#------------------------------------------------------------------------------
#$Date: 2016-03-24 16:08:07 +0100 (jue 24 de mar de 2016) $
#$Revision: 179678 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/00/7000022.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7000022
loop_
_publ_author_name
'Favier, Isabelle'
'Gomez, Montserrat'
'Granell, Jaume'
'Martinez, Manuel'
'Solans, Xavier'
'Font-Bardia, Merce'
_publ_section_title
;
 Kinetico-mechanistic studies of C-H bond activation on new Pd
 complexes containing N,N'-chelating ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              123
_journal_page_last               132
_journal_paper_doi               10.1039/b415613g
_journal_year                    2005
_chemical_formula_sum            'C12 H17 Cl3 N2 Pd'
_chemical_formula_weight         402.03
_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-97
_cell_angle_alpha                117.14(2)
_cell_angle_beta                 100.86(2)
_cell_angle_gamma                91.26(3)
_cell_formula_units_Z            2
_cell_length_a                   7.651(4)
_cell_length_b                   10.646(2)
_cell_length_c                   10.904(2)
_cell_measurement_temperature    293(2)
_cell_volume                     770.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'four cicle diffractometer'
_diffrn_measurement_method       ω-2θ-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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4478
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0304P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                2659
_reflns_number_total             4478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b415613g.txt
_cod_data_source_block           E-2Cl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.44911(4) 0.42584(4) 0.22358(4) 0.03639(11) Uani 1 1 d . . .
Cl1 Cl -0.1130(2) -0.11381(16) -0.43877(15) 0.0791(5) Uani 1 1 d . . .
Cl2 Cl 0.54575(17) 0.21676(14) 0.20769(14) 0.0596(4) Uani 1 1 d . . .
Cl3 Cl 0.72509(15) 0.48802(16) 0.20033(15) 0.0638(4) Uani 1 1 d . . .
N1 N 0.2175(4) 0.3730(4) 0.2600(4) 0.0409(9) Uani 1 1 d . . .
N2 N 0.3559(5) 0.6202(4) 0.2559(4) 0.0455(9) Uani 1 1 d . . .
C1 C -0.0549(6) 0.0078(5) -0.2585(5) 0.0468(11) Uani 1 1 d . . .
C2 C -0.1768(6) 0.0238(5) -0.1788(5) 0.0476(12) Uani 1 1 d . . .
H2 H -0.2909 -0.0269 -0.2200 0.057 Uiso 1 1 calc R . .
C3 C -0.1299(6) 0.1159(5) -0.0360(6) 0.0457(12) Uani 1 1 d . . .
C4 C 0.0397(5) 0.1924(5) 0.0269(4) 0.0377(10) Uani 1 1 d . . .
C5 C 0.1606(6) 0.1744(5) -0.0603(5) 0.0528(13) Uani 1 1 d . . .
H5 H 0.2740 0.2263 -0.0215 0.063 Uiso 1 1 calc R . .
C6 C 0.1140(7) 0.0824(5) -0.1998(5) 0.0570(14) Uani 1 1 d . . .
H6 H 0.1963 0.0694 -0.2561 0.068 Uiso 1 1 calc R . .
C7 C 0.0771(5) 0.2849(5) 0.1794(5) 0.0387(10) Uani 1 1 d . . .
H7 H -0.0126 0.2793 0.2242 0.046 Uiso 1 1 calc R . .
C8 C 0.2125(6) 0.4625(5) 0.4091(4) 0.0458(11) Uani 1 1 d . . .
H8 H 0.3238 0.4634 0.4694 0.055 Uiso 1 1 calc R . .
H8A H 0.1150 0.4232 0.4316 0.055 Uiso 1 1 calc R . .
C9 C 0.1866(6) 0.6111(5) 0.4364(5) 0.0542(13) Uani 1 1 d . . .
H9 H 0.1844 0.6668 0.5355 0.065 Uiso 1 1 calc R . .
H9A H 0.0695 0.6084 0.3817 0.065 Uiso 1 1 calc R . .
C10 C 0.3223(6) 0.6883(5) 0.4038(5) 0.0541(13) Uani 1 1 d . . .
H10 H 0.4357 0.7039 0.4691 0.065 Uiso 1 1 calc R . .
H10A H 0.2857 0.7811 0.4237 0.065 Uiso 1 1 calc R . .
C11 C 0.1830(7) 0.5941(7) 0.1526(6) 0.0564(14) Uani 1 1 d . . .
