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_7249009
_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 Cl4 N8 Zn'
_chemical_formula_sum            'C16 H14 Cl4 N8 Zn'
_chemical_formula_weight         525.52
_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             2024-02-23
_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                107.838(2)
_cell_angle_beta                 95.257(2)
_cell_angle_gamma                94.091(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8207(2)
_cell_length_b                   11.4820(2)
_cell_length_c                   12.1835(3)
_cell_measurement_reflns_used    14686
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.5230
_cell_measurement_theta_min      3.4350
_cell_volume                     1031.35(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.8117
_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     -2.00  48.00   0.50    2.00    --    3.51-115.00 131.00  100
  2  \w     -8.00  66.00   0.50    2.00    --    3.51  57.00  90.00  148
  3  \w     -8.00  66.00   0.50    2.00    --    3.51  57.00 -30.00  148
  4  \w      0.00  70.00   0.50    2.00    --    3.51  37.00-120.00  140
  5  \w     -8.00  66.00   0.50    2.00    --    3.51  57.00-150.00  148
  6  \w    -27.00  21.00   0.50    2.00    --   -4.14  77.00-150.00   96
  7  \w    -27.00  21.00   0.50    2.00    --   -4.14  77.00-120.00   96
  8  \w    -15.00  32.00   0.50    2.00    --   -4.14 -99.00 150.00   94
  9  \w    -27.00  21.00   0.50    2.00    --   -4.14  77.00 -60.00   96
 10  \w    -10.00  25.00   0.50    2.00    --   -4.14  19.00-180.00   70
;
_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      0.0026582000
_diffrn_orient_matrix_UB_12      0.0291953000
_diffrn_orient_matrix_UB_13      0.0606405000
_diffrn_orient_matrix_UB_21      -0.0909187000
_diffrn_orient_matrix_UB_22      -0.0127366000
_diffrn_orient_matrix_UB_23      -0.0044835000
_diffrn_orient_matrix_UB_31      0.0106918000
_diffrn_orient_matrix_UB_32      -0.0569525000
_diffrn_orient_matrix_UB_33      0.0098567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18484
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.322
_diffrn_reflns_theta_min         3.341
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0266P)^2^+0.5338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4655
_reflns_number_total             5027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           ZnACP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_database_code               7249009
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C32 H28 Cl8 N16 Zn2 '
_chemical_oxdiff_usercomment     'COLOURLESS BLOCKS'
_shelx_estimated_absorpt_t_max   0.735
_shelx_estimated_absorpt_t_min   0.682
_diffrn_oxdiff_digest_frames
;
01679abb1f5c6134b664c7463849077e76000268e8b
;
_diffrn_oxdiff_digest_hkl
;
0114970d96d5535d5ec3ff9d231c6e16866595
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C10'(H10C,H10D)
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              4929
_shelx_hkl_checksum              97740
_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 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.680