Cyclopalladated imine catalysts in Heck arylation: search for the catalytic species
Nowotny, Mathias; Hanefeld, Ulf; Koningsveld, Henk van; Maschmeyer, Thomas; Chemical Communications  (2000) 1877–; doi:10.1039/b004502k

data_7111027
_publ_section_title
;
 Cyclopalladated imine catalysts in Heck arylation: search for the
 catalytic species
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1877
_journal_paper_doi               10.1039/b004502k
_journal_year                    2000
_chemical_formula_sum            'C17 H17 F6 N O2 Pd'
_chemical_formula_weight         487.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                77.57(7)
_cell_angle_beta                 87.72(4)
_cell_angle_gamma                79.55(14)
_cell_formula_units_Z            2
_cell_length_a                   8.314(6)
_cell_length_b                   9.565(5)
_cell_length_c                   12.293(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.2
_cell_measurement_theta_min      13.0
_cell_volume                     938.8(10)
_computing_cell_refinement       'cad4 SETANG LS'
_computing_data_collection       'cad4 DATCOL'
_computing_data_reduction        'xtal DIFDAT ADDREF SORTRF'
_computing_molecular_graphics    'xtal ORTEP'
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    'xtal FOURR'
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .009
_diffrn_reflns_av_sigmaI/netI    .016
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5916
_diffrn_reflns_reduction_process 'No monochr Lp applied'
_diffrn_reflns_theta_max         30.26
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.057
_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
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_exptl_crystal_size_max          .27
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .18
_refine_diff_density_max         .869
_refine_diff_density_min         -.893
_refine_ls_extinction_coef       .00000
_refine_ls_goodness_of_fit_all   2.651
_refine_ls_goodness_of_fit_ref   2.947
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .059
_refine_ls_R_factor_gt           .037
_refine_ls_shift/su_max          .592
_refine_ls_shift/su_mean         .04
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     1/sigma
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .037
_refine_ls_wR_factor_ref         .037
_reflns_d_resolution_high        .705
_reflns_d_resolution_low         11.976
_reflns_Friedel_coverage         0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4488
_reflns_number_total             5559
_reflns_threshold_expression     'F    > 2.50 sig(F   )'
_cod_data_source_file            b004502ksup1.cif
_cod_data_source_block           MAT1
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_original_formula_sum        'C17 H17 F6 N1 O2 Pd1'
_cod_database_code               7111027