00  22.00   0.50   40.00    --  -25.00   0.00   0.00  110
;
_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      0.0623681000
_diffrn_orient_matrix_UB_12      -0.0608795000
_diffrn_orient_matrix_UB_13      -0.0044288000
_diffrn_orient_matrix_UB_21      0.0009251000
_diffrn_orient_matrix_UB_22      -0.0123865000
_diffrn_orient_matrix_UB_23      0.0504891000
_diffrn_orient_matrix_UB_31      -0.1263844000
_diffrn_orient_matrix_UB_32      -0.0304423000
_diffrn_orient_matrix_UB_33      -0.0111163000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.410
_diffrn_reflns_Laue_measured_fraction_max 0.410
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3803
_diffrn_reflns_point_group_measured_fraction_full 0.410
_diffrn_reflns_point_group_measured_fraction_max 0.410
_diffrn_reflns_theta_full        25.040
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36099
_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    1.609
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.124
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         516
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0810P)^2^+0.4842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                309
_reflns_number_total             516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5086sup1.cif
_cod_data_source_block           0.28GPa
_cod_original_cell_volume        714.6(6)
_cod_database_code               2108911
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4N4NO3H7
_reflns_odcompleteness_completeness 40.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
3.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
;
_shelx_res_checksum              46239
_shelx_hkl_checksum              84536
_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 2.274
_oxdiff_exptl_absorpt_empirical_full_min 0.784
_cod_database_fobs_code 2108911