Crystal engineering and structural diversity of 2-aminopyridinium hypodiphosphates obtained by crystallization and dehydration
Budzikur, Daria; Kinzhybalo, Vasyl; Ślepokura, Katarzyna; CrystEngComm  (2022) –; doi:10.1039/D2CE00261B

data_7245026
_publ_section_title
;
 Crystal engineering and structural diversity of 2-aminopyridinium
 hypodiphosphates obtained by crystallization and dehydration
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00261B
_journal_year                    2022
_chemical_formula_moiety
'4(C5 H7 N2), 2(H3 P2 O6), (H2 P2 O6), 0.1(H2 O)'
_chemical_formula_sum            'C20 H36.2 N8 O18.1 P6'
_chemical_formula_weight         864.19
_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     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-02-24 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.61(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.706(5)
_cell_length_b                   10.656(4)
_cell_length_c                   24.802(7)
_cell_measurement_reflns_used    13370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.3890
_cell_measurement_theta_min      3.2340
_cell_volume                     3598(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.970
_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  0.1243
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            86594
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         74.824
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         7170
_refine_ls_number_restraints     446
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1628
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1198P)^2^+6.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3580
_reflns_number_total             7170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00261b4.cif
_cod_data_source_block           2ampyr11-dehh
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C20 H36.20 N8 O18.10 P6'
_cod_database_code               7245026
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              71770