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_7250651
_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 H20 N4 O2'
_chemical_formula_weight         324.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 93.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.149(4)
_cell_length_b                   9.6466(19)
_cell_length_c                   9.3799(19)
_cell_measurement_reflns_used    861
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2095
_cell_measurement_theta_min      2.392
_cell_volume                     1639.9(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8358
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.248
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9982
_exptl_absorpt_correction_T_min  0.9677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2892
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0513P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2069
_reflns_number_total             2892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00130g2.cif
_cod_data_source_block           4OK
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7250651
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              24823
_shelx_hkl_checksum              12687