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_7249011
_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 H10 Cl4 N8 Zn, C6 H5 Cl N4'
_chemical_formula_sum            'C18 H15 Cl5 N12 Zn'
_chemical_formula_weight         642.04
_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                102.553(3)
_cell_angle_beta                 90.641(3)
_cell_angle_gamma                108.110(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9888(2)
_cell_length_b                   10.2584(4)
_cell_length_c                   18.2501(6)
_cell_measurement_reflns_used    13054
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.4510
_cell_measurement_theta_min      3.6690
_cell_volume                     1209.50(8)
_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    '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 0.9977
_diffrn_measured_fraction_theta_max 0.8371
_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      1.00  54.00   0.50    2.00    --    6.67-119.00 -90.00  106
  2  \w     23.00  75.00   0.50    2.00    --    6.67-157.00 114.00  104
  3  \w      4.00  73.00   0.50    2.00    --    6.67  37.00   0.00  138
  4  \w    -42.00  16.00   0.50    2.00    --   -7.30 -77.00 150.00  116
  5  \w    -77.00  -1.00   0.50    2.00    --   -7.30 -19.00-150.00  152
  6  \w    -56.00   4.00   0.50    2.00    --   -7.30 -57.00   0.00  120
  7  \w    -24.00  16.00   0.50    2.00    --   -7.30 -77.00  90.00   80
  8  \w     -7.00  55.00   0.50    2.00    --   -7.30  37.00-150.00  124
  9  \w    -41.00   2.00   0.50    2.00    --   -7.30 -77.00 -90.00   86
 10  \w    -31.00  12.00   0.50    2.00    --   -7.30 -77.00 -30.00   86
 11  \w    -27.00  13.00   0.50    2.00    --   -7.30  77.00-120.00   80
 12  \w    -19.00  40.00   0.50    2.00    --   -7.30  57.00  90.00  118
;
_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      0.0710229000
_diffrn_orient_matrix_UB_12      0.0167338000
_diffrn_orient_matrix_UB_13      -0.0267531000
_diffrn_orient_matrix_UB_21      0.0709524000
_diffrn_orient_matrix_UB_22      0.0483468000
_diffrn_orient_matrix_UB_23      0.0292614000
_diffrn_orient_matrix_UB_31      0.0375034000
_diffrn_orient_matrix_UB_32      -0.0545586000
_diffrn_orient_matrix_UB_33      0.0049962000
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.523
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62837
_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    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0291P)^2^+0.4662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5412
_reflns_number_total             6767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           ZnMCP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_original_cell_volume        1209.49(7)
_cod_database_code               7249011
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N Cl Zn O'
_chemical_oxdiff_usercomment     'COLOURLESS BLOCK'
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.653
_diffrn_oxdiff_digest_frames
;
01a9ba8e4da903250a2881db7afc7ad5bc00026c29b
;
_diffrn_oxdiff_digest_hkl
;
01c55eea311b47602e1056cc84a2bb5dbf921c
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C2'(H2'), C8(H8), C8'(H8'), C2"(H2"), C8"(H8")
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C10'(H10D,H10E,H10F), C10"(H10G,H10H,H10I)
;
_shelx_res_checksum              32043
_shelx_hkl_checksum              47108
_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 1.889
_oxdiff_exptl_absorpt_empirical_full_min 0.661