Versatility of Iminophosphoranes and Noninnocent Behavior of the 1,5-Cyclooctadiene Ligand in Palladium(II) Complexes. Synthesis of σ-Allyl Derivatives
Aguilar, David; Aznárez, Francisco; Bielsa, Raquel; Falvello, Larry R.; Navarro, Rafael; Urriolabeitia, Esteban P.; Organometallics 26 (2007) 6397–; doi:10.1021/om700707j

data_4073885
_publ_section_title
;
 Versatility of Iminophosphoranes and Noninnocent Behavior of the
 1,5-Cyclooctadiene Ligand in Palladium(II) Complexes. Synthesis of
 \s-Allyl Derivatives
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6397
_journal_paper_doi               10.1021/om700707j
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C33 H34 Cl4 N P Pd'
_chemical_formula_weight         723.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 103.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.369(4)
_cell_length_b                   12.150(2)
_cell_length_c                   27.890(6)
_cell_measurement_reflns_used    13209
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      32.0493
_cell_measurement_theta_min      2.9617
_cell_volume                     6376(2)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction Ltd., 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction Ltd., 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction Ltd., 2006)
;
_computing_molecular_graphics    'Diamond (Brandenburg, 2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir-92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type
;
four-circle device with CCD 
;
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25791
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  1.0837
_exptl_absorpt_correction_T_min  0.9245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.878
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0657P)^2^+6.1296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                5240
_reflns_number_total             7078
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om700707js2.cif
_cod_data_source_block           est
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               4073885