# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Mikael Hakansson'
_publ_contact_author_email       HSON@CHEM.GU.SE

_publ_section_title              
;

;
loop_
_publ_author_name
'Mikael Hakansson'
'Anders Lennartson'

# Attachment '1a_new.cif'

data_1a
_database_code_depnum_ccdc_archive 'CCDC 699737'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;Pentasodium tris(2,2?-oxydiacetato)-dysprosium(III)
bis(tetrafluoroborate) hexahydrate
;
_chemical_name_common            
;
Pentasodium tris(2,2?-oxydiacetato)-dysprosium(iii)
bis(tetrafluoroborate) hexahydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 B2 Dy F8 Na5 O21'
_chemical_formula_sum            'C12 H24 B2 Dy F8 Na5 O21'
_chemical_formula_weight         955.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2'
_symmetry_int_tables_number      155
_symmetry_space_group_name_Hall  'R 3 2"'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   9.638(2)
_cell_length_b                   9.638(2)
_cell_length_c                   27.840(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2239.6(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    289(2)
_cell_measurement_reflns_used    5017
_cell_measurement_theta_min      4.39
_cell_measurement_theta_max      26.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1401
_exptl_absorpt_coefficient_mu    2.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3377
_exptl_absorpt_correction_T_max  0.7612
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_source_type              RU-H3R
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5017
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         4.39
_diffrn_reflns_theta_max         26.00
_reflns_number_total             960
_reflns_number_gt                959
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    'CrystalClear(Rigaku, 2000)'
_computing_structure_refinement  'SIR92 (Altomare et al., 1993)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0166P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack (1983), 392 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.029(16)
_refine_ls_number_reflns         960
_refine_ls_number_parameters     76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0555
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.3403(4) 0.1880(9) 0.76794(13) 0.0207(14) Uani 1 1 d . . .
C2 C 0.2858(5) 0.0480(5) 0.80145(15) 0.0272(9) Uani 1 1 d . . .
H2B H 0.1928 0.0324 0.8194 0.033 Uiso 1 1 calc R . .
H2A H 0.2560 -0.0487 0.7832 0.033 Uiso 1 1 calc R . .
O1 O 0.4124(4) 0.0791(4) 0.8333 0.0243(9) Uani 1 2 d S . .
O2 O 0.4780(3) 0.3066(3) 0.77509(10) 0.0237(6) Uani 1 1 d . . .
O3 O 0.2524(4) 0.1741(4) 0.73364(11) 0.0363(8) Uani 1 1 d . . .
O4 O 0.5928(4) 0.4805(4) 0.69107(12) 0.0388(10) Uani 1 1 d . . .
F1 F 0.3333 0.6667 0.78578(16) 0.0720(15) Uani 1 3 d S . .
F2 F 0.2475(8) 0.5131(3) 0.71985(12) 0.0614(8) Uani 1 1 d . . .
Na1 Na 0.3333 0.3815(3) 0.6667 0.0443(7) Uani 1 2 d S . .
Na2 Na 0.0000 0.0000 0.69996(8) 0.0278(5) Uani 1 3 d S . .
Dy1 Dy 0.6667 0.3333 0.8333 0.01566(14) Uani 1 6 d S . .
B1 B 0.3333 0.6667 0.7369(2) 0.0344(15) Uani 1 3 d S . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O3 1.238(5) . ?
C1 O2 1.261(5) . ?
C1 C2 1.503(8) . ?
C2 O1 1.415(4) . ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
O1 Dy1 2.450(4) . ?
O2 Dy1 2.352(3) . ?
O3 Na2 2.352(3) . ?
O3 Na1 2.554(4) . ?
O4 Na1 2.289(3) . ?
F1 B1 1.359(8) . ?
F2 B1 1.370(4) . ?
F2 Na1 2.353(6) . ?
Na2 O4 2.472(4) 12_446 ?

