Adenosine hypodiphosphate ester, an analogue of ADP: analysis of the adenine–hypodiphosphate interaction mode in hypodiphosphate nucleotides and adenine salts
Otreba, Marta; Budzikur, Daria; Górecki, Łukasz; Ślepokura, Katarzyna A.; Acta Crystallographica Section C 74 (2018) 571–583; doi:10.1107/S2053229618005089

data_2021098
_publ_section_title
;
 Adenosine hypodiphosphate ester, an analogue of ADP: analysis of the
 adenine--hypodiphosphate interaction mode in hypodiphosphate nucleotides
 and adenine salts
;
_journal_coeditor_code           JX3010
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              571
_journal_page_last               583
_journal_paper_doi               10.1107/S2053229618005089
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '2C5 H6 N5 +, H2 P2 O6 2-, 2H2 O'
_chemical_formula_moiety         '2(C5 H6 N5 +), (H2 P2 O6 2-), 2(H2 O)'
_chemical_formula_sum            'C10 H18 N10 O8 P2'
_chemical_formula_weight         468.28
_chemical_name_systematic
;
Bis(adeninium) hypodiphosphorate dihydrate
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.62(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.515(2)
_cell_length_b                   11.955(2)
_cell_length_c                   7.064(2)
_cell_measurement_reflns_used    8199
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      36.59
_cell_measurement_theta_min      3.30
_cell_volume                     882.1(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Kuma KM4-CCD kappa-geometry diffractometer with a Sapphire2 CCD camera'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12503
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.901
_diffrn_reflns_theta_min         3.367
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.623
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0811P)^2^+0.4292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                3125
_reflns_number_total             3613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3010sup1.cif
_cod_data_source_block           3_dadopp13
_cod_database_code               2021098
_cod_database_fobs_code          2021098
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.951
_shelx_hkl_checksum              22683
_shelx_res_checksum              18976