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_1573526
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.512(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6711(3)
_cell_length_b                   4.92720(10)
_cell_length_c                   19.3744(4)
_cell_measurement_reflns_used    6372
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      76.1010
_cell_measurement_theta_min      4.1930
_cell_volume                     1509.10(5)
_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_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5384
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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   -114.00 -13.00   1.00    3.00    --  -41.23 -57.00 120.00  101
  2  \w   -114.00 -13.00   1.00    3.00    --  -41.23 -57.00-150.00  101
  3  \w    -39.00  26.00   1.00    3.00    --   41.23 -19.00 -60.00   65
  4  \w     39.00 109.00   1.00    6.00    --  112.00-111.00 -60.00   70
  5  \w     29.00 107.00   1.00    6.00    --  112.00 -94.00-150.00   78
  6  \w     84.00 158.00   1.00    6.00    --  112.00  30.00-150.00   74
  7  \w     86.00 158.00   1.00    6.00    --  112.00  45.00 -30.00   72
  8  \w     59.00 158.00   1.00    6.00    --  112.00  15.00 -60.00   99
  9  \w     59.00 158.00   1.00    6.00    --  112.00  15.00   0.00   99
 10  \w     36.00 106.00   1.00    6.00    --  112.00 -77.00 -60.00   70
 11  \w     40.00  71.00   1.00    6.00    --  112.00 -61.00  30.00   31
 12  \w    -95.00  -6.00   1.00    3.00    --  -41.23 125.00-150.00   89
 13  \w    -66.00  32.00   1.00    3.00    --  -41.23  57.00 150.00   98
 14  \w   -116.00 -17.00   1.00    3.00    --  -41.23 -37.00   0.00   99
 15  \w     40.00  71.00   1.00    6.00    --  112.00 -61.00  90.00   31
 16  \w     86.00 158.00   1.00    6.00    --  112.00  45.00 120.00   72
 17  \w     82.00 158.00   1.00    6.00    --  112.00  77.00   0.00   76
 18  \w     83.00 158.00   1.00    6.00    --  112.00  61.00 150.00   75
 19  \w     36.00 106.00   1.00    6.00    --  112.00 -77.00  90.00   70
 20  \w     86.00 158.00   1.00    6.00    --  112.00  45.00  60.00   72
 21  \w   -114.00 -13.00   1.00    3.00    --  -41.23 -57.00  30.00  101
 22  \w   -114.00 -13.00   1.00    3.00    --  -41.23 -57.00 -60.00  101
 23  \w    -33.00  42.00   1.00    3.00    --   41.23 -37.00   0.00   75
 24  \w     83.00 158.00   1.00    6.00    --  112.00  61.00  90.00   75
 25  \w     40.00  71.00   1.00    6.00    --  112.00 -61.00-150.00   31
 26  \w     40.00  71.00   1.00    6.00    --  112.00 -61.00 120.00   31
 27  \w     82.00 158.00   1.00    6.00    --  112.00  77.00-150.00   76
 28  \w     36.00 106.00   1.00    6.00    --  112.00 -77.00   0.00   70
 29  \w     40.00  71.00   1.00    6.00    --  112.00 -61.00   0.00   31
 30  \w   -115.00 -10.00   1.00    3.00    --  -41.23 -71.00 -10.49  105
 31  \w      6.00  95.00   1.00    3.00    --   41.23-125.00   0.00   89
 32  \w    -33.00  42.00   1.00    3.00    --   41.23 -37.00-150.00   75
 33  \w     82.00 158.00   1.00    6.00    --  112.00  77.00 -30.00   76
 34  \w     82.00 158.00   1.00    6.00    --  112.00  77.00-120.00   76
 35  \w     82.00 158.00   1.00    6.00    --  112.00  77.00 -90.00   76
 36  \w     82.00 158.00   1.00    6.00    --  112.00  77.00-180.00   76
 37  \w     83.00 158.00   1.00    6.00    --  112.00  61.00 120.00   75
 38  \w     40.00  71.00   1.00    6.00    --  112.00 -61.00 -60.00   31
 39  \w   -116.00 -17.00   1.00    3.00    --  -41.23 -37.00-150.00   99
 40  \w   -114.00 -13.00   1.00    3.00    --  -41.23 -57.00  60.00  101
 41  \w     17.00 116.00   1.00    3.00    --   41.23  37.00-120.00   99
 42  \w     83.00 156.00   1.00    6.00    --  112.00  61.00  60.00   73
;
_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      0.0729892000
_diffrn_orient_matrix_UB_12      -0.0152011000
_diffrn_orient_matrix_UB_13      -0.0326135000
_diffrn_orient_matrix_UB_21      -0.0639374000
_diffrn_orient_matrix_UB_22      0.0275765000
_diffrn_orient_matrix_UB_23      -0.0770802000
_diffrn_orient_matrix_UB_31      0.0092394000
_diffrn_orient_matrix_UB_32      0.3110018000
_diffrn_orient_matrix_UB_33      0.0052561000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12238
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.244
_diffrn_reflns_theta_min         4.814
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_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    1.331
_exptl_crystal_description       block
_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          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0011(2)
_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   1.031
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0553P)^2^+0.6357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1318
_reflns_number_total             1554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5049.cif
_cod_data_source_block           etysuc
_cod_database_code               1573526
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C12 H12 N2,C4 H6 O4'
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.857
_olex2_refinement_description
;
;
_shelx_res_checksum              27483
_shelx_hkl_checksum              2980
_ins_header
;
TITL ETYSUC in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  16.671128   4.927171  19.374423  90.0000 108.5123  90.0000
ZERR    4.00   0.000317   0.000109   0.000368   0.0000   0.0021   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H N O
UNIT 64.00 72.00 8.00 16.00
SIZE 0.04 0.10 0.20
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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.803