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_4088329
_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         'C21 H35 N2 P1'
_chemical_formula_sum            'C21 H35 N2 P'
_chemical_formula_weight         346.50
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                93.7880(10)
_cell_angle_beta                 100.6860(10)
_cell_angle_gamma                90.5700(10)
_cell_formula_units_Z            4
_cell_length_a                   10.1402(3)
_cell_length_b                   14.3567(4)
_cell_length_c                   14.9971(4)
_cell_measurement_reflns_used    279
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      1.4
_cell_volume                     2140.18(10)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.951
_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  0.053
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34078
_diffrn_reflns_theta_full        25.187
_diffrn_reflns_theta_max         29.287
_diffrn_reflns_theta_min         1.385
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.964
_exptl_crystal_size_mid          0.544
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.30
_refine_ls_extinction_coef       14.022
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9092
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.0005751
_refine_ls_shift/su_mean         0.0000207
_refine_ls_structure_factor_coef Fsqd
_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: 
 11.9 14.7 5.91 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1187
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.0965
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7472
_reflns_number_total             11102
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.10
_oxford_diffrn_Wilson_scale      2.59
_oxford_refine_ls_r_factor_ref   0.0477
_oxford_refine_ls_scale          0.4787(4)
_oxford_reflns_number_all        11071
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om5b01019_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C21 H35 N2 P1'
_cod_database_code               4088329