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
O3 C1 O2 124.9(6) . . ?
O3 C1 C2 117.9(4) . . ?
O2 C1 C2 116.9(4) . . ?
O1 C2 C1 108.8(3) . . ?
O1 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
O1 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
H2B C2 H2A 108.3 . . ?
C2 O1 Dy1 122.5(2) . . ?
C1 O2 Dy1 127.9(3) . . ?
C1 O3 Na2 142.4(4) . . ?
C1 O3 Na1 123.6(4) . . ?
Na2 O3 Na1 93.98(11) . . ?
Na1 O4 Na2 97.82(12) . 10_556 ?
B1 F2 Na1 128.0(4) . . ?
O4 Na1 O4 165.1(2) 11_556 . ?
O4 Na1 F2 101.18(19) 11_556 11_556 ?
O4 Na1 F2 89.48(18) . 11_556 ?
O4 Na1 F2 101.18(19) . . ?
F2 Na1 F2 88.72(19) 11_556 . ?
O4 Na1 O3 83.40(12) . 11_556 ?
F2 Na1 O3 172.10(17) . 11_556 ?
O4 Na1 O3 83.40(12) 11_556 . ?
O4 Na1 O3 87.25(12) . . ?
F2 Na1 O3 84.86(11) . . ?
O3 Na1 O3 101.89(19) 11_556 . ?
O3 Na2 O3 105.16(11) . 3 ?
O3 Na2 O4 85.80(11) . 12_446 ?
O3 Na2 O4 83.96(11) 3 12_446 ?
O3 Na2 O4 162.92(14) . 10_456 ?
O4 Na2 O4 82.33(13) 12_446 10_456 ?
O3 Na2 O4 162.92(14) 3 11_556 ?
O3 Na2 O4 85.80(11) 2 11_556 ?
O3 Na2 Na1 145.33(9) 3 . ?
O3 Na2 Na1 101.01(9) 2 . ?
O4 Na2 Na1 77.21(9) 12_446 . ?
O4 Na2 Na1 119.55(10) 10_456 . ?
O3 Na2 Na1 145.33(9) . 2 ?
O3 Na2 Na1 145.33(9) 2 3 ?
O4 Na2 Na1 77.21(9) 10_456 3 ?
O4 Na2 Na1 119.55(10) 11_556 3 ?
O2 Dy1 O2 88.18(14) 16_556 . ?
O2 Dy1 O2 147.83(14) 17_656 . ?
O2 Dy1 O2 127.64(14) 18_546 . ?
O2 Dy1 O2 77.72(11) 2_655 . ?
O2 Dy1 O1 63.82(7) . . ?
O2 Dy1 O1 135.91(7) 3_665 . ?
O1 Dy1 O1 120.000(1) 2_655 . ?
F1 B1 F2 110.3(3) . . ?
F2 B1 F2 108.6(3) 3_565 . ?
F1 B1 F2 110.3(3) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.110

# Attachment '1b_new.cif'

data_1b
_database_code_depnum_ccdc_archive 'CCDC 721015'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;Pentasodium tris(2,2?-oxydiacetato)-erbium(III)
bis(tetrafluoroborate) hexahydrate
;
_chemical_name_common            
;
Pentasodium tris(2,2?-oxydiacetato)-erbium(iii)
bis(tetrafluoroborate) hexahydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 B2 Er F8 Na5 O21'
_chemical_formula_sum            'C12 H24 B2 Er F8 Na5 O21'
_chemical_formula_weight         960.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_int_tables_number      155

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   9.6578(15)
_cell_length_b                   9.6578(15)
_cell_length_c                   27.923(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2255.5(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    289(2)
_cell_measurement_reflns_used    4432
_cell_measurement_theta_min      4.93
_cell_measurement_theta_max      25.96

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1407
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4205
_exptl_absorpt_correction_T_max  0.5494
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      289(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Rigaku RU-H3R'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4432
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         4.93
_diffrn_reflns_theta_max         25.96
_reflns_number_total             873
_reflns_number_gt                872
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    'CrystalClear(Rigaku, 2000)'
_computing_structure_refinement  'SIR92 (Altomare et al., 1993)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0458P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack (1983), 359 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.051(17)
_refine_ls_number_reflns         873
_refine_ls_number_parameters     76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0149
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0403
_refine_ls_goodness_of_fit_ref   1.428
_refine_ls_restrained_S_all      1.428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.6589(5) 0.8121(11) 0.23228(15) 0.0204(17) Uani 1 1 d . . .
C2 C 0.7139(6) 0.9515(6) 0.19854(19) 0.0257(10) Uani 1 1 d . . .
H2B H 0.7440 1.0486 0.2165 0.031 Uiso 1 1 calc R . .
H2A H 0.8063 0.9664 0.1806 0.031 Uiso 1 1 calc R . .
O1 O 0.5857(5) 0.9190(5) 0.1667 0.0221(11) Uani 1 2 d S . .
O2 O 0.5189(4) 0.6903(4) 0.22457(13) 0.0209(7) Uani 1 1 d . . .
O3 O 0.7451(5) 0.8215(5) 0.26606(15) 0.0321(9) Uani 1 1 d . . .
O4 O 0.4063(5) 0.5201(5) 0.30931(16) 0.0360(10) Uani 1 1 d . . .
F1 F 0.6667 0.3333 0.2143(2) 0.072(2) Uani 1 3 d S . .
F2 F 0.7587(10) 0.4870(5) 0.28042(18) 0.0565(14) Uani 1 1 d . . .
Na1 Na 0.6667 0.6185(4) 0.3333 0.0417(8) Uani 1 2 d S . .
Na2 Na 1.0000 1.0000 0.29968(11) 0.0249(6) Uani 1 3 d S . .
Er1 Er 0.3333 0.6667 0.1667 0.0124(2) Uani 1 6 d S . .
B1 B 0.6667 0.3333 0.2629(3) 0.0318(16) Uani 1 3 d S . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O3 1.231(6) . ?
C1 O2 1.291(6) . ?
C1 C2 1.506(9) . ?
C2 O1 1.426(5) . ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
O1 Er1 2.437(5) . ?
O2 Er1 2.339(3) . ?
O3 Na2 2.381(4) . ?
O3 Na1 2.542(5) . ?
O4 Na1 2.299(4) . ?
O4 Na2 2.468(5) 16_565 ?
F1 B1 1.359(11) . ?
F2 B1 1.383(5) . ?
F2 Na1 2.391(8) . ?
Na1 O4 2.299(4) 17_655 ?
Na2 O4 2.468(5) 18 ?

