Rational design of a second generation catalyst for preparation of allylsilanes using the silyl-heck reaction.
McAtee, Jesse R.; Yap, Glenn P. A.; Watson, Donald A.; Journal of the American Chemical Society 136 (2014) 10166–10172; doi:10.1021/ja505446y

data_4122159
_publ_section_title
;
 Rational design of a second generation catalyst for preparation of
 allylsilanes using the silyl-heck reaction.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10166
_journal_page_last               10172
_journal_paper_doi               10.1021/ja505446y
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C16 H19 P'
_chemical_formula_weight         242.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   12.982(6)
_cell_length_c                   13.323(5)
_cell_measurement_reflns_used    1146
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.84
_cell_measurement_theta_min      3.00
_cell_volume                     1367.6(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.960
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_point_group_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.696
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6757
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
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_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
; 
 Flack x determined using 636 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.1497P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.440
_reflns_Friedel_fraction_full    0.664
_reflns_Friedel_fraction_max     0.574
_reflns_number_gt                2197
_reflns_number_total             2551
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           donw038
_cod_depositor_comments
'Adding full bibliography for 4122159--4122167.cif.'
_cod_database_code               4122159
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.958
_shelxl_version_number           2013-2
_shelx_res_checksum              51706
_shelx_hkl_checksum              62621