Reversible phase transformations upon water uptake/removal in crystalline material of a bipodal N-donor ligand and evaluation of the stability of the hydrates formed
Chaudhary, Simran; Wiśniewski, Marek; Hoser, Anna; Maria Losus, Renny; Rafiński, Zbigniew; Dobrzańska, Liliana; CrystEngComm 27 (2025) 3891–3898; doi:10.1039/D5CE00130G

data_7250650
_publ_section_title
;
 Reversible phase transformations upon water uptake/removal in crystalline
 material of a bipodal N-donor ligand and evaluation of the stability of
 the hydrates formed
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              3891
_journal_page_last               3898
_journal_paper_doi               10.1039/D5CE00130G
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C18 H16 N4'
_chemical_formula_weight         288.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-11-05 deposited with the CCDC.	2025-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                62.525(4)
_cell_angle_beta                 75.236(3)
_cell_angle_gamma                80.607(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0492(3)
_cell_length_b                   9.5052(4)
_cell_length_c                   9.9724(3)
_cell_measurement_reflns_used    10905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.8600
_cell_measurement_theta_min      5.0510
_cell_volume                     734.86(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2019/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.293
_diffrn_reflns_theta_min         5.062
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0507P)^2^+0.2042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2660
_reflns_number_total             3044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00130g2.cif
_cod_data_source_block           1
_cod_database_code               7250650
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              43424
_shelx_hkl_checksum              1231