X/Y Platinum(II) complexes: some features of supramolecular assembly via halogen bonding
Gitlina, Anastasiia Yu.; Petrovskii, Stanislav; Luginin, Maksim; Melnikov, Alexei S.; Rychagova, Elena A.; Ketkov, Sergey Yu.; Grachova, Elena V.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02970K

data_7714133
_publ_section_title
;
 X/Y Platinum(II) complexes: some features of supramolecular assembly via
 halogen bonding
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02970K
_journal_year                    2023
_chemical_formula_moiety         'C18 H12 Br I N2 Pt S'
_chemical_formula_sum            'C18 H12 Br I N2 Pt S'
_chemical_formula_weight         690.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-08-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-18 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.48680(10)
_cell_length_b                   18.57310(10)
_cell_length_c                   16.48480(10)
_cell_measurement_reflns_used    107889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.9830
_cell_measurement_theta_min      2.6360
_cell_volume                     7191.04(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -118.00 -36.00   0.50    0.30    --  -47.35 -51.00  -2.00  164
  2  \w   -107.00 -34.00   0.50    1.00    -- -106.00 106.00  11.00  146
  3  \w   -159.00 -92.00   0.50    1.00    -- -106.00 -51.00  -2.00  134
  4  \w     44.00  92.00   0.50    1.00    --  113.25 -75.00 157.00   96
  5  \w    -24.00   1.00   0.50    0.30    --  -47.35  19.00 -60.00   50
  6  \w   -114.00 -82.00   0.50    0.30    --  -47.35-125.00 150.00   64
  7  \w     75.00 117.00   0.50    0.30    --   47.35 125.00 -90.00   84
  8  \w    -26.00   1.00   0.50    0.30    --   47.35 -19.00-180.00   54
  9  \w    -70.00 -35.00   0.50    1.00    -- -106.00  61.00-120.00   70
 10  \w    -71.00 -46.00   0.50    1.00    -- -106.00  61.00 -60.00   50
 11  \w    -75.00 -36.00   0.50    1.00    -- -106.00 125.00-150.00   78
 12  \w     43.00  68.00   0.50    1.00    --  113.25 -61.00 120.00   50
 13  \w    110.00 165.00   0.50    1.00    --  113.25  30.00  90.00  110
 14  \w     55.00  96.00   0.50    1.00    --  113.25 -77.00 -60.00   82
 15  \w     42.00  67.00   0.50    1.00    --  113.25 -61.00 -30.00   50
 16  \w     46.00  71.00   0.50    1.00    --  113.25 -61.00-150.00   50
 17  \w      2.00  57.00   0.50    0.30    --   47.35 -51.00  -2.00  110
 18  \w   -119.00 -79.00   0.50    0.30    --  -47.35 -37.00-180.00   80
 19  \w    -95.00 -32.00   0.50    0.30    --  -47.35 -57.00 -90.00  126
 20  \w    -26.00  26.00   0.50    0.30    --  -47.35  37.00 150.00  104
 21  \w     74.00 109.00   0.50    0.30    --   47.35 125.00  60.00   70
 22  \w     34.00  78.00   0.50    0.30    --   47.35  57.00 -60.00   88
 23  \w     94.00 119.00   0.50    0.30    --   47.35  57.00 -60.00   50
 24  \w    -24.00  13.00   0.50    0.30    --   47.35 -19.00-150.00   74
 25  \w     83.00 119.00   0.50    0.30    --   47.35 125.00-150.00   72
 26  \w   -162.00-136.00   0.50    1.00    -- -106.00 -94.00  90.00   52
 27  \w    -63.00 -37.00   0.50    1.00    -- -106.00  61.00 150.00   52
 28  \w   -113.00 -84.00   0.50    1.00    -- -106.00 -94.00  90.00   58
 29  \w   -109.00 -83.00   0.50    1.00    -- -106.00 -77.00-101.99   52
 30  \w   -108.00 -83.00   0.50    1.00    -- -106.00 -77.00 -81.76   50
 31  \w   -177.00 -92.00   0.50    1.00    -- -106.00 -61.00-150.00  170
 32  \w   -121.00 -93.00   0.50    1.00    -- -106.00 -30.00 -90.00   56
 33  \w   -139.00 -92.00   0.50    1.00    -- -106.00 -48.00-125.70   94
 34  \w    -70.00 -38.00   0.50    1.00    -- -106.00  61.00 120.00   64
 35  \w   -115.00 -89.00   0.50    1.00    -- -106.00 -61.00 -58.93   52
 36  \w   -125.00 -94.00   0.50    1.00    -- -106.00 -49.00 -85.10   62
 37  \w   -110.00 -84.00   0.50    1.00    -- -106.00 -77.00 -90.00   52
 38  \w   -172.00-136.00   0.50    1.00    -- -106.00 -61.00 -58.93   72
 39  \w   -118.00 -92.00   0.50    1.00    -- -106.00 -50.00 -77.93   52
 40  \w   -109.00 -83.00   0.50    1.00    -- -106.00 -78.00 -91.52   52
 41  \w   -166.00-140.00   0.50    1.00    -- -106.00 -77.00 -81.76   52
 42  \w   -175.00-149.00   0.50    1.00    -- -106.00 -72.00 -71.85   52
 43  \w   -105.00 -79.00   0.50    1.00    -- -106.00 -90.00 -92.43   52
 44  \w   -110.00 -85.00   0.50    1.00    -- -106.00 -72.00 -71.85   50
 45  \w   -108.00 -83.00   0.50    1.00    -- -106.00 -77.00 -60.00   50
 46  \w    -97.00 -72.00   0.50    1.00    -- -106.00 125.00-120.00   50
 47  \w    -60.00 -34.00   0.50    1.00    -- -106.00 125.00-120.00   52
 48  \w   -177.00-145.00   0.50    1.00    -- -106.00 -77.00-120.00   64
 49  \w    -80.00 -34.00   0.50    1.00    -- -106.00  77.00-120.00   92
