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_4089044
_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 Cl0.15 I1.85 N3 Pd'
_chemical_formula_sum            'C38 H45 Cl0.15 I1.85 N3 Pd'
_chemical_formula_weight         890.61
_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             2015-12-17
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                101.143(4)
_cell_angle_beta                 96.316(4)
_cell_angle_gamma                102.930(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2685(3)
_cell_length_b                   11.7625(4)
_cell_length_c                   18.2798(8)
_cell_measurement_reflns_used    56433
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      30.1070
_cell_measurement_theta_min      1.9120
_cell_volume                     1881.10(13)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9968
_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    -46.00  96.00   1.00    5.03    --   25.04   0.00 120.00  142
  2  \w     -4.00  94.00   1.00    5.03    --   25.04  77.00-180.00   98
  3  \w     -4.00  94.00   1.00    5.03    --   25.04  77.00  60.00   98
  4  \w    -43.00  44.00   1.00    5.03    --   25.04 -57.00  30.00   87
  5  \w      3.00  96.00   1.00    5.03    --   25.04  38.00-180.00   93
  6  \w    -20.00  66.00   1.00    5.03    --   25.04 -99.00 -30.00   86
  7  \w     -4.00  94.00   1.00    5.03    --   25.04  77.00-120.00   98
  8  \w    -20.00  66.00   1.00    5.03    --   25.04 -99.00-120.00   86
  9  \w      7.00  93.00   1.00    5.03    --   25.04  57.00   0.00   86
 10  \w    -46.00  47.00   1.00    5.03    --   25.04 -38.00  90.00   93
 11  \w     -8.00  73.00   1.00    5.03    --   25.04-113.00 117.53   81
 12  \w    -95.00  48.00   1.00    5.03    --  -23.50   0.00 -60.00  143
 13  \w    -95.00  48.00   1.00    5.03    --  -23.50   0.00 -90.00  143
 14  \w    -97.00 -35.00   1.00    5.03    --  -23.50-178.00-120.00   62
 15  \w    -97.00 -35.00   1.00    5.03    --  -23.50-178.00   0.00   62
 16  \w    -95.00  48.00   1.00    5.03    --  -23.50   0.00-180.00  143
 17  \w    -95.00  48.00   1.00    5.03    --  -23.50   0.00-150.00  143
 18  \w    -95.00  48.00   1.00    5.03    --  -23.50   0.00-120.00  143
 19  \w     34.00 100.00   1.00    5.03    --   25.04-178.00-120.00   66
 20  \w      7.00  93.00   1.00    5.03    --   25.04  57.00 120.00   86
 21  \w     -4.00  94.00   1.00    5.03    --   25.04  77.00 -60.00   98
 22  \w    -95.00  31.00   1.00    5.03    --  -23.50   0.00   0.00  126
 23  \w    -95.00  48.00   1.00    5.03    --  -23.50   0.00 -30.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0787877000
_diffrn_orient_matrix_UB_12      0.0217131000
_diffrn_orient_matrix_UB_13      0.0033322000
_diffrn_orient_matrix_UB_21      0.0084386000
_diffrn_orient_matrix_UB_22      -0.0036949000
_diffrn_orient_matrix_UB_23      0.0384278000
_diffrn_orient_matrix_UB_31      0.0069140000
_diffrn_orient_matrix_UB_32      -0.0595293000
_diffrn_orient_matrix_UB_33      -0.0107871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            110480
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.823
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.709
_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    1.572
_exptl_crystal_description       fragment
_exptl_crystal_F_000             881.5
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.126
_refine_diff_density_max         2.945
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0273P)^2^+3.4228P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10194
_reflns_number_total             10943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00662_si_010.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        1881.08(14)
_cod_database_code               4089044
_chemical_oxdiff_formula         'C38 H46 I2 N2 Pd'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_date_sample_data_collection 2015-12-16
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.801
_shelx_hkl_checksum              48763
_shelx_res_checksum              30182
_shelxl_version_number           2013-2