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_7713486
_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_formula_moiety         'C46 H56 Br2 N4 Pt, C2 H4 Cl4'
_chemical_formula_sum            'C48 H60 Br2 Cl4 N4 Pt'
_chemical_formula_weight         1189.71
_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             2020-06-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2023-05-17 deposited with the CCDC.	2023-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.18770(10)
_cell_length_b                   13.2995(2)
_cell_length_c                   15.2041(2)
_cell_measurement_reflns_used    13169
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9450
_cell_measurement_theta_min      4.4040
_cell_volume                     2451.67(5)
_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 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_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     32.00 123.00   0.50    0.05    --   46.87  21.00  39.00  182
  2  \w     92.00 178.00   0.50    0.14    --  106.69  21.00  39.00  172
  3  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00-120.00   74
  4  \w     34.00 105.00   0.50    0.14    --  106.69 -94.00-180.00  142
  5  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00 -60.00   74
  6  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00   0.00   74
  7  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00  30.00   74
  8  \w     40.00  71.00   0.50    0.14    --  106.69 -61.00  90.00   62
  9  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00 120.00   74
 10  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00 150.00   74
 11  \w     34.00 105.00   0.50    0.14    --  106.69 -94.00  90.00  142
 12  \w     35.00  71.00   0.50    0.14    --  106.69 -61.00  60.00   72
 13  \w     36.00  63.00   0.50    0.14    --  106.69 -61.00 -30.00   54
 14  \w     34.00  71.00   0.50    0.14    --  106.69 -61.00 -90.00   74
 15  \w    -28.00  31.00   0.50    0.05    --   46.87 -21.00-126.00  118
 16  \w    -31.00  29.00   0.50    0.05    --  -46.87  21.00  39.00  120
 17  \w    -51.00 -16.00   0.50    0.14    --  -88.50  45.00 -90.00   70
 18  \w    -51.00 -16.00   0.50    0.14    --  -88.50  45.00 -30.00   70
 19  \w    -51.00 -16.00   0.50    0.14    --  -88.50  45.00   0.00   70
 20  \w    -51.00 -16.00   0.50    0.14    --  -88.50  45.00  30.00   70
 21  \w    -71.00 -15.00   0.50    0.14    --  -88.50  61.00 -30.00  112
 22  \w    -51.00 -16.00   0.50    0.14    --  -88.50  45.00-120.00   70
 23  \w   -123.00 -32.00   0.50    0.05    --  -46.87 -21.00-126.00  182
 24  \w    -28.00  30.00   0.50    0.05    --   46.87 -19.00  90.00  116
 25  \w    -27.00  43.00   0.50    0.05    --   46.87 -37.00 120.00  140
 26  \w    -71.00 -15.00   0.50    0.14    --  -88.50  61.00 120.00  112
 27  \w   -120.00 -87.00   0.50    0.05    --  -46.87-125.00   0.00   66
 28  \w   -164.00 -73.00   0.50    0.14    --  -88.50 -21.00-126.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0942689000
_diffrn_orient_matrix_UB_12      0.0230968000
_diffrn_orient_matrix_UB_13      -0.0571810000
_diffrn_orient_matrix_UB_21      0.0851485000
_diffrn_orient_matrix_UB_22      -0.0218038000
_diffrn_orient_matrix_UB_23      0.0796788000
_diffrn_orient_matrix_UB_31      0.0026594000
_diffrn_orient_matrix_UB_32      -0.1114017000
_diffrn_orient_matrix_UB_33      -0.0274941000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23592
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.506
_diffrn_reflns_theta_min         4.427
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method
'Crystals prepared from a solution of hexane and dichloromethane.'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.099
_refine_diff_density_min         -2.028
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0693P)^2^+0.5713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4574
_reflns_number_total             4967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01483e2.cif
_cod_data_source_block           hpd123a
_cod_database_code               7713486
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pt C H'
_chemical_oxdiff_usercomment     AK-67
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C6(H6A,H6B), C15(H15A,H15B), C7(H7A,H7B), C12(H12A,H12B),
 C14(H14A,H14B), C13(H13A,H13B), C9(H9A,H9B), C8(H8A,H8B), C5(H5A,H5B),
 C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C22(H22), C3(H3), C23(H23), C19(H19), C20(H20)
;
_olex2_exptl_crystal_mounting_method 'nylon 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 1.631
_oxdiff_exptl_absorpt_empirical_full_min 0.679