Reactivity of Ortho-Palladated Phenol Derivatives with Unsaturated Molecules. Carbodiimide Insertion into a C−Pd Bond and/or O−H Phenol Addition to a Carbodiimide
Vicente, José; Abad, José Antonio; López-Sáez, María-José; Jones, Peter G.; Organometallics 25 (2006) 1851–; doi:10.1021/om0601652

data_4075260
_publ_section_title
;
 Reactivity of Ortho-Palladated Phenol Derivatives with Unsaturated
 Molecules. Carbodiimide Insertion into a C&#x2212;Pd Bond and/or
 O&#x2212;H Phenol Addition to a Carbodiimide
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1851
_journal_paper_doi               10.1021/om0601652
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C32 H27 F3 N4 O4 Pd S'
_chemical_formula_weight         727.04
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.035(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8541(11)
_cell_length_b                   12.0079(11)
_cell_length_c                   18.6470(14)
_cell_measurement_reflns_used    6062
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      2.2
_cell_volume                     3054.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_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  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56753
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment
'NH free with DFIX, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8924
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                6151
_reflns_number_total             8924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0601652si20060221_051410.cif
_cod_data_source_block           raiser
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075260