P,N-Chelate Complexes of Pd(II) and Pt(II) Based on a Phosphaalkene Motif: A Catalyst for the Overman−Claisen Rearrangement
Dugal-Tessier, Julien; Dake, Gregory R.; Gates, Derek P.; Organometallics 26 (2007) 6481–; doi:10.1021/om700784x

data_4073983
_publ_section_title
;
 P,N-Chelate Complexes of Pd(II) and Pt(II) Based on a Phosphaalkene
 Motif:&#x00A0; A Catalyst for the Overman&#x2212;Claisen Rearrangement
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6481
_journal_paper_doi               10.1021/om700784x
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C23 H24 Cl6 N P Pd'
_chemical_formula_weight         664.50
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                86.2920(10)
_cell_angle_beta                 88.6850(10)
_cell_angle_gamma                69.9040(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8650(3)
_cell_length_b                   11.7091(4)
_cell_length_c                   12.5723(5)
_cell_measurement_reflns_used    7323
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.34
_cell_volume                     1360.96(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22041
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6431
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.1902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                5069
_reflns_number_total             6431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700784x-file001.cif
_cod_data_source_block           dg039
_cod_database_code               4073983