Phosphine-alkene ligand-mediated alkyl-alkyl and alkyl-halide elimination processes from palladium(II)
Luke Tuxworth; Lise Baiget; Andreas Phanopoulos; Owen J. Metters; Andrei S. Batsanov; Mark A. Fox; Judith A. K. Howard; Philip W. Dyer; Chem.Commun. 48 (2012) 10413–; doi:10.1039/c2cc35623f

data_7108472
_publ_section_title
;
 Phosphine-alkene ligand-mediated alkyl-alkyl and alkyl-halide elimination
 processes from palladium(II)
;
_journal_name_full               Chem.Commun.
_journal_page_first              10413
_journal_paper_doi               10.1039/c2cc35623f
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C44 H36 N2 P2 Pd'
_chemical_formula_sum            'C44 H36 N2 P2 Pd'
_chemical_formula_weight         761.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-06-28
_audit_creation_method
;
Olex2 1.1-beta (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                70.057(7)
_cell_angle_beta                 74.120(7)
_cell_angle_gamma                81.517(7)
_cell_formula_units_Z            2
_cell_length_a                   11.9327(6)
_cell_length_b                   12.2787(6)
_cell_length_c                   13.2937(6)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    120
_cell_measurement_theta_max      34.325
_cell_measurement_theta_min      2.328
_cell_volume                     1757.92(17)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40908
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.8887
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP 2012/1, R(int)=0.044 before correction'
_exptl_crystal_colour            off-white
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.782
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         14631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                11656
_reflns_number_total             14631
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc35623f.txt
_cod_data_source_block           4
_cod_database_code               7108472