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_4021802
_publ_section_title
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 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            'C17 H22 I N5'
_chemical_formula_weight         423.30
_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                103.268(2)
_cell_angle_beta                 96.557(2)
_cell_angle_gamma                109.701(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0453(12)
_cell_length_b                   9.4904(13)
_cell_length_c                   12.2205(17)
_cell_measurement_reflns_used    3323
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.336
_cell_measurement_theta_min      4.891
_cell_volume                     940.0(2)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5593
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58914
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.292
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0397P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                3526
_reflns_number_total             3989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060795dsi20060414_122728_1.cif
_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_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4021802