Mechanistic significance of the si-o-pd bond in the palladium-catalyzed cross-coupling reactions of arylsilanolates.
Tymonko, Steven A.; Smith, Russell C.; Ambrosi, Andrea; Ober, Michael H.; Wang, Hao; Denmark, Scott E.; Journal of the American Chemical Society 137 (2015) 6200–6218; doi:10.1021/jacs.5b02518

data_4123655
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Mechanistic significance of the si-o-pd bond in the palladium-catalyzed
 cross-coupling reactions of arylsilanolates.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6200
_journal_page_last               6218
_journal_paper_doi               10.1021/jacs.5b02518
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C50 H45 F3 Fe O2 P2 Pd Si'
_chemical_formula_sum            'C50 H45 F3 Fe O2 P2 Pd Si'
_chemical_formula_weight         987.14
_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
_audit_update_record
; 
2005-04-27   text and data added, srw 
;
_cell_angle_alpha                104.725(3)
_cell_angle_beta                 97.998(3)
_cell_angle_gamma                97.617(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8243(5)
_cell_length_b                   11.9643(7)
_cell_length_c                   20.2965(10)
_cell_measurement_reflns_used    4398
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2249.5(2)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga70fas
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42149
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.97547
_exptl_absorpt_correction_T_min  0.88858
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1008
_exptl_crystal_id                ga70fas
_exptl_crystal_preparation
; 
The data crystal was excised from a cluster of severely twinned 
and interconnected crystals.  Every effort was made to remove all 
crystallites; however, a few segments (<0.005 mm) could not be 
removed.  The data crystal was mounted using oil (Parantone-N, 
Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (-1 0 1) 
scattering planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0422P)^2^+1.9984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                5853
_reflns_number_total             8501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b02518_si_007.cif
_cod_data_source_block           ga70fas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4123655--4123660.cif.
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4123655