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_7022718
_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            'C30 H38 Cl6 N4 Pd'
_chemical_formula_weight         773.74
_chemical_name_systematic
;
?
;
_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                 91.862(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8530(16)
_cell_length_b                   12.240(2)
_cell_length_c                   15.180(3)
_cell_measurement_reflns_used    33188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      1.14
_cell_volume                     3315.4(9)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_computing_molecular_graphics
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 1998)'
;
_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 Q210'
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'synchrotron BM'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49147
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.369
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1843P)^2^+12.9847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2597
_refine_ls_wR_factor_ref         0.2755
_reflns_number_gt                5438
_reflns_number_total             6716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32895c.txt
_cod_data_source_block           d:\as31ch42
_cod_original_cell_volume        3315.4(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7022718