Synthesis and structures of n1-allenyl and/or -propargyl Pd(II) complexes and their reactivity toward trimethylsilyl pseudohalides, organic thiols, and N-heterocyclic carbene ligands
Yong-Joo Kim; Hyun-Kyung Kim; Jung-Hyun Lee; Zhen Nu Zheng; Soon W. Lee; Inorganica Chimica Acta 398 (2013) 54–63; doi:10.1016/j.ica.2012.12.011

data_1513200
_publ_section_title
;
 Synthesis and structures of n1-allenyl and/or -propargyl Pd(II) complexes
 and their reactivity toward trimethylsilyl pseudohalides, organic thiols,
 and N-heterocyclic carbene ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              54
_journal_page_last               63
_journal_paper_doi               10.1016/j.ica.2012.12.011
_journal_volume                  398
_journal_year                    2013
_chemical_formula_moiety         'C25 H29 Cl P2 Pd'
_chemical_formula_sum            'C25 H29 Cl P2 Pd'
_chemical_formula_weight         533.27
_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
_cell_angle_alpha                89.9700(10)
_cell_angle_beta                 81.7740(10)
_cell_angle_gamma                74.2890(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2242(3)
_cell_length_b                   9.4337(3)
_cell_length_c                   15.2031(4)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.71
_cell_volume                     1259.41(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17602
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.9085
_exptl_absorpt_correction_T_min  0.8135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0325P)^2^+0.7903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                5301
_reflns_number_total             6031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-398-54-63-1.cif
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      'P -1   '
_cod_database_code               1513200