Luminescence in the Solid State of Phosphine-EWO Ligands with Fluorinated Chalcone Skeletons and their PdX2 complexes. Metal-promoted Phosphorescence Enhancement
Ponce-de-León, Jaime; Peñas-Defrutos, Marconi N.; Vélez Blasco, Andrea; Aullon, Gabriel; Espinet, Pablo; Dalton Transactions  (2023) –; doi:10.1039/D3DT00408B

data_7712281
_publ_section_title
;
 Luminescence in the Solid State of Phosphine-EWO Ligands with Fluorinated
 Chalcone Skeletons and their PdX2 complexes. Metal-promoted
 Phosphorescence Enhancement
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00408B
_journal_year                    2023
_chemical_formula_moiety         'C42 H42 Cl2 F8 O2 P2 Pd, C6 H14'
_chemical_formula_sum            'C48 H56 Cl2 F8 O2 P2 Pd'
_chemical_formula_weight         1056.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2023-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                74.065(5)
_cell_angle_beta                 70.863(5)
_cell_angle_gamma                78.505(5)
_cell_formula_units_Z            1
_cell_length_a                   9.5648(5)
_cell_length_b                   11.8739(7)
_cell_length_c                   11.8921(8)
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    294
_cell_measurement_theta_max      25.4210
_cell_measurement_theta_min      3.6270
_cell_volume                     1218.03(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.807
_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    -36.00  56.00   1.00   12.40    --  -10.64  57.00 120.00   92
  2  \w    -82.00  12.00   1.00   12.40    --  -10.64 -57.00 -30.00   94
  3  \w     35.00 101.00   1.00   12.40    --   12.20 178.00 -30.00   66
;
_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      -0.0088543000
_diffrn_orient_matrix_UB_12      0.0556061000
_diffrn_orient_matrix_UB_13      -0.0402652000
_diffrn_orient_matrix_UB_21      -0.0279927000
_diffrn_orient_matrix_UB_22      0.0272592000
_diffrn_orient_matrix_UB_23      0.0504462000
_diffrn_orient_matrix_UB_31      0.0734169000
_diffrn_orient_matrix_UB_32      0.0089923000
_diffrn_orient_matrix_UB_33      -0.0058534000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8436
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.629
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0367P)^2^+0.2077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4239
_reflns_number_total             5555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00408b3.cif
_cod_data_source_block           1-L3
_cod_original_cell_volume        1218.03(14)
_cod_database_code               7712281
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C40 H30 Cl2 F3 O P2 Pd'
_chemical_oxdiff_usercomment     yellow
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.909
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C52-C53
 1.6 with sigma of 0.02
 C51-C52
 1.6 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C31(H31), C41(H41)
3.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
3.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C53(H53B,H53A,H53C)
;
_shelx_res_checksum              5674
_shelx_hkl_checksum              29308
_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 1.392
_oxdiff_exptl_absorpt_empirical_full_min 0.798