Practical Heck-Mizoroki coupling protocol for challenging substrates mediated by an N-heterocyclic carbene-ligated palladacycle.
Kantchev, Eric Assen B.; Peh, Guang-Rong; Zhang, Chi; Ying, Jackie Y.; Organic letters 10 (2008) 3949–3952; doi:10.1021/ol8012809

data_1504806
_publ_section_title
;
 Practical Heck-Mizoroki coupling protocol for challenging substrates
 mediated by an N-heterocyclic carbene-ligated palladacycle.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              3949
_journal_page_last               3952
_journal_paper_doi               10.1021/ol8012809
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C30 H36.5 Cl N3 O0.25 Pd'
_chemical_formula_weight         584.97
_chemical_name_common            IMes-Pd(dmba)Cl
_chemical_name_systematic
; 
 (chloro (1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene)
(k2-N,C-dimethylbenzylamine)palladium (II) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.2240(10)
_cell_angle_beta                 71.8720(10)
_cell_angle_gamma                84.4660(10)
_cell_formula_units_Z            4
_cell_length_a                   13.5773(6)
_cell_length_b                   13.5923(6)
_cell_length_c                   15.9863(7)
_cell_measurement_reflns_used    5576
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.37
_cell_volume                     2790.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35633
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.8847
_exptl_absorpt_correction_T_min  0.7987
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         12801
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.8171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                10935
_reflns_number_total             12801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol8012809_si_001.cif
_cod_data_source_block           6419a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30 H36.50 Cl N3 O0.25 Pd'
_cod_database_code               1504806