Pyridyl-Supported Pyrazolyl-N-Heterocyclic Carbene Ligands and the Catalytic Activity of Their Palladium Complexes in Suzuki-Miyaura Reactions
Fanlong Zeng; Zhengkun Yu; Journal of Organic Chemistry 71 (2006) 5274–5281; doi:10.1021/jo060795d

data_4021805
_publ_section_title
;
 Pyridyl-Supported Pyrazolyl-N-Heterocyclic Carbene Ligands and the
 Catalytic Activity of Their Palladium Complexes in Suzuki-Miyaura Reactions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5274
_journal_page_last               5281
_journal_paper_doi               10.1021/jo060795d
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C26 H34 Cl2 N5 O1.5 Pd'
_chemical_formula_weight         617.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.812(3)
_cell_length_b                   15.838(2)
_cell_length_c                   14.956(2)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.382
_cell_measurement_theta_min      5.144
_cell_volume                     5403.8(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(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  0.1584
_diffrn_reflns_av_sigmaI/netI    0.1275
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30407
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78162
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.096
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                2975
_reflns_number_total             5888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060795dsi20060414_122728_4.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C26 H34 Cl2 N5 O1.50 Pd'
_cod_database_code               4021805