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
O3 C1 O2 123.8(7) . . ?
O3 C1 C2 119.4(5) . . ?
O2 C1 C2 116.8(5) . . ?
O1 C2 C1 108.3(4) . . ?
O1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
O1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
H2B C2 H2A 108.4 . . ?
C2 O1 Er1 123.0(3) . . ?
C1 O2 Er1 127.3(4) . . ?
C1 O3 Na2 140.5(5) . . ?
C1 O3 Na1 125.4(4) . . ?
Na2 O3 Na1 93.93(14) . . ?
Na1 O4 Na2 98.03(17) . 16_565 ?
B1 F2 Na1 125.3(5) . . ?
O4 Na1 O4 164.6(3) 17_655 . ?
O4 Na1 F2 88.3(2) . 17_655 ?
O4 Na1 F2 102.8(2) . . ?
F2 Na1 F2 88.4(3) 17_655 . ?
O4 Na1 O3 83.57(16) . 17_655 ?
F2 Na1 O3 170.4(2) . 17_655 ?
O4 Na1 O3 83.57(16) 17_655 . ?
O4 Na1 O3 86.88(15) . . ?
F2 Na1 O3 84.63(15) . . ?
O3 Na1 O3 103.0(3) 17_655 . ?
O3 Na2 O3 105.48(14) . 3_675 ?
O3 Na2 O4 86.04(15) . 18 ?
O3 Na2 O4 162.40(18) . 16_665 ?
O3 Na2 O4 86.05(15) 3_675 16_665 ?
O4 Na2 O4 82.02(17) 18 16_665 ?
O3 Na2 O4 83.54(15) . 17_655 ?
O3 Na2 O4 162.40(18) 3_675 17_655 ?
O3 Na2 O4 86.04(15) 2_765 17_655 ?
O2 Er1 O2 146.82(18) 12_455 3_565 ?
O2 Er1 O2 77.47(14) 2_665 3_565 ?
O2 Er1 O2 88.29(18) 10_565 . ?
O2 Er1 O2 146.82(18) 11 . ?
O2 Er1 O2 128.81(17) 12_455 . ?
O2 Er1 O1 73.41(9) 10_565 . ?
O2 Er1 O1 135.85(9) 11 . ?
O2 Er1 O1 64.40(9) . . ?
O1 Er1 O1 120.000(1) 2_665 . ?
F1 B1 F2 110.7(4) . . ?
F2 B1 F2 108.2(4) 3_665 . ?

_diffrn_measured_fraction_theta_max 0.868
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.853
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.196

# Attachment '1c_new.cif'

data_1c
_database_code_depnum_ccdc_archive 'CCDC 721016'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;Pentasodium tris(2,2?-oxydiacetato)-praseodymium(III)
bis(tetrafluoroborate) hexahydrate
;
_chemical_name_common            
;
Pentasodium tris(2,2?-oxydiacetato)-praseodymium(iii)
bis(tetrafluoroborate) hexahydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H24 B2 F8 Na5 O21 Pr1'
_chemical_formula_sum            'C12 H24 B2 F8 Na5 O21 Pr1'
_chemical_formula_weight         933.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2'
_symmetry_int_tables_number      155
_symmetry_space_group_name_Hall  'R 3 2"'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   9.710(2)
_cell_length_b                   9.710(2)
_cell_length_c                   28.170(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2300.2(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    289(2)
_cell_measurement_reflns_used    6034
_cell_measurement_theta_min      4.34
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1380
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      289(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Rigaku RU-H3R'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6034
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         4.34
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1155
_reflns_number_gt                1153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    'CrystalClear(Rigaku, 2000)'
_computing_structure_refinement  'SIR92 (Altomare et al., 1993)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0501P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack (1983), 483 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_number_reflns         1155
_refine_ls_number_parameters     76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C 0.6641(5) 0.8192(13) 0.23319(13) 0.0387(14) Uani 1 1 d . . .
C2 C 0.7188(5) 0.9593(6) 0.19902(18) 0.0461(10) Uani 1 1 d . . .
H2A H 0.7470 1.0555 0.2167 0.055 Uiso 1 1 calc R . .
H2B H 0.8120 0.9751 0.1817 0.055 Uiso 1 1 calc R . .
O1 O 0.5941(4) 0.9274(4) 0.1667 0.0388(9) Uani 1 2 d S . .
O2 O 0.5302(4) 0.7009(4) 0.22634(11) 0.0419(7) Uani 1 1 d . . .
O3 O 0.7524(5) 0.8347(5) 0.26716(14) 0.0611(12) Uani 1 1 d . . .
O4 O 0.4112(4) 0.5230(4) 0.30932(14) 0.0578(11) Uani 1 1 d . . .
F1 F 0.6667 0.3333 0.2153(2) 0.101(2) Uani 1 3 d S . .
F2 F 0.7483(10) 0.4868(4) 0.28077(15) 0.0891(11) Uani 1 1 d . . .
Na1 Na 0.6667 0.6179(4) 0.3333 0.0677(9) Uani 1 2 d S . .
Na2 Na 1.0000 1.0000 0.30064(9) 0.0384(5) Uani 1 3 d S . .
Pr1 Pr 0.3333 0.6667 0.1667 0.02591(15) Uani 1 6 d S . .
B1 B 0.6667 0.3333 0.2635(3) 0.0538(17) Uani 1 3 d S . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O3 1.243(6) . ?
C1 O2 1.246(7) . ?
C1 C2 1.528(11) . ?
C2 O1 1.421(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O1 C2 1.420(5) 12_455 ?
O1 Pr1 2.532(4) . ?
O2 Pr1 2.440(3) . ?
O3 Na2 2.321(4) . ?
O3 Na1 2.617(5) . ?
O4 Na1 2.274(4) . ?
O4 Na2 2.475(5) 16_565 ?
F1 B1 1.359(10) . ?
F2 B1 1.380(4) . ?
F2 Na1 2.335(8) . ?
Na1 F2 2.335(8) 17_655 ?

