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_4089045
_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 H44 Cl I2 N3 Pd'
_chemical_formula_sum            'C38 H44 Cl I2 N3 Pd'
_chemical_formula_weight         938.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-01
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                102.384(2)
_cell_angle_beta                 97.461(2)
_cell_angle_gamma                103.547(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2753(3)
_cell_length_b                   11.7753(3)
_cell_length_c                   18.6313(5)
_cell_measurement_reflns_used    34238
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.1430
_cell_measurement_theta_min      3.9690
_cell_volume                     1897.19(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -122.00 -35.00   1.00    1.75    --  -38.50-178.00  90.00   87
  2  \w   -116.00  -5.00   1.00    1.75    --  -38.50 -19.00  90.00  111
  3  \w    -64.00  30.00   1.00    1.75    --  -38.50  57.00 -60.00   94
  4  \w     13.00 115.00   1.00    1.75    --   43.20  77.00-120.00  102
  5  \w     18.00 112.00   1.00    1.75    --   43.20  57.00-150.00   94
  6  \w     18.00 112.00   1.00    1.75    --   43.20  57.00  30.00   94
  7  \w     13.00 115.00   1.00    1.75    --   43.20  77.00  30.00  102
  8  \w     23.00 114.00   1.00    1.75    --   43.20  38.00 -60.00   91
  9  \w      1.00  82.00   1.00    1.75    --   43.20 -99.00  30.00   81
 10  \w     13.00 115.00   1.00    1.75    --   43.20  77.00 150.00  102
 11  \w     13.00 115.00   1.00    1.75    --   43.20  77.00 -60.00  102
 12  \w     15.00 113.00   1.00    1.75    --   43.20  71.00 103.00   98
 13  \w     57.00 127.00   1.00    1.75    --   43.20 178.00-150.00   70
 14  \w     31.00 109.00   1.00    7.50    --  111.00 -94.00 -60.00   78
 15  \w     41.00 122.00   1.00    7.50    --  111.00-125.00  60.00   81
 16  \w     89.00 178.00   1.00    7.50    --  111.00  45.00 120.00   89
 17  \w     31.00 109.00   1.00    7.50    --  111.00 -94.00 120.00   78
 18  \w     41.00 122.00   1.00    7.50    --  111.00-125.00   0.00   81
 19  \w     81.00 178.00   1.00    7.50    --  111.00  77.00 150.00   97
 20  \w     81.00 178.00   1.00    7.50    --  111.00  77.00  60.00   97
 21  \w     81.00 178.00   1.00    7.50    --  111.00  77.00 -30.00   97
 22  \w     85.00 178.00   1.00    7.50    --  111.00  61.00 120.00   93
 23  \w     41.00 122.00   1.00    7.50    --  111.00-125.00-120.00   81
 24  \w     84.00 178.00   1.00    7.50    --  111.00  64.00  -2.07   94
 25  \w     87.00 178.00   1.00    7.50    --  111.00  54.00 -95.19   91
 26  \w     85.00 178.00   1.00    7.50    --  111.00  61.00-150.00   93
 27  \w     31.00 109.00   1.00    7.50    --  111.00 -94.00  60.00   78
 28  \w     81.00 178.00   1.00    7.50    --  111.00  77.00 -60.00   97
 29  \w     85.00 178.00   1.00    7.50    --  111.00  61.00 -60.00   93
 30  \w     85.00 178.00   1.00    7.50    --  111.00  61.00  90.00   93
 31  \w     40.00 141.00   1.00    7.50    --  111.00 -77.00 150.00  101
 32  \w     87.00 178.00   1.00    7.50    --  111.00  54.00 -69.18   91
 33  \w     81.00 178.00   1.00    7.50    --  111.00  77.00   0.00   97
 34  \w     85.00 178.00   1.00    7.50    --  111.00  61.00 150.00   93
 35  \w     85.00 178.00   1.00    7.50    --  111.00  61.00-120.00   93
 36  \w     85.00 178.00   1.00    7.50    --  111.00  61.00-180.00   93
 37  \w     85.00 178.00   1.00    7.50    --  111.00  61.00  60.00   93
 38  \w     81.00 178.00   1.00    7.50    --  111.00  77.00  30.00   97
 39  \w     81.00 178.00   1.00    7.50    --  111.00  77.00 120.00   97
 40  \w     85.00 178.00   1.00    7.50    --  111.00  61.00 -30.00   93
 41  \w     81.00 178.00   1.00    7.50    --  111.00  77.00-180.00   97
 42  \w     85.00 178.00   1.00    7.50    --  111.00  61.00 -90.00   93
 43  \w     82.00 178.00   1.00    7.50    --  111.00  71.00 103.00   96
 44  \w     81.00 178.00   1.00    7.50    --  111.00  77.00-150.00   97
 45  \w     81.00 178.00   1.00    7.50    --  111.00  75.00-159.12   97
 46  \w     85.00 178.00   1.00    7.50    --  111.00  61.00  30.00   93
 47  \w     83.00 178.00   1.00    7.50    --  111.00  70.00   1.51   95
 48  \w     85.00 178.00   1.00    7.50    --  111.00  59.00 -49.62   93
 49  \w     18.00 112.00   1.00    1.75    --   43.20  57.00  90.00   94
 50  \w     23.00 114.00   1.00    1.75    --   43.20  38.00-180.00   91
 51  \w     18.00 112.00   1.00    1.75    --   43.20  57.00 -90.00   94
 52  \w     13.00 115.00   1.00    1.75    --   43.20  77.00 -90.00  102
 53  \w     23.00 114.00   1.00    1.75    --   43.20  38.00 -30.00   91
 54  \w     18.00 112.00   1.00    1.75    --   43.20  57.00-180.00   94
 55  \w     13.00 115.00   1.00    1.75    --   43.20  77.00-180.00  102
 56  \w    -42.00 129.00   1.00    1.75    --   43.20   0.00-180.00  171
 57  \w    -42.00 129.00   1.00    1.75    --   43.20   0.00-150.00  171
 58  \w    -42.00 129.00   1.00    1.75    --   43.20   0.00-120.00  171
 59  \w    -42.00 129.00   1.00    1.75    --   43.20   0.00 -90.00  171
 60  \w    -42.00  70.00   1.00    1.75    --   43.20   0.00 -60.00  112
 61  \w     18.00 112.00   1.00    1.75    --   43.20  57.00   0.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1443973000
_diffrn_orient_matrix_UB_12      0.0825993000
_diffrn_orient_matrix_UB_13      0.0539356000
_diffrn_orient_matrix_UB_21      0.0019395000
_diffrn_orient_matrix_UB_22      -0.0982921000
_diffrn_orient_matrix_UB_23      0.0426856000
_diffrn_orient_matrix_UB_31      0.0969347000
_diffrn_orient_matrix_UB_32      -0.0535746000
_diffrn_orient_matrix_UB_33      -0.0519987000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            68190
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.996
_diffrn_reflns_theta_min         2.473
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.584
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.136
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       needle
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.387
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+2.2614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6873
_reflns_number_total             7465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00662_si_011.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        1897.19(9)
_cod_database_code               4089045
_chemical_oxdiff_formula         'C38 H44 Cl1 I2 N3 Pd'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2015-11-30
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.683
_shelx_hkl_checksum              5604
_shelx_res_checksum              81903
_shelxl_version_number           2014-3