Reactivity toward Neutral N- and P-Donor Ligands of Eight-Membered Palladacycles Arising from Monoinsertion of Alkynes into the Pd‒C Bond of Orthopalladated Homoveratrylamine and Phentermine. A New Example of the Transphobia Effect
Oliva-Madrid, María-José; García-López, José-Antonio; Saura-Llamas, Isabel; Bautista, Delia; Vicente, José; Organometallics 33 (2014) 33–; doi:10.1021/om401090b

data_4082541
_publ_section_title
;
 Reactivity toward Neutral N- and P-Donor Ligands of Eight-Membered
 Palladacycles Arising from Monoinsertion of Alkynes into the Pd--C Bond
 of Orthopalladated Homoveratrylamine and Phentermine. A New Example of
 the Transphobia Effect
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              33
_journal_paper_doi               10.1021/om401090b
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C88 H86 Br2 Cl8 N2 O4 P2 Pd2'
_chemical_formula_weight         1953.75
_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                 113.482(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.7668(11)
_cell_length_b                   17.2559(11)
_cell_length_c                   15.0620(8)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.36
_cell_volume                     4235.3(4)
_computing_cell_refinement       'SAINT V8.1????C (Bruker AXS Inc., 2011)'
_computing_data_collection       'APEX2 201?.? (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.1????C (Bruker AXS Inc., 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'high brilliance microfocus sealed tube'
_diffrn_radiation_type
'high brilliance microfocus sealed tube MoK\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            223246
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.267
_refine_diff_density_min         -1.865
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment
'NH2 free with SADI, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         10566
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+17.7675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                8399
_reflns_number_total             10566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401090b_si_002.cif
_cod_data_source_block           isu60_sp1
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               4082541