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_7712282
_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         'C54 H58 Cl2 F8 O2 P2 Pd, 2(C3 H6 O)'
_chemical_formula_sum            'C60 H70 Cl2 F8 O4 P2 Pd'
_chemical_formula_weight         1246.40
_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     iterative
_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                74.659(4)
_cell_angle_beta                 89.730(4)
_cell_angle_gamma                88.099(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9875(4)
_cell_length_b                   10.2176(3)
_cell_length_c                   15.2240(8)
_cell_measurement_reflns_used    4041
_cell_measurement_temperature    209.9(6)
_cell_measurement_theta_max      27.1310
_cell_measurement_theta_min      3.9870
_cell_volume                     1497.39(11)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      209.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.804
_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    -20.00  53.00   1.00   25.72    --   12.20 -99.00  90.00   73
  2  \w    -15.00  80.00   1.00   25.72    --   12.20  57.00 -30.00   95
  3  \w    -61.00  38.00   1.00   25.72    --   12.20 -57.00-180.00   99
;
_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      0.0255889000
_diffrn_orient_matrix_UB_12      0.0148071000
_diffrn_orient_matrix_UB_13      -0.0449741000
_diffrn_orient_matrix_UB_21      -0.0652896000
_diffrn_orient_matrix_UB_22      -0.0039740000
_diffrn_orient_matrix_UB_23      -0.0170433000
_diffrn_orient_matrix_UB_31      -0.0114791000
_diffrn_orient_matrix_UB_32      0.0703731000
_diffrn_orient_matrix_UB_33      -0.0045808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10840
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.755
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       cube
_exptl_crystal_F_000             644
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0345P)^2^+0.7179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5228
_reflns_number_total             6875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00408b3.cif
_cod_data_source_block           1-L2
_cod_database_code               7712282
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C27 H29 Cl2 F4 O P Pd'
_chemical_oxdiff_usercomment     colourless
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.894
_reflns_odcompleteness_completeness 98.97
_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.a Ternary CH refined with riding coordinates:
 C31(H31), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              65879
_shelx_hkl_checksum              49949
_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.819