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_2108923
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                88.714(3)
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_cell_angle_gamma                92.480(3)
_cell_formula_units_Z            4
_cell_length_a                   5.0927(2)
_cell_length_b                   10.2465(3)
_cell_length_c                   13.6617(4)
_cell_measurement_reflns_used    2734
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9780
_cell_measurement_theta_min      5.8430
_cell_volume                     703.45(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.830
_diffrn_measured_fraction_theta_max 0.719
_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    -65.00  45.40   0.80   10.00    --   13.31 -57.00   0.00  138
  2  \w    -65.00  45.40   0.80   10.00    --   13.31 -57.00-120.00  138
  3  \w     35.00 105.40   0.80   10.00    --   13.31 178.00-120.00   88
  4  \w    -78.00 -38.00   0.80   10.00    --   13.31 178.00  60.00   50
  5  \w    -19.00  90.60   0.80   10.00    --   13.31  57.00   0.00  137
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0816041000
_diffrn_orient_matrix_UB_12      0.0559751000
_diffrn_orient_matrix_UB_13      -0.0077217000
_diffrn_orient_matrix_UB_21      0.0454957000
_diffrn_orient_matrix_UB_22      0.0029692000
_diffrn_orient_matrix_UB_23      0.0517141000
_diffrn_orient_matrix_UB_31      0.1057552000
_diffrn_orient_matrix_UB_32      -0.0407447000
_diffrn_orient_matrix_UB_33      -0.0054176000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.830
_diffrn_reflns_Laue_measured_fraction_max 0.719
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6317
_diffrn_reflns_point_group_measured_fraction_full 0.830
_diffrn_reflns_point_group_measured_fraction_max 0.719
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.169
_diffrn_reflns_theta_min         2.517
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92191
_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    1.635
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.332
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2045
_reflns_number_total             2716
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9939\% 
 around [-0.02 1.00 0.03] (reciprocal) or [0.00 1.00 -0.00] (direct)
;
_cod_data_source_file            xk5086sup1.cif
_cod_data_source_block           100K
_cod_database_code               2108923
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4N4NO3H7
_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:
 C11(H11), C12(H12), C13(H13), C21(H21), C22(H22), C23(H23)
2.b X=CH2 refined with riding coordinates:
 N13(H13A,H13B), N14(H14A,H14B), N23(H23A,H23B), N24(H24A,H24B)
;
_shelx_res_checksum              90610
_shelx_hkl_checksum              32791
_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 1.126
_oxdiff_exptl_absorpt_empirical_full_min 0.895
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_cod_database_fobs_code 2108923