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_1569228
_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         '1.143(C22 H10 F10 N2 Pd)'
_chemical_formula_sum            'C25.14 H11.43 F11.43 N2.29 Pd1.14'
_chemical_formula_weight         684.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-29
_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                90
_cell_angle_beta                 109.505(4)
_cell_angle_gamma                90
_cell_formula_units_Z            7
_cell_length_a                   9.8649(3)
_cell_length_b                   34.9214(14)
_cell_length_c                   13.1305(5)
_cell_measurement_reflns_used    5439
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0260
_cell_measurement_theta_min      3.6870
_cell_volume                     4263.8(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.814
_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  29.00   0.50   11.70    --  -10.48 -99.00  90.00   98
  2  \w    -24.00  85.00   0.50   11.70    --   12.36  19.00   0.00  218
;
_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      -0.0513001000
_diffrn_orient_matrix_UB_12      0.0087601000
_diffrn_orient_matrix_UB_13      0.0196565000
_diffrn_orient_matrix_UB_21      0.0248746000
_diffrn_orient_matrix_UB_22      0.0183170000
_diffrn_orient_matrix_UB_23      -0.0089606000
_diffrn_orient_matrix_UB_31      -0.0506792000
_diffrn_orient_matrix_UB_32      0.0001388000
_diffrn_orient_matrix_UB_33      -0.0530977000
_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  0.0285
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18369
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.763
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471
_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 white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6804
_reflns_number_total             9904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02076b2.cif
_cod_data_source_block           17-3-21-def
_cod_depositor_comments
'Adding full bibliography for 1569224--1569228.cif.'
_cod_database_code               1569228
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C22 H10 F10 N2 Pd'
_chemical_oxdiff_usercomment     colorless
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C011(H011), C012(H012), C015(H015), C018(H018), C019(H019), C01C(H01C),
 C01D(H01D), C01G(H01G), C01H(H01H), C01J(H01J), C01K(H01K), C01Q(H01Q),
 C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Y(H01Y)
;
_shelx_res_checksum              12760
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.797