Reactivity of hydroxo complexes of palladium(II) towards nitriles: formation of carboxamide and imino ether derivatives of palladium(II)
Ruiz, José; Cutillas, Natalia; Rodríguez, Venancio; Sampedro, José; López, Gregorio; Chaloner, Penny A.; Hitchcock, Peter B.; Journal of the Chemical Society, Dalton Transactions  (1999) 2939–; doi:10.1039/a903262b

data_7027497
_publ_section_title
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 Reactivity of hydroxo complexes of palladium(II) towards nitriles:
 formation of carboxamide and imino ether derivatives of palladium(II)
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2939
_journal_paper_doi               10.1039/a903262b
_journal_year                    1999
_chemical_formula_sum            'C18 H12 F10 N2 O2 Pd'
_chemical_formula_weight         584.70
_chemical_name_common
; 

 [Pd(C6F5)2{NC(Me)OMe}2] 

;
_chemical_name_systematic
; 

  ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_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                 94.71(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.243(3)
_cell_length_b                   14.634(6)
_cell_length_c                   15.865(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2138.7(12)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6541
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.073
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_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_reflns         6204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_obs          0.0470
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.6716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1212
_refine_ls_wR_factor_obs         0.1010
_reflns_number_observed          3852
_reflns_number_total             6204
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903262bsup1.cif
_cod_data_source_block           feb1895
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+1.6716P] 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^)+(0.0463P)^2^+1.6716P] 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      P2(1)/n
_cod_database_code               7027497