Managing negative linear compressibility and thermal expansion through steric hindrance: a case study of 1,2-bis(4'-pyridyl)ethane cocrystals.
Patyk-Kaźmierczak, Ewa; Szymańska, Kornelia; Kaźmierczak, Michał; IUCrJ 12 (2025) –; doi:10.1107/S2052252524011734

data_1573498
_publ_section_title
;
 Managing negative linear compressibility and thermal expansion through
 steric hindrance: a case study of 1,2-bis(4'-pyridyl)ethane cocrystals.
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524011734
_journal_volume                  12
_journal_year                    2025
_chemical_formula_moiety         'C12 H12 N2, C4 H6 O4'
_chemical_formula_sum            'C16 H18 N2 O4'
_chemical_formula_weight         302.32
_chemical_name_systematic        '4,4'-Ethane-1,2-diyldipyridine succinic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2023-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.551(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6147(11)
_cell_length_b                   4.8463(4)
_cell_length_c                   19.3274(11)
_cell_measurement_reflns_used    991
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      71.8310
_cell_measurement_theta_min      5.6390
_cell_volume                     1466.51(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5384
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_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     10.00  36.00   1.00    5.00    --   40.98-125.00 -90.00   26
  2  \w     19.00 107.00   1.00    5.00    --   40.98  37.00   0.00   88
  3  \w     57.00  83.00   1.00    5.00    --   40.98-125.00 -60.00   26
  4  \w    -29.00  41.00   1.00    5.00    --   40.98 -37.00-150.00   70
  5  \w     71.00 146.00   1.00    7.50    --  103.83 179.00   0.00   75
  6  \w     86.00 156.00   1.00    7.50    --  103.83  77.00 -30.00   70
  7  \w     38.00 144.00   1.00    7.50    --  103.83 179.00 120.00  106
  8  \w     30.00 106.00   1.00    7.50    --  103.83 -77.00 120.00   76
  9  \w     83.00 140.00   1.00    7.50    --  103.83 111.00-120.00   57
 10  \w     54.00  86.00   1.00    7.50    --  103.83-111.00   0.00   32
 11  \w     71.00 101.00   1.00    7.50    --  103.83-111.00 -60.00   30
 12  \w     44.00  69.00   1.00    7.50    --  103.83 -61.00 150.00   25
 13  \w     40.00  66.00   1.00    7.50    --  103.83 -61.00  30.00   26
;
_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      0.0983062000
_diffrn_orient_matrix_UB_12      0.0075577000
_diffrn_orient_matrix_UB_13      0.0311077000
_diffrn_orient_matrix_UB_21      -0.0015836000
_diffrn_orient_matrix_UB_22      0.3096993000
_diffrn_orient_matrix_UB_23      -0.0183397000
_diffrn_orient_matrix_UB_31      -0.0038838000
_diffrn_orient_matrix_UB_32      0.0712715000
_diffrn_orient_matrix_UB_33      0.0765084000
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2776
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.945
_diffrn_reflns_theta_min         5.652
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method
;Single crystals were grown by slow evaporation of a solution obtained 
dissolving 4,4'-ethane-1,2-diyldipyridine and succinic acid in 1:1 
mol ratio in hot methanol 99.8%.
;
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1064P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                997
_reflns_number_total             1405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5049.cif
_cod_data_source_block           etysuc_100K
_cod_database_code               1573498
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C4 H6 O4, C12 H12 N2'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
;
_shelx_res_checksum              67585
_shelx_hkl_checksum              75163
_ins_header
;
TITL ETYSUC_100 in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  16.614702   4.846273  19.327432  90.0000 109.5515  90.0000
ZERR    4.00   0.001143   0.000358   0.001122   0.0000   0.0074   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H N O
UNIT 64.00 72.00 8.00 16.00
REM  CrysAlisPro recorded range (K): Min=99.7; max=100.1; aver:99.9
TEMP -173
SIZE 0.04 0.09 0.14
TREF
HKLF 4
END
;
_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 14.010
_oxdiff_exptl_absorpt_empirical_full_min 0.378