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_2021099
_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-'
_chemical_formula_moiety         '2(C5 H6 N5 +), (H2 P2 O6 2-)'
_chemical_formula_sum            'C10 H14 N10 O6 P2'
_chemical_formula_weight         432.25
_chemical_name_systematic
;
Bis(adeninium) hypodiphosphorate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.888(5)
_cell_length_b                   11.093(4)
_cell_length_c                   11.487(4)
_cell_measurement_reflns_used    5596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.06
_cell_measurement_theta_min      3.90
_cell_volume                     1609.6(10)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur PX kappa-geometry diffractometer
with an Onyx CCD camera
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9109
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         77.754
_diffrn_reflns_theta_min         5.307
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.510
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0969P)^2^+1.9080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                1547
_reflns_number_total             1638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3010sup1.cif
_cod_data_source_block           4_pp12l_100
_cod_database_code               2021099
_cod_database_fobs_code          2021099
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.772
_shelx_hkl_checksum              37468
_shelx_res_checksum              38005