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_1565866
_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           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0533(2)
_cell_length_b                   8.7742(2)
_cell_length_c                   10.0552(2)
_cell_measurement_reflns_used    2554
_cell_measurement_temperature    250.0(1)
_cell_measurement_theta_max      64.7340
_cell_measurement_theta_min      6.6920
_cell_volume                     622.29(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      N~2~
_diffrn_ambient_temperature      250.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5357
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     13.00 116.00   1.00    1.25    --   41.73  77.00 150.00  103
  2  \w     13.00  88.00   1.00    1.25    --   41.73-125.00  60.00   75
  3  \w     40.00  99.00   1.00    1.25    --   41.73  37.00 -90.00   59
  4  \w     16.00  51.00   1.00    2.50    --   88.44 -45.00 150.00   35
  5  \w     36.00 158.00   1.00    2.50    --   88.44  15.00  60.00  122
  6  \w      8.00 106.00   1.00    2.50    --   88.44 -94.00 120.00   98
  7  \w     37.00  77.00   1.00    2.50    --   88.44 -45.00  90.00   40
  8  \w     44.00  70.00   1.00    2.50    --   88.44 -45.00-120.00   26
  9  \w     16.00 109.00   1.00    2.50    --   88.44 -94.00-120.00   93
 10  \w     26.00  75.00   1.00    2.50    --   88.44 -45.00   0.00   49
 11  \w     42.00  81.00   1.00    2.50    --   88.44 -94.00   0.00   39
 12  \w     85.00 111.00   1.00    2.50    --   88.44 125.00  90.00   26
 13  \w    116.00 146.00   1.00    2.50    --   88.44 125.00  90.00   30
 14  \w     68.00 107.00   1.00    2.50    --   88.44-125.00  90.00   39
 15  \w     75.00 156.00   1.00    2.50    --   88.44  61.00 -90.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0560155000
_diffrn_orient_matrix_UB_12      -0.0094470000
_diffrn_orient_matrix_UB_13      0.1478208000
_diffrn_orient_matrix_UB_21      -0.0480815000
_diffrn_orient_matrix_UB_22      -0.1713134000
_diffrn_orient_matrix_UB_23      0.0006184000
_diffrn_orient_matrix_UB_31      0.2055681000
_diffrn_orient_matrix_UB_32      -0.0374516000
_diffrn_orient_matrix_UB_33      -0.0401516000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3654
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        64.632
_diffrn_reflns_theta_max         64.632
_diffrn_reflns_theta_min         6.696
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70489
_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            colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 379 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.487(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0428P)^2^+0.2471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                1006
_reflns_number_total             1038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5042.cif
_cod_data_source_block           C4H2N5Cl1@250K_phase_alpha
_cod_database_code               1565866
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4H2N5Cl1
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.53
_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              69350
_shelx_hkl_checksum              38771
_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 1.547
_oxdiff_exptl_absorpt_empirical_full_min 0.809