Highly Active Pd(II) PCP-Type Catalysts for the Heck Reaction
Manuela Ohff; Andreas Ohff; Milko E. van der Boom; David Milstein; Journal of the American Chemical Society 119 (1997) 11687–11688; doi:10.1021/ja9729692

data_4117066
_publ_section_title
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 Highly Active Pd(II) PCP-Type Catalysts for the Heck Reaction
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11687
_journal_page_last               11688
_journal_paper_doi               10.1021/ja9729692
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C38 H58 F3 O2 P2 Pd'
_chemical_formula_weight         772.18
_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
_cell_angle_alpha                107.90(3)
_cell_angle_beta                 109.15(3)
_cell_angle_gamma                95.55(3)
_cell_formula_units_Z            2
_cell_length_a                   11.738(2)
_cell_length_b                   12.183(2)
_cell_length_c                   15.259(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1913.6(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0119
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7131
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    0.614
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_F_000             810
_refine_diff_density_max         1.604
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_obs          0.0645
_refine_ls_shift/esd_max         -0.027
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+3.0117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1799
_refine_ls_wR_factor_obs         0.1523
_reflns_number_observed          5076
_reflns_number_total             7026
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9729692_1.cif
_cod_data_source_block           m88
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+3.0117P] 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^)+(0.0936P)^2^+3.0117P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1913.6(6)
_cod_database_code               4117066