Palladium mono-<i>N</i>-protected amino acid complexes: experimental validation of the ligand cooperation model in C-H activation.
Fernández-Moyano, Sara; Salamanca, Vanesa; Albéniz, Ana C; Chemical science 14 (2023) 6688–6694; doi:10.1039/d3sc02076b

data_1569225
_publ_section_title
;
 Palladium mono-<i>N</i>-protected amino acid complexes: experimental
 validation of the ligand cooperation model in C-H activation.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6688
_journal_page_last               6694
_journal_paper_doi               10.1039/d3sc02076b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C14 H11 F5 N2 O2 Pd'
_chemical_formula_sum            'C14 H10 F5 N2 O2 Pd'
_chemical_formula_weight         439.64
_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             2021-12-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                107.490(6)
_cell_angle_beta                 107.025(6)
_cell_angle_gamma                100.307(6)
_cell_formula_units_Z            4
_cell_length_a                   10.0930(7)
_cell_length_b                   11.7688(8)
_cell_length_c                   14.7684(9)
_cell_measurement_reflns_used    3718
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      26.8100
_cell_measurement_theta_min      4.0380
_cell_volume                     1529.8(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.816
_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    -34.00  62.00   1.00   18.83    --  -10.64  57.00 -30.00   96
  2  \w    -76.00  15.00   1.00   18.83    --  -10.64 -57.00-180.00   91
  3  \w     35.00 101.00   1.00   18.83    --   12.51 178.00-180.00   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      -0.0372833000
_diffrn_orient_matrix_UB_12      0.0425935000
_diffrn_orient_matrix_UB_13      0.0170026000
_diffrn_orient_matrix_UB_21      0.0314203000
_diffrn_orient_matrix_UB_22      0.0403527000
_diffrn_orient_matrix_UB_23      -0.0202854000
_diffrn_orient_matrix_UB_31      -0.0594195000
_diffrn_orient_matrix_UB_32      -0.0304079000
_diffrn_orient_matrix_UB_33      -0.0472826000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10727
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.596
_diffrn_reflns_theta_min         3.522
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.651
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0357P)^2^+0.1994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5081
_reflns_number_total             7020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02076b2.cif
_cod_data_source_block           exp_576
_cod_depositor_comments
'Adding full bibliography for 1569224--1569228.cif.'
_cod_original_cell_volume        1529.75(19)
_cod_database_code               1569225
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C14 H10 F5 N2 O2 Pd'
_chemical_oxdiff_usercomment     'colourless block'
_reflns_odcompleteness_completeness 98.55
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N00C(H00C), N00F(H00g)
2.b Secondary CH2 refined with riding coordinates:
 C00M(H00a,H00b), C00N(H00h,H00i)
2.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00Q(H00Q), C00T(H00T), C00V(H00V), C00X(H00X), C010(H010),
 C011(H011), C017(H017), C018(H018), C019(H019)
2.d Idealised Me refined as rotating group:
 C00R(H00d,H00e,H00f), C00Z(H00j,H00k,H00l)
;
_shelx_res_checksum              9185
_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 2.002
_oxdiff_exptl_absorpt_empirical_full_min 0.654