Selective and adaptable access to N,N'-asymmetrically substituted imidazol-2-ylidene bis-NHC ligands: Pd(II) complexes featuring wide variation in N-alkyl and aryl steric bulk.
Gardiner, Michael G.; Ho, Curtis C.; Mackay, Felicity M.; McGuinness, David S.; Tucker, Matthew; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7447–7457; doi:10.1039/c3dt32895c

data_7022715
_publ_section_title
;
 Selective and adaptable access to N,N'-asymmetrically substituted
 imidazol-2-ylidene bis-NHC ligands: Pd(II) complexes featuring wide
 variation in N-alkyl and aryl steric bulk.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7447
_journal_page_last               7457
_journal_paper_doi               10.1039/c3dt32895c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C36 H52 I2 N4 O2'
_chemical_formula_weight         826.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.474(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4130(12)
_cell_length_b                   12.4050(16)
_cell_length_c                   17.8960(8)
_cell_measurement_reflns_used    36688
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.94
_cell_measurement_theta_min      1.17
_cell_volume                     3864.4(6)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_computing_molecular_graphics
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)'
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'ADSC Q315'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  '3-ID1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'Synchrotron ID'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80553
_diffrn_reflns_theta_full        30.94
_diffrn_reflns_theta_max         30.94
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.458
_refine_diff_density_min         -2.004
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         11973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+7.5168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1537
_reflns_number_gt                8050
_reflns_number_total             11973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32895c.txt
_cod_data_source_block           d:\30ch40a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7022715