Effect of Bromine Substitution on Blue Phosphorescent trans-(N-Heterocyclic Carbene)Pt(II) Acetylide Complexes
Khan, Amran; Gobeze, Habtom B.; Islam, Tanjila; Arman, Hadi; Schanze, Kirk; Dalton Transactions  (2023) –; doi:10.1039/D3DT01483E

data_7713487
_publ_section_title
;
 Effect of Bromine Substitution on Blue Phosphorescent
 trans-(N-Heterocyclic Carbene)Pt(II) Acetylide Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01483E
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C46 H54 Br4 N4 Pt'
_chemical_formula_sum            'C46 H54 Br4 N4 Pt'
_chemical_formula_weight         1177.660
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_audit_creation_date             2022-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-05-17 deposited with the CCDC.	2023-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 148.017(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6051(12)
_cell_length_b                   28.2889(3)
_cell_length_c                   12.9480(7)
_cell_measurement_reflns_used    38201
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9330
_cell_measurement_theta_min      3.1340
_cell_volume                     4385.6(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9855
_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    -94.00 -19.00   0.50    0.16    --  -46.62 136.00 -57.00  150
  2  \w   -119.00 -69.00   0.50    0.16    --  -46.62-132.00  55.00  100
  3  \w    -91.00 -17.00   0.50    0.16    --  -46.62 132.00 124.00  148
  4  \w   -119.00 -66.00   0.50    0.16    --  -46.62-136.00-122.00  106
  5  \w     38.00  99.00   0.50    0.16    --   46.62-132.00  55.00  122
  6  \w     41.00 102.00   0.50    0.16    --   46.62-136.00-122.00  122
  7  \w    -91.00 -17.00   0.50    0.66    --  -88.50 132.00 124.00  148
  8  \w   -160.00 -69.00   0.50    0.66    --  -88.50-132.00  55.00  182
  9  \w    -94.00 -19.00   0.50    0.66    --  -88.50 136.00 -57.00  150
 10  \w   -159.00 -66.00   0.50    0.66    --  -88.50-136.00-122.00  186
 11  \w     41.00 120.00   0.50    0.66    --  106.69-136.00-122.00  158
 12  \w     88.00 178.00   0.50    0.66    --  106.69 136.00 -57.00  180
 13  \w     91.00 178.00   0.50    0.66    --  106.69 132.00 124.00  174
 14  \w     38.00 117.00   0.50    0.66    --  106.69-132.00  55.00  158
 15  \w   -119.00 -83.00   0.50    0.16    --  -46.62 -57.00   0.00   72
 16  \w   -119.00 -83.00   0.50    0.16    --  -46.62 -57.00  60.00   72
 17  \w    -30.00  29.00   0.50    0.16    --  -46.62  19.00-120.00  118
 18  \w    -86.00 -13.00   0.50    0.16    --  -46.62 125.00  90.00  146
 19  \w   -119.00 -83.00   0.50    0.16    --  -46.62 -57.00 -30.00   72
 20  \w   -119.00 -83.00   0.50    0.16    --  -46.62 -57.00  90.00   72
 21  \w   -119.00 -88.00   0.50    0.16    --  -46.62-125.00 120.00   62
 22  \w     83.00 120.00   0.50    0.16    --   46.62  57.00  60.00   74
 23  \w    -51.00 -16.00   0.50    0.66    --  -88.50  45.00  60.00   70
 24  \w   -160.00-101.00   0.50    0.66    --  -88.50 -77.00 -30.00  118
 25  \w   -160.00-101.00   0.50    0.66    --  -88.50 -77.00   0.00  118
 26  \w    -51.00 -16.00   0.50    0.66    --  -88.50  45.00-180.00   70
 27  \w   -160.00 -73.00   0.50    0.66    --  -88.50 -52.00 111.13  174
 28  \w    -51.00 -16.00   0.50    0.66    --  -88.50  45.00  90.00   70
 29  \w    -51.00 -16.00   0.50    0.66    --  -88.50  45.00 -30.00   70
 30  \w     34.00  71.00   0.50    0.66    --  106.69 -61.00 -60.00   74
 31  \w     91.00 178.00   0.50    0.66    --  106.69  30.00  60.00  174
 32  \w    101.00 178.00   0.50    0.66    --  106.69  77.00-180.00  154
 33  \w     89.00 178.00   0.50    0.66    --  106.69  15.00 -30.00  178
 34  \w     91.00 178.00   0.50    0.66    --  106.69  30.00-120.00  174
 35  \w     34.00  71.00   0.50    0.66    --  106.69 -61.00 -90.00   74
 36  \w     34.00 105.00   0.50    0.66    --  106.69 -94.00  60.00  142
 37  \w     34.00 101.00   0.50    0.66    --  106.69 -77.00-120.00  134
 38  \w     34.00 111.00   0.50    0.66    --  106.69-125.00 -90.00  154
