Why excess cyanide can be detrimental to Pd-catalyzed cyanation of haloarenes. Facile formation and characterization of [Pd(CN)(3)(H)](2-) and [Pd(CN)(3)(Ph)](2-).
Dobbs, Kerwin D; Marshall, William J; Grushin, Vladimir V; Journal of the American Chemical Society 129 (2007) 30–31; doi:10.1021/ja066931d

data_4101764
_publ_section_title
;
 Why excess cyanide can be detrimental to Pd-catalyzed cyanation of
 haloarenes. Facile formation and characterization of [Pd(CN)(3)(H)](2-)
 and [Pd(CN)(3)(Ph)](2-).
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              30
_journal_page_last               31
_journal_paper_doi               10.1021/ja066931d
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C123.5 H100.5 N8.5 P6 Pd1.5'
_chemical_formula_weight         2049.04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.699(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   63.105(9)
_cell_length_b                   15.236(3)
_cell_length_c                   21.642(3)
_cell_measurement_temperature    293(2)
_cell_volume                     20799(6)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1559
_diffrn_reflns_limit_h_max       74
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30987
_diffrn_reflns_theta_full        25.55
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       wedge
_exptl_crystal_F_000             8480
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         31015
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.367
_refine_ls_R_factor_all          0.1843
_refine_ls_R_factor_gt           0.1043
_refine_ls_shift/su_max          0.155
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2563
_refine_ls_wR_factor_ref         0.3089
_reflns_number_gt                15483
_reflns_number_total             31015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066931dsi20060926_050342.cif
_cod_data_source_block           05187
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C123.50 H100.50 N8.50 P6 Pd1.50'
_cod_database_code               4101764