Supramolecular architecture of theophylline polymorphs, monohydrate and co-crystals with iodine: study from the energetic viewpoint
Konovalova, Irina S.; Shishkina, Svitlana V.; Wyshusek, Maik; Patzer, Michael; Reiss, Guido J.; RSC Advances 14 (2024) 29774–29788; doi:10.1039/D4RA04368E

data_7249352
_publ_section_title
;
 Supramolecular architecture of theophylline polymorphs, monohydrate and
 co-crystals with iodine: study from the energetic viewpoint
;
_journal_issue                   41
_journal_name_full               'RSC Advances'
_journal_page_first              29774
_journal_page_last               29788
_journal_paper_doi               10.1039/D4RA04368E
_journal_volume                  14
_journal_year                    2024
_chemical_formula_sum            'C14 H20 N8 O6'
_chemical_formula_weight         396.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-05-22 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.558(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.46150(10)
_cell_length_b                   15.3156(3)
_cell_length_c                   13.0669(3)
_cell_measurement_reflns_used    9283
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      33.9050
_cell_measurement_theta_min      4.1010
_cell_volume                     885.11(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 16.2678
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32288
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        32.493
_diffrn_reflns_theta_max         32.493
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       needle
_exptl_crystal_F_000             416
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2147 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6403
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0551
_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^)+(0.0300P)^2^+0.3600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5154
_reflns_number_total             6403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra04368e2.cif
_cod_data_source_block           Theo_hydrat115
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7249352
_shelx_shelxl_version_number     2019/2
_shelx_res_checksum              83133
_shelx_hkl_checksum              83877