Selective Oxygen Atom Insertion into an Aryl‒Palladium Bond
Behnia, Ava; Boyle, Paul D.; Blacquiere, Johanna M.; Puddephatt, Richard J.; Organometallics 35 (2016) 2645–; doi:10.1021/acs.organomet.6b00387

data_4086643
_publ_section_title
;
 Selective Oxygen Atom Insertion into an Aryl--Palladium Bond
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2645
_journal_paper_doi               10.1021/acs.organomet.6b00387
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C32 H41 N2 O0.5 Pd'
_chemical_formula_weight         568.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.239(9)
_cell_length_b                   21.009(7)
_cell_length_c                   25.246(8)
_cell_measurement_reflns_used    9563
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.79
_cell_volume                     11795(7)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL-2014
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            216309
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.084
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         14656
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0367P)^2^+44.4895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10587
_reflns_number_total             14656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00387_si_003.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
'Adding full bibliography for 4086643--4086646.cif.'
_cod_original_formula_sum        'C32 H41 N2 O0.50 Pd'
_cod_database_code               4086643
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              87413
_shelx_hkl_checksum              71536