Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm
#=============================================================================

# PROCESSING SUMMARY

_journal_coden_Cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?

#=============================================================================

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Daniel M. Toebbens'
_publ_contact_author_address     
;University of Innsbruck
Institute of Mineralogy and Crystallography
Innrain 52
A-6020 Innsbruck
Austria
;
_publ_contact_author_email       daniel.toebbens@uibk.ac.at
_publ_contact_author_phone       +435125075532
_publ_requested_coeditor_name    ?
_publ_requested_category         ?

# Definition of non standard CIF items (Reliability indices used in FULLPROF)

loop_
_publ_manuscript_incl_extra_item
_publ_manuscript_incl_extra_info
_publ_manuscript_incl_extra_defn
# Name Explanation Standard?
# ------ ----------- ---------
'_pd_proc_ls_prof_cR_factor' 'Prof. R-factor CORRECTED for background' no
'_pd_proc_ls_prof_cwR_factor' 'wProf.R-factor CORRECTED for background' no
'_pd_proc_ls_prof_cwR_expected' 'wProf.Expected CORRECTED for background' no
'_pd_proc_ls_prof_chi2' 'Chi-square for all considered points' no
'_pd_proc_ls_prof_echi2' 'Chi-2 for points with Bragg contribution' no
#=============================================================================

# 3. TITLE AND AUTHOR LIST

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address
D.M.Toebbens
;University of Innsbruck
Institute of Mineralogy and Petrography
Innrain 52
A-6020 Innsbruck
Austria
;
M.Hummel
;University of Innsbruck
Institute of General, Inorganic and Theoretical Chemistry
Innrain 52a
A-6020 Innsbruck
Austria
;
R.Kaindl
;University of Innsbruck
Institute of Mineralogy and Petrography
Innrain 52
A-6020 Innsbruck
Austria
;
H.Schottenberger
;University of Innsbruck
Institute of General, Inorganic and Theoretical Chemistry
Innrain 52a
A-6020 Innsbruck
Austria
;
V.Kahlenberg
;University of Innsbruck
Institute of Mineralogy and Petrography
Innrain 52
A-6020 Innsbruck
Austria
;

#=============================================================================

# 4. TEXT

_publ_section_synopsis           
; ?
;
_publ_section_abstract           
; ?
;
_publ_section_comment            
; ?
;
_publ_section_exptl_prep         
# Details of the preparation of the sample(s)
# should be given here.
; ?
;
_publ_section_exptl_refinement   
; ?
;
_publ_section_references         
; ?
;
_publ_section_figure_captions    
; ?
;
_publ_section_acknowledgements   
; ?
;

#=============================================================================

#=============================================================================
# If more than one structure is reported, the remaining sections should be
# completed per structure. For each data set, replace the '?' in the
# data_? line below by a unique identifier.

data_Mg[acacac]2
_database_code_depnum_ccdc_archive 'CCDC 657357'

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 'bis(3-acetyl-2,4-pentandionato-O2,O3)magnesium(II)'
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H18 Mg O6'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C14 H18 Mg O6'
_chemical_formula_iupac          ?
_chemical_formula_weight         306.59
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
mg 5.42040 2.82750 2.17350 79.26110 1.22690 0.38080 2.30730 7.19370 0.85840
0.16500 0.17700
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/A'
_symmetry_space_group_name_Hall  '-P 2yab'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x+1/2,y+1/2,-z
-x,-y,-z
x+1/2,-y+1/2,z

_cell_length_a                   8.31089(9)
_cell_length_b                   12.15064(12)
_cell_length_c                   8.06761(9)
_cell_angle_alpha                90.00000
_cell_angle_beta                 106.7228(8)
_cell_angle_gamma                90.00000
_cell_volume                     780.233(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    297(1)
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane
_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'
_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'
_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min. The pressure at which the sample was
# prepared is in kPa. The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; 'external standard'
;

