Chelate Palladium(II) Complexes with Saturated N-Phosphanyl-N-Heterocyclic Carbene Ligands: Synthesis and Catalysis
Marchenko, Anatoliy; Koidan, Georgyi; Hurieva, Anastasiia N.; Vlasenko, Yurii; Kostyuk, Aleksandr; Biffis, Andrea; Organometallics 35 (2016) 762–; doi:10.1021/acs.organomet.5b01019

data_4088331
_publ_section_title
;
 Chelate Palladium(II) Complexes with Saturated
 N-Phosphanyl-N-Heterocyclic Carbene Ligands: Synthesis and Catalysis
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              762
_journal_paper_doi               10.1021/acs.organomet.5b01019
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C46 H73 Cl4 N6 P2 Pd2'
_chemical_formula_sum            'C46 H73 Cl4 N6 P2 Pd2'
_chemical_formula_weight         1126.68
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 103.744(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8616(3)
_cell_length_b                   28.4967(10)
_cell_length_c                   12.2214(4)
_cell_measurement_reflns_used    7936
_cell_measurement_temperature    123
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2659.56(16)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24815
_diffrn_reflns_theta_full        25.927
_diffrn_reflns_theta_max         26.456
_diffrn_reflns_theta_min         1.429
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.56
_refine_ls_extinction_coef       14.587
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0940
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.0015784
_refine_ls_shift/su_mean         0.0000197
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.21 -1.14 0.607 -0.276 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0373
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0320
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4420
_reflns_number_total             5439
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.14
_oxford_diffrn_Wilson_scale      7.89
_oxford_refine_ls_r_factor_ref   0.0346
_oxford_refine_ls_scale          0.3605(4)
_oxford_reflns_number_all        5414
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om5b01019_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4088331