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_4114954
_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_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         'C58 H100 P4 Pd2, C7 H8'
_chemical_formula_sum            'C65 H108 P4 Pd2'
_chemical_formula_weight         1226.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2001-06-25
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2001-06-25 - Report on C65 H108 P4 Pd2 (6)
             by Anthony C. Willis and A. David Rae
             for Mikael K. Retboll and Eric Wenger
2001-06-26 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                80.6763(5)
_cell_angle_beta                 85.7074(4)
_cell_angle_gamma                89.8127(6)
_cell_formula_units_Z            4
_cell_length_a                   13.9055(2)
_cell_length_b                   19.0192(2)
_cell_length_c                   24.0778(3)
_cell_measurement_reflns_used    332477
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.546
_cell_volume                     6265.88(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'RAELS2000 (2000)'
_computing_structure_solution
;
PATTY in DIRDIF92  (Beurskens, 1992)
;
_diffrn_ambient_temperature      150.0
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.00903
_diffrn_orient_matrix_UB_12      0.00386
_diffrn_orient_matrix_UB_13      0.07145
_diffrn_orient_matrix_UB_21      0.03612
_diffrn_orient_matrix_UB_22      -0.03912
_diffrn_orient_matrix_UB_23      -0.00196
_diffrn_orient_matrix_UB_31      0.02512
_diffrn_orient_matrix_UB_32      0.03293
_diffrn_orient_matrix_UB_33      -0.00816
_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  0.059
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            124400
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       rod
_exptl_crystal_F_000             2600.00
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.28
_refine_diff_density_min         -1.95
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.1163
_refine_ls_goodness_of_fit_ref   1.8672
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     244
_refine_ls_number_reflns         17995
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.3
_refine_ls_shift/su_mean         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0016|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1412
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                17995
_reflns_number_total             28627
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja0264091_s2_6.cif
_cod_data_source_block           mxr5
_cod_original_cell_volume        6265.9(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C65 H108 P4 Pd2 '
_cod_database_code               4114954