Investigations of Benzyl and Aryl Palladium Complexes with Pendant Hydroxy Substituents and Their Transformation into Benzolactones on Carbonylation
Lindsell, W. Edward; Palmer, Daniel D.; Preston, Peter N.; Rosair, Georgina M.; Jones, Ray V. H.; Whitton, Alan J.; Organometallics 24 (2005) 1119–; doi:10.1021/om049131p

data_4075692
_publ_section_title
;
 Investigations of Benzyl and Aryl Palladium Complexes with Pendant
 Hydroxy Substituents and Their Transformation into Benzolactones on
 Carbonylation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1119
_journal_paper_doi               10.1021/om049131p
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C56 H54 O8 P2 Pd2, 4(C H2 Cl2)'
_chemical_formula_sum            'C60 H62 Cl8 O8 P2 Pd2'
_chemical_formula_weight         1469.44
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.594(9)
_cell_angle_beta                 71.833(11)
_cell_angle_gamma                89.336(11)
_cell_formula_units_Z            1
_cell_length_a                   10.3038(11)
_cell_length_b                   11.9421(14)
_cell_length_c                   14.743(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      15.03
_cell_measurement_theta_min      3.16
_cell_volume                     1581.6(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6348
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.8751
_exptl_absorpt_correction_T_min  0.7617
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et al.,1968'
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+3.7332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                4648
_reflns_number_total             5373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049131psi20041109_111226.cif
_cod_data_source_block           25
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
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_cell_volume        1581.6(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075692