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_4063926
_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         'C18 H15 F3 N4 Pd, 2(C F3 O3 S)'
_chemical_formula_sum            'C20 H15 F9 N4 O6 Pd S2'
_chemical_formula_weight         748.88
_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                107.230(2)
_cell_angle_beta                 100.385(2)
_cell_angle_gamma                102.965(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7061(9)
_cell_length_b                   12.7990(12)
_cell_length_c                   13.5092(13)
_cell_measurement_reflns_used    2780
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.49
_cell_volume                     1351.0(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15234
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.7031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5886
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.4034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                4640
_reflns_number_total             5886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101037k_si_002.cif
_cod_data_source_block           '[(tfmm-phen)Pd(NCCH3)2][OTf]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063926