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_4114951
_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         'C38 H64 B Br O2 P2 Pd '
_chemical_formula_sum            'C38 H64 B Br O2 P2 Pd'
_chemical_formula_weight         811.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2001-06-14
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2001-06-14 - Report on C38 H64 B Br O2 P2 Pd (3d)
              by Anthony C. Willis and A. David Rae
              for Mikael K. Retboll and Eric Wenger
2001-06-14 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6632(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7037(1)
_cell_length_b                   12.4606(1)
_cell_length_c                   36.1403(4)
_cell_measurement_reflns_used    61277
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.263
_cell_volume                     3906.56(7)
_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      200.0
_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      -0.08926
_diffrn_orient_matrix_UB_12      -0.05305
_diffrn_orient_matrix_UB_13      0.05006
_diffrn_orient_matrix_UB_21      -0.03183
_diffrn_orient_matrix_UB_22      0.07125
_diffrn_orient_matrix_UB_23      0.01875
_diffrn_orient_matrix_UB_31      -0.01539
_diffrn_orient_matrix_UB_32      -0.00080
_diffrn_orient_matrix_UB_33      -0.02309
_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  0.045
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            46354
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.743
_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    1.380
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.25
_refine_diff_density_min         -1.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.5846
_refine_ls_goodness_of_fit_ref   2.2637
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     120
_refine_ls_number_reflns         5487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0631
_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         0.1397
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                5487
_reflns_number_total             6896
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja0264091_s2_3.cif
_cod_data_source_block           mxr4
_cod_original_cell_volume        3906.56(6)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C38 H64 B Br O2 P2 Pd '
_cod_database_code               4114951