Dynamic pedal motion and thermal expansion in an ionic co-crystal with 1,2-bis(4-pyridyl) ethylene
Zhang, Yuchen; Jiao, Yijia; Guo, Yan; Cen, Peipei; Zhang, Zhenyi; Liu, Xiangyu; RSC Advances 15 (2025) 33531–33535; doi:10.1039/D5RA04941E

data_7250856
_publ_section_title
;
 Dynamic pedal motion and thermal expansion in an ionic co-crystal with
 1,2-bis(4-pyridyl) ethylene
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              33531
_journal_page_last               33535
_journal_paper_doi               10.1039/D5RA04941E
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C12 H11 N2, C24 H20 B'
_chemical_formula_sum            'C36 H31 B N2'
_chemical_formula_weight         502.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-02-10 deposited with the CCDC.	2025-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.622(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4237(12)
_cell_length_b                   10.4916(12)
_cell_length_c                   23.340(3)
_cell_measurement_reflns_used    1152
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      64.33
_cell_measurement_theta_min      3.87
_cell_volume                     2740.0(6)
_computing_cell_refinement       ZC5-1-CIF
_computing_data_reduction        ZC5-1-CIF
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      140.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15965
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.384
_diffrn_reflns_theta_min         3.867
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1209 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.7756.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0072(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     415
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1112P)^2^+1.6006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.2358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2669
_reflns_number_total             4955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra04941e2.cif
_cod_data_source_block           20231203_nx_140k_0m
_cod_original_cell_volume        2740.1(5)
_cod_database_code               7250856
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.924
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim N1 \\sim C25 \\sim C29 \\sim C25A \\sim C29A \\sim C26 \\sim C28 \\sim
C26A \\sim C28A \\sim C27 \\sim C27A \\sim C30 \\sim C30A \\sim C31 \\sim C31A
\\sim C32 \\sim C32A \\sim C33 \\sim C36 \\sim C33A \\sim C36A \\sim C34 \\sim
C35 \\sim C34A \\sim C35A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Same fragment restrains
{C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A} sigma
for 1-2: 0.01, 1-3: 0.04
as in
{C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36}
4. Others
 Sof(H2B)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=
 Sof(C32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(H2A)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2A), N2(H2B), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C33(H33), C34(H34), C35(H35), C36(H36), C25A(H25A), C26A(H26A), C28A(H28A),
 C29A(H29A), C30A(H30A), C31A(H31A), C33A(H33A), C34A(H34A), C35A(H35A),
 C36A(H36A), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20),
  C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              36232
_olex2_submission_special_instructions 'No special instructions were received'