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_7249012
_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         '2(C24 H18 Cl3.917 N8 Zn)'
_chemical_formula_sum            'C48 H36 Cl7.91 N16 Zn2'
_chemical_formula_weight         1248.25
_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
_audit_creation_date             2024-03-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.232(2)
_cell_angle_beta                 96.974(2)
_cell_angle_gamma                92.585(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9320(2)
_cell_length_b                   14.3027(3)
_cell_length_c                   19.3085(4)
_cell_measurement_reflns_used    17436
_cell_measurement_temperature    260.89
_cell_measurement_theta_max      75.6630
_cell_measurement_theta_min      3.8030
_cell_volume                     2719.67(10)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      260.89
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.961
_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    -71.00  21.34   0.38    2.00    --  -38.50  93.00 -31.00  243
  2  \w      0.00  80.94   0.38    2.00    --   49.56 -93.00-143.00  213
  3  \w     34.00 105.06   0.38    2.00    --  102.63 -93.00-143.00  187
  4  \w   -101.00 -23.86   0.38    2.00    --  -38.50 -64.00-159.86  203
  5  \w   -108.00 -34.28   0.38    2.00    --  -38.50 -19.00  60.00  194
  6  \w     46.00 115.16   0.38    2.00    --   49.56  37.00   0.00  182
  7  \w    -17.00  52.16   0.38    2.00    --   49.56 -37.00  90.00  182
  8  \w    -17.00  52.16   0.38    2.00    --   49.56 -37.00   0.00  182
  9  \w    -13.00  60.34   0.38    2.00    --   49.56 -57.00-120.00  193
 10  \w     95.00 171.00   0.38    2.00    --  102.63  15.00  30.00  200
 11  \w     40.00 116.00   0.38    2.00    --  102.63 -61.00  60.00  200
 12  \w     90.00 163.72   0.38    2.00    --  102.63  61.00-120.00  194
 13  \w     40.00 111.06   0.38    2.00    --  102.63-125.00-150.00  187
 14  \w     38.00 125.02   0.38    2.00    --  102.63 -77.00-150.00  229
 15  \w     95.00 171.00   0.38    2.00    --  102.63  15.00-180.00  200
 16  \w     92.00 165.34   0.38    2.00    --  102.63  55.00  56.97  193
 17  \w     98.00 165.64   0.38    2.00    --  102.63  45.00 -90.00  178
 18  \w     34.00 106.20   0.38    2.00    --  102.63 -94.00  60.00  190
 19  \w     98.00 165.64   0.38    2.00    --  102.63  45.00 120.00  178
 20  \w     34.00 106.20   0.38    2.00    --  102.63 -94.00 -30.00  190
 21  \w     90.00 163.72   0.38    2.00    --  102.63  61.00-180.00  194
 22  \w     38.00 125.02   0.38    2.00    --  102.63 -77.00  60.00  229
 23  \w     34.00 106.20   0.38    2.00    --  102.63 -94.00-150.00  190
 24  \w     97.00 164.64   0.38    2.00    --  102.63 125.00 120.00  178
 25  \w    103.00 165.70   0.38    2.00    --  102.63  77.00   0.00  165
 26  \w     40.00 111.06   0.38    2.00    --  102.63-125.00   0.00  187
 27  \w     34.00 106.20   0.38    2.00    --  102.63 -94.00  90.00  190
 28  \w     97.00 164.64   0.38    2.00    --  102.63 125.00  60.00  178
 29  \w     40.00 116.00   0.38    2.00    --  102.63 -61.00 -60.00  200
 30  \w    103.00 165.70   0.38    2.00    --  102.63  77.00 150.00  165
 31  \w    104.00 170.12   0.38    2.00    --  102.63  93.00 -31.00  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  0.0501
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42962
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.786
_diffrn_reflns_theta_min         4.615
_exptl_absorpt_coefficient_mu    5.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62741
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             1261
_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          0.14
_refine_diff_density_max         1.832
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1440P)^2^+1.6062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8426
_reflns_number_total             11029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           ZnBCP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_database_code               7249012
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.537
_shelx_estimated_absorpt_t_min   0.375
_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), C10A(H10A,H10B), C00Z(H00A,H00B), C01Y(H01B,H01C)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A), C8(H8), C8A(H8A), C12(H12), C12A(H12A), C13(H13),
 C13A(H13A), C14(H14), C14A(H14A), C15(H15), C15A(H15A), C16(H16), C16A(H16A),
 C01A(H01A), C01G(H01G), C01L(H01L), C01M(H01M), C01R(H01R), C01W(H01W),
 C01X(H01X), C01Z(H01Z), C011(H011), C013(H013), C019(H019), C020(H020),
 C021(H021), C022(H022)
;
_shelx_res_checksum              53169
_shelx_hkl_checksum              86211
_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
;