Aryl Ether Cleavage by Group 9 and 10 Transition Metals: Stoichiometric Studies of Selectivity and Mechanism
Edouard, Guy A.; Kelley, Paul; Herbert, David E.; Agapie, Theodor; Organometallics  (2015) –; doi:10.1021/acs.organomet.5b00710

data_4086333
_publ_section_title
;
 Aryl Ether Cleavage by Group 9 and 10 Transition Metals: Stoichiometric
 Studies of Selectivity and Mechanism
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.5b00710
_journal_year                    2015
_chemical_formula_moiety         'C39 H56 N2 O P2 Pd, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C41 H59 B2 F8 N3 O P2 Pd'
_chemical_formula_weight         951.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                82.133(2)
_cell_angle_beta                 86.587(2)
_cell_angle_gamma                86.032(2)
_cell_formula_units_Z            4
_cell_length_a                   12.3085(5)
_cell_length_b                   17.2927(7)
_cell_length_c                   21.7237(9)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.46
_cell_measurement_theta_min      2.28
_cell_volume                     4563.5(3)
_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-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            165477
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         38.839
_diffrn_reflns_theta_min         0.947
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       slab
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.699
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1125
_refine_ls_number_reflns         48987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+4.1090P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33605
_reflns_number_total             48987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00710_si_001.cif
_cod_data_source_block           ta47_sad
_cod_database_code               4086333
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.923
_diffrn_reflns_sigmai/neti       0.0565
_shelxl_version_number           2012-4
_shelx_res_checksum              82167
_shelx_hkl_checksum              49469