C12 C 0.4790(7) 0.7206(6) 0.2459(6) 0.0657(15) Uani 1 1 d . . .
H12 H 0.4436 0.8142 0.2901 0.079 Uiso 1 1 calc R . .
H12A H 0.4754 0.6924 0.1483 0.079 Uiso 1 1 calc R . .
H12B H 0.5986 0.7210 0.2929 0.079 Uiso 1 1 calc R . .
H3 H -0.219(5) 0.132(4) 0.028(4) 0.022(9) Uiso 1 1 d . . .
H11 H 0.193(4) 0.550(4) 0.043(4) 0.019(9) Uiso 1 1 d . . .
H11A H 0.141(7) 0.681(5) 0.201(5) 0.068(18) Uiso 1 1 d . . .
H11B H 0.088(5) 0.523(4) 0.147(4) 0.032(11) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd N2 87.30(15) . . ?
N1 Pd Cl3 175.14(11) . . ?
N2 Pd Cl3 94.20(11) . . ?
N1 Pd Cl2 89.50(11) . . ?
N2 Pd Cl2 174.77(12) . . ?
Cl3 Pd Cl2 88.66(6) . . ?
C7 N1 C8 117.0(3) . . ?
C7 N1 Pd 133.0(3) . . ?
C8 N1 Pd 109.9(3) . . ?
C12 N2 C11 108.0(4) . . ?
C12 N2 C10 108.2(4) . . ?
C11 N2 C10 108.9(4) . . ?
C12 N2 Pd 115.6(3) . . ?
C11 N2 Pd 110.0(3) . . ?
C10 N2 Pd 105.9(3) . . ?
C2 C1 C6 121.3(4) . . ?
C2 C1 Cl1 118.9(4) . . ?
C6 C1 Cl1 119.8(4) . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3 122(2) . . ?
C4 C3 H3 117(2) . . ?
C3 C4 C5 117.8(4) . . ?
C3 C4 C7 116.7(4) . . ?
C5 C4 C7 125.5(4) . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C1 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
N1 C7 C4 128.7(4) . . ?
N1 C7 H7 115.7 . . ?
C4 C7 H7 115.7 . . ?
N1 C8 C9 110.3(4) . . ?
N1 C8 H8 109.6 . . ?
C9 C8 H8 109.6 . . ?
N1 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
H8 C8 H8A 108.1 . . ?
C8 C9 C10 117.3(4) . . ?
C8 C9 H9 108.0 . . ?
C10 C9 H9 108.0 . . ?
C8 C9 H9A 108.0 . . ?
C10 C9 H9A 108.0 . . ?
H9 C9 H9A 107.2 . . ?
C9 C10 N2 118.3(4) . . ?
C9 C10 H10 107.7 . . ?
N2 C10 H10 107.7 . . ?
C9 C10 H10A 107.7 . . ?
N2 C10 H10A 107.7 . . ?
H10 C10 H10A 107.1 . . ?
N2 C11 H11 115.2(19) . . ?
N2 C11 H11A 98(3) . . ?
H11 C11 H11A 123(4) . . ?
N2 C11 H11B 115(2) . . ?
H11 C11 H11B 102(3) . . ?
H11A C11 H11B 103(4) . . ?
N2 C12 H12 109.5 . . ?
N2 C12 H12A 109.5 . . ?
H12 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd N1 2.010(3) . ?
Pd N2 2.099(4) . ?
Pd Cl3 2.2922(16) . ?
Pd Cl2 2.3021(14) . ?
Cl1 C1 1.750(5) . ?
N1 C7 1.286(5) . ?
N1 C8 1.471(5) . ?
N2 C12 1.463(6) . ?
N2 C11 1.494(6) . ?
N2 C10 1.513(6) . ?
C1 C2 1.354(6) . ?
C1 C6 1.375(6) . ?
C2 C3 1.377(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(6) . ?
C3 H3 1.03(4) . ?
C4 C5 1.403(6) . ?
C4 C7 1.460(6) . ?
C5 C6 1.349(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.496(7) . ?
C8 H8 0.9700 . ?
C8 H8A 0.9700 . ?
C9 C10 1.500(7) . ?
C9 H9 0.9700 . ?
C9 H9A 0.9700 . ?
C10 H10 0.9700 . ?
C10 H10A 0.9700 . ?
C11 H11 1.09(3) . ?
C11 H11A 0.93(5) . ?
C11 H11B 1.01(4) . ?
C12 H12 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
