#------------------------------------------------------------------------------
#$Date: 2024-09-06 02:15:56 +0200 (Fri 06 de Sep de 2024) $
#$Revision: 294518 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/90/7249004.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7249004
loop_
_publ_author_name
'Panda, Subhra Jyoti'
'Agrawalla, Suraj Kumar'
'Purohit, Chandra Shekhar'
_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         'C8 H7 Cl3 Hg N4'
_chemical_formula_sum            'C8 H7 Cl3 Hg N4'
_chemical_formula_weight         466.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
;
2024-06-24 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.751(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2883(13)
_cell_length_b                   7.9852(4)
_cell_length_c                   15.3182(8)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      78.2400
_cell_measurement_theta_min      5.9400
_cell_volume                     2465.8(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_environment      N~2~
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9918
_diffrn_measured_fraction_theta_max 0.9590
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -106.00 -20.00   0.50    1.00    --  -38.50 152.00  29.00  172
  2  ω    -85.00  -3.00   0.50    1.00    --  -38.50 121.00-130.00  164
  3  ω     24.00  96.00   0.50    1.00    --   49.56-121.00 146.00  144
  4  ω     81.00 165.00   0.50    2.00    --  107.46 152.00  29.00  168
  5  ω     44.00 110.00   0.50    2.00    --  107.46-121.00 146.00  132
  6  ω     44.00 131.00   0.50    2.00    --  107.46-152.00 -13.00  174
  7  ω     99.00 171.00   0.50    2.00    --  107.46 121.00-130.00  144
  8  ω   -105.00 -35.00   0.50    1.00    --  -38.50 -37.00 -30.00  140
  9  ω    -42.00  28.00   0.50    1.00    --  -38.50  37.00-120.00  140
 10  ω     42.00 109.00   0.50    1.00    --   49.56-152.00 -13.00  134
 11  ω     62.00 113.00   0.50    1.00    --   49.56  57.00-120.00  102
 12  ω    144.00 170.00   0.50    2.00    --  107.46  61.00  30.00   52
 13  ω     46.00  73.00   0.50    2.00    --  107.46-125.00  90.00   54
 14  ω     46.00 121.00   0.50    2.00    --  107.46 -61.00 -90.00  150
 15  ω    132.00 172.00   0.50    2.00    --  107.46  45.00   0.00   80
 16  ω     46.00  77.00   0.50    2.00    --  107.46 -94.00-180.00   62
 17  ω     50.00 131.00   0.50    2.00    --  107.46 -77.00  30.00  162
 18  ω     88.00 113.00   0.50    2.00    --  107.46-125.00  90.00   50
 19  ω     98.00 170.00   0.50    2.00    --  107.46 125.00  60.00  144
 20  ω    105.00 130.00   0.50    2.00    --  107.46  30.00  30.00   50
 21  ω    138.00 175.00   0.50    2.00    --  107.46  30.00  30.00   74
 22  ω     43.00 110.00   0.50    2.00    --  107.46 -45.00  90.00  134
 23  ω    117.00 175.00   0.50    2.00    --  107.46  30.00 150.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0752369000
_diffrn_orient_matrix_UB_12      0.0199441000
_diffrn_orient_matrix_UB_13      0.0468422000
_diffrn_orient_matrix_UB_21      0.0099917000
_diffrn_orient_matrix_UB_22      -0.1878832000
_diffrn_orient_matrix_UB_23      -0.0149083000
_diffrn_orient_matrix_UB_31      0.0081222000
_diffrn_orient_matrix_UB_32      0.0402715000
_diffrn_orient_matrix_UB_33      -0.0940966000
_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  0.0736
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8384
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.708
_diffrn_reflns_theta_min         4.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    28.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39961
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_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          0.18
_refine_diff_density_max         1.733
_refine_diff_density_min         -2.780
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0557
_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/[σ²(Fo²)+(0.0798P)²+107.0663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2340
_reflns_number_total             2555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00341a2.cif
_cod_data_source_block           HgACP
_cod_depositor_comments
'Adding full bibliography for 7249004--7249012.cif.'
