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_4067997
_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         'C32 H46 Cl2 F3 O2 P Pd'
_chemical_formula_sum            'C32 H46 Cl2 F3 O2 P Pd'
_chemical_formula_weight         727.96
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.680(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.770(3)
_cell_length_b                   9.2842(4)
_cell_length_c                   18.4678(11)
_cell_measurement_reflns_used    3481
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.89
_cell_measurement_theta_min      4.79
_cell_volume                     6811.5(7)
_computing_cell_refinement       'APEX2 (BRUKER, V2010.11-3, 2010)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT (BRUKER, V7.68A, 2010)'
_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 0.985
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w,and/f 0.5 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1528
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19868
_diffrn_reflns_theta_full        68.02
_diffrn_reflns_theta_max         68.02
_diffrn_reflns_theta_min         4.79
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.644
_exptl_absorpt_correction_T_max  0.6758
_exptl_absorpt_correction_T_min  0.2729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.1061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+216.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2446
_refine_ls_wR_factor_ref         0.2637
_reflns_number_gt                3668
_reflns_number_total             6113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200988f_si_001.cif
_cod_data_source_block           amg3808_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        6811.4(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4067997