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
O3 C1 O2 124.7(8) . . ?
O3 C1 C2 117.7(6) . . ?
O2 C1 C2 117.4(5) . . ?
O1 C2 C1 109.3(3) . . ?
O1 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O1 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
C2 O1 C2 115.3(5) 12_455 . ?
C2 O1 Pr1 122.4(3) 12_455 . ?
C2 O1 Pr1 122.4(3) . . ?
C1 O2 Pr1 128.1(4) . . ?
C1 O3 Na2 144.1(5) . . ?
C1 O3 Na1 121.9(5) . . ?
Na2 O3 Na1 93.99(13) . . ?
Na1 O4 Na2 99.10(15) . 16_565 ?
B1 F2 Na1 130.1(5) . . ?
O4 Na1 O4 163.9(3) 17_655 . ?
O4 Na1 F2 90.6(2) . 17_655 ?
O4 Na1 F2 100.9(2) . . ?
F2 Na1 F2 88.7(2) 17_655 . ?
O4 Na1 O3 82.04(15) . 17_655 ?
F2 Na1 O3 173.9(2) . 17_655 ?
O4 Na1 O3 82.03(15) 17_655 . ?
O4 Na1 O3 87.60(14) . . ?
F2 Na1 O3 173.9(2) 17_655 . ?
F2 Na1 O3 85.92(13) . . ?
O3 Na1 O3 99.6(2) 17_655 . ?
O3 Na2 O3 104.61(14) . 3_675 ?
O3 Na2 O4 85.76(14) . 18 ?
O3 Na2 O4 163.75(16) . 16_665 ?
O4 Na2 O4 82.84(14) 18 16_665 ?
O3 Na2 O4 84.29(14) . 17_655 ?
O3 Na2 O4 163.75(16) 3_675 17_655 ?
O3 Na2 O4 85.76(14) 2_765 17_655 ?
O4 Na2 O4 82.83(14) 16_665 17_655 ?
O2 Pr1 O2 150.42(16) 10_565 2_665 ?
O2 Pr1 O2 125.23(16) 11 2_665 ?
O2 Pr1 O2 88.68(17) 11 3_565 ?
O2 Pr1 O2 150.42(16) 11 . ?
O2 Pr1 O2 125.24(16) 12_455 . ?
O2 Pr1 O2 77.77(13) 2_665 . ?
O2 Pr1 O2 77.78(13) 3_565 . ?
O2 Pr1 O1 75.21(8) 10_565 . ?
O2 Pr1 O1 135.66(8) 11 . ?
O2 Pr1 O1 62.62(8) . . ?
O1 Pr1 O1 120.000(1) . 3_565 ?
F1 B1 F2 110.6(4) . . ?
F2 B1 F2 108.3(4) 3_665 . ?
F2 B1 F2 108.3(4) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.705
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.114

# Attachment '2_new.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 721017'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;Trisodium tris(2,2?-oxydiacetato)-gadolinium(III)
hexaahydrate
;
_chemical_name_common            
'Trisodium tris(2,2?-oxydiacetato)-gadolinium(iii) hexaahydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Gd Na3 O15, 8(H2 O)'
_chemical_formula_sum            'C12 H28 Gd Na3 O23'
_chemical_formula_weight         766.57

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'
Gd Gd -0.1653 3.9035 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C c'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_int_tables_number      9