_cod_database_code               7249004
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N Cl Hg'
_chemical_oxdiff_usercomment     'LIGHT YELLOW BLOCK'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.081
_shelx_estimated_absorpt_t_min   0.056
_diffrn_oxdiff_ac3_digest_hkl    0129136fc2a11e4d7f8780048212e9d4b3575f
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C11(H11)
2.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B)
;
_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 4.760
_oxdiff_exptl_absorpt_empirical_full_min 0.536
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1 Hg 0.500000 0.000000 0.500000 0.0274(2) Uani 1 2 d S . P . .
Hg2 Hg 0.500000 0.12117(9) 0.750000 0.0283(2) Uani 1 2 d S T P . .
Cl1 Cl 0.71610(19) 0.6648(5) 0.5732(2) 0.0556(10) Uani 1 1 d . . . . .
Cl2 Cl 0.42581(15) 0.0950(4) 0.36071(18) 0.0359(6) Uani 1 1 d . . . . .
Cl3 Cl 0.40924(13) 0.0673(4) 0.61525(16) 0.0319(6) Uani 1 1 d . . . . .
N1 N 0.6188(5) 0.4749(13) 0.4792(7) 0.029(2) Uani 1 1 d . . . . .
N3 N 0.5450(5) 0.3097(13) 0.5381(6) 0.029(2) Uani 1 1 d . . . . .
N7 N 0.6460(5) 0.5359(13) 0.7281(6) 0.032(2) Uani 1 1 d . . . . .
N9 N 0.5633(5) 0.3457(13) 0.7011(6) 0.031(2) Uani 1 1 d . . . . .
C2 C 0.5687(6) 0.3625(15) 0.4724(8) 0.029(2) Uani 1 1 d . . . . .
H2 H 0.548254 0.316160 0.412907 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5783(5) 0.3792(13) 0.6206(7) 0.024(2) Uani 1 1 d . . . . .
C5 C 0.6274(6) 0.4942(13) 0.6359(7) 0.025(2) Uani 1 1 d . . . . .
C6 C 0.6489(6) 0.5345(16) 0.5615(8) 0.033(3) Uani 1 1 d . . . . .
C8 C 0.6053(6) 0.4403(17) 0.7634(8) 0.035(3) Uani 1 1 d . . . . .
H8 H 0.607440 0.442972 0.826357 0.042 Uiso 1 1 calc R U . . .
C10 C 0.6912(7) 0.6658(18) 0.7820(9) 0.048(4) Uani 1 1 d . . . . .
H10A H 0.691783 0.761171 0.740972 0.057 Uiso 1 1 calc R U . . .
H10B H 0.673942 0.707326 0.830775 0.057 Uiso 1 1 calc R U . . .
C11 C 0.7572(7) 0.6079(17) 0.8237(11) 0.047(3) Uani 1 1 d . . . . .
H11 H 0.781451 0.569841 0.785158 0.056 Uiso 1 1 calc R U . . .
C12 C 0.7866(9) 0.605(2) 0.9156(12) 0.066(5) Uani 1 1 d . . . . .
H12A H 0.763110 0.642387 0.955227 0.079 Uiso 1 1 calc R U . . .
H12B H 0.830813 0.565202 0.940958 0.079 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Hg1 Cl2 180.0 5_656 . ?
Cl2 Hg1 N3 89.3(2) . . ?
Cl2 Hg1 N3 89.3(2) 5_656 5_656 ?
Cl2 Hg1 N3 90.7(2) 5_656 . ?
Cl2 Hg1 N3 90.7(2) . 5_656 ?
N3 Hg1 N3 180.0 . 5_656 ?
Cl3 Hg2 Cl3 159.10(16) 2_656 . ?
Cl3 Hg2 N9 91.4(2) 2_656 . ?
Cl3 Hg2 N9 91.4(2) . 2_656 ?
Cl3 Hg2 N9 103.7(2) 2_656 2_656 ?
Cl3 Hg2 N9 103.7(2) . . ?
N9 Hg2 N9 88.3(5) 2_656 . ?
C6 N1 C2 116.1(10) . . ?
C2 N3 Hg1 109.1(7) . . ?
C2 N3 C4 111.4(10) . . ?
C4 N3 Hg1 129.2(7) . . ?
C5 N7 C8 104.9(9) . . ?
C5 N7 C10 131.6(11) . . ?
C8 N7 C10 123.0(11) . . ?
C4 N9 Hg2 134.5(7) . . ?
C8 N9 Hg2 120.0(8) . . ?
