Room temperature rapid functionalization of E-H bonds (E = O, N, S) via the metal-ligand cooperation mechanism.
Scharf, Adam; Goldberg, Israel; Vigalok, Arkadi; Inorganic chemistry 53 (2014) 12–14; doi:10.1021/ic402315a

data_4337449
_publ_section_title
;
 Room temperature rapid functionalization of E-H bonds (E = O, N, S) via
 the metal-ligand cooperation mechanism.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12
_journal_page_last               14
_journal_paper_doi               10.1021/ic402315a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C30 H35 F N2 P Pd, C2 F3 O2'
_chemical_formula_sum            'C32 H35 F4 N2 O2 P Pd'
_chemical_formula_weight         692.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.968(2)
_cell_angle_beta                 80.708(2)
_cell_angle_gamma                82.083(2)
_cell_formula_units_Z            4
_cell_length_a                   12.9990(7)
_cell_length_b                   17.0995(9)
_cell_length_c                   17.4393(9)
_cell_measurement_reflns_used    10101
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      1.87
_cell_volume                     3691.6(3)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-2012, (Sheldrick, 2012)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45867
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.9164
_exptl_absorpt_correction_T_min  0.8422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, Bruker-AXS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         12632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+2.4050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                10101
_reflns_number_total             12632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402315a_si_005.cif
_cod_data_source_block           ar101sq
_cod_database_code               4337449