Oxidatively Resistant Ligands for Palladium-Catalyzed Aerobic Alcohol Oxidation
Pearson, David M.; Conley, Nicholas R.; Waymouth, Robert M.; Organometallics 30 (2011) 1445–; doi:10.1021/om101037k

data_4063928
_publ_section_title
;
 Oxidatively Resistant Ligands for Palladium-Catalyzed Aerobic Alcohol
 Oxidation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1445
_journal_paper_doi               10.1021/om101037k
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C20 H13 Cl F2 N3 Pd, C F3 O3 S '
_chemical_formula_sum            'C21 H13 Cl F5 N3 O3 Pd S'
_chemical_formula_weight         624.25
_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                102.481(4)
_cell_angle_beta                 99.258(2)
_cell_angle_gamma                105.172(3)
_cell_formula_units_Z            2
_cell_length_a                   6.5952(14)
_cell_length_b                   12.156(3)
_cell_length_c                   14.847(3)
_cell_measurement_reflns_used    4198
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.60
_cell_volume                     1091.4(4)
_computing_cell_refinement       'Bruker SAINT v7.34'
_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_data_reduction        'Bruker SAINT v7.34'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12266
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_correction_T_min  0.8037
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.792
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+2.3782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                4243
_reflns_number_total             5286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101037k_si_002.cif
_cod_data_source_block           '[(odfp-phen)Pd(NCCH3)(Cl)][OTf]'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063928