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   17.535(4)
_cell_length_b                   8.4677(16)
_cell_length_c                   19.207(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.483(16)
_cell_angle_gamma                90.00
_cell_volume                     2653.7(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    289(2)
_cell_measurement_reflns_used    7088
_cell_measurement_theta_min      4.24
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4758
_exptl_absorpt_correction_T_max  0.7670
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      289(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_source_type              RU-H3R
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7088
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.24
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3974
_reflns_number_gt                3871
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    'CrystalClear(Rigaku, 2000)'
_computing_structure_refinement  'SIR92 (Altomare et al., 1993)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0401P)²+2.0052P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.315(9)
_refine_ls_number_reflns         3974
_refine_ls_number_parameters     353
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.0542
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_restrained_S_all      0.905
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O16 O 0.6882(5) 0.5328(6) 0.7531(4) 0.0717(18) Uani 1 1 d . . .
O17 O 0.7746(3) 0.7192(6) 0.9300(3) 0.0421(12) Uani 1 1 d . . .
O18 O 0.5553(4) 0.4264(6) 0.8344(3) 0.0360(12) Uani 1 1 d . . .
O19 O 0.4893(4) 1.1064(7) 0.9222(3) 0.0462(13) Uani 1 1 d . . .
O20 O 0.6583(3) 1.1593(6) 0.8879(3) 0.0399(12) Uani 1 1 d . . .
O21 O 0.3766(3) 1.6401(7) 0.3603(3) 0.0447(13) Uani 1 1 d . . .
O22 O 0.7730(3) 1.2505(8) 0.8208(3) 0.0551(15) Uani 1 1 d . . .
O23 O 0.3945(4) 1.0035(7) 0.5012(3) 0.0609(13) Uani 1 1 d . . .
Na3 Na 0.4862(2) 1.4349(3) 0.4059(2) 0.0241(7) Uani 1 1 d . . .
C1 C 0.8747(4) 0.8961(9) 0.5139(4) 0.0223(11) Uani 1 1 d . . .
C2 C 0.9269(6) 1.0296(9) 0.5606(6) 0.0302(18) Uani 1 1 d . . .
H2A H 0.9811 0.9903 0.5902 0.036 Uiso 1 1 calc R . .
H2B H 0.9327 1.1123 0.5280 0.036 Uiso 1 1 calc R . .
C3 C 0.9445(4) 1.1701(7) 0.6723(3) 0.0250(14) Uani 1 1 d . . .
H3A H 0.9573 1.2737 0.6579 0.030 Uiso 1 1 calc R . .
H3B H 0.9951 1.1102 0.6921 0.030 Uiso 1 1 calc R . .
C4 C 0.9072(4) 1.1869(7) 0.7319(4) 0.0204(14) Uani 1 1 d . . .
C5 C 0.9111(4) 0.6870(9) 0.7100(4) 0.0244(14) Uani 1 1 d . . .
C6 C 0.8456(6) 0.5719(8) 0.6624(6) 0.034(2) Uani 1 1 d . . .
H6A H 0.8628 0.5247 0.6245 0.041 Uiso 1 1 calc R . .
H6B H 0.8382 0.4880 0.6937 0.041 Uiso 1 1 calc R . .
C7 C 0.7078(7) 0.5595(7) 0.5776(6) 0.037(2) Uani 1 1 d . . .
H7A H 0.6925 0.4762 0.6046 0.045 Uiso 1 1 calc R . .
H7B H 0.7264 0.5110 0.5408 0.045 Uiso 1 1 calc R . .
C8 C 0.6357(5) 0.6624(8) 0.5393(4) 0.0273(16) Uani 1 1 d . . .
C9 C 0.6368(4) 1.1864(7) 0.5038(4) 0.0187(13) Uani 1 1 d . . .
C10 C 0.5952(4) 1.1778(7) 0.5602(3) 0.0204(12) Uani 1 1 d . . .
H10A H 0.5829 1.2835 0.5725 0.024 Uiso 1 1 calc R . .
H10B H 0.5441 1.1200 0.5390 0.024 Uiso 1 1 calc R . .
C11 C 0.6098(6) 1.0553(7) 0.6750(6) 0.030(2) Uani 1 1 d . . .
H11A H 0.5548 1.0191 0.6460 0.036 Uiso 1 1 calc R . .
H11B H 0.6052 1.1466 0.7038 0.036 Uiso 1 1 calc R . .
C12 C 0.6556(4) 0.9252(7) 0.7284(4) 0.0190(15) Uani 1 1 d . . .
Gd1 Gd 0.76805(3) 0.947136(15) 0.62250(3) 0.01385(7) Uani 1 1 d . . .
O1 O 0.8111(3) 0.8548(5) 0.5250(3) 0.0279(11) Uani 1 1 d . . .
O2 O 0.8888(3) 1.0919(6) 0.6090(3) 0.0223(9) Uani 1 1 d . . .
O3 O 0.8327(3) 1.1482(5) 0.7135(2) 0.0232(9) Uani 1 1 d . . .
O4 O 0.9001(3) 0.8350(5) 0.4670(3) 0.0301(10) Uani 1 1 d . . .
O5 O 0.9519(3) 1.2419(6) 0.7939(2) 0.0322(10) Uani 1 1 d . . .
O6 O 0.8909(3) 0.8303(5) 0.7046(3) 0.0269(10) Uani 1 1 d . . .
O7 O 0.7721(4) 0.6527(3) 0.6284(4) 0.0253(7) Uani 1 1 d . . .
O8 O 0.6458(3) 0.8109(5) 0.5452(3) 0.0306(11) Uani 1 1 d . . .
O9 O 0.9794(3) 0.6355(6) 0.7486(3) 0.0381(11) Uani 1 1 d . . .
O10 O 0.5717(3) 0.5960(7) 0.5020(3) 0.0411(12) Uani 1 1 d . . .
O11 O 0.7093(3) 1.1333(5) 0.5238(2) 0.0261(10) Uani 1 1 d . . .
O12 O 0.6483(3) 1.0994(7) 0.6268(2) 0.0206(8) Uani 1 1 d . . .
O13 O 0.7204(3) 0.8754(6) 0.7197(3) 0.0246(10) Uani 1 1 d . . .
O14 O 0.5977(2) 1.2424(5) 0.4412(2) 0.0232(8) Uani 1 1 d . . .
O15 O 0.6285(3) 0.8763(5) 0.7740(3) 0.0351(11) Uani 1 1 d . . .
Na2 Na 0.5458(3) 0.9641(3) 0.8417(2) 0.0263(7) Uani 1 1 d . . .
Na1 Na 0.64274(13) 0.6440(2) 0.84212(10) 0.0361(4) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
O16 Na1 2.334(5) . ?
O17 Na1 2.397(6) . ?
O18 Na1 2.367(6) . ?
O19 Na2 2.439(6) . ?
O20 Na2 2.476(7) . ?
O21 Na3 2.500(7) . ?
Na3 O14 2.443(5) . ?
C1 O4 1.255(8) . ?
C1 O1 1.259(8) . ?
C1 C2 1.522(11) . ?
C2 O2 1.428(10) . ?
C3 O2 1.415(8) . ?
C3 C4 1.520(9) . ?
C4 O5 1.250(8) . ?
C4 O3 1.265(8) . ?
C5 O9 1.233(9) . ?
C5 O6 1.258(8) . ?
C5 C6 1.528(12) . ?
C6 O7 1.392(10) . ?
C7 O7 1.429(11) . ?
C7 C8 1.489(12) . ?
C8 O10 1.224(9) . ?
C8 O8 1.269(8) . ?
C9 O14 1.240(8) . ?
C9 O11 1.268(8) . ?
C9 C10 1.512(9) . ?
C10 O12 1.440(7) . ?
C11 O12 1.383(10) . ?
C11 C12 1.519(9) . ?
C12 O15 1.212(8) . ?
C12 O13 1.278(8) . ?
Gd1 O6 2.370(5) . ?
Gd1 O13 2.387(4) . ?
Gd1 O11 2.390(4) . ?
Gd1 O1 2.393(4) . ?
Gd1 O3 2.406(4) . ?
Gd1 O8 2.409(5) . ?
Gd1 O7 2.496(3) . ?
Gd1 O12 2.491(5) . ?
Gd1 O2 2.541(5) . ?
O15 Na1 2.325(4) . ?
O15 Na2 2.393(6) . ?

