Phosphines with Tethered Electron-Withdrawing Olefins as Ligands for Efficient Pd-Catalyzed Aryl-Alkyl Coupling
Gioria, Estefanía; Martínez-Ilarduya, Jesús M.; García-Cuadrado, Domingo; Miguel, Jesús A.; Genov, Miroslav; Espinet, Pablo; Organometallics 32 (2013) 4255–; doi:10.1021/om4004303

data_4081210
_publ_section_title
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 Phosphines with Tethered Electron-Withdrawing Olefins as Ligands for
 Efficient Pd-Catalyzed Aryl-Alkyl Coupling
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4255
_journal_paper_doi               10.1021/om4004303
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C27 H17 Cl2 F4 O P Pd'
_chemical_formula_weight         641.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 118.328(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6534(6)
_cell_length_b                   12.7998(3)
_cell_length_c                   14.6608(6)
_cell_measurement_reflns_used    8701
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4610
_cell_measurement_theta_min      2.7747
_cell_volume                     2420.49(19)
_computing_cell_refinement
; 
'Wed Nov 04 17:40:42 2009' 
;
_computing_data_collection
; 
'Wed Nov 04 17:40:42 2009' 
;
_computing_data_reduction
; 
'Wed Nov 04 17:40:42 2009' 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13091
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
'Wed Nov 04 17:40:42 2009' 
;
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.2460
_exptl_crystal_size_mid          0.2075
_exptl_crystal_size_min          0.0763
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+2.3214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                3518
_reflns_number_total             4363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4004303_si_002.cif
_cod_data_source_block           11
_cod_database_code               4081210