_diffrn_ambient_temperature      297
_diffrn_source                   'sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  'curved Ge(111)'
_diffrn_measurement_device_type  'STOE STADI MP'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'linear PSD'
_diffrn_detector_type            STOE # make or model of detector
_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        11795
_pd_meas_2theta_range_min        2.06000
_pd_meas_2theta_range_max        120.00000
_pd_meas_2theta_range_inc        0.010001

#=============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     TCH-Pseudo-Voigt
_pd_proc_ls_background_function  'linear interpolation'
_pd_proc_ls_pref_orient_corr     
; ?
;

# The following profile R-factors are NOT CORRECTED for background
# The sum is extended to all non-excluded points.
# These are the current CIF standard

_pd_proc_ls_prof_R_factor        3.0871
_pd_proc_ls_prof_wR_factor       4.1182
_pd_proc_ls_prof_wR_expected     3.8105

# The following profile R-factors are CORRECTED for background
# The sum is extended to all non-excluded points.
# These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       18.3533
_pd_proc_ls_prof_cwR_factor      13.9841
_pd_proc_ls_prof_cwR_expected    12.9394

# The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            1.1680
_pd_proc_ls_prof_echi2           1.1953

# Items related to LS refinement

_refine_ls_R_I_factor            4.2413
_refine_ls_number_reflns         1224
_refine_ls_number_parameters     67
_refine_ls_number_restraints     21
_refine_ls_shift/su_max          0.05

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        2.0842
_pd_proc_2theta_range_max        120.0242
_pd_proc_2theta_range_inc        0.010001
_pd_proc_wavelength              1.540560

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    EXPO2004
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
Mg 0.50000 0.50000 0.00000 0.0319(16) 1.00000 Uiso Mg
O1 0.3958(6) 0.4878(3) 0.2029(6) 0.0409(9) 1.00000 Uiso O
O2 0.2807(6) 0.4329(3) -0.1337(6) 0.0409(9) 1.00000 Uiso O
O3 0.0936(6) 0.1612(4) 0.0412(6) 0.0409(9) 1.00000 Uiso O
C1 0.2546(7) 0.4278(6) 0.3932(6) 0.0409(9) 1.00000 Uiso C
H1a 0.1717(7) 0.3622(6) 0.4084(6) 0.0409(9) 1.00000 Uiso H
H1b 0.3685(7) 0.4259(6) 0.5004(6) 0.0409(9) 1.00000 Uiso H
H1c 0.1926(7) 0.5063(6) 0.3912(6) 0.0409(9) 1.00000 Uiso H
C2 0.2984(8) 0.4121(5) 0.2247(6) 0.0409(9) 1.00000 Uiso C
C3 0.2221(9) 0.3346(4) 0.0931(5) 0.0409(9) 1.00000 Uiso C
C4 0.1965(8) 0.3598(6) -0.0830(5) 0.0409(9) 1.00000 Uiso C
C5 0.0654(7) 0.2980(5) -0.2223(7) 0.0409(9) 1.00000 Uiso C
H5a 0.0028(7) 0.2385(5) -0.1623(7) 0.0409(9) 1.00000 Uiso H
H5b 0.1261(7) 0.2558(5) -0.3063(7) 0.0409(9) 1.00000 Uiso H
H5c -0.0261(7) 0.3557(5) -0.2976(7) 0.0409(9) 1.00000 Uiso H
C6 0.1869(10) 0.2226(4) 0.1441(6) 0.0409(9) 1.00000 Uiso C
C7 0.2526(8) 0.1772(5) 0.3284(6) 0.0409(9) 1.00000 Uiso C
H7a 0.3341(8) 0.2375(5) 0.4102(6) 0.0409(9) 1.00000 Uiso H
H7b 0.1477(8) 0.1599(5) 0.3787(6) 0.0409(9) 1.00000 Uiso H
H7c 0.3224(8) 0.1022(5) 0.3267(6) 0.0409(9) 1.00000 Uiso H

# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg O1 2.0657 . . yes
Mg O2 2.0047 . . yes
Mg O3 2.0984 . 2_555 yes
Mg O1 2.0657 . 3_665 yes
Mg O2 2.0047 . 3_665 yes
Mg O3 2.0984 . 4_555 yes
O1 C2 1.2705 . . yes
O2 C4 1.2691 . . yes
O3 C6 1.2151 . . yes
C1 C2 1.5171 . . no
C2 C3 1.4243 . . no
C3 C4 1.4084 . . no
C3 C6 1.4752 . . no
C4 C5 1.5196 . . no
C6 C7 1.5317 . . no
C1 H1A 1.0834 . . no
C1 H1B 1.0832 . . no
C1 H1C 1.0820 . . no
C5 H5A 1.0829 . . no
C5 H5B 1.0832 . . no
C5 H5C 1.0830 . . no
C7 H7A 1.0835 . . no
C7 H7B 1.0828 . . no
C7 H7C 1.0825 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mg O2 82.74 . . . yes
O1 Mg O3 88.38 . . 2_555 yes
O1 Mg O1 180.00 . . 3_665 yes
O1 Mg O2 97.26 . . 3_665 yes
O1 Mg O3 91.62 . . 4_555 yes
O2 Mg O3 93.22 . . 2_555 yes
O1 Mg O2 97.26 3_665 . . yes
O2 Mg O2 180.00 . . 3_665 yes
O2 Mg O3 86.78 . . 4_555 yes
O1 Mg O3 91.62 3_665 . 2_555 yes
O2 Mg O3 86.78 3_665 . 2_555 yes
O3 Mg O3 180.00 2_555 . 4_555 yes
O1 Mg O2 82.74 3_665 . 3_665 yes
O1 Mg O3 88.38 3_665 . 4_555 yes
O2 Mg O3 93.22 3_665 . 4_555 yes
Mg O1 C2 126.21 . . . yes
Mg O2 C4 127.70 . . . yes
Mg O3 C6 144.68 2_545 . . yes
O1 C2 C1 111.08 . . . yes
O1 C2 C3 122.70 . . . yes
C1 C2 C3 125.51 . . . no
C2 C3 C4 120.92 . . . no
C2 C3 C6 118.91 . . . no
C4 C3 C6 119.83 . . . no
O2 C4 C3 122.69 . . . yes
O2 C4 C5 116.87 . . . yes
C3 C4 C5 120.44 . . . no
O3 C6 C3 120.97 . . . yes
O3 C6 C7 114.91 . . . yes
C3 C6 C7 123.99 . . . no
C2 C1 H1A 109.47 . . . no
C2 C1 H1B 109.44 . . . no
C2 C1 H1C 109.48 . . . no
H1A C1 H1B 109.39 . . . no
H1A C1 H1C 109.55 . . . no
H1B C1 H1C 109.49 . . . no
C4 C5 H5A 109.50 . . . no
C4 C5 H5B 109.43 . . . no
C4 C5 H5C 109.46 . . . no
H5A C5 H5B 109.50 . . . no
H5A C5 H5C 109.44 . . . no
H5B C5 H5C 109.50 . . . no
C6 C7 H7A 109.48 . . . no
C6 C7 H7B 109.46 . . . no
C6 C7 H7C 109.48 . . . no
H7A C7 H7B 109.43 . . . no
H7A C7 H7C 109.49 . . . no
H7B C7 H7C 109.48 . . . no

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C3 C6 O3 165.33 . . . . no
C2 C3 C6 C7 -10.45 . . . . no
C4 C3 C6 O3 -21.27 . . . . no
C4 C3 C6 C7 162.95 . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?

