# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2_Eu
#TrackingRef '1_Eu.cif'


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

_audit_creation_method           'Manual editing plus fullprof.2k'
_audit_creation_date             '16 April 2010'

#=============================================================================
# CHEMICAL DATA

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H11 Eu O7 P2'
_chemical_formula_weight         433.07


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
EU 24.62740 2.38790 19.08860 0.19420 13.76030 13.75460 2.92270 123.17400
2.57450 -7.71800 11.27600
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
P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490
0.28300 0.43400
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

#=============================================================================
# POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

_cell_length_a                   5.6110(4)
_cell_length_b                   9.3974(6)
_cell_length_c                   11.4933(8)
_cell_angle_alpha                75.069(3)
_cell_angle_beta                 81.651(3)
_cell_angle_gamma                80.964(4)
_cell_volume                     574.80(7)
_exptl_crystal_density_diffrn    2.502
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_cell_special_details            
;
?
;

_pd_spec_mounting                
;
Glass slide
;

_pd_spec_mount_mode              Reflection
_pd_spec_shape                   'Flat sheet'


#=============================================================================
# EXPERIMENTAL DATA


_exptl_special_details           
;
?
;

_pd_instr_location               
;
Conventional powder diffractometer instrument belonging to the
University of Aveiro and located at the Central Analytical Laboratory
;

_pd_calibration_special_details  
;
LaB6 standard
;

_diffrn_ambient_temperature      298
_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           X-ray
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  None
_diffrn_measurement_method       Bragg-Brentano
_diffrn_detector_type            'X Celerator detector'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;
Data were collected in a continuous mode over the angular range 4-110.
;

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


_pd_meas_number_of_points        5286
_pd_meas_2theta_range_min        4.00703
_pd_meas_2theta_range_max        109.99242
_pd_meas_2theta_range_inc        0.020054

#=============================================================================
# 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     Cauchy
_pd_proc_ls_background_function  'Fixed Points'
_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        2.0887
_pd_proc_ls_prof_wR_factor       2.9078
_pd_proc_ls_prof_wR_expected     0.8401

# 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       21.8433
_pd_proc_ls_prof_cwR_factor      15.2340
_pd_proc_ls_prof_cwR_expected    4.4014

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

_pd_proc_ls_prof_chi2            11.9797
_pd_proc_ls_prof_echi2           12.2141

# Items related to LS refinement

_refine_ls_R_I_factor            11.7383
_refine_ls_number_reflns         3003
_refine_ls_number_parameters     50
_refine_ls_number_restraints     16

# 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        3.9864
_pd_proc_2theta_range_max        109.9718
_pd_proc_2theta_range_inc        0.020054
_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    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    'Crystal Impact Diamond 3.2'
_computing_publication_material  ?

#=============================================================================
# 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
_atom_site_type_symbol
EU1 1.1232(7) 0.1928(4) -0.0051(4) 0.01267 1.00000 Uiso EU
O1W 0.756(5) 0.229(3) 0.125(2) 0.01267 1.00000 Uiso O
O1 0.956(2) 0.3896(11) -0.1296(19) 0.01267 1.00000 Uiso O
O2 0.5332(14) 0.5143(15) -0.1583(17) 0.01267 1.00000 Uiso O
O3 0.822(3) 0.6421(16) -0.0950(20) 0.01267 1.00000 Uiso O
O4 1.0915(15) -0.0779(15) 0.1232(17) 0.01267 1.00000 Uiso O
O5 1.423(2) 0.0523(10) 0.1457(18) 0.01267 1.00000 Uiso O
O6 1.5190(19) -0.2052(14) 0.1210(19) 0.01267 1.00000 Uiso O
P1 0.8027(13) 0.5353(6) -0.1729(3) 0.01267 1.00000 Uiso P
P2 1.3292(13) -0.1020(8) 0.1758(2) 0.01267 1.00000 Uiso P
C1 0.893(6) 0.6613(10) -0.3175(9) 0.01267 1.00000 Uiso C
C2 0.96400 0.57640 -0.40960 0.01267 1.00000 Uiso C
C3 0.78500 0.59040 -0.48180 0.01267 1.00000 Uiso C
C4 0.81800 0.51550 -0.57180 0.01267 1.00000 Uiso C
C5 1.232(6) -0.1815(11) 0.3353(8) 0.01267 1.00000 Uiso C
C6 1.12100 -0.08500 0.41840 0.01267 1.00000 Uiso C
C7 1.23700 -0.06360 0.50880 0.01267 1.00000 Uiso C
C8 1.11900 0.01840 0.58910 0.01267 1.00000 Uiso C

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

#=============================================================================
# DISTANCES AND ANGLES / MOLECULAR GEOMETRY

_geom_special_details            ?


