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_4114950
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Eric Wenger '
_publ_contact_author_phone       ' 61 2 6125 4425 '
_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_formula_moiety         'C48 H82 B Br O2 P2 Pd '
_chemical_formula_sum            'C48 H82 B Br O2 P2 Pd'
_chemical_formula_weight         950.24
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_date             2001-04-17
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
mxr3_-_numabs/averaged
2001-04-17 - Report on C48 H82 B Br O2 P2 Pd (3b)
             by    Anthony C. Willis
             for Mikael K. Retboll and Eric Wenger
2001-04-19 - passes checkcif tests with minor warnings
             *  note disorder of C6 H12 B O2 unit across y = 1/4.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3184(3)
_cell_length_b                   22.7581(4)
_cell_length_c                   10.5870(1)
_cell_measurement_reflns_used    114415
_cell_measurement_temperature    200.
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.546
_cell_volume                     4895.52(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution
;
PATTY in DIRDIF92  (Beurskens, 1992)
;
_diffrn_ambient_temperature      200.0
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            59885
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008.00
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.100
_refine_ls_goodness_of_fit_ref   1.993
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.064
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.086
_refine_ls_wR_factor_ref         0.077
_reflns_number_gt                4042
_reflns_number_total             4440
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ja0264091_s2_2.cif
_cod_data_source_block           mxr3
_cod_original_cell_volume        4895.5(1)
_cod_original_sg_symbol_Hall     -p_2ac_2n
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C48 H82 B Br O2 P2 Pd '
_cod_database_code               4114950