Synthesis of Ortho-Palladated Phenol Derivatives. Study of Their Reactivity with Carbon Monoxide and Isonitriles
Vicente, José; Abad, José-Antonio; Förtsch, Walter; Jones, Peter G.; Fischer, Axel K.; Organometallics 20 (2001) 2704–; doi:10.1021/om010074z

data_4077289
_publ_section_title
;
 Synthesis of Ortho-Palladated Phenol Derivatives. Study of Their
 Reactivity with Carbon Monoxide and Isonitriles
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2704
_journal_paper_doi               10.1021/om010074z
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C39 H41 F3 N4 O5 Pd S'
_chemical_formula_weight         841.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                112.118(3)
_cell_angle_beta                 95.685(3)
_cell_angle_gamma                101.822(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5339(3)
_cell_length_b                   14.9785(4)
_cell_length_c                   17.2207(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1957.95(12)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens 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      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Siemens SMART 1000 CCD'
_diffrn_measurement_method       \w-scans
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13301
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   'multiple scans (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    'cation methyls and OH rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9338
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0312P)^2^+1.2668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                7934
_reflns_number_total             9338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010074z.cif
_cod_data_source_block           foerst
_cod_original_cell_volume        1957.95(10)
_cod_database_code               4077289