Bimetallic Pd(III) complexes in palladium-catalysed carbon-heteroatom bond formation
David C. Powers; Tobias Ritter; Nature Chemistry 1 (2009) 302–309; doi:10.1038/nchem.246

data_1551900
_publ_section_title
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 Bimetallic Pd(III) complexes in palladium-catalysed carbon-heteroatom
 bond formation
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              302
_journal_page_last               309
_journal_paper_doi               10.1038/nchem.246
_journal_volume                  1
_journal_year                    2009
_chemical_compound_source        'chemical synthesis'
_chemical_formula_iupac
;
[Pd (C2 H3 O2) (C13 H8 N) Cl]2 . (C6 H5 I) . (C H2 Cl2)
;
_chemical_formula_moiety
;
((Pd 3+) (C2 H3 O2 1-) (C13 H8 N 1-) (Cl 1-))2, C6 H5 I, C H2 Cl2
;
_chemical_formula_structural
;
(Pd (C2 H3 O2) (C13 H8 N) Cl)2 (C6 H5 I) (C H2 Cl2)
;
_chemical_formula_sum            'C37 H29 Cl4 I N2 O4 Pd2'
_chemical_formula_weight         1047.12
_chemical_name_common            tr040
_chemical_name_systematic
; 
(Acetato){10-benzo[<i>h</i>]quinolinato)chloropalladium(III) Dimer
. Iodobenzene . Dichloromethane Solvate
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 117.053(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7605(5)
_cell_length_b                   17.7508(5)
_cell_length_c                   14.1762(4)
_cell_measurement_reflns_used    5273
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.99
_cell_measurement_theta_min      2.29
_cell_volume                     3756.1(2)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006b)'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_data_reduction
;
SAINT V7.34A (Bruker AXS, 2006b), SADABS (Bruker AXS, 2004),
PLATON (Spek, 2003)
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL v6.12 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w scans, 2762 0.5\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37194
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.106
_exptl_absorpt_correction_T_max  0.9395
_exptl_absorpt_correction_T_min  0.7430
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The Squeeze/Bypass procedure yielded total void volumes and electron
counts of 639.4 \%A^3^ and 203 e, respectively.  For Z = 4, this
gives V~l~ = 159.8 \%A^3^ and 51 e.  These values may be compared to
the expectation values of V~l~ = 186.5 \%A^3^ and 94 e, V~l~ = 192.1
\%A^3^ and 42 e, and V~l~ = 106.8 \%A^3^ and 42 e for iodobenzene,
pentane and dichloromethane, respectively.  The void volume observed,
i.e., 159.8 \%A^3^, is too small to accommodate iodobenzene or pentane.
Hence, the Squeeze/Bypass results suggest that, of these three
possibilities, dichloromethane is the probable solvent in the lattice.

Note 1.  The researchers have indicated that dichloromethane resonances
were observed in their NMR spectrum for the compound.

Note 2.  In a parallel test, the iodobenzene site was squeezed out
yielding V~l~ = 191.9 \%A^3^ and 91 e.  These observed values are in
excellent agreement with the expectation values of V~l~ = 186.5 \%A^3^
and 94 e.  Hence, that parallel test gives us confidence that the
iodobenzene site is indeed occupied by an iodobenzene molecule, and
that the void volume calculated for the solvent site, i.e., 159.8 \%A^3^,
is indeed probably reliable enough to exclude iodobenzene and pentane
as argued above.
;
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3313
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.5903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                2701
_reflns_number_total             3313
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nchem.246-s3.cif
_cod_data_source_block           tr040
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3756.13(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1551900