Highly active PdII cyclometallated imine catalysts for the Heck reaction
Ohff, Manuela; Ohff, Andreas; Milstein, David; Chemical Communications  (1999) 357–; doi:10.1039/a809883b

data_7110445
_publ_section_title
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 Highly active PdII cyclometallated imine catalysts for the Heck reaction
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              357
_journal_paper_doi               10.1039/a809883b
_journal_year                    1999
_chemical_formula_sum            'C26 H28 F6 N2 O4 Pd2'
_chemical_formula_weight         759.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.044(3)
_cell_length_b                   16.976(3)
_cell_length_c                   19.725(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.21
_cell_volume                     5655.1(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega scan'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23194
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.346
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.107
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     733
_refine_ls_number_reflns         12988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_obs          0.0618
_refine_ls_shift/esd_max         0.068
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1464
_refine_ls_wR_factor_obs         0.1068
_reflns_number_observed          8420
_reflns_number_total             12993
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809883bsup1.cif
_cod_data_source_block           m104
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] 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^)+(0.0465P)^2^+0.0000P] 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        5655.1(18)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110445