Orthopalladation of iminophosphoranes: synthesis, structure and study of stability
Bielsa, Raquel; Navarro, Rafael; Soler, Tatiana; Urriolabeitia, Esteban P.; Dalton Transactions  (2008) 1203–1214; doi:10.1039/b714485g

data_7003218
_publ_section_title
;
 Orthopalladation of iminophosphoranes: synthesis, structure and study
 of stability
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1203
_journal_page_last               1214
_journal_paper_doi               10.1039/b714485g
_journal_year                    2008
_chemical_formula_moiety         'C27 H27 N3 O P Pd, Cl O4'
_chemical_formula_sum            'C27 H27 Cl N3 O5 P Pd'
_chemical_formula_weight         646.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.6200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1099(11)
_cell_length_b                   13.2935(11)
_cell_length_c                   16.0085(13)
_cell_measurement_reflns_used    3529
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.23
_cell_volume                     2673.4(4)
_computing_cell_refinement       'Bruker SMART V5.624'
_computing_data_collection       'Bruker SMART V5.624'
_computing_data_reduction        'Bruker SAINT V6.02A'
_computing_molecular_graphics    'SHELXTL Rel. 5.05/V (Siemens, 1996)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17019
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.9224
_exptl_absorpt_correction_T_min  0.7984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker/Siemens SADABS V2.03'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0442P)^2^+1.2381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                4746
_reflns_number_total             6119
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b714485g.txt
_cod_data_source_block           7b
_cod_original_cell_volume        2673.3(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003218