Crystal structures of potassium and cesium salts of adenine: the role of alkali cations
Kaur, Sarabjeet; Harvey, Jeremy; Van Meervelt, Luc; Kirschhock, Christine E. A.; CrystEngComm 26 (2024) 6805–6812; doi:10.1039/D4CE00892H

data_7249534
_publ_section_title
;
 Crystal structures of potassium and cesium salts of adenine: the role of
 alkali cations
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              6805
_journal_page_last               6812
_journal_paper_doi               10.1039/D4CE00892H
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C5 H4 K N5'
_chemical_formula_sum            'C5 H4 K N5'
_chemical_formula_weight         173.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-21 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.802(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.6480(6)
_cell_length_b                   7.4057(5)
_cell_length_c                   7.1220(7)
_cell_measurement_reflns_used    2790
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8810
_cell_measurement_theta_min      3.1130
_cell_volume                     320.81(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9631
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  25.00   1.00    5.00    --  -17.15 -99.00 -30.00   45
  2  \w     -7.00  91.00   1.00    5.00    --   18.87  38.00   0.00   98
  3  \w    -25.00  92.00   1.00    5.00    --   18.87  19.00 -60.00  117
  4  \w    -86.00   4.00   1.00    5.00    --  -17.15 -57.00  90.00   90
  5  \w    -80.00  -7.00   1.00    5.00    --  -17.15 133.00 -25.00   73
  6  \w    -93.00 -35.00   1.00    5.00    --  -17.15-178.00  60.00   58
  7  \w    -39.00 -14.00   1.00    5.00    --  -17.15  57.00-120.00   25
  8  \w    -93.00 -35.00   1.00    5.00    --  -17.15-178.00 150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0928666000
_diffrn_orient_matrix_UB_12      0.0478063000
_diffrn_orient_matrix_UB_13      0.0691968000
_diffrn_orient_matrix_UB_21      0.0527430000
_diffrn_orient_matrix_UB_22      -0.0829861000
_diffrn_orient_matrix_UB_23      0.0409465000
_diffrn_orient_matrix_UB_31      0.0468748000
_diffrn_orient_matrix_UB_32      -0.0012713000
_diffrn_orient_matrix_UB_33      -0.0734441000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3436
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.326
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_description       plate
_exptl_crystal_F_000             176
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 543 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1286
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0399P)^2^+0.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                1255
_reflns_number_total             1286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00892h2.cif
_cod_data_source_block           ck103
_cod_depositor_comments
'Adding full bibliography for 7249534--7249535.cif.'
_cod_original_cell_volume        320.81(5)
_cod_database_code               7249534
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C5H5N4K1
_chemical_oxdiff_usercomment     K-adenine
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.753
_diffrn_oxdiff_ac4_digest_frames
;
01c594f93e35bd9bae4aed681b356a41600002871fb
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All K(H,H,H,H) groups
;
_shelx_res_checksum              55988
_shelx_hkl_checksum              62648
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.593
_oxdiff_exptl_absorpt_empirical_full_min 0.693