#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/49/2204981.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2204981
loop_
_publ_author_name
'Calmuschi, Beatrice'
'Englert, Ulli'
_publ_section_title
(S)-(Acetylacetonato-κ²O,O')[2-(1-aminoethyl)phenyl-κ²C¹,N]palladium(II)
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m164
_journal_page_last               m165
_journal_paper_doi               10.1107/S1600536804032842
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Pd (C8 H10 N) (C5 H7 O2)]'
_chemical_formula_moiety         'C13 H17 N O2 Pd'
_chemical_formula_sum            'C13 H17 N O2 Pd'
_chemical_formula_weight         325.68
_chemical_name_systematic
;
(S)-(Acetylacetonato-κ²O,O')[2-(1-aminoethyl)phenyl-
κ²C¹,N]palladium(II)
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5872(11)
_cell_length_b                   10.5872(11)
_cell_length_c                   11.9509(12)
_cell_measurement_reflns_used    8096
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      1.92
_cell_volume                     1339.6(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18582
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.5829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.217
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3327
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0196
_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)+(0.0750P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                3225
_reflns_number_total             3327
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ww6314.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2204981
_cod_database_fobs_code          2204981
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Pd1 -0.465800(13) -0.628078(15) -0.229710(18) 0.02152(5) Uani d . 1 Pd
O2 -0.58375(13) -0.77878(15) -0.23734(19) 0.0295(3) Uani d . 1 O
O1 -0.61100(15) -0.5015(2) -0.27234(16) 0.0281(4) Uani d . 1 O
N1 -0.3416(2) -0.48553(19) -0.20198(17) 0.0239(4) Uani d . 1 N
H1A -0.3465 -0.4277 -0.2626 0.031 Uiso calc R 1 H
H1B -0.3664 -0.4418 -0.1361 0.031 Uiso calc R 1 H
C6 -0.2087(2) -0.6656(2) -0.15828(17) 0.0233(4) Uani d . 1 C
C7 -0.2070(2) -0.5269(2) -0.18905(19) 0.0263(5) Uani d . 1 C
H7 -0.1663 -0.5193 -0.2624 0.034 Uiso calc R 1 H
C5 -0.1040(2) -0.7289(2) -0.11536(19) 0.0280(5) Uani d . 1 C
H5 -0.0261 -0.6820 -0.0998 0.036 Uiso calc R 1 H
C2 -0.3249(2) -0.8620(2) -0.16023(18) 0.0252(4) Uani d . 1 C
H2 -0.4022 -0.9096 -0.1764 0.033 Uiso calc R 1 H
C8 -0.1366(2) -0.4403(2) -0.1081(2) 0.0354(6) Uani d . 1 C
H8A -0.1781 -0.4424 -0.0349 0.046 Uiso calc R 1 H
H8B -0.1373 -0.3537 -0.1372 0.046 Uiso calc R 1 H
H8C -0.0491 -0.4693 -0.1004 0.046 Uiso calc R 1 H
C10 -0.7268(2) -0.5346(3) -0.2754(2) 0.0312(5) Uani d . 1 C
C11 -0.7733(2) -0.6576(2) -0.2624(2) 0.0335(5) Uani d . 1 C
H11 -0.8652 -0.6674 -0.2670 0.044 Uiso calc R 1 H
C12 -0.7040(2) -0.7676(2) -0.2437(2) 0.0324(5) Uani d . 1 C
C1 -0.3219(2) -0.7321(2) -0.18036(18) 0.0228(4) Uani d . 1 C
C4 -0.1091(2) -0.8581(2) -0.0944(2) 0.0298(5) Uani d . 1 C
H4 -0.0354 -0.9020 -0.0636 0.039 Uiso calc R 1 H
C3 -0.2202(2) -0.9250(2) -0.1177(2) 0.0280(5) Uani d . 1 C
H3 -0.2241 -1.0161 -0.1039 0.036 Uiso calc R 1 H
C9 -0.8187(2) -0.4283(3) -0.2942(3) 0.0382(6) Uani d . 1 C
H9A -0.8100 -0.3660 -0.2340 0.050 Uiso calc R 1 H
H9B -0.9050 -0.4617 -0.2945 0.050 Uiso calc R 1 H
H9C -0.8008 -0.3878 -0.3662 0.050 Uiso calc R 1 H
C13 -0.7751(2) -0.8898(3) -0.2268(4) 0.0563(8) Uani d . 1 C
H13A -0.7345 -0.9570 -0.2702 0.073 Uiso calc R 1 H
H13B -0.8625 -0.8793 -0.2520 0.073 Uiso calc R 1 H
H13C -0.7743 -0.9122 -0.1473 0.073 Uiso calc R 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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_publ_flag
C1 Pd1 O2 92.86(8) yes
C1 Pd1 N1 82.28(9) yes
O2 Pd1 N1 172.55(8) yes
C1 Pd1 O1 173.94(9) yes
O2 Pd1 O1 92.30(7) yes
N1 Pd1 O1 92.26(10) yes
C12 O2 Pd1 122.82(15) ?
