Preparation of Benzyne Complexes of Group 10 Metals by Intramolecular Suzuki Coupling of ortho-Metalated Phenylboronic Esters: Molecular Structure of the First Benzyne-Palladium(0) Complex
Mikael Retbøll; Alison J. Edwards; A. David Rae; Anthony C. Willis; Martin A. Bennett; Eric Wenger; Journal of the American Chemical Society 124 (2002) 8348–8360; doi:10.1021/ja0264091

data_4114952
_publ_contact_author_address
;
R.S.C. A.N.U.
;
_publ_contact_author_name        'Eric Wenger'
_publ_section_title
;
 Preparation of Benzyne Complexes of Group 10 Metals by Intramolecular
 Suzuki Coupling of ortho-Metalated Phenylboronic Esters: Molecular
 Structure of the First Benzyne-Palladium(0) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8348
_journal_page_last               8360
_journal_paper_doi               10.1021/ja0264091
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C42 H70 Ni P2 + C6 H6 '
_chemical_formula_sum            'C48 H76 Ni P2'
_chemical_formula_weight         773.794
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             01-20-11
_audit_creation_method           'maXus +CRYSTALS_ver_12-03-99'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1217(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.99820(10)
_cell_length_b                   28.9827(3)
_cell_length_c                   15.1034(2)
_cell_measurement_reflns_used    90596
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     4351.63(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) + maXus(Mackay et al., 1999)
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR97 (Altomare et al, 1999) 
;
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.05691
_diffrn_orient_matrix_UB_12      -0.04549
_diffrn_orient_matrix_UB_13      0.06936
_diffrn_orient_matrix_UB_21      -0.02844
_diffrn_orient_matrix_UB_22      -0.01009
_diffrn_orient_matrix_UB_23      0.01672
_diffrn_orient_matrix_UB_31      0.00285
_diffrn_orient_matrix_UB_32      -0.05900
_diffrn_orient_matrix_UB_33      -0.03074
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            75271
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0867
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         3614
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.029526
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
0.474    0.211    0.245    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0452
_reflns_d_resolution_high        0.62
_reflns_d_resolution_low         1.86
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3614
_reflns_number_total             9960
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ja0264091_s2_4.cif
_cod_data_source_block           EXW21z
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C48 H76 Ni P2 '
_cod_database_code               4114952