 39  \w     95.00 178.00   0.50    0.66    --  106.69 125.00   0.00  166
 40  \w     34.00 111.00   0.50    0.66    --  106.69-125.00-180.00  154
 41  \w     34.00 101.00   0.50    0.66    --  106.69 -77.00  60.00  134
 42  \w     34.00 108.00   0.50    0.66    --  106.69-112.00 122.24  148
 43  \w     34.00  71.00   0.50    0.66    --  106.69 -61.00  90.00   74
 44  \w     34.00  71.00   0.50    0.66    --  106.69 -61.00  30.00   74
 45  \w     34.00 111.00   0.50    0.66    --  106.69-125.00   0.00  154
 46  \w     34.00  71.00   0.50    0.66    --  106.69 -61.00-120.00   74
 47  \w   -122.00 -31.00   0.50    0.16    --  -46.62 -19.00 120.00  182
 48  \w     31.00 120.00   0.50    0.16    --   46.62  55.00-124.30  178
 49  \w     31.00 120.00   0.50    0.16    --   46.62  54.00  43.82  178
 50  \w     31.00 120.00   0.50    0.16    --   46.62  54.00 -81.38  178
 51  \w     31.00 120.00   0.50    0.16    --   46.62  54.00  87.47  178
 52  \w     31.00 120.00   0.50    0.16    --   46.62  53.00 -26.05  178
 53  \w     31.00 120.00   0.50    0.16    --   46.62  54.00  11.23  178
 54  \w     31.00 120.00   0.50    0.16    --   46.62  55.00 115.82  178
 55  \w     31.00 120.00   0.50    0.16    --   46.62  53.00-169.83  178
 56  \w     31.00 120.00   0.50    0.16    --   46.62  55.00 151.02  178
 57  \w   -160.00 -78.00   0.50    0.66    --  -88.50 -51.00   5.23  164
 58  \w   -160.00 -73.00   0.50    0.66    --  -88.50 -52.00 151.56  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9855
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14040
_diffrn_reflns_point_group_measured_fraction_full 0.8939
_diffrn_reflns_point_group_measured_fraction_max 0.8526
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.77
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    10.530
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.989
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       plank
_exptl_crystal_F_000             2281.774
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.043
_refine_diff_density_max         3.3190
_refine_diff_density_min         -1.2521
_refine_diff_density_rms         0.1157
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.2751(14)
_refine_ls_d_res_high            0.7919
_refine_ls_d_res_low             14.1445
_refine_ls_goodness_of_fit_ref   1.0468
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    88
_refine_ls_number_parameters     497
_refine_ls_number_reflns         14040
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0468
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          -0.0973
_refine_ls_shift/su_mean         0.0036
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+36.7044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         1.631
_reflns_limit_h_max              28
_reflns_limit_h_min              -26
_reflns_limit_k_max              35
_reflns_limit_k_min              -35
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                13964
_reflns_number_total             14040
_reflns_threshold_expression     I>=2u(I)
_twin_special_details
;
Component 2 rotated by -179.9722\% 
 around [-0.89 -0.00 0.45] (reciprocal) or [-0.99 0.00 0.16] (direct)
;
_cod_data_source_file            d3dt01483e2.cif
_cod_data_source_block           hpd290c_twin1_hklf4
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               7713487
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5372(17)
 0.4628(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C25(H25), C10(H10), C19(H19), C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C29(H29a,H29b), C26(H26a,H26b), C23(H23a,H23b), C21(H21a,
 H21b), C22(H22a,H22b), C6(H6a,H6b), C30(H30a,H30b), C28(H28a,H28b), C24(H24a,
 H24b), C27(H27a,H27b), C14(H14a,H14b), C13(H13a,H13b), C12(H12a,H12b), C9(H9a,
 H9b), C20(H20a,H20b), C7(H7a,H7b), C5(H5a,H5b), C8(H8a,H8b), C15(H15a,H15b)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C44(H44), C34(H34), C46(H46), C38(H38), C18(H18), C42(H42),
 C17(H17), C2(H2), C3(H3)
;
_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
;