Structural variety and dehydration in 3-aminopyridine–hypodiphosphoric acid–water system
Budzikur-Maciąg, Daria; Kinzhybalo, Vasyl; Ślepokura, Katarzyna; CrystEngComm 25 (2023) 3826–3836; doi:10.1039/D3CE00186E

data_7246916
_publ_section_title
;
 Structural variety and dehydration in 3-aminopyridine--hypodiphosphoric
 acid--water system
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3826
_journal_page_last               3836
_journal_paper_doi               10.1039/D3CE00186E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'4(C5 N2 H7), 2(H3 P2 O6), H2 P2 O6, 2(H2 O)'
_chemical_formula_sum            'C20 H40 N8 O20 P6'
_chemical_formula_weight         898.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                73.10(2)
_cell_angle_beta                 81.56(2)
_cell_angle_gamma                81.96(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6024(14)
_cell_length_b                   13.234(2)
_cell_length_c                   13.848(2)
_cell_measurement_reflns_used    33264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.7290
_cell_measurement_theta_min      1.8860
_cell_volume                     1829.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89059
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         48.011
_diffrn_reflns_theta_min         1.904
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76055
_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    1.631
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         27745
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16336
_reflns_number_total             27745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00186e4.cif
_cod_data_source_block           3AminoPyr11_21_100_00
_cod_depositor_comments
;
Adding full bibliography for 7246911--7246916.cif.

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10 H20 N4 O10 P3'
_cod_original_formula_weight         449.21
_cod_original_formula_moiety
'2(C5 N2 H7), (H2 P2 O6), 0.5(H4 P2 O6), (H2 O)'
_cod_original_formula_units_Z            4
_cod_database_code               7246916
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              77944