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_4082538
_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            'C44 H43 Cl5 N P Pd'
_chemical_formula_weight         900.41
_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                72.231(2)
_cell_angle_beta                 70.129(2)
_cell_angle_gamma                81.274(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9200(8)
_cell_length_b                   14.2254(12)
_cell_length_c                   14.6750(11)
_cell_measurement_reflns_used    8753
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.42
_cell_volume                     2038.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25010
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.9044
_exptl_absorpt_correction_T_min  0.7656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment
'NH2 free with SADI; rigid methyl, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9562
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+1.4408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                9148
_reflns_number_total             9562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401090b_si_002.cif
_cod_data_source_block           jah445s
_cod_database_code               4082538