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_1569227
_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         'C8 H10 N2 O6 Pd, 2(C16 H36 N)'
_chemical_formula_sum            'C40 H82 N4 O6 Pd'
_chemical_formula_weight         821.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-04-11 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.492(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3972(5)
_cell_length_b                   12.8302(4)
_cell_length_c                   19.2798(5)
_cell_measurement_reflns_used    6100
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.6970
_cell_measurement_theta_min      4.0050
_cell_volume                     4546.5(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 (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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.840
_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    -16.00  12.00   1.00   36.72    --  -10.48-101.00 -76.00   28
  2  \w    -72.00  78.00   1.00   36.72    --  -10.48   0.00 -90.00  150
  3  \w     66.00  94.00   1.00   36.72    --   12.36 178.00 -60.00   28
;
_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      -0.0026190000
_diffrn_orient_matrix_UB_12      0.0276079000
_diffrn_orient_matrix_UB_13      0.0316730000
_diffrn_orient_matrix_UB_21      0.0170700000
_diffrn_orient_matrix_UB_22      0.0437207000
_diffrn_orient_matrix_UB_23      -0.0148548000
_diffrn_orient_matrix_UB_31      -0.0345097000
_diffrn_orient_matrix_UB_32      0.0195260000
_diffrn_orient_matrix_UB_33      -0.0115264000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12298
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.618
_diffrn_reflns_theta_min         3.347
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91373
_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    1.200
_exptl_crystal_description       cube
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.268
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5396
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0650P)^2^+3.0891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4494
_reflns_number_total             5396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02076b2.cif
_cod_data_source_block           vs-983-1-1
_cod_depositor_comments
'Adding full bibliography for 1569224--1569228.cif.'
_cod_database_code               1569227
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C15 H10 N2 O3 F5 Pd'
_chemical_oxdiff_usercomment     'YELLOW CRISTAL'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C1AA
 1.55 with sigma of 0.01
 C2-C0AA
 1.55 with sigma of 0.01
3. Others
 Fixed Sof: H2BC(0.5) H2BD(0.5) H2AA(0.5) H2AB(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C00A(H00A,H00B), C00B(H00C,H00D), C00C(H00E,H00F), C00D(H00Z,
 H), C00E(H00G,H00H), C00F(H00I,H00J), C00G(H00K,H00L), C00I(H00M,H00N),
 C00J(H00O,H00P), C00M(H00T,H00U), C1(H1A,H1B), C2(H2BC,H2BD), C2(H2AA,H2AB)
4.b Idealised Me refined as rotating group:
 C(HA,HB,HC), C00K(H00Q,H00R,H00S), C00O(H00V,H00W,H00X), C00P(H00Y,HD,HE),
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              43066
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.825