Structural landscape studies of aminopyridinium hypodiphosphates: dehydration and polymorphism in 4-aminopyridinium salts
Budzikur-Maciąg, Daria; Kinzhybalo, Vasyl; Ślepokura, Katarzyna; CrystEngComm 26 (2024) 6861–6872; doi:10.1039/D4CE01048E

data_7249606
_publ_section_title
;
 Structural landscape studies of aminopyridinium hypodiphosphates:
 dehydration and polymorphism in 4-aminopyridinium salts
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              6861
_journal_page_last               6872
_journal_paper_doi               10.1039/D4CE01048E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '2(C5 H7 N2), (H2 P2 O6), (H4 P2 O6), 2(H2 O)'
_chemical_formula_sum            'C10 H24 N4 O14 P4'
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
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_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2024-08-15 deposited with the CCDC.	2024-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.97(2)
_cell_angle_gamma                90
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_cell_length_b                   18.528(3)
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_cell_measurement_temperature    100(2)
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_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'four-circle diffractometer'
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'Agilent Technologies Xcalibur R, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30195
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         3.174
_diffrn_source                   'fine-focus sealed X-ray tube'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.453
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5756
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.1974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4944
_reflns_number_total             5756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01048e2.cif
_cod_data_source_block           4amino11m-smart
_cod_depositor_comments
'Adding full bibliography for 7249606--7249610.cif.'
_cod_original_cell_volume        1120.5(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249606
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.905
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              91808
_shelx_hkl_checksum              58917