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_1569224
_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         'C11 H5 Br2 F5 N Pd, C16 H36 N'
_chemical_formula_sum            'C27 H41 Br2 F5 N2 Pd'
_chemical_formula_weight         754.84
_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             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                75.651(9)
_cell_angle_beta                 87.092(8)
_cell_angle_gamma                71.514(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8832(12)
_cell_length_b                   10.4913(12)
_cell_length_c                   16.8579(14)
_cell_measurement_reflns_used    2624
_cell_measurement_temperature    298
_cell_measurement_theta_max      75.0480
_cell_measurement_theta_min      4.5570
_cell_volume                     1605.3(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 (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      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.941
_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    -63.00  33.00   1.00    1.73    --  -41.06  37.00-120.00   96
  2  \w   -111.00 -17.00   1.00    1.73    --  -41.06 -37.00  60.00   94
  3  \w    -74.00  24.00   1.00    1.73    --  -41.06  77.00 -30.00   98
  4  \w     35.00 112.00   1.00    6.92    --  110.01 -77.00   0.00   77
  5  \w     65.00 116.00   1.00    6.92    --  110.01-125.00   0.00   51
  6  \w     50.00 136.00   1.00    6.92    --  110.01 -45.00  90.00   86
  7  \w     34.00 107.00   1.00    6.92    --  110.01 -94.00 120.00   73
  8  \w     37.00 130.00   1.00    6.92    --  110.01 -45.00-150.00   93
  9  \w     31.00 161.00   1.00    6.92    --  110.01 -15.00 -30.00  130
 10  \w     37.00 108.00   1.00    6.92    --  110.01-125.00 -90.00   71
 11  \w    118.00 176.00   1.00    6.92    --  110.01  45.00 150.00   58
;
_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      -0.0693213000
_diffrn_orient_matrix_UB_12      0.1547540000
_diffrn_orient_matrix_UB_13      -0.0022682000
_diffrn_orient_matrix_UB_21      0.0209336000
_diffrn_orient_matrix_UB_22      -0.0330630000
_diffrn_orient_matrix_UB_23      0.0936813000
_diffrn_orient_matrix_UB_31      0.1476291000
_diffrn_orient_matrix_UB_32      0.0213810000
_diffrn_orient_matrix_UB_33      -0.0111624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9382
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.190
_diffrn_reflns_theta_min         4.583
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.985
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.500
_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    1.562
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1003P)^2^+0.3096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.2009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4380
_reflns_number_total             6236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02076b2.cif
_cod_data_source_block           sfm-199
_cod_depositor_comments
'Adding full bibliography for 1569224--1569228.cif.'
_cod_database_code               1569224
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C27H41Br2F5N2Pd
_chemical_oxdiff_usercomment     Yellow
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Secondary CH2 refined with riding coordinates:
 C00C(H00A,H00B), C00D(H00C,H00D), C00I(H00E,H00F), C00K(H00G,H00H), C00L(H00I,
 H00J), C00O(H00K,H00L), C00P(H00M,H00N), C00Q(H00O,H00P), C00S(H00Q,H00R),
 C00V(H00S,H00T), C00W(H00U,H00V), C00X(H00W,H00X)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00), C00F(H0AA), C00R(H1AA), C00T(H2AA), C00U(H3AA)
2.c Idealised Me refined as rotating group:
 C00Y(H00Y,H,HA), C00Z(H00Z,HB,HC), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F)
;
_shelx_res_checksum              75558
_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 1.920
_oxdiff_exptl_absorpt_empirical_full_min 0.647