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_4088330
_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_absolute_configuration ad
_chemical_formula_moiety         'C18 H29 Cl2 N2 P1 Pd1'
_chemical_formula_sum            'C18 H29 Cl2 N2 P Pd'
_chemical_formula_weight         481.72
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4381(16)
_cell_length_b                   12.831(2)
_cell_length_c                   17.115(3)
_cell_measurement_reflns_used    2400
_cell_measurement_temperature    173
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2072.6(6)
_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      173
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.934
_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  0.042
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7586
_diffrn_reflns_theta_full        25.209
_diffrn_reflns_theta_max         26.535
_diffrn_reflns_theta_min         1.984
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.64
_refine_ls_abs_structure_details 'Flack (1983), 1548 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.09(5)
_refine_ls_extinction_coef       8.559
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0722
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.0003980
_refine_ls_shift/su_mean         0.0000164
_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: 
 4.02 -2.46 3.23 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0525
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0503
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3460
_reflns_number_total             3839
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.21
_oxford_diffrn_Wilson_scale      6.97
_oxford_refine_ls_r_factor_ref   0.0455
_oxford_refine_ls_scale          0.3896(9)
_oxford_reflns_number_all        3822
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om5b01019_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        2072.5(6)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C18 H29 Cl2 N2 P1 Pd1'
_cod_database_code               4088330