Versatile Behavior of the Schiff Base Ligand 2,5-Me2C6H3C(H)═N(2,4,6-Me3C6H2) toward Cyclometalation Reactions: C(sp2,phenyl)−H vs C(sp3,methyl)−H Activation
Vázquez-García, Digna; Fernández, Alberto; López-Torres, Margarita; Rodríguez, Antonio; Gómez-Blanco, Nina; Viader, Carlos; Vila, José M.; Fernández, Jesús J.; Organometallics 29 (2010) 3303–; doi:10.1021/om100238w

data_4065985
_publ_section_title
;
 Versatile Behavior of the Schiff Base Ligand
 2,5-Me2C6H3C(H)&#x2550;N(2,4,6-Me3C6H2) toward Cyclometalation Reactions:
 C(sp2,phenyl)&#x2212;H vs C(sp3,methyl)&#x2212;H Activation
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3303
_journal_paper_doi               10.1021/om100238w
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C36 H41 Cl2 N2 O0.5 Pd2'
_chemical_formula_weight         793.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-01-27T11:37:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   29.948(5)
_cell_length_b                   29.948(5)
_cell_length_c                   10.397(5)
_cell_measurement_reflns_used    4070
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.189
_cell_measurement_theta_min      4.711
_cell_volume                     8076(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17915
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3609
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                3108
_reflns_number_total             4477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100238w_si_002.cif
_cod_data_source_block           0731819_0s
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C36 H41 Cl2 N2 O0.50 Pd2'
_cod_database_code               4065985