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_4089040
_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         'C38 H45 Cl1.06 I0.95 N3 Pd'
_chemical_formula_sum            'C38 H45 Cl1.06 I0.94 N3 Pd'
_chemical_formula_weight         807.46
_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                 100.47(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.537(2)
_cell_length_b                   24.824(3)
_cell_length_c                   15.418(2)
_cell_measurement_reflns_used    9018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.601
_cell_measurement_theta_min      2.3215
_cell_volume                     3589.4(10)
_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 0.947
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            187613
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.044
_diffrn_reflns_theta_min         1.574
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+4.3390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8624
_reflns_number_total             9067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00662_si_008.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089040
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.689
_shelx_estimated_absorpt_t_max   0.909
_shelx_res_checksum              44165
_shelx_hkl_checksum              73448