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
? ? ? ? ? ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
_database_code_depnum_ccdc_archive 'CCDC 775633'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3_Gd
#TrackingRef '2_Gd.cif'


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

_audit_creation_method           'Manual editing plus fullprof.2k'
_audit_creation_date             '16 April 2010'

#=============================================================================
# CHEMICAL DATA


_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H11 Gd O7 P2'
_chemical_formula_weight         438.36


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
GD 25.07090 2.25341 19.07980 0.18195 13.85180 12.93310 3.54545 101.39799
2.41960 -9.24200 11.94600
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
P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490
0.28300 0.43400
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

#=============================================================================
# POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

_cell_length_a                   5.6010(4)
_cell_length_b                   9.3849(7)
_cell_length_c                   11.4837(8)
_cell_angle_alpha                75.205(4)
_cell_angle_beta                 81.625(4)
_cell_angle_gamma                81.120(4)
_cell_volume                     573.06(7)
_exptl_crystal_density_diffrn    2.502
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_cell_special_details            
;
?
;

_pd_spec_mounting                
;
Glass slide
;

_pd_spec_mount_mode              Reflection
_pd_spec_shape                   'Flat sheet'


#=============================================================================
# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_pd_instr_location               
;
Conventional powder diffractometer instrument belonging to the
University of Aveiro and located at the Central Analytical Laboratory
;

_pd_calibration_special_details  
;
LaB6 standard
;

_diffrn_ambient_temperature      298
_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           X-ray
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  None
_diffrn_measurement_method       Bragg-Brentano
_diffrn_detector_type            'X Celerator detector'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;
Data were collected in a continuous mode over the angular range 4-110.
;

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

_pd_meas_number_of_points        5286
_pd_meas_2theta_range_min        4.00703
_pd_meas_2theta_range_max        109.99242
_pd_meas_2theta_range_inc        0.020054

#=============================================================================
# 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     Cauchy
_pd_proc_ls_background_function  'Fixed Points'
_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        1.8004
_pd_proc_ls_prof_wR_factor       2.5623
_pd_proc_ls_prof_wR_expected     0.7615

# 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       22.9998
_pd_proc_ls_prof_cwR_factor      15.4725
_pd_proc_ls_prof_cwR_expected    4.5984

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

_pd_proc_ls_prof_chi2            11.3214
_pd_proc_ls_prof_echi2           11.5085

# Items related to LS refinement

_refine_ls_R_I_factor            12.1287
_refine_ls_number_reflns         3018
_refine_ls_number_parameters     50
_refine_ls_number_restraints     16

# 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        3.9874
_pd_proc_2theta_range_max        109.9728
_pd_proc_2theta_range_inc        0.020054
_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    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    'Crystal Impact Diamond 3.2'
_computing_publication_material  ?

#=============================================================================
# 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
_atom_site_type_symbol
GD1 1.1205(8) 0.1937(5) -0.0043(4) 0.01267 1.00000 Uiso GD
O1W 0.767(5) 0.231(3) 0.126(3) 0.01267 1.00000 Uiso O
O1 0.952(2) 0.3872(12) -0.1329(19) 0.01267 1.00000 Uiso O
O2 0.5295(14) 0.5104(16) -0.1607(18) 0.01267 1.00000 Uiso O
O3 0.811(3) 0.6315(17) -0.084(2) 0.01267 1.00000 Uiso O
O4 1.0931(15) -0.0816(15) 0.1245(17) 0.01267 1.00000 Uiso O
O5 1.418(2) 0.0578(10) 0.1420(19) 0.01267 1.00000 Uiso O
O6 1.5262(18) -0.2001(14) 0.1193(20) 0.01267 1.00000 Uiso O
P1 0.7986(13) 0.5361(7) -0.1730(4) 0.01267 1.00000 Uiso P
P2 1.3323(13) -0.0997(8) 0.1766(2) 0.01267 1.00000 Uiso P
C1 0.891(7) 0.6616(11) -0.3176(9) 0.01267 1.00000 Uiso C
C2 0.96400 0.57640 -0.40960 0.01267 1.00000 Uiso C
C3 0.78500 0.59040 -0.48180 0.01267 1.00000 Uiso C
C4 0.81800 0.51550 -0.57180 0.01267 1.00000 Uiso C
C5 1.239(6) -0.1815(12) 0.3362(8) 0.01267 1.00000 Uiso C
C6 1.12100 -0.08500 0.41840 0.01267 1.00000 Uiso C
C7 1.23700 -0.06360 0.50880 0.01267 1.00000 Uiso C
C8 1.11900 0.01840 0.58910 0.01267 1.00000 Uiso C

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

#=============================================================================
# DISTANCES AND ANGLES / MOLECULAR GEOMETRY

_geom_special_details            ?


