Crystal engineering with ambidentate thiocyanate: thiocyanate nitrogen as a halogen bond acceptor in platinum(ii) complexes
Antonova, Elina V.; Kashina, Maria V.; Ivanov, Daniil M.; Bokach, Nadezhda A.; Kinzhalov, Mikhail A.; CrystEngComm 27 (2025) 6942–6948; doi:10.1039/D5CE00678C

data_7250973
_publ_section_title
;
 Crystal engineering with ambidentate thiocyanate: thiocyanate nitrogen as
 a halogen bond acceptor in platinum(ii) complexes
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6942
_journal_page_last               6948
_journal_paper_doi               10.1039/D5CE00678C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C19 H11 Br2 N3 Pt S, C H3 N O2'
_chemical_formula_sum            'C20 H14 Br2 N4 O2 Pt S'
_chemical_formula_weight         729.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-02 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.414(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1208(3)
_cell_length_b                   9.1619(3)
_cell_length_c                   25.3184(9)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100.2(4)
_cell_measurement_theta_max      29.1660
_cell_measurement_theta_min      3.3490
_cell_volume                     2113.83(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.102a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.2(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_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    -29.00   4.00   1.00  190.91    --   -9.54 -77.00-180.00   33
  2  \w    -63.00  34.00   1.00  190.91    --   11.41 -38.00 -90.00   97
  3  \w     47.00  77.00   1.00  190.91    --   11.41-143.00  15.00   30
  4  \w     -9.00  19.00   1.00  190.91    --   11.41 -99.00 -30.00   28
  5  \w     18.00  76.00   1.00  190.91    --   11.41  38.00  90.00   58
  6  \w    -22.00  22.00   1.00  190.91    --   -9.54 -77.00  30.00   44
  7  \w    -43.00   3.00   1.00  190.91    --   11.41 -38.00 -90.00   46
  8  \w    -53.00  45.00   1.00  190.91    --   11.41 -19.00  60.00   98
  9  \w     28.00  70.00   1.00  190.91    --   11.41-129.00-173.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0060681000
_diffrn_orient_matrix_UB_12      -0.0523619000
_diffrn_orient_matrix_UB_13      -0.0206069000
_diffrn_orient_matrix_UB_21      -0.0036257000
_diffrn_orient_matrix_UB_22      0.0569990000
_diffrn_orient_matrix_UB_23      -0.0189735000
_diffrn_orient_matrix_UB_31      0.0775149000
_diffrn_orient_matrix_UB_32      -0.0014689000
_diffrn_orient_matrix_UB_33      -0.0013127000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26250
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.490
_diffrn_reflns_theta_min         3.153
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0195P)^2^+4.3169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4268
_reflns_number_total             5135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00678c5.cif
_cod_data_source_block           18192_sev-586_auto
_cod_depositor_comments
'Adding full bibliography for 7250969--7250973.cif.'
_cod_database_code               7250973
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Pt N3 S Br3 C18 H10 '
_shelx_estimated_absorpt_t_max   0.227
_shelx_estimated_absorpt_t_min   0.144
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C8(H8), C15(H15), C17(H17), C18(H18), C11(H11), C3(H3), C9(H9),
 C5(H5), C10(H10), C4(H4)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              17996
_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 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.536