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
Na1 O18 Na3 91.93(19) . 2_575 ?
O10 Na3 O4 99.1(2) 1_565 3_455 ?
O10 Na3 O14 87.3(2) 1_565 . ?
O4 Na3 O14 102.32(18) 3_455 . ?
O10 Na3 O18 81.7(2) 1_565 2_574 ?
O4 Na3 O18 169.6(2) 3_455 2_574 ?
O14 Na3 O18 88.0(2) . 2_574 ?
O10 Na3 O21 93.4(2) 1_565 . ?
O4 Na3 O21 82.8(2) 3_455 . ?
O14 Na3 O21 174.6(3) . . ?
O18 Na3 O21 86.8(2) 2_574 . ?
O10 Na3 O5 155.1(2) 1_565 4_474 ?
O4 Na3 O5 102.4(2) 3_455 4_474 ?
O14 Na3 O5 75.87(15) . 4_474 ?
O18 Na3 O5 79.4(2) 2_574 4_474 ?
O21 Na3 O5 101.6(2) . 4_474 ?
O10 Na3 Na1 91.67(18) 1_565 2_574 ?
O4 Na3 Na1 146.62(15) 3_455 2_574 ?
O14 Na3 Na1 46.41(12) . 2_574 ?
O18 Na3 Na1 43.19(14) 2_574 2_574 ?
O21 Na3 Na1 128.2(2) . 2_574 ?
O5 Na3 Na1 63.41(13) 4_474 2_574 ?
O10 Na3 Na2 126.14(16) 1_565 2_574 ?
O4 Na3 Na2 98.08(13) 3_455 2_574 ?
O14 Na3 Na2 39.08(14) . 2_574 ?
O18 Na3 Na2 89.59(14) 2_574 2_574 ?
O21 Na3 Na2 139.27(18) . 2_574 ?
O5 Na3 Na2 38.09(12) 4_474 2_574 ?
Na1 Na3 Na2 51.38(5) 2_574 2_574 ?
O4 C1 O1 125.2(6) . . ?
O4 C1 C2 115.8(6) . . ?
O1 C1 C2 119.0(6) . . ?
O2 C2 C1 109.6(7) . . ?
O2 C3 C4 109.8(5) . . ?
O5 C4 O3 125.8(6) . . ?
O5 C4 C3 117.4(6) . . ?
O3 C4 C3 116.8(6) . . ?
O9 C5 O6 124.9(7) . . ?
O9 C5 C6 119.0(7) . . ?
O6 C5 C6 116.0(6) . . ?
O7 C6 C5 109.3(5) . . ?
O7 C7 C8 109.2(5) . . ?
O10 C8 O8 125.1(7) . . ?
O10 C8 C7 116.8(6) . . ?
O8 C8 C7 118.1(7) . . ?
O14 C9 O11 124.4(6) . . ?
O14 C9 C10 118.2(6) . . ?
O11 C9 C10 117.4(6) . . ?
O12 C10 C9 109.5(5) . . ?
O12 C11 C12 112.4(6) . . ?
O15 C12 O13 125.7(6) . . ?
O15 C12 C11 119.0(6) . . ?
O13 C12 C11 115.3(6) . . ?
O6 Gd1 O13 82.32(17) . . ?
O6 Gd1 O11 145.68(17) . . ?
O13 Gd1 O11 128.03(15) . . ?
O6 Gd1 O1 85.05(18) . . ?
O13 Gd1 O1 146.16(11) . . ?
O11 Gd1 O1 76.26(16) . . ?
O6 Gd1 O3 74.96(15) . . ?
O13 Gd1 O3 79.54(17) . . ?
O11 Gd1 O3 93.50(11) . . ?
O1 Gd1 O3 126.86(15) . . ?
O6 Gd1 O8 126.66(11) . . ?
O13 Gd1 O8 82.71(17) . . ?
O11 Gd1 O8 78.41(16) . . ?
O1 Gd1 O8 79.97(17) . . ?
O3 Gd1 O8 149.68(16) . . ?
O6 Gd1 O7 63.17(17) . . ?
O13 Gd1 O7 73.91(19) . . ?
O11 Gd1 O7 133.79(18) . . ?
O1 Gd1 O7 72.36(18) . . ?
O3 Gd1 O7 132.53(17) . . ?
O8 Gd1 O7 63.50(18) . . ?
O6 Gd1 O12 139.95(16) . . ?
O13 Gd1 O12 64.20(14) . . ?
O11 Gd1 O12 63.99(14) . . ?
O1 Gd1 O12 134.99(16) . . ?
O3 Gd1 O12 77.76(16) . . ?
O8 Gd1 O12 72.42(17) . . ?
O7 Gd1 O12 121.76(19) . . ?
O6 Gd1 O2 71.42(17) . . ?
O13 Gd1 O2 138.28(17) . . ?
O11 Gd1 O2 74.54(16) . . ?