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
? ? ? ? ? ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
_database_code_depnum_ccdc_archive 'CCDC 775634'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3_Tb
#TrackingRef '3_Tb.cif'


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

_audit_creation_method           'Manual editing plus fullprof.2k'
_audit_creation_date             '16 April 2010'

#=============================================================================
# CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C8 H11 O7 P2 Tb'
_chemical_formula_weight         ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

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
TB 25.89760 2.24256 18.21850 0.19614 14.31670 12.66480 2.95354 115.36200
3.58224 -9.49800 9.24200
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
P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490
0.28300 0.43400
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

#=============================================================================
# POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

_cell_length_a                   5.5882(5)
_cell_length_b                   9.3484(8)
_cell_length_c                   11.4594(10)
_cell_angle_alpha                75.325(4)
_cell_angle_beta                 81.698(4)
_cell_angle_gamma                81.177(5)
_cell_volume                     568.76(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_cell_special_details            
;
?
;

_pd_spec_mounting                
;
Glass slide
;

_pd_spec_mount_mode              Reflection
_pd_spec_shape                   'Flat sheet'


#=============================================================================
# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_pd_instr_location               
;
Conventional powder diffractometer instrument belonging to the
University of Aveiro and located at the Central Analytical Laboratory
;

_pd_calibration_special_details  
;
LaB6 standard
;

_diffrn_ambient_temperature      298
_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           X-ray
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  None
_diffrn_measurement_method       Bragg-Brentano
_diffrn_detector_type            'X Celerator detector'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;
Data were collected in a continuous mode over the angular range 4-110.
;


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

_pd_meas_number_of_points        5286
_pd_meas_2theta_range_min        4.00703
_pd_meas_2theta_range_max        109.99242
_pd_meas_2theta_range_inc        0.020054

#=============================================================================
# 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     Cauchy
_pd_proc_ls_background_function  'Fixed Points'
_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        2.2193
_pd_proc_ls_prof_wR_factor       2.9608
_pd_proc_ls_prof_wR_expected     0.7439

# 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       23.0321
_pd_proc_ls_prof_cwR_factor      15.3831
_pd_proc_ls_prof_cwR_expected    3.8653

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

_pd_proc_ls_prof_chi2            15.8387
_pd_proc_ls_prof_echi2           16.0889

# Items related to LS refinement

_refine_ls_R_I_factor            12.8350
_refine_ls_number_reflns         3005
_refine_ls_number_parameters     50
_refine_ls_number_restraints     16

# 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        4.0110
_pd_proc_2theta_range_max        109.9964
_pd_proc_2theta_range_inc        0.020054
_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    ?
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    'Crystal Impact Diamond 3.2'
_computing_publication_material  ?

#=============================================================================
# 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
_atom_site_type_symbol
TB1 1.1186(8) 0.1924(5) -0.0046(4) 0.01267 1.00000 Uiso TB
O1W 0.770(5) 0.232(3) 0.119(2) 0.01267 1.00000 Uiso O
O1 0.948(2) 0.3846(13) -0.1344(19) 0.01267 1.00000 Uiso O
O2 0.5243(14) 0.5107(17) -0.1543(18) 0.01267 1.00000 Uiso O
O3 0.815(3) 0.6210(18) -0.0709(19) 0.01267 1.00000 Uiso O
O4 1.1009(16) -0.0787(15) 0.1160(17) 0.01267 1.00000 Uiso O
O5 1.422(2) 0.0605(10) 0.1438(19) 0.01267 1.00000 Uiso O
O6 1.5309(19) -0.1991(14) 0.1213(20) 0.01267 1.00000 Uiso O
P1 0.7956(13) 0.5374(7) -0.1695(3) 0.01267 1.00000 Uiso P
P2 1.3329(13) -0.0959(8) 0.1762(2) 0.01267 1.00000 Uiso P
C1 0.881(7) 0.6607(10) -0.3166(9) 0.01267 1.00000 Uiso C
C2 0.96400 0.57640 -0.40960 0.01267 1.00000 Uiso C
C3 0.78500 0.59040 -0.48180 0.01267 1.00000 Uiso C
C4 0.81800 0.51550 -0.57180 0.01267 1.00000 Uiso C
C5 1.243(6) -0.1808(12) 0.3358(8) 0.01267 1.00000 Uiso C
C6 1.12100 -0.08500 0.41840 0.01267 1.00000 Uiso C
C7 1.23700 -0.06360 0.50880 0.01267 1.00000 Uiso C
C8 1.11900 0.01840 0.58910 0.01267 1.00000 Uiso C

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

#=============================================================================
# DISTANCES AND ANGLES / MOLECULAR GEOMETRY

_geom_special_details            ?


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
? ? ? ? ? ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
_database_code_depnum_ccdc_archive 'CCDC 775635'