Stochastic hydration of a high-nitrogen-content molecular compound recrystallized under pressure
Olejniczak, Anna; Katrusiak, Anna; Podsiadło, Marcin; Katrusiak, Andrzej; IUCrJ 9 (2022) 49–54; doi:10.1107/S2052252521010381

data_1565884
_publ_section_title
;
 Stochastic hydration of a high-nitrogen-content molecular compound
 recrystallized under pressure
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              49
_journal_page_last               54
_journal_paper_doi               10.1107/S2052252521010381
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'C4 H2 Cl N5'
_chemical_formula_sum            'C4 H2 Cl N5'
_chemical_formula_weight         155.56
_chemical_name_systematic        6-chloro-1,2,3,4-tetrazolo[1,5-b]pyridazine
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-06-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.668(2)
_cell_length_b                   6.2042(7)
_cell_length_c                   8.780(4)
_cell_measurement_reflns_used    734
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.0650
_cell_measurement_theta_min      4.4200
_cell_volume                     581.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         540000
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.509
_diffrn_measured_fraction_theta_max 0.456
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  \f    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  \f    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  \f    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  \w    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  \w    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  \w    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  \w    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  \w    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  \w    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  \w    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  \w    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  \w    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  \w    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  \w    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  \w    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method
;
HP omega scans - for more details see:
A. Budzianowski, A. Katrusiak in High-Pressure Crystallography
(Eds.: A. Katrusiak, P. F. McMillan),
Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168       
;
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0333657000
_diffrn_orient_matrix_UB_12      0.0095614000
_diffrn_orient_matrix_UB_13      0.0695271000
_diffrn_orient_matrix_UB_21      -0.0423276000
_diffrn_orient_matrix_UB_22      -0.0729669000
_diffrn_orient_matrix_UB_23      0.0349857000
_diffrn_orient_matrix_UB_31      0.0389363000
_diffrn_orient_matrix_UB_32      -0.0875212000
_diffrn_orient_matrix_UB_33      -0.0215685000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.509
_diffrn_reflns_Laue_measured_fraction_max 0.456
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2992
_diffrn_reflns_point_group_measured_fraction_full 0.509
_diffrn_reflns_point_group_measured_fraction_max 0.456
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.115
_diffrn_reflns_theta_min         4.453
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       plate
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0468P)^2^+0.1183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                225
_reflns_number_total             321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5042.cif
_cod_data_source_block           C4H2N5Cl1@0_54GPa_phase_alpha_prim_xH2O
_cod_database_code               1565884
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4H2N5Cl1
_reflns_odcompleteness_completeness 44.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8)
;
_shelx_res_checksum              48201
_shelx_hkl_checksum              11644
_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 1.326
_oxdiff_exptl_absorpt_empirical_full_min 0.911