O1 Gd1 O2 64.13(15) . . ?
O3 Gd1 O2 62.89(15) . . ?
O8 Gd1 O2 139.01(16) . . ?
O7 Gd1 O2 118.39(18) . . ?
O12 Gd1 O2 119.84(9) . . ?
C1 O1 Gd1 126.5(4) . . ?
C3 O2 C2 113.0(6) . . ?
C3 O2 Gd1 118.5(4) . . ?
C2 O2 Gd1 119.6(4) . . ?
C4 O3 Gd1 123.4(4) . . ?
C1 O4 Na3 131.6(4) . 3_545 ?
C4 O5 Na2 138.1(4) . 3 ?
C4 O5 Na3 117.7(4) . 4_575 ?
Na2 O5 Na3 102.7(2) 3 4_575 ?
C5 O6 Gd1 128.1(4) . . ?
C6 O7 C7 114.4(4) . . ?
C6 O7 Gd1 121.2(4) . . ?
C7 O7 Gd1 121.2(4) . . ?
C8 O8 Gd1 126.4(5) . . ?
C5 O9 Na2 143.7(5) . 3_545 ?
C8 O10 Na3 156.0(5) . 1_545 ?
C9 O11 Gd1 124.5(4) . . ?
C11 O12 C10 113.8(6) . . ?
C11 O12 Gd1 120.5(4) . . ?
C10 O12 Gd1 119.2(3) . . ?
C12 O13 Gd1 126.9(4) . . ?
C9 O14 Na3 128.8(4) . . ?
C9 O14 Na1 131.9(4) . 2_574 ?
Na3 O14 Na1 88.62(16) . 2_574 ?
C9 O14 Na2 113.0(4) . 2_574 ?
Na3 O14 Na2 102.9(2) . 2_574 ?
Na1 O14 Na2 79.38(16) 2_574 2_574 ?
C12 O15 Na1 134.9(4) . . ?
C12 O15 Na2 139.7(4) . . ?
Na1 O15 Na2 85.32(16) . . ?
O9 Na2 O15 90.5(2) 3_455 . ?
O9 Na2 O19 88.5(2) 3_455 . ?
O15 Na2 O19 164.9(3) . . ?
O9 Na2 O5 96.6(2) 3_455 3_445 ?
O15 Na2 O5 90.91(19) . 3_445 ?
O19 Na2 O5 104.1(2) . 3_445 ?
O9 Na2 O20 88.1(2) 3_455 . ?
O15 Na2 O20 80.8(2) . . ?
O19 Na2 O20 84.2(2) . . ?
O5 Na2 O20 170.5(2) 3_445 . ?
O9 Na2 O14 171.2(3) 3_455 2_575 ?
O15 Na2 O14 94.29(18) . 2_575 ?
O19 Na2 O14 88.8(2) . 2_575 ?
O5 Na2 O14 75.89(16) 3_445 2_575 ?
O20 Na2 O14 100.0(2) . 2_575 ?
O9 Na2 Na1 131.6(2) 3_455 . ?
O15 Na2 Na1 46.44(12) . . ?
O19 Na2 Na1 139.2(2) . . ?
O5 Na2 Na1 68.49(13) 3_445 . ?
O20 Na2 Na1 102.23(19) . . ?
O14 Na2 Na1 50.33(11) 2_575 . ?
O9 Na2 Na3 133.64(17) 3_455 2_575 ?
O15 Na2 Na3 100.98(14) . 2_575 ?
O19 Na2 Na3 90.55(18) . 2_575 ?
O5 Na2 Na3 39.21(15) 3_445 2_575 ?
O20 Na2 Na3 137.87(16) . 2_575 ?
O14 Na2 Na3 37.99(13) 2_575 2_575 ?
Na1 Na2 Na3 57.63(9) . 2_575 ?
O15 Na1 O16 85.65(19) . . ?
O15 Na1 O18 133.6(2) . . ?
O16 Na1 O18 91.6(2) . . ?
O15 Na1 O17 92.8(2) . . ?
O16 Na1 O17 97.0(3) . . ?
O18 Na1 O17 133.4(2) . . ?
O15 Na1 O14 95.96(16) . 2_575 ?
O16 Na1 O14 177.9(2) . 2_575 ?
O18 Na1 O14 88.26(16) . 2_575 ?
O17 Na1 O14 81.63(17) . 2_575 ?
O15 Na1 Na2 48.24(13) . . ?
O16 Na1 Na2 131.62(19) . . ?
O18 Na1 Na2 109.15(17) . . ?
O17 Na1 Na2 98.73(15) . . ?
O14 Na1 Na2 50.29(13) 2_575 . ?
O15 Na1 Na3 115.31(14) . 2_575 ?
O16 Na1 Na3 135.29(19) . 2_575 ?
O18 Na1 Na3 44.88(14) . 2_575 ?
O17 Na1 Na3 119.25(16) . 2_575 ?
O14 Na1 Na3 44.97(11) 2_575 2_575 ?
Na2 Na1 Na3 70.99(10) . 2_575 ?