#=============================================================================
# Additional structures (last six sections and associated data_? identifiers)
# may be added at this point.
#=============================================================================

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# Attachment 'Pd[acacac]2.cif'
#=============================================================================

#=============================================================================
# If more than one structure is reported, the remaining sections should be
# completed per structure. For each data set, replace the '?' in the
# data_? line below by a unique identifier.

data_Pd[acacac]2
_database_code_depnum_ccdc_archive 'CCDC 657358'

#=============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 'bis(3-acetyl-2,4-pentandionato-O2,O3)palladium(II)'
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H18 O6 Pd'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C14 H18 O6 Pd'
_chemical_formula_iupac          ?
_chemical_formula_weight         388.70
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
pd 19.33190 0.69866 15.50170 7.98929 5.29537 25.20520 0.60584 76.89860 5.26593
-0.05900 3.93400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304
0.00000 0.00000
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P B C A'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
x+1/2,-y+1/2,-z
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
-x,-y,-z
-x+1/2,y+1/2,z
x,-y+1/2,z+1/2
x+1/2,y,-z+1/2

_cell_length_a                   13.39752(15)
_cell_length_b                   13.43165(8)
_cell_length_c                   8.49767(4)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_volume                     1529.16(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane
_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'
_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'
_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min. The pressure at which the sample was
# prepared is in kPa. The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#=============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; 'external standard'
;

_diffrn_ambient_temperature      296
_diffrn_source                   'sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  'curved Ge(111)'
_diffrn_measurement_device_type  'STOE STADI MP'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'linear PSD'
_diffrn_detector_type            STOE # make or model of detector
_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        12794
_pd_meas_2theta_range_min        2.06000
_pd_meas_2theta_range_max        129.99001
_pd_meas_2theta_range_inc        0.010001

#=============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     ?
_pd_proc_ls_background_function  ?
_pd_proc_ls_pref_orient_corr     
; ?
;

# The following profile R-factors are NOT CORRECTED for background
# The sum is extended to all non-excluded points.
# These are the current CIF standard

_pd_proc_ls_prof_R_factor        5.5913
_pd_proc_ls_prof_wR_factor       7.1901
_pd_proc_ls_prof_wR_expected     6.3130

# The following profile R-factors are CORRECTED for background
# The sum is extended to all non-excluded points.
# These items are not in the current CIF standard, but are defined above

_pd_proc_ls_prof_cR_factor       17.1073
_pd_proc_ls_prof_cwR_factor      15.2119
_pd_proc_ls_prof_cwR_expected    13.3563

# The following items are not in the CIF standard, but are defined above

_pd_proc_ls_prof_chi2            1.2972
_pd_proc_ls_prof_echi2           1.3257

# Items related to LS refinement

_refine_ls_R_I_factor            3.8205
_refine_ls_number_reflns         1349
_refine_ls_number_parameters     79
_refine_ls_number_restraints     21
_refine_ls_shift/su_max          0.05

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        2.0657
_pd_proc_2theta_range_max        129.9957
_pd_proc_2theta_range_inc        0.010001
_pd_proc_wavelength              1.540560

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_structure_solution    FOX
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    ?
_computing_publication_material  ?

#=============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
Pd 0.00000 0.00000 0.00000 0.0267(3) 1.00000 Uiso Pd
C1 0.2153(7) -0.0155(8) -0.3701(11) 0.0378(11) 1.00000 Uiso C
C2 0.1272(7) 0.0224(7) -0.2760(9) 0.0378(11) 1.00000 Uiso C
C3 0.0664(6) 0.0983(6) -0.3349(8) 0.0378(11) 1.00000 Uiso C
C4 -0.0191(6) 0.1350(6) -0.2601(8) 0.0378(11) 1.00000 Uiso C
C5 -0.0714(9) 0.2213(5) -0.3359(11) 0.0378(11) 1.00000 Uiso C
C6 0.0968(8) 0.1505(6) -0.4826(5) 0.0378(11) 1.00000 Uiso C
C7 0.1618(7) 0.2413(4) -0.4792(17) 0.0378(11) 1.00000 Uiso C
O1 0.1116(8) -0.0285(5) -0.1513(7) 0.0378(11) 1.00000 Uiso O
O2 -0.0584(7) 0.1048(5) -0.1327(6) 0.0378(11) 1.00000 Uiso O
O3 0.0684(8) 0.1229(5) -0.6108(6) 0.0378(11) 1.00000 Uiso O
H1a 0.2250(7) 0.0301(8) -0.4739(11) 0.36(3) 1.00000 Uiso H
H1b 0.2821(7) -0.0120(8) -0.2985(11) 0.36(3) 1.00000 Uiso H
H1c 0.2018(7) -0.0919(8) -0.4050(11) 0.36(3) 1.00000 Uiso H
H5a -0.0328(9) 0.2416(5) -0.4432(11) 0.36(3) 1.00000 Uiso H
H5b -0.1476(9) 0.2004(5) -0.3634(11) 0.36(3) 1.00000 Uiso H
H5c -0.0717(9) 0.2840(5) -0.2559(11) 0.36(3) 1.00000 Uiso H
H7a 0.1820(7) 0.2581(4) -0.3587(17) 0.36(3) 1.00000 Uiso H
H7b 0.1216(7) 0.3037(4) -0.5292(17) 0.36(3) 1.00000 Uiso H
H7c 0.2287(7) 0.2276(4) -0.5473(17) 0.36(3) 1.00000 Uiso H

# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

#=============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd O1 2.0087 . . yes
Pd O2 1.9660 . . yes
Pd O1 2.0087 . 5_566 yes
Pd O2 1.9660 . 5_566 yes
O1 C2 1.2783 . . yes
O2 C4 1.2704 . . yes
O3 C6 1.2120 . . yes
C1 C2 1.5138 . . no
C2 C3 1.3976 . . no
C3 C4 1.3997 . . no
C3 C6 1.4942 . . no
C4 C5 1.4998 . . no
C6 C7 1.4989 . . no
C1 H1A 1.0817 . . no
C1 H1B 1.0832 . . no
C1 H1C 1.0834 . . no
C5 H5A 1.0831 . . no
C5 H5B 1.0843 . . no
C5 H5C 1.0823 . . no
C7 H7A 1.0829 . . no
C7 H7B 1.0831 . . no
C7 H7C 1.0826 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd O2 93.76 . . . yes
O1 Pd O1 180.00 . . 5_566 yes
O1 Pd O2 86.24 . . 5_566 yes
O1 Pd O2 86.24 5_566 . . yes
O2 Pd O2 180.00 . . 5_566 yes
O1 Pd O2 93.76 5_566 . 5_566 yes
Pd O1 C2 123.39 . . . yes
Pd O2 C4 123.54 . . . yes
O1 C2 C1 112.68 . . . yes
O1 C2 C3 126.28 . . . yes
C1 C2 C3 120.70 . . . no
C2 C3 C4 124.84 . . . no
C2 C3 C6 118.96 . . . no
C4 C3 C6 116.06 . . . no
O2 C4 C3 127.86 . . . yes
O2 C4 C5 114.78 . . . yes
C3 C4 C5 117.35 . . . no
O3 C6 C3 121.73 . . . yes
O3 C6 C7 116.65 . . . yes
C3 C6 C7 121.60 . . . no
C2 C1 H1A 109.51 . . . no
C2 C1 H1B 109.44 . . . no
C2 C1 H1C 109.45 . . . no
H1A C1 H1B 109.52 . . . no
H1A C1 H1C 109.46 . . . no
H1B C1 H1C 109.44 . . . no
C4 C5 H5A 109.45 . . . no
C4 C5 H5B 109.41 . . . no
C4 C5 H5C 109.47 . . . no
H5A C5 H5B 109.47 . . . no
H5A C5 H5C 109.55 . . . no
H5B C5 H5C 109.47 . . . no
C6 C7 H7A 109.45 . . . no
C6 C7 H7B 109.46 . . . no
C6 C7 H7C 109.41 . . . no
H7A C7 H7B 109.51 . . . no
H7A C7 H7C 109.51 . . . no
H7B C7 H7C 109.48 . . . no

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C3 C6 O3 -92.09 . . . . no
C2 C3 C6 C7 89.56 . . . . no
C4 C3 C6 O3 92.10 . . . . no
C4 C3 C6 C7 -86.25 . . . . no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


