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_7249010
_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         'C16 H14 Cd2 Cl6 N8'
_chemical_formula_sum            'C16 H14 Cd2 Cl6 N8'
_chemical_formula_weight         755.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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
;
2024-06-02 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                102.283(4)
_cell_angle_beta                 92.670(4)
_cell_angle_gamma                110.237(6)
_cell_formula_units_Z            2
_cell_length_a                   7.9194(5)
_cell_length_b                   11.2800(7)
_cell_length_c                   14.7285(5)
_cell_measurement_reflns_used    10651
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.1320
_cell_measurement_theta_min      4.6890
_cell_volume                     1195.82(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9638
_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    -65.00  31.00   0.50    0.50    --  -38.50   5.00-112.00  192
  2  \w   -108.00 -12.00   0.50    0.50    --  -38.50  -5.00  71.00  192
  3  \w    -20.00  76.00   0.50    0.50    --   49.56  -5.00  71.00  192
  4  \w     23.00 119.00   0.50    0.50    --   49.56   5.00-112.00  192
  5  \w     38.00 134.00   0.50    1.20    --  107.46  -5.00  71.00  192
  6  \w     81.00 177.00   0.50    1.20    --  107.46   5.00-112.00  192
  7  \w    -86.00  -6.00   0.50    0.50    --  -38.50 125.00 150.00  160
  8  \w   -101.00 -27.00   0.50    0.50    --  -38.50 -57.00  60.00  148
  9  \w    -17.00  53.00   0.50    0.50    --   49.56 -37.00 -60.00  140
 10  \w     28.00  99.00   0.50    0.50    --   49.56-125.00  30.00  142
 11  \w    103.00 172.00   0.50    1.20    --  107.46  77.00  90.00  138
 12  \w     45.00 121.00   0.50    1.20    --  107.46 -61.00 -60.00  152
 13  \w     39.00 107.00   0.50    1.20    --  107.46 -94.00 150.00  136
 14  \w    103.00 172.00   0.50    1.20    --  107.46  45.00 -90.00  138
 15  \w     45.00 121.00   0.50    1.20    --  107.46 -61.00   0.00  152
 16  \w     45.00 113.00   0.50    1.20    --  107.46-125.00 -60.00  136
 17  \w    104.00 176.00   0.50    1.20    --  107.46  30.00 150.00  144
 18  \w    104.00 176.00   0.50    1.20    --  107.46  30.00  30.00  144
 19  \w     45.00 113.00   0.50    1.20    --  107.46-125.00  90.00  136
 20  \w     39.00 111.00   0.50    1.20    --  107.46 -30.00   0.00  144
 21  \w     43.00 112.00   0.50    1.20    --  107.46 -45.00-150.00  138
 22  \w     45.00 113.00   0.50    1.20    --  107.46-125.00-120.00  136
 23  \w     45.00 121.00   0.50    1.20    --  107.46 -61.00  90.00  152
 24  \w     43.00 112.00   0.50    1.20    --  107.46 -45.00 -60.00  138
 25  \w     97.00 170.00   0.50    1.20    --  107.46 125.00  30.00  146
 26  \w     45.00 121.00   0.50    1.20    --  107.46 -61.00  60.00  152
 27  \w     45.00 121.00   0.50    1.20    --  107.46 -61.00-180.00  152
 28  \w     39.00 107.00   0.50    1.20    --  107.46 -94.00 -90.00  136
 29  \w     39.00 107.00   0.50    1.20    --  107.46 -94.00 -60.00  136
 30  \w     39.00 107.00   0.50    1.20    --  107.46 -94.00 120.00  136
 31  \w    103.00 172.00   0.50    1.20    --  107.46  77.00 -90.00  138
 32  \w     39.00 107.00   0.50    1.20    --  107.46 -94.00 -30.00  136
 33  \w   -101.00 -42.00   0.50    0.50    --  -38.50 -68.00-133.11  118
 34  \w   -101.00 -20.00   0.50    0.50    --  -38.50 -69.00 -53.41  162
;
_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      0.1487861000
_diffrn_orient_matrix_UB_12      0.1339157000
_diffrn_orient_matrix_UB_13      0.0068223000
_diffrn_orient_matrix_UB_21      -0.1461173000
_diffrn_orient_matrix_UB_22      0.0610224000
_diffrn_orient_matrix_UB_23      -0.0026304000
_diffrn_orient_matrix_UB_31      0.0142558000
_diffrn_orient_matrix_UB_32      0.0295653000
_diffrn_orient_matrix_UB_33      0.1077338000
_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  0.0894
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18182
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.736
_diffrn_reflns_theta_min         4.308
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
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    2.099
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.441
_refine_diff_density_min         -2.084
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1100P)^2^+6.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4052
_reflns_number_total             4909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           CdACP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_original_cell_volume        1195.82(12)
_cod_database_code               7249010
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N Cl Cd'
_chemical_oxdiff_usercomment     'COLOURLESS NEEDLES'
_shelx_estimated_absorpt_t_max   0.137
_shelx_estimated_absorpt_t_min   0.093
_diffrn_oxdiff_digest_frames
;
01694699db74250f73b001cbc59e08b88b00029d344
;
_diffrn_oxdiff_digest_hkl
;
0139b43a66a72b979625b06b0b1b05b5181b67
;
_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(H10C,H10D), C10'(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2'(H2'), C8(H8), C8'(H8'), C11(H11), C11'(H11')
2.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B), C12'(H12C,H12D)
;
_shelx_res_checksum              1024
_shelx_hkl_checksum              13547
_olex2_exptl_crystal_mounting_method 'Mounted on the nylon 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 2.288
_oxdiff_exptl_absorpt_empirical_full_min 0.603