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_7249607
_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         '(C5 H7 N2), (H3 P2 O6)'
_chemical_formula_sum            'C5 H10 N2 O6 P2'
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_space_group_name_H-M_alt        'P 1 21/n 1'
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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
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_cell_length_b                   15.099(4)
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_cell_volume                     1003.2(5)
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_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
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_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      110(2)
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_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.468
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.468
_diffrn_reflns_limit_h_max       8
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_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8299
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
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_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       plate
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_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.464
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_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0549
_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^)+(0.1005P)^2^+0.7205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1989
_reflns_number_total             2319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01048e2.cif
_cod_data_source_block           4AMINO12_aa
_cod_depositor_comments
'Adding full bibliography for 7249606--7249610.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249607
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              26234
_shelx_hkl_checksum              594