 50  \w   -177.00-100.00   0.50    1.00    -- -106.00 -61.00-120.00  154
 51  \w   -116.00 -91.00   0.50    1.00    -- -106.00 -58.00 -69.41   50
 52  \w   -173.00-121.00   0.50    1.00    -- -106.00 -58.00 -69.41  104
 53  \w   -109.00 -84.00   0.50    1.00    -- -106.00 -75.00 -77.62   50
 54  \w    -67.00 -38.00   0.50    1.00    -- -106.00  61.00-180.00   58
 55  \w   -148.00 -90.00   0.50    1.00    -- -106.00 -59.00-131.30  116
 56  \w   -109.00 -84.00   0.50    1.00    -- -106.00 -77.00-120.00   50
 57  \w   -177.00-117.00   0.50    1.00    -- -106.00 -45.00 -30.00  120
 58  \w   -112.00 -87.00   0.50    1.00    -- -106.00 -67.00-136.01   50
 59  \w   -112.00 -87.00   0.50    1.00    -- -106.00 -67.00-106.48   50
 60  \w   -117.00 -92.00   0.50    1.00    -- -106.00 -15.00 -90.00   50
 61  \w   -108.00 -83.00   0.50    1.00    -- -106.00 -78.00 -84.19   50
 62  \w   -121.00 -96.00   0.50    1.00    -- -106.00 -45.00-150.00   50
 63  \w   -124.00 -90.00   0.50    1.00    -- -106.00 -60.00 -82.73   68
 64  \w   -176.00-131.00   0.50    1.00    -- -106.00 -61.00 -90.00   90
 65  \w   -127.00 -90.00   0.50    1.00    -- -106.00 -61.00 -90.00   74
 66  \w     52.00 100.00   0.50    1.00    --  113.25 -77.00 -30.00   96
 67  \w     71.00  97.00   0.50    1.00    --  113.25 -94.00 150.00   52
 68  \w    144.00 171.00   0.50    1.00    --  113.25  61.00 -90.00   54
 69  \w     44.00  69.00   0.50    1.00    --  113.25 -61.00 -60.00   50
 70  \w     43.00  84.00   0.50    1.00    --  113.25 -77.00  60.00   82
 71  \w    133.00 176.00   0.50    1.00    --  113.25  45.00  60.00   86
 72  \w     43.00  69.00   0.50    1.00    --  113.25 -61.00  90.00   52
 73  \w     42.00  67.00   0.50    1.00    --  113.25 -61.00-120.00   50
 74  \w    131.00 176.00   0.50    1.00    --  113.25  61.00  30.00   90
 75  \w    102.00 129.00   0.50    1.00    --  113.25  45.00  60.00   54
 76  \w    149.00 174.00   0.50    1.00    --  113.25  61.00 -60.00   50
 77  \w    148.00 173.00   0.50    1.00    --  113.25 125.00  90.00   50
 78  \w     80.00 131.00   0.50    1.00    --  113.25 125.00  90.00  102
 79  \w     43.00  82.00   0.50    1.00    --  113.25-125.00 150.00   78
 80  \w    111.00 160.00   0.50    1.00    --  113.25  30.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0404878000
_diffrn_orient_matrix_UB_12      0.0708879000
_diffrn_orient_matrix_UB_13      0.0171014000
_diffrn_orient_matrix_UB_21      0.0357707000
_diffrn_orient_matrix_UB_22      -0.0563040000
_diffrn_orient_matrix_UB_23      0.0483711000
_diffrn_orient_matrix_UB_31      0.0372196000
_diffrn_orient_matrix_UB_32      -0.0231834000
_diffrn_orient_matrix_UB_33      -0.0651603000
_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  0.1178
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            128082
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.489
_diffrn_reflns_theta_max         67.489
_diffrn_reflns_theta_min         3.033
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    31.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.550
_exptl_crystal_description       prism
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.568
_refine_diff_density_min         -7.071
_refine_diff_density_rms         0.412
_refine_ls_abs_structure_details
;
 Flack x determined using 5504 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.492(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12891
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          12.343
_refine_ls_shift/su_mean         0.147
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0829P)^2^+454.5717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                12810
_reflns_number_total             12891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02970k3.cif
_cod_data_source_block           0ver0-21856_cwo-pt4br
_cod_database_code               7714133
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C19 H12 Br I N2 S Pt'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12D(H12D), C11A(H11A), C1A(H1A), C1B(H1B), C11B(H11B), C2D(H2D), C4A(H4A),
 C12A(H12A), C10C(H10C), C3A(H3A), C9C(H9C), C11D(H11D), C5D(H5D), C2C(H2C),
 C5C(H5C), C6A(H6A), C4C(H4C), C8D(H8D), C4B(H4B), C5A(H5A), C11C(H11C),
 C9D(H9D), C12C(H12C), C1C(H1C), C8B(H8B), C5B(H5B), C2A(H2A), C10A(H10A),
 C12B(H12B), C3B(H3B), C10D(H10D), C6C(H6C), C2B(H2B), C3D(H3D), C8C(H8C),
 C4D(H4D), C7A(H7A), C7B(H7B), C10B(H10B), C1D(H1D), C6B(H6B), C8A(H8A),
 C9A(H9A), C7C(H7C), C7D(H7D), C3C(H3C), C9B(H9B), C6D(H6D)
;
_shelx_res_checksum              96909
_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 2.755
_oxdiff_exptl_absorpt_empirical_full_min 0.423