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_4114949
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       WENGER@RSC.ANU.EDU.AU
_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         ' C48 H46 B1 Br1 Ni1 O2 P2, 1.5 C7 H8 '
_chemical_formula_sum            'C58.5 H58 B Br Ni O2 P2'
_chemical_formula_weight         1004.39
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             01-18-10
_audit_creation_method           'CRYSTALS_ver_12-03-99 + maXus'
_audit_update_record
;
Preparation of Benzyne Complexes of Group 10 Metals by 
Intramolecular Suzuki Coupling of ortho-Metallated Phenylboronic 
Esters: Molecular Structure of the First Benzyne-Palladium(0) Complex
by Mikael Retb\/oll, Alison J. Edwards, A. David Rae, Anthony C. Willis, 
Martin A. Bennett and Eric Wenger
;
_cell_angle_alpha                85.1981(4)
_cell_angle_beta                 88.5163(4)
_cell_angle_gamma                72.3410(4)
_cell_formula_units_Z            2
_cell_length_a                   9.92980(10)
_cell_length_b                   12.95530(10)
_cell_length_c                   20.4921(3)
_cell_measurement_reflns_used    72803
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2503.14(5)
_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)  + maXus(Mackay et al., 1999)
;
_computing_structure_solution
; 
SIR97 (Altomare et al, 1999)
;
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.09320
_diffrn_orient_matrix_UB_12      -0.03402
_diffrn_orient_matrix_UB_13      -0.03640
_diffrn_orient_matrix_UB_21      0.05383
_diffrn_orient_matrix_UB_22      -0.00637
_diffrn_orient_matrix_UB_23      -0.06054
_diffrn_orient_matrix_UB_31      0.00921
_diffrn_orient_matrix_UB_32      -0.04455
_diffrn_orient_matrix_UB_33      0.01812
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75844
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0706
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         5981
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.007106
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
0.311    0.923E-010.137    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0318
_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              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5981
_reflns_number_total             11494
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            ja0264091_s2_1.cif
_cod_data_source_block           EXW19z
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C58.50 H58 B1 Br1 Ni1 O2 P2 '
_cod_database_code               4114949