Two ligands transfer from Ag to Pd: En Route to (SIPr)Pd(CF2H)(X) and its Application in One-pot C-H Borylation/Difluoromethylation.
Zhao, Haiwei; Herbert, Simon; Kinzel, Tom; Zhang, Wei; Shen, Qilong; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b03296

data_4037886
_publ_section_title
;
 Two ligands transfer from Ag to Pd: En Route to (SIPr)Pd(CF2H)(X) and its
 Application in One-pot C-H Borylation/Difluoromethylation.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b03296
_journal_year                    2020
_chemical_formula_sum            'C30 H42 F2 N2 O2 Pd'
_chemical_formula_weight         607.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.227(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5050(6)
_cell_length_b                   17.9473(7)
_cell_length_c                   13.6621(6)
_cell_measurement_reflns_used    4786
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.604
_cell_measurement_theta_min      4.829
_cell_volume                     3057.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14280
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_min         1.877
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.115
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1285P)^2^+0.4215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3627
_reflns_number_total             5679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03296_si_002.cif
_cod_data_source_block           mo_d8v19005_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4037886
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.938
_shelxl_version_number           2013-4
_shelx_res_checksum              90847
_shelx_hkl_checksum              71980