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_7249007
_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         'C24 H18 Cl8 Hg3 N8'
_chemical_formula_sum            'C24 H18 Cl8 Hg3 N8'
_chemical_formula_weight         1303.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.382(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6958(4)
_cell_length_b                   8.2297(2)
_cell_length_c                   13.5675(3)
_cell_measurement_reflns_used    8459
_cell_measurement_temperature    294.97(10)
_cell_measurement_theta_max      79.3690
_cell_measurement_theta_min      6.1120
_cell_volume                     1608.61(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9789
_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    -79.00   8.00   0.50    1.00    --  -38.50 108.00  62.00  174
  2  \w     14.00  91.00   0.50    1.00    --   49.56-108.00 -34.00  154
  3  \w    104.00 178.00   0.50    2.00    --  111.00 108.00  62.00  148
  4  \w     43.00 108.00   0.50    2.00    --  111.00-108.00 -34.00  130
  5  \w   -105.00 -35.00   0.50    1.00    --  -38.50 -37.00 -90.00  140
  6  \w   -105.00 -35.00   0.50    1.00    --  -38.50 -37.00 -30.00  140
  7  \w    -17.00  53.00   0.50    1.00    --   49.56 -37.00-180.00  140
  8  \w     38.00 113.00   0.50    1.00    --   49.56  57.00 150.00  150
  9  \w    -17.00  53.00   0.50    1.00    --   49.56 -37.00 -30.00  140
 10  \w    108.00 178.00   0.50    2.00    --  111.00  30.00-120.00  140
 11  \w     43.00 114.00   0.50    2.00    --  111.00 -30.00 120.00  142
 12  \w     43.00 114.00   0.50    2.00    --  111.00 -30.00  60.00  142
 13  \w    103.00 178.00   0.50    2.00    --  111.00  15.00 120.00  150
 14  \w     48.00 124.00   0.50    2.00    --  111.00 -61.00 -30.00  152
 15  \w     43.00 106.00   0.50    2.00    --  111.00 -94.00   0.00  126
 16  \w     47.00 134.00   0.50    2.00    --  111.00 -77.00 -60.00  174
 17  \w     47.00 116.00   0.50    2.00    --  111.00 -45.00   0.00  138
 18  \w     47.00 116.00   0.50    2.00    --  111.00 -45.00 150.00  138
 19  \w     43.00 103.00   0.50    2.00    --  111.00 -94.00-180.00  120
 20  \w     47.00 112.00   0.50    2.00    --  111.00 -45.00  90.00  130
;
_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      -0.1001691000
_diffrn_orient_matrix_UB_12      -0.0409737000
_diffrn_orient_matrix_UB_13      0.0095858000
_diffrn_orient_matrix_UB_21      -0.0263576000
_diffrn_orient_matrix_UB_22      -0.0265295000
_diffrn_orient_matrix_UB_23      -0.1144887000
_diffrn_orient_matrix_UB_31      0.0265487000
_diffrn_orient_matrix_UB_32      -0.1807436000
_diffrn_orient_matrix_UB_33      0.0146899000
_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  0.0739
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13220
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.604
_diffrn_reflns_theta_min         6.144
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    31.564
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.532
_refine_diff_density_min         -2.145
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+9.5119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2967
_reflns_number_total             3415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           HgBCP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_database_code               7249007
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N Cl Hg'
_chemical_oxdiff_usercomment     'colourless white block'
_shelx_estimated_absorpt_t_max   0.049
_shelx_estimated_absorpt_t_min   0.035
_diffrn_oxdiff_digest_frames
;
014c286bca5e9de38ebfe2c3fdf737bbd800029b3f7
;
_diffrn_oxdiff_digest_hkl
;
0114ac105ceb8d9cf81d6050d4c12bae28e097
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              95906
_shelx_hkl_checksum              91500
_olex2_exptl_crystal_mounting_method 'mounted on a 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 3.268
_oxdiff_exptl_absorpt_empirical_full_min 0.376