Chelating N-Heterocyclic Carbene Alkoxide as a Supporting Ligand for PdII/IV C-H Bond Functionalization Catalysis
Polly L. Arnold; Melanie S. Sanford; Stephen M. Pearson; Journal of the American Chemical Society 131 (2009) 13912–13913; doi:10.1021/ja905713t

data_4105088
_publ_contact_author_address
;
School of Chemistry
Joseph Black Building, University of Edinburgh,
West Mains Road, Edinburgh, EH9 3JJ, UK.
;
_publ_contact_author_email       Polly.Arnold@ed.ac.uk
_publ_contact_author_fax         '+44 131 650 6453'
_publ_contact_author_name        'Polly L Arnold'
_publ_contact_author_phone       '+44 131 650 5429'
_publ_section_title
;
 Chelating N-Heterocyclic Carbene Alkoxide as a Supporting Ligand for
 PdII/IV C-H Bond Functionalization Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13912
_journal_page_last               13913
_journal_paper_doi               10.1021/ja905713t
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C23 H25 Cl2 N3 O Pd, C3 H6 O'
_chemical_formula_sum            'C26 H31 Cl2 N3 O2 Pd'
_chemical_formula_weight         594.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 97.18
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5786(7)
_cell_length_b                   12.6706(6)
_cell_length_c                   15.1481(8)
_cell_measurement_reflns_used    6726
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.21
_cell_volume                     2585.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP (Farrugia, 1997)'
_computing_publication_material  'enCIFer (Allen et all., 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Brucker SMART APEX CCD area detector'
_diffrn_measurement_method       'Phi and Omega 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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60537
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.8227
_exptl_absorpt_correction_T_min  0.7551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       Block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.1554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                5766
_reflns_number_total             6431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905713t_si_003.cif
_cod_data_source_block           smp232_compd_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105088