Structural aspects of dehydration and rehydration in the adenosine 5′-diphosphate (ADP)–potassium–water system
Kaszubowski, Oskar; Ślepokura, Katarzyna; CrystEngComm 25 (2023) 4592–4603; doi:10.1039/D3CE00395G

data_7247123
_publ_section_title
;
 Structural aspects of dehydration and rehydration in the adenosine
 5&#x2032;-diphosphate (ADP)--potassium--water system
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4592
_journal_page_last               4603
_journal_paper_doi               10.1039/D3CE00395G
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'H5 O2, K, C20 H28 N10 O20 P4, 4.25(H2 O)'
_chemical_formula_sum            'C20 H41.5 K N10 O26.25 P4'
_chemical_formula_weight         1005.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-02-16 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.352(6)
_cell_length_b                   10.990(3)
_cell_length_c                   6.7232(11)
_cell_measurement_reflns_used    2813
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      71.6360
_cell_measurement_theta_min      3.3300
_cell_volume                     1947.1(8)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300(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 0.987
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6961
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.141
_diffrn_reflns_theta_min         3.354
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.745
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       needle
_exptl_crystal_F_000             1041
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 778 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.073(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1322P)^2^+0.5051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.531
_reflns_Friedel_fraction_full    0.779
_reflns_Friedel_fraction_max     0.707
_reflns_number_gt                2686
_reflns_number_total             3340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00395g3.cif
_cod_data_source_block           IVa
_cod_depositor_comments
'Adding full bibliography for 7247122--7247126.cif.'
_cod_original_formula_sum        'C20 H41.50 K N10 O26.25 P4'
_cod_database_code               7247123
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.400
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              96368