Silylpalladium Cations Enable the Oxidative Addition of C(sp<sup>3</sup>)-O Bonds.
Wierschen, Andreas L.; Romano, Neyen; Lee, Stephen J.; Gagné, Michel R; Journal of the American Chemical Society 141 (2019) 16024–16032; doi:10.1021/jacs.9b08178

data_4128307
_publ_section_title
;
 Silylpalladium Cations Enable the Oxidative Addition of
 C(sp<sup>3</sup>)-O Bonds.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16024
_journal_page_last               16032
_journal_paper_doi               10.1021/jacs.9b08178
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C79.50 H54 B1 Cl1 F24 O1 P2 Pd1'
_chemical_formula_sum            'C79.5 H54 B Cl F24 O P2 Pd'
_chemical_formula_weight         1695.86
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2019-05-08
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_cell_angle_alpha                115.2667(13)
_cell_angle_beta                 96.9948(16)
_cell_angle_gamma                103.7856(18)
_cell_formula_units_Z            2
_cell_length_a                   14.6401(3)
_cell_length_b                   17.2051(4)
_cell_length_c                   17.9300(4)
_cell_measurement_reflns_used    8314
_cell_measurement_temperature    150
_cell_measurement_theta_max      67
_cell_measurement_theta_min      3
_cell_volume                     3836.00(17)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60658
_diffrn_reflns_theta_full        26.132
_diffrn_reflns_theta_max         67.005
_diffrn_reflns_theta_min         2.818
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.581
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             1706.000
_exptl_crystal_size_max          0.382
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.51
_refine_diff_density_min         -0.96
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         13175
_refine_ls_number_restraints     474
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.0463905
_refine_ls_shift/su_mean         0.0013169
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 9.53P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1781
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1781
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                11294
_reflns_number_total             13236
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0751
_oxford_refine_ls_scale          0.09451(3)
_oxford_reflns_number_all        13175
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '19019a_0m in P-1'
_cod_data_source_file            ja9b08178_si_002.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C79.50 H54 B1 Cl1 F24 O1 P2 Pd1'
_cod_database_code               4128307