Unraveling the High Activity of Ylide-Functionalized Phosphines in Palladium-Catalyzed Amination Reactions: A Comparative Study with CyJohnPhos and PtBu3
Scharf, Lennart T.; Rodstein, Ilja; Schmidt, Michelle; Scherpf, Thorsten; Gessner, Viktoria H.; ACS Catalysis  (2019) 999–; doi:10.1021/acscatal.9b04666

data_4517272
_publ_section_title
;
 Unraveling the High Activity of Ylide-Functionalized Phosphines in
 Palladium-Catalyzed Amination Reactions: A Comparative Study with
 CyJohnPhos and PtBu3
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              999
_journal_paper_doi               10.1021/acscatal.9b04666
_journal_year                    2019
_chemical_formula_moiety         'C43 H76 Cl N P2 Pd'
_chemical_formula_sum            'C43 H76 Cl N P2 Pd'
_chemical_formula_weight         810.83
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_atom_sites_solution_hydrogens   mixed
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_cell_length_c                   15.5260(9)
_cell_measurement_reflns_used    13580
_cell_measurement_temperature    99.90(14)
_cell_measurement_theta_max      76.1600
_cell_measurement_theta_min      3.6490
_cell_volume                     2102.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
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_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.90(14)
_diffrn_detector                 'CCD plate'
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.060
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
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_exptl_absorpt_correction_T_min  0.672
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         7969
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.3349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7119
_reflns_number_total             7969
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           ST147
_cod_database_code               4517272
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              93043
_shelx_hkl_checksum              19300