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_7246914
_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         '2(C5 N2 H7), (H2 P2 O6), (C5 N2 H6)'
_chemical_formula_sum            'C15 H22 N6 O6 P2'
_chemical_formula_weight         444.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-02-23 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.014(2)
_cell_length_b                   13.556(2)
_cell_length_c                   12.259(2)
_cell_measurement_reflns_used    28552
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.1520
_cell_measurement_theta_min      4.8230
_cell_volume                     1996.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       '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 1.000
_diffrn_measured_fraction_theta_max 0.991
_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           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40672
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         75.704
_diffrn_reflns_theta_min         4.864
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65551
_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    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1716 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3967
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0520P)^2^+0.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                3884
_reflns_number_total             3967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00186e4.cif
_cod_data_source_block           3amino31-deh
_cod_depositor_comments
'Adding full bibliography for 7246911--7246916.cif.'
_cod_database_code               7246914
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              85840