Palladium(ii) complexes with chelating N-phosphanyl acyclic diaminocarbenes: synthesis, characterization and catalytic performance in Suzuki couplings.
Marchenko, Anatoliy; Koidan, Georgyi; Hurieva, Anastasiya; Vlasenko, Yurii; Kostyuk, Aleksandr; Biffis, Andrea; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1967–1975; doi:10.1039/c5dt02250a

data_7036005
_publ_section_title
;
 Palladium(ii) complexes with chelating N-phosphanyl acyclic
 diaminocarbenes: synthesis, characterization and catalytic performance in
 Suzuki couplings.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1967
_journal_page_last               1975
_journal_paper_doi               10.1039/c5dt02250a
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C22 H39 Cl2 N2 O1 P1 Pd1'
_chemical_formula_sum            'C22 H39 Cl2 N2 O P Pd'
_chemical_formula_weight         555.84
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/cc13wwgb
_audit_update_record
;
2014-12-16 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2299(2)
_cell_length_b                   16.7796(3)
_cell_length_c                   9.6743(2)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    123
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     1296.54(5)
_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 0.993
_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  0.026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15750
_diffrn_reflns_theta_full        26.096
_diffrn_reflns_theta_max         26.629
_diffrn_reflns_theta_min         2.169
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.420
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.45
_refine_ls_abs_structure_details 'Flack (1983), 2285 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_extinction_coef       4.509
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1025
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.0461381
_refine_ls_shift/su_mean         0.0032966
_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: 
 1.26 -0.440 1.32 -0.128 0.412 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0170
_refine_ls_wR_factor_gt          0.0169
_refine_ls_wR_factor_ref         0.0169
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              21
_reflns_limit_k_min              -19
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                5001
_reflns_number_total             5091
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.17
_oxford_diffrn_Wilson_scale      4.42
_oxford_refine_ls_r_factor_ref   0.0164
_oxford_refine_ls_scale          0.6695(4)
_oxford_reflns_number_all        5071
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c5dt02250a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7036005--7036009.cif.'
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C22 H39 Cl2 N2 O1 P1 Pd1'
_cod_database_code               7036005