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_7249535
_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_formula_moiety         'C5 H4 Cs N5'
_chemical_formula_sum            'C5 H4 Cs N5'
_chemical_formula_weight         267.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7149(8)
_cell_length_b                   11.1762(8)
_cell_length_c                   10.8144(9)
_cell_measurement_reflns_used    4030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1370
_cell_measurement_theta_min      3.0620
_cell_volume                     1536.77(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -94.00 -34.00   1.00    2.50    --  -17.15 178.00  60.00   60
  2  \w    -25.00  92.00   1.00    2.50    --   19.03  19.00  60.00  117
  3  \w    -87.00 -62.00   1.00    2.50    --  -17.15 -77.00-150.00   25
  4  \w    -43.00  55.00   1.00    2.50    --  -17.15  38.00 -30.00   98
;
_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      -0.0235396000
_diffrn_orient_matrix_UB_12      0.0353504000
_diffrn_orient_matrix_UB_13      -0.0469545000
_diffrn_orient_matrix_UB_21      0.0294668000
_diffrn_orient_matrix_UB_22      -0.0311588000
_diffrn_orient_matrix_UB_23      -0.0453976000
_diffrn_orient_matrix_UB_31      -0.0411516000
_diffrn_orient_matrix_UB_32      -0.0424729000
_diffrn_orient_matrix_UB_33      -0.0058685000
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8275
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.356
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49290
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.777
_refine_diff_density_min         -3.401
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0521P)^2^+16.5633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1336
_reflns_number_total             1571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00892h2.cif
_cod_data_source_block           ck104
_cod_depositor_comments
'Adding full bibliography for 7249534--7249535.cif.'
_cod_database_code               7249535
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C5H4N5Cs1
_chemical_oxdiff_usercomment     'Cs adenine'
_shelx_estimated_absorpt_t_max   0.329
_shelx_estimated_absorpt_t_min   0.200
_diffrn_oxdiff_ac4_digest_frames
;
017a3f1033c37a4ed9412e60b250994e7600028f87a
;
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8)
;
_shelx_res_checksum              64197
_shelx_hkl_checksum              80159
_olex2_date_sample_data_collection 2022-11-10
_olex2_date_sample_submission    2022-11-10
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.745