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_7249006
_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         'C12 H9 Cd Cl3 N4'
_chemical_formula_sum            'C12 H9 Cd Cl3 N4'
_chemical_formula_weight         427.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-24 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.316(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7616(5)
_cell_length_b                   13.8750(3)
_cell_length_c                   17.3043(7)
_cell_measurement_reflns_used    4391
_cell_measurement_temperature    295.90(10)
_cell_measurement_theta_max      74.9040
_cell_measurement_theta_min      5.5150
_cell_volume                     3056.7(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_temperature      295.90
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.957
_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   -103.00 -52.84   0.38    1.00    --  -38.50-161.00 -91.00  132
  2  \w    -81.00  -0.06   0.38    1.00    --  -38.50 117.00 146.00  213
  3  \w   -108.00 -27.06   0.38    1.00    --  -38.50 161.00 -63.00  213
  4  \w     21.00  91.30   0.38    1.00    --   48.56-117.00  58.00  185
  5  \w     47.00 116.16   0.38    1.00    --   48.56-161.00 -91.00  182
  6  \w     74.00 157.22   0.38    4.00    --  102.63 161.00 -63.00  219
  7  \w     49.00 108.28   0.38    4.00    --  102.63-161.00 -91.00  156
  8  \w     74.00  99.08   0.38    4.00    --  102.63-117.00  58.00   66
  9  \w    102.00 164.70   0.38    4.00    --  102.63 117.00 146.00  165
 10  \w   -104.00 -38.64   0.38    1.00    --  -38.50 -19.00  60.00  172
 11  \w     74.00 108.20   0.38    1.00    --   48.56  57.00 150.00   90
 12  \w     41.00 110.16   0.38    4.00    --  102.63-125.00  30.00  182
 13  \w     82.00 108.22   0.38    4.00    --  102.63-125.00 120.00   69
 14  \w     78.00 105.36   0.38    4.00    --  102.63 -45.00-120.00   72
 15  \w    110.00 161.30   0.38    4.00    --  102.63  45.00 -30.00  135
 16  \w     40.00  97.00   0.38    4.00    --  102.63 -30.00   0.00  150
 17  \w     65.00 100.72   0.38    4.00    --  102.63 -94.00 -90.00   94
 18  \w    106.00 163.76   0.38    4.00    --  102.63  77.00 -90.00  152
 19  \w     64.00 104.28   0.38    4.00    --  102.63 -94.00  30.00  106
 20  \w    110.00 161.30   0.38    4.00    --  102.63 125.00  30.00  135
 21  \w     42.00 101.28   0.38    4.00    --  102.63 -45.00   0.00  156
 22  \w     46.00  75.26   0.38    4.00    --  102.63 -45.00-120.00   77
 23  \w    100.00 166.12   0.38    4.00    --  102.63  45.00  60.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11218
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.788
_diffrn_reflns_theta_min         4.217
_exptl_absorpt_coefficient_mu    16.226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53077
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3052
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0793P)^2^+12.5054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2592
_reflns_number_total             3052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           cdbcp
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_database_code               7249006
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.169
_shelx_estimated_absorpt_t_min   0.118
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C12-C11 \\sim C18-C11 \\sim C13-C12 \\sim C18-C17 \\sim C14-C13 \\sim C9-C17
\\sim C9-C3 \\sim C15-C14 ~
 C16-C15 \\sim C7-C3 \\sim C7-C11 \\sim C16-C11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C16(0.5) H16(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C14(0.5)
 H14(0.5) C15(0.5) H15(0.5) C7(0.5) H7(0.5) C18(0.5) H18(0.5) C3(0.5) H3(0.5)
 C17(0.5) H17(0.5) C9(0.5) H9(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C16(H16), C12(H12), C13(H13), C14(H14), C15(H15), C7(H7),
 C18(H18), C3(H3), C17(H17), C9(H9)
5.c Fitted hexagon refined as free rotating group:
 C16(C11,C12,C13,C14,C15)
;
_shelx_res_checksum              91770
_shelx_hkl_checksum              96674
_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
;