Isoelectronic Pt(II) Complexes of Cyclometalating C^N^N Ligands with Phenyl/(Benzo)thiophenyl and Pyridyl/(Benzo)thiazolyl Moieties
Krause, Maren; Friedel, Joshua; Buss, Stefan; Bruenkink, Dana; Berger, Annemarie; Strassert, Cristian Alejandro; Doltsinis, Nikos; Klein, Axel; Dalton Transactions  (2022) –; doi:10.1039/D2DT02688K

data_7711373
_publ_section_title
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 Isoelectronic Pt(II) Complexes of Cyclometalating C^N^N Ligands with
 Phenyl/(Benzo)thiophenyl and Pyridyl/(Benzo)thiazolyl Moieties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02688K
_journal_year                    2022
_chemical_formula_moiety         'C40 H36 N2 Pt S'
_chemical_formula_sum            'C40 H36 N2 Pt S'
_chemical_formula_weight         771.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27ynwr
_audit_creation_date             2021-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.192(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1805(4)
_cell_length_b                   37.3146(19)
_cell_length_c                   6.7184(2)
_cell_measurement_reflns_used    5667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6500
_cell_measurement_theta_min      1.7290
_cell_volume                     3252.1(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 360.00   1.00    5.00  90.00  10.00   0.00    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0106031000
_diffrn_orient_matrix_UB_12      0.0145639000
_diffrn_orient_matrix_UB_13      0.0005834000
_diffrn_orient_matrix_UB_21      -0.0408320000
_diffrn_orient_matrix_UB_22      0.0034549000
_diffrn_orient_matrix_UB_23      -0.0339016000
_diffrn_orient_matrix_UB_31      -0.0095130000
_diffrn_orient_matrix_UB_32      0.0013953000
_diffrn_orient_matrix_UB_33      0.0776731000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56076
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.1144
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.720
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            47026
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_theta_full        19.661
_diffrn_reflns_theta_max         27.447
_diffrn_reflns_theta_min         1.508
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48059
_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            orange
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.684
_refine_diff_density_min         -5.115
_refine_diff_density_rms         0.280
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         10871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.1016
_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/[\s^2^(Fo^2^)+101.3431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6373
_reflns_number_total             10871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02688k3.cif
_cod_data_source_block           '[Pt(ph(tbppy)btz)(CCPh)]'
_cod_database_code               7711373
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PtSN2C40H36
_reflns_odcompleteness_completeness 96.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     20.52
_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:
 C24(H24), C18(H18), C8(H8), C5(H5), C10(H10), C38(H38), C2(H2), C20(H20),
 C17(H17), C36(H36), C39(H39), C22(H22), C37(H37), C3(H3), C4(H4), C40(H40),
 C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              83155
_ins_header
;
TITL k203_avarageBG_finalize in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.56076  13.180467  37.314571   6.718448  90.0000 100.1918  90.0000
ZERR    4.00   0.000427   0.001861   0.000218   0.0000   0.0030   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N S Pt
UNIT 160.00 144.00 8.00 4.00 4.00
TREF
HKLF 4
END
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.472
_oxdiff_exptl_absorpt_empirical_full_min 0.619