Abnormal-NHC Palladium(II) Complexes: Rational Synthesis, Structural Elucidation, and Catalytic Activity
Rottschäfer, Dennis; Schürmann, Christian J.; Lamm, Jan-Hendrik; Paesch, Alexander N.; Neumann, Beate; Ghadwal, Rajendra S.; Organometallics 35 (2016) 3421–; doi:10.1021/acs.organomet.6b00662

data_4089043
_publ_section_title
;
 Abnormal-NHC Palladium(II) Complexes: Rational Synthesis, Structural
 Elucidation, and Catalytic Activity
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3421
_journal_paper_doi               10.1021/acs.organomet.6b00662
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C66 H80 Cl2 N4 Pd, 4(C7 H8)'
_chemical_formula_sum            'C94 H112 Cl2 N4 Pd'
_chemical_formula_weight         1475.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.25(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.581(2)
_cell_length_b                   12.031(2)
_cell_length_c                   20.983(3)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2995
_cell_measurement_theta_min      2.2335
_cell_volume                     4131.4(11)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.30C'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            108043
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.380
_diffrn_reflns_theta_min         1.457
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.4288
_exptl_absorpt_correction_T_min  0.3755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         7593
_refine_ls_number_restraints     918
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+4.8748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6226
_reflns_number_total             7593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00662_si_004.cif
_cod_data_source_block           p21n_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089043
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              33769
_shelx_hkl_checksum              25107