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_1573480
_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 H4 O4'
_chemical_formula_sum            'C16 H16 N2 O4'
_chemical_formula_weight         300.31
_chemical_name_systematic        '1,2-bis(4-Pyridyl)ethane fumaric 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             2024-05-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.002(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6876(7)
_cell_length_b                   4.7329(2)
_cell_length_c                   19.6859(9)
_cell_measurement_reflns_used    2278
_cell_measurement_temperature    145.05(10)
_cell_measurement_theta_max      71.2150
_cell_measurement_theta_min      4.2670
_cell_volume                     1461.02(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      145.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0294
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_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    -87.00  -6.00   1.00    1.00    --  -35.87 125.00 -60.00   81
  2  \w     19.00 103.00   1.00    1.00    --   35.87  57.00 -30.00   84
  3  \w     19.00 103.00   1.00    1.00    --   35.87  57.00-180.00   84
  4  \w      6.00  87.00   1.00    1.00    --   35.87-125.00 -90.00   81
  5  \w     19.00 103.00   1.00    1.00    --   35.87  57.00-120.00   84
  6  \w     88.00 158.00   1.00    1.50    --  105.44  45.00 -60.00   70
  7  \w     38.00 109.00   1.00    1.50    --  105.44-111.00 120.00   71
  8  \w     87.00 158.00   1.00    1.50    --  105.44  61.00 -30.00   71
  9  \w     67.00 158.00   1.00    1.50    --  105.44  15.00-150.00   91
 10  \w     88.00 158.00   1.00    1.50    --  105.44  45.00-120.00   70
 11  \w     38.00 109.00   1.00    1.50    --  105.44-111.00-150.00   71
 12  \w     67.00 158.00   1.00    1.50    --  105.44  15.00  90.00   91
 13  \w     38.00 132.00   1.00    1.50    --  105.44 -77.00 -60.00   94
 14  \w    -31.00  53.00   1.00    1.00    --   35.87 -57.00  90.00   84
 15  \w     19.00 103.00   1.00    1.00    --   35.87  57.00 120.00   84
 16  \w    -31.00  10.00   1.00    1.00    --   35.87 -57.00 -90.00   41
 17  \w     19.00 103.00   1.00    1.00    --   35.87  57.00  60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0882354000
_diffrn_orient_matrix_UB_12      0.0092509000
_diffrn_orient_matrix_UB_13      0.0600061000
_diffrn_orient_matrix_UB_21      -0.0396550000
_diffrn_orient_matrix_UB_22      -0.1147205000
_diffrn_orient_matrix_UB_23      0.0545864000
_diffrn_orient_matrix_UB_31      0.0175577000
_diffrn_orient_matrix_UB_32      -0.3043931000
_diffrn_orient_matrix_UB_33      -0.0187036000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.995
_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       3
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4130
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.603
_diffrn_reflns_theta_min         4.781
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1394
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0790P)^2^+0.3412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1262
_reflns_number_total             1394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yc5049.cif
_cod_data_source_block           etyfum_145k_b
_cod_database_code               1573480
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C4H404, N2C12H12'
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.729
_olex2_refinement_description
;
1. Restrained distances
 H1A-O1
 1 with sigma of 0.02
;
_shelx_res_checksum              74526
_shelx_hkl_checksum              11473
_ins_header
;
TITL ETYFUM_145K_B in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  16.687588   4.732853  19.685869  90.0000 110.0020  90.0000
ZERR    4.00   0.000736   0.000178   0.000876   0.0000   0.0051   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H N
UNIT 64.00 1664.00 8.00
REM  CrysAlisPro recorded range (K): Min=145.0; max=145.1; aver:145.1
TEMP -128
SIZE 0.16 0.29 0.41
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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.837