C10 O1 Pd1 122.36(18) ?
C7 N1 Pd1 114.55(15) ?
C7 N1 H1A 108.6 ?
Pd1 N1 H1A 108.6 ?
C7 N1 H1B 108.6 ?
Pd1 N1 H1B 108.6 ?
H1A N1 H1B 107.6 ?
C5 C6 C1 120.3(2) ?
C5 C6 C7 123.1(2) ?
C1 C6 C7 116.6(2) ?
N1 C7 C6 107.31(17) ?
N1 C7 C8 110.8(2) ?
C6 C7 C8 115.73(19) ?
N1 C7 H7 107.6 ?
C6 C7 H7 107.6 ?
C8 C7 H7 107.6 ?
C4 C5 C6 120.5(2) ?
C4 C5 H5 119.7 ?
C6 C5 H5 119.7 ?
C3 C2 C1 121.1(2) ?
C3 C2 H2 119.4 ?
C1 C2 H2 119.4 ?
C7 C8 H8A 109.5 ?
C7 C8 H8B 109.5 ?
H8A C8 H8B 109.5 ?
C7 C8 H8C 109.5 ?
H8A C8 H8C 109.5 ?
H8B C8 H8C 109.5 ?
O1 C10 C11 126.1(2) ?
O1 C10 C9 114.9(2) ?
C11 C10 C9 119.0(2) ?
C12 C11 C10 127.5(2) ?
C12 C11 H11 116.2 ?
C10 C11 H11 116.2 ?
O2 C12 C11 127.6(2) ?
O2 C12 C13 114.1(2) ?
C11 C12 C13 118.3(2) ?
C2 C1 C6 118.5(2) ?
C2 C1 Pd1 125.75(16) ?
C6 C1 Pd1 115.66(17) ?
C5 C4 C3 119.6(2) ?
C5 C4 H4 120.2 ?
C3 C4 H4 120.2 ?
C2 C3 C4 120.0(2) ?
C2 C3 H3 120.0 ?
C4 C3 H3 120.0 ?
C10 C9 H9A 109.5 ?
C10 C9 H9B 109.5 ?
H9A C9 H9B 109.5 ?
C10 C9 H9C 109.5 ?
H9A C9 H9C 109.5 ?
H9B C9 H9C 109.5 ?
C12 C13 H13A 109.5 ?
C12 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
C12 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 C1 1.970(2) yes
Pd1 O2 2.0281(15) yes
Pd1 N1 2.0288(19) yes
Pd1 O1 2.1017(17) yes
O2 C12 1.280(3) yes
O1 C10 1.275(3) yes
N1 C7 1.499(3) ?
N1 H1A 0.9500 ?
N1 H1B 0.9500 ?
C6 C5 1.393(3) ?
C6 C1 1.414(3) ?
C6 C7 1.514(3) ?
C7 C8 1.527(3) ?
C7 H7 0.9800 ?
C5 C4 1.391(3) ?
C5 H5 0.9800 ?
C2 C3 1.390(3) ?
C2 C1 1.397(3) ?
C2 H2 0.9800 ?
C8 H8A 0.9801 ?
C8 H8B 0.9801 ?
C8 H8C 0.9801 ?
C10 C11 1.401(4) ?
C10 C9 1.504(3) ?
C11 C12 1.395(3) ?
C11 H11 0.9800 ?
C12 C13 1.510(3) ?
C4 C3 1.401(3) ?
C4 H4 0.9800 ?
C3 H3 0.9800 ?
C9 H9A 0.9801 ?
C9 H9B 0.9801 ?
C9 H9C 0.9801 ?
C13 H13A 0.9801 ?
C13 H13B 0.9801 ?
C13 H13C 0.9801 ?
