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_4114953
_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_compound_source
;
?
;
_chemical_formula_moiety         ' C42 H70 P2 Pd, C6 H6 '
_chemical_formula_sum            'C48 H76 P2 Pd'
_chemical_formula_weight         821.48
_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
_audit_creation_date             02-30-01
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2002-01-30 - Report on C48 H76 P2 Pd
              by Anthony C. Willis
              for  Mikael K. Retboll and Eric Wenger
2002-01-30 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1577(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1512(1)
_cell_length_b                   29.5301(3)
_cell_length_c                   15.0770(2)
_cell_measurement_reflns_used    112853
_cell_measurement_temperature    200
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1
_cell_volume                     4484.35(9)
_computing_cell_refinement
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
  COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
teXsan (MSC, 1992-1997)
;
_computing_publication_material
;
  CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
  CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
  SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            68283
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' red  '
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             1756.482
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.10
_refine_diff_density_min         -1.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.8962
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         4548
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.013088
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979,
0.260    -3.46    -.173    -1.50
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0350
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4548
_reflns_number_total             8375
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ja0264091_s2_5.cif
_cod_data_source_block           mxr9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C48 H76 P2 Pd1 '
_cod_database_code               4114953