#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:08:07 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179678 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/00/7000021.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_7000021
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            'C16 H25 Cl N2 O5 Pd'
_chemical_formula_weight         467.23
_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                93.169(14)
_cell_angle_beta                 99.090(10)
_cell_angle_gamma                115.404(9)
_cell_formula_units_Z            2
_cell_length_a                   10.1620(10)
_cell_length_b                   10.5199(17)
_cell_length_c                   10.5800(10)
_cell_measurement_temperature    293(2)
_cell_volume                     999.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.785
_diffrn_measured_fraction_theta_max 0.785
_diffrn_measurement_device_type  'Image plate detector diffractometer'
_diffrn_measurement_method       phi-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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43084
_diffrn_reflns_theta_full        31.65
_diffrn_reflns_theta_max         31.65
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisme
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0574P)²+0.2894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                5155
_reflns_number_total             5288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b415613g.txt
_cod_data_source_block           E-2AcO
_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               7000021
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 0.574890(14) 0.187744(13) 0.382432(14) 0.03194(7) Uani 1 1 d . . .
Cl1 Cl 0.84669(10) 0.75134(9) 0.00099(9) 0.0741(2) Uani 1 1 d . . .
O1 O 0.75750(18) 0.1860(2) 0.3308(2) 0.0478(4) Uani 1 1 d . . .
O2 O 0.6406(2) -0.0214(2) 0.2030(2) 0.0567(5) Uani 1 1 d . . .
O3 O 0.7053(2) 0.25858(19) 0.56123(19) 0.0445(4) Uani 1 1 d . . .
O4 O 0.7666(3) 0.4767(2) 0.5119(3) 0.0660(6) Uani 1 1 d . . .
N1 N 0.4512(2) 0.11107(19) 0.2052(2) 0.0368(3) Uani 1 1 d . . .
N2 N 0.3918(2) 0.1955(2) 0.4376(2) 0.0389(4) Uani 1 1 d . . .
C1 C 0.7472(3) 0.5543(3) 0.1596(3) 0.0472(5) Uani 1 1 d . . .
C2 C 0.7398(3) 0.5805(3) 0.0327(3) 0.0472(5) Uani 1 1 d . . .
C3 C 0.6498(3) 0.4763(3) -0.0682(3) 0.0557(6) Uani 1 1 d . . .
H3 H 0.6468 0.4962 -0.1528 0.067 Uiso 1 1 calc R . .
C4 C 0.5636(3) 0.3415(3) -0.0423(3) 0.0491(5) Uani 1 1 d . . .
H4 H 0.5014 0.2705 -0.1102 0.059 Uiso 1 1 calc R . .
C5 C 0.5687(2) 0.3106(2) 0.0847(2) 0.0398(4) Uani 1 1 d . . .
C6 C 0.6615(3) 0.4187(3) 0.1853(2) 0.0450(5) Uani 1 1 d . . .
H6 H 0.6658 0.3996 0.2703 0.054 Uiso 1 1 calc R . .
C7 C 0.4657(2) 0.1662(2) 0.1007(2) 0.0403(4) Uani 1 1 d . . .
H7 H 0.4034 0.1076 0.0255 0.048 Uiso 1 1 calc R . .
C8 C 0.3268(3) -0.0301(2) 0.2012(3) 0.0453(5) Uani 1 1 d . . .
H8A H 0.3625 -0.0906 0.2463 0.054 Uiso 1 1 calc R . .
H8B H 0.2832 -0.0744 0.1122 0.054 Uiso 1 1 calc R . .
C9 C 0.2106(2) -0.0123(3) 0.2655(3) 0.0518(6) Uani 1 1 d . . .
C10 C 0.2621(3) 0.0497(3) 0.4059(3) 0.0502(5) Uani 1 1 d . . .
H10 H 0.2888 -0.0148 0.4535 0.060 Uiso 1 1 calc R . .
H10A H 0.1789 0.0539 0.4369 0.060 Uiso 1 1 calc R . .
C11 C 0.3556(3) 0.3004(3) 0.3708(3) 0.0501(5) Uani 1 1 d . . .
C12 C 0.4170(3) 0.2393(4) 0.5786(3) 0.0578(6) Uani 1 1 d . . .
H12 H 0.4408 0.1737 0.6252 0.069 Uiso 1 1 calc R . .
H12A H 0.3285 0.2397 0.5994 0.069 Uiso 1 1 calc R . .
H12B H 0.4979 0.3330 0.6022 0.069 Uiso 1 1 calc R . .
C13 C 0.7512(2) 0.0860(3) 0.2510(2) 0.0445(5) Uani 1 1 d . . .
C14 C 0.8975(4) 0.1096(5) 0.2179(5) 0.1031(19) Uani 1 1 d . . .
H14 H 0.8906 0.0211 0.1808 0.124 Uiso 1 1 calc R . .
H14A H 0.9737 0.1466 0.2949 0.124 Uiso 1 1 calc R . .
H14B H 0.9217 0.1762 0.1569 0.124 Uiso 1 1 calc R . .
C15 C 0.7834(3) 0.3945(3) 0.5833(3) 0.0473(5) Uani 1 1 d . . .
C16 C 0.8983(4) 0.4500(4) 0.7063(4) 0.0760(10) Uani 1 1 d . . .
H16 H 0.9071 0.5400 0.7416 0.091 Uiso 1 1 calc R . .
