Highly luminescent palladium(ii) complexes with sub-millisecond blue to green phosphorescent excited states. Photocatalysis and highly efficient PSF-OLEDs
Chow, Pui-Keong; Cheng, Gang; Tong, Glenna So Ming; Ma, Chensheng; Kwok, Wai-Ming; Ang, Wai-Hung; Chung, Clive Yik-Sham; Yang, Chen; Wang, Feng; Che, Chi-Ming; Chem. Sci. 7 (2016) 6083–; doi:10.1039/C6SC00462H

data_1543440
_publ_section_title
;
 Highly luminescent palladium(ii) complexes with sub-millisecond blue to
 green phosphorescent excited states. Photocatalysis and highly efficient
 PSF-OLEDs
;
_journal_issue                   9
_journal_name_full               'Chem. Sci.'
_journal_page_first              6083
_journal_paper_doi               10.1039/C6SC00462H
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C43 H36 F2 N2 O Pd'
_chemical_formula_sum            'C43 H36 F2 N2 O Pd'
_chemical_formula_weight         741.14
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/cc1kn029
_audit_creation_date             2015-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2016-01-22 deposited with the CCDC.
2016-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4424(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2388(13)
_cell_length_b                   14.5866(13)
_cell_length_c                   15.9868(14)
_cell_measurement_reflns_used    9460
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.96
_cell_measurement_theta_min      4.28
_cell_volume                     3408.3(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39920
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.107
_diffrn_reflns_theta_min         3.538
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.781
_exptl_absorpt_correction_T_max  0.7300
_exptl_absorpt_correction_T_min  0.5883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1390 before and 0.1145 after correction.
The Ratio of minimum to maximum transmission is 0.8059.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0709P)^2^+2.1032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5863
_reflns_number_total             6015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00462h2.cif
_cod_data_source_block           SamsonPd1
_cod_depositor_comments
'Adding full bibliography for 1543439--1543440.cif.'
_cod_database_code               1543440
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.646
_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. Restrained distances
 C39-C38 \\sim C40-C38 \\sim C41-C38 \\sim C39A-C38A \\sim C41A-C38A \\sim
C40A-C38A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41) = Uanis(C40A)
Uanis(C40) = Uanis(C41A)
Uanis(C39) = Uanis(C39A)
Uanis(C38) = Uanis(C38A)
4. Others
 Sof(C38A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(C38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C13(H13), C14(H14), C15(H15),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C31(H31), C32(H32), C35(H35),
  C36(H36), C42(H42)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C39A(H39D,H39E,H39F),
 C40A(H40D,H40E,H40F), C41A(H41D,H41E,H41F)
;
_olex2_submission_special_instructions 'No special instructions were received'