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_7246915
_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         '6(C5 N2 H7), (H2 P2 O6), (P2 O4), 2(H2 O)'
_chemical_formula_sum            'C30 H48 N12 O14 P4'
_chemical_formula_weight         924.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 106.49(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0257(13)
_cell_length_b                   14.6592(14)
_cell_length_c                   12.1537(11)
_cell_measurement_reflns_used    10827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.5840
_cell_measurement_theta_min      4.8420
_cell_volume                     2054.4(4)
_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-2016/6 (Sheldrick, 2016)'
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0134
_diffrn_reflns_av_unetI/netI     0.0087
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14175
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        63.825
_diffrn_reflns_theta_max         63.825
_diffrn_reflns_theta_min         4.848
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60659
_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    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.3036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3234
_reflns_number_total             3311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00186e4.cif
_cod_data_source_block           3Aminopyr31-100
_cod_depositor_comments
'Adding full bibliography for 7246911--7246916.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7246915
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.492
_shelx_estimated_absorpt_t_max   0.858
_shelx_res_checksum              64985