C8 N9 C4 103.7(10) . . ?
N1 C2 H2 115.7 . . ?
N3 C2 N1 128.6(11) . . ?
N3 C2 H2 115.7 . . ?
N3 C4 N9 123.2(10) . . ?
N3 C4 C5 125.5(10) . . ?
C5 C4 N9 111.2(10) . . ?
N7 C5 C6 135.9(11) . . ?
C4 C5 N7 107.0(9) . . ?
C4 C5 C6 117.0(11) . . ?
N1 C6 Cl1 116.8(9) . . ?
N1 C6 C5 121.0(12) . . ?
C5 C6 Cl1 122.2(10) . . ?
N7 C8 H8 123.4 . . ?
N9 C8 N7 113.3(10) . . ?
N9 C8 H8 123.4 . . ?
N7 C10 H10A 108.9 . . ?
N7 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 N7 113.3(13) . . ?
C11 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C10 C11 H11 118.8 . . ?
C12 C11 C10 122.4(16) . . ?
C12 C11 H11 118.8 . . ?
C11 C12 H12A 120.0 . . ?
C11 C12 H12B 120.0 . . ?
H12A C12 H12B 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1 Cl2 2.336(3) 5_656 ?
Hg1 Cl2 2.336(3) . ?
Hg1 N3 2.649(10) . ?
Hg1 N3 2.649(10) 5_656 ?
Hg2 Cl3 2.369(2) 2_656 ?
Hg2 Cl3 2.369(2) . ?
Hg2 N9 2.499(10) . ?
Hg2 N9 2.499(10) 2_656 ?
Cl1 C6 1.731(13) . ?
N1 C2 1.372(15) . ?
N1 C6 1.307(16) . ?
N3 C2 1.330(13) . ?
N3 C4 1.354(14) . ?
N7 C5 1.380(14) . ?
N7 C8 1.390(16) . ?
N7 C10 1.474(16) . ?
N9 C4 1.394(13) . ?
N9 C8 1.316(15) . ?
C2 H2 0.9500 . ?
C4 C5 1.354(15) . ?
C5 C6 1.395(15) . ?
C8 H8 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.42(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.35(2) . ?
C12 H12A 0.9500 . ?
C12 H12B 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hg1 N3 C2 N1 -150.2(11) . . . . ?
Hg1 N3 C4 N9 -39.5(15) . . . . ?
Hg1 N3 C4 C5 143.7(9) . . . . ?
Hg2 N9 C4 N3 17.5(17) . . . . ?
Hg2 N9 C4 C5 -165.2(8) . . . . ?
Hg2 N9 C8 N7 168.0(8) . . . . ?
N3 C4 C5 N7 178.0(11) . . . . ?
N3 C4 C5 C6 -5.2(17) . . . . ?
N7 C5 C6 Cl1 1(2) . . . . ?
N7 C5 C6 N1 -178.4(12) . . . . ?
N7 C10 C11 C12 -117.8(16) . . . . ?
N9 C4 C5 N7 0.8(13) . . . . ?
N9 C4 C5 C6 177.6(10) . . . . ?
C2 N1 C6 Cl1 175.5(9) . . . . ?
C2 N1 C6 C5 -4.7(17) . . . . ?
C2 N3 C4 N9 179.8(11) . . . . ?
C2 N3 C4 C5 3.0(16) . . . . ?
C4 N3 C2 N1 -1.5(18) . . . . ?
C4 N9 C8 N7 1.0(14) . . . . ?
C4 C5 C6 Cl1 -174.2(9) . . . . ?
C4 C5 C6 N1 6.0(17) . . . . ?
C5 N7 C8 N9 -0.5(15) . . . . ?
C5 N7 C10 C11 -93.0(16) . . . . ?
C6 N1 C2 N3 2.5(19) . . . . ?
C8 N7 C5 C4 -0.2(13) . . . . ?
C8 N7 C5 C6 -176.1(13) . . . . ?
C8 N7 C10 C11 96.1(17) . . . . ?
C8 N9 C4 N3 -178.3(11) . . . . ?
C8 N9 C4 C5 -1.1(13) . . . . ?
C10 N7 C5 C4 -172.4(13) . . . . ?
C10 N7 C5 C6 12(2) . . . . ?
C10 N7 C8 N9 172.5(12) . . . . ?
