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_7250652
_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 H17 N4 O0.5'
_chemical_formula_weight         297.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 102.478(2)
_cell_angle_gamma                90
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_cell_length_c                   26.6872(5)
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_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      3.3810
_cell_volume                     2926.82(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.948
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.310
_diffrn_reflns_theta_min         3.392
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95565
_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    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0457P)^2^+1.8118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2631
_reflns_number_total             2997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00130g2.cif
_cod_data_source_block           2cor
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C18 H17 N4 O0.50'
_cod_database_code               7250652
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              19330
_shelx_hkl_checksum              27100