Characterization of Two Stable Degradants of PalladiumtBuXPhos Catalyst and a Unique Dearomatization Reaction
Allgeier, Alan M.; Shaw, Bradley J.; Hwang, Tsang-Lin; Milne, Jacqueline E.; Tedrow, Jason S.; Wilde, Christopher N.; Organometallics 31 (2012) 519–; doi:10.1021/om200988f

data_4067998
_publ_section_title
;
 Characterization of Two Stable Degradants of PalladiumtBuXPhos Catalyst
 and a Unique Dearomatization Reaction
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              519
_journal_paper_doi               10.1021/om200988f
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C33 H46 F3 N O2 P Pd'
_chemical_formula_sum            'C33 H46 F3 N O2 P Pd'
_chemical_formula_weight         683.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                79.179(4)
_cell_angle_beta                 82.501(4)
_cell_angle_gamma                89.990(4)
_cell_formula_units_Z            4
_cell_length_a                   8.049(2)
_cell_length_b                   16.945(5)
_cell_length_c                   25.181(7)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.45
_cell_volume                     3343.5(16)
_computing_cell_refinement       'APEX2 (BRUKER, V5-0, 2008)'
_computing_data_collection       'COSMO (BRUKER, V1.58, 2007)'
_computing_data_reduction        'SAINT (BRUKER, V7.56A, 2008)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_publication_material
'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48389
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.8234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.243
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         12550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+41.2143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2247
_reflns_number_gt                8470
_reflns_number_total             12550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200988f_si_001.cif
_cod_data_source_block           amg4508_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_cell_volume        3343.7(17)
_cod_database_code               4067998