Crystallographic insight into the binding modes of group 12 metal cations with N7-alkylated purines
Panda, Subhra Jyoti; Agrawalla, Suraj Kumar; Purohit, Chandra Shekhar; CrystEngComm 26 (2024) 4418–4430; doi:10.1039/D4CE00341A

data_7249004
_publ_section_title
;
 Crystallographic insight into the binding modes of group 12 metal cations
 with N7-alkylated purines
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4418
_journal_page_last               4430
_journal_paper_doi               10.1039/D4CE00341A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C8 H7 Cl3 Hg N4'
_chemical_formula_sum            'C8 H7 Cl3 Hg N4'
_chemical_formula_weight         466.12
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.751(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2883(13)
_cell_length_b                   7.9852(4)
_cell_length_c                   15.3182(8)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      78.2400
_cell_measurement_theta_min      5.9400
_cell_volume                     2465.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9918
_diffrn_measured_fraction_theta_max 0.9590
_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   -106.00 -20.00   0.50    1.00    --  -38.50 152.00  29.00  172
  2  \w    -85.00  -3.00   0.50    1.00    --  -38.50 121.00-130.00  164
  3  \w     24.00  96.00   0.50    1.00    --   49.56-121.00 146.00  144
  4  \w     81.00 165.00   0.50    2.00    --  107.46 152.00  29.00  168
  5  \w     44.00 110.00   0.50    2.00    --  107.46-121.00 146.00  132
  6  \w     44.00 131.00   0.50    2.00    --  107.46-152.00 -13.00  174
  7  \w     99.00 171.00   0.50    2.00    --  107.46 121.00-130.00  144
  8  \w   -105.00 -35.00   0.50    1.00    --  -38.50 -37.00 -30.00  140
  9  \w    -42.00  28.00   0.50    1.00    --  -38.50  37.00-120.00  140
 10  \w     42.00 109.00   0.50    1.00    --   49.56-152.00 -13.00  134
 11  \w     62.00 113.00   0.50    1.00    --   49.56  57.00-120.00  102
 12  \w    144.00 170.00   0.50    2.00    --  107.46  61.00  30.00   52
 13  \w     46.00  73.00   0.50    2.00    --  107.46-125.00  90.00   54
 14  \w     46.00 121.00   0.50    2.00    --  107.46 -61.00 -90.00  150
 15  \w    132.00 172.00   0.50    2.00    --  107.46  45.00   0.00   80
 16  \w     46.00  77.00   0.50    2.00    --  107.46 -94.00-180.00   62
 17  \w     50.00 131.00   0.50    2.00    --  107.46 -77.00  30.00  162
 18  \w     88.00 113.00   0.50    2.00    --  107.46-125.00  90.00   50
 19  \w     98.00 170.00   0.50    2.00    --  107.46 125.00  60.00  144
 20  \w    105.00 130.00   0.50    2.00    --  107.46  30.00  30.00   50
 21  \w    138.00 175.00   0.50    2.00    --  107.46  30.00  30.00   74
 22  \w     43.00 110.00   0.50    2.00    --  107.46 -45.00  90.00  134
 23  \w    117.00 175.00   0.50    2.00    --  107.46  30.00 150.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0752369000
_diffrn_orient_matrix_UB_12      0.0199441000
_diffrn_orient_matrix_UB_13      0.0468422000
_diffrn_orient_matrix_UB_21      0.0099917000
_diffrn_orient_matrix_UB_22      -0.1878832000
_diffrn_orient_matrix_UB_23      -0.0149083000
_diffrn_orient_matrix_UB_31      0.0081222000
_diffrn_orient_matrix_UB_32      0.0402715000
_diffrn_orient_matrix_UB_33      -0.0940966000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8384
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.708
_diffrn_reflns_theta_min         4.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    28.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.733
_refine_diff_density_min         -2.780
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0798P)^2^+107.0663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2340
_reflns_number_total             2555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           HgACP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_database_code               7249004
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N Cl Hg'
_chemical_oxdiff_usercomment     'LIGHT YELLOW BLOCK'
_shelx_estimated_absorpt_t_max   0.081
_shelx_estimated_absorpt_t_min   0.056
_diffrn_oxdiff_ac3_digest_hkl    0129136fc2a11e4d7f8780048212e9d4b3575f
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C11(H11)
2.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B)
;
_shelx_res_checksum              24684
_shelx_hkl_checksum              70677
_olex2_exptl_crystal_mounting_method 'Mounted on the loop'
_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 4.760
_oxdiff_exptl_absorpt_empirical_full_min 0.536