H16A H 0.9923 0.4616 0.6887 0.091 Uiso 1 1 calc R . .
H16B H 0.8689 0.3839 0.7673 0.091 Uiso 1 1 calc R . .
O5 O 0.9652(3) 0.7438(3) 0.4612(3) 0.0730(7) Uani 1 1 d . . .
H1 H 0.787(4) 0.611(4) 0.210(4) 0.048(8) Uiso 1 1 d . . .
H5 H 0.926(5) 0.674(5) 0.475(5) 0.082(15) Uiso 1 1 d . . .
H9 H 0.118(4) -0.112(4) 0.264(4) 0.069(11) Uiso 1 1 d . . .
H9A H 0.175(4) 0.046(4) 0.212(4) 0.059(9) Uiso 1 1 d . . .
H11 H 0.275(4) 0.301(3) 0.397(3) 0.049(8) Uiso 1 1 d . . .
H11A H 0.340(3) 0.278(3) 0.280(4) 0.043(8) Uiso 1 1 d . . .
H11B H 0.435(4) 0.392(4) 0.398(3) 0.048(8) 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'
O O 0.0106 0.0060 '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 O1 93.51(8) . . ?
N1 Pd O3 177.01(6) . . ?
O1 Pd O3 84.21(8) . . ?
N1 Pd N2 87.53(8) . . ?
O1 Pd N2 178.36(6) . . ?
O3 Pd N2 94.80(8) . . ?
C13 O1 Pd 122.79(14) . . ?
C15 O3 Pd 113.70(17) . . ?
C7 N1 C8 118.6(2) . . ?
C7 N1 Pd 129.56(15) . . ?
C8 N1 Pd 111.82(16) . . ?
C12 N2 C11 107.0(2) . . ?
C12 N2 C10 107.1(2) . . ?
C11 N2 C10 110.8(2) . . ?
C12 N2 Pd 112.69(16) . . ?
C11 N2 Pd 109.96(15) . . ?
C10 N2 Pd 109.25(15) . . ?
C2 C1 C6 118.9(2) . . ?
C2 C1 H1 120(3) . . ?
C6 C1 H1 121(3) . . ?
C3 C2 C1 121.9(2) . . ?
C3 C2 Cl1 119.33(19) . . ?
C1 C2 Cl1 118.8(2) . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 C7 125.2(2) . . ?
C4 C5 C7 115.8(2) . . ?
C1 C6 C5 120.4(2) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
N1 C7 C5 127.9(2) . . ?
N1 C7 H7 116.0 . . ?
C5 C7 H7 116.0 . . ?
N1 C8 C9 108.6(2) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
C10 C9 C8 115.4(2) . . ?
C10 C9 H9 104(2) . . ?
C8 C9 H9 111(2) . . ?
C10 C9 H9A 112(2) . . ?
C8 C9 H9A 106(2) . . ?
H9 C9 H9A 108(3) . . ?
C9 C10 N2 116.2(2) . . ?
C9 C10 H10 108.2 . . ?
N2 C10 H10 108.2 . . ?
C9 C10 H10A 108.2 . . ?
N2 C10 H10A 108.2 . . ?
H10 C10 H10A 107.4 . . ?
N2 C11 H11 107(2) . . ?
N2 C11 H11A 110.5(19) . . ?
H11 C11 H11A 113(3) . . ?
N2 C11 H11B 109(2) . . ?
H11 C11 H11B 107(3) . . ?
H11A C11 H11B 109(3) . . ?
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 . . ?
O2 C13 O1 126.0(2) . . ?
O2 C13 C14 119.3(3) . . ?
O1 C13 C14 114.6(2) . . ?
C13 C14 H14 109.5 . . ?
C13 C14 H14A 109.5 . . ?
H14 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O4 C15 O3 124.0(2) . . ?
O4 C15 C16 120.4(3) . . ?
O3 C15 C16 115.6(3) . . ?
C15 C16 H16 109.5 . . ?
C15 C16 H16A 109.5 . . ?
H16 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16 C16 H16B 109.5 . . ?
H16A C16 H16B 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 1.991(2) . ?
Pd O1 2.0224(17) . ?
Pd O3 2.0235(19) . ?
Pd N2 2.0683(19) . ?
Cl1 C2 1.740(2) . ?
O1 C13 1.284(3) . ?
O2 C13 1.211(3) . ?
O3 C15 1.289(3) . ?
O4 C15 1.228(4) . ?
N1 C7 1.277(3) . ?
N1 C8 1.473(3) . ?
N2 C12 1.485(4) . ?
N2 C11 1.485(3) . ?
N2 C10 1.507(3) . ?
C1 C2 1.382(4) . ?
C1 C6 1.386(3) . ?
C1 H1 0.70(4) . ?
C2 C3 1.371(4) . ?
C3 C4 1.381(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(3) . ?
C5 C7 1.467(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.525(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.503(4) . ?
C9 H9 1.06(4) . ?
C9 H9A 1.00(4) . ?
C10 H10 0.9700 . ?
C10 H10A 0.9700 . ?
C11 H11 0.90(3) . ?
C11 H11A 0.95(4) . ?
C11 H11B 0.94(3) . ?
C12 H12 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C13 C14 1.501(4) . ?
C14 H14 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C15 C16 1.499(4) . ?
C16 H16 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
O5 H5 0.70(5) . ?
