Ligand driven σ,π-η3 structural rearrangements of organopalladium complexes: their relevance to the CO/styrene copolymerisation reaction
Milani, Barbara; Paronetto, Federica; Zangrando, Ennio; Journal of the Chemical Society, Dalton Transactions  (2000) 3055–; doi:10.1039/b005492p

data_7010055
_publ_section_title
;
 Ligand driven \s,\p-\h3 structural rearrangements of organopalladium
 complexes: their relevance to the CO/styrene copolymerisation reaction
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3055
_journal_paper_doi               10.1039/b005492p
_journal_year                    2000
_chemical_formula_moiety
'([(CH2)3 (P(C6H5)2)2] (C9 H15 O) Pd 1+ ) (P F6 1-)'
_chemical_formula_structural
'[(P(Ph)2)-(CH2)3-(P(Ph)2) (C8 H12 (O C H3)) Pd] (P F6)'
_chemical_formula_sum            'C36 H41 F6 O P3 Pd'
_chemical_formula_weight         803.00
_chemical_name_systematic
;
bis[1,3-(diphenylphosphino)propane]-
[eta-3-(1-methoxy-2-cicloocten-1-yl]-palladium(II) 
exafluorophosphate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.01(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.716(2)
_cell_length_b                   18.008(2)
_cell_length_c                   18.978(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      12.5
_cell_volume                     3626.5(11)
_computing_cell_refinement       'CELDIM (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'WinGX 1.63 (Farrugia, 1999)'
_computing_molecular_graphics    'Ortep3/Windows (Farrugia,1997)'
_computing_publication_material  'WinGX 1.63 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega 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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8741
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7874
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.975
_refine_ls_goodness_of_fit_obs   1.189
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_restrained_S_obs      1.189
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1389
_refine_ls_wR_factor_obs         0.1256
_reflns_number_observed          4692
_reflns_number_total             8213
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b005492p.txt
_cod_data_source_block           codp
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0762P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7010055
_diffrn_standards_decay_corr_max 1.022
_diffrn_standards_decay_corr_min 0.943