Mechanistic Insight into the Regioselective Palladation of Indole Derivatives: Tetranuclear Indolyl Palladacycles with High C2–Pd or C3–Pd Bond Selectivity
Li, Yang; Wang, Wen-Hua; He, Ke-Han; Shi, Zhang-Jie; Organometallics 31 (2012) 4397–; doi:10.1021/om300284t

data_4078508
_publ_section_title
;
 Mechanistic Insight into the Regioselective Palladation of Indole
 Derivatives: Tetranuclear Indolyl Palladacycles with High C2--Pd or
 C3--Pd Bond Selectivity
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4397
_journal_paper_doi               10.1021/om300284t
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C44 H50 N2 O10 Pd4'
_chemical_formula_weight         1192.46
_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                102.2830(10)
_cell_angle_beta                 97.2550(10)
_cell_angle_gamma                113.191(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3044(12)
_cell_length_b                   13.5915(15)
_cell_length_c                   15.5969(18)
_cell_measurement_reflns_used    2119
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.374
_cell_measurement_theta_min      2.308
_cell_volume                     2277.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.1192
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11832
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.8555
_exptl_absorpt_correction_T_min  0.7183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1757
_refine_ls_R_factor_gt           0.0803
_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^)+(0.0931P)^2^+15.2309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2595
_reflns_number_gt                3381
_reflns_number_total             7850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300284t_si_002.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078508