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.916
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.072

# Attachment '3_new.cif'

data_3
_database_code_depnum_ccdc_archive 'CCDC 721018'
_chemical_name_systematic        
;Ammonium trisodium tris(2,2?-oxydiacetato)-praseodymium(III)tiocyanate
tetraahydrate
;
_audit_creation_method           SHELXL-97
_chemical_name_common            
;
Ammonium trisodium tris(2,2?-oxydiacetato)-
praseodymium(iii)tiocyanate tetraahydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H24 N2 Na3 O19 Pr S'
_chemical_formula_sum            'C13 H24 N2 Na3 O19 Pr S'
_chemical_formula_weight         754.29

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_int_tables_number      2

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

_cell_length_a                   9.1741(11)
_cell_length_b                   9.3387(16)
_cell_length_c                   17.7642(16)
_cell_angle_alpha                83.75(2)
_cell_angle_beta                 72.724(10)
_cell_angle_gamma                86.44(2)
_cell_volume                     1443.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    289(2)
_cell_measurement_reflns_used    8956
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      289(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_source_type              RU-H3R
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8956
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4584
_reflns_number_gt                4293
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    'CrystalClear(Rigaku, 2000)'
_computing_structure_refinement  'SIR92 (Altomare et al., 1993)'
_computing_molecular_graphics    
'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0589P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4584
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
C1 C 0.6695(4) 0.2054(4) 0.8264(3) 0.0266(9) Uani 1 1 d . . .
C2 C 0.5659(5) 0.2371(5) 0.9167(3) 0.0327(10) Uani 1 1 d . . .
H2A H 0.5220 0.1490 0.9467 0.039 Uiso 1 1 calc R . .
H2B H 0.6276 0.2774 0.9446 0.039 Uiso 1 1 calc R . .
C3 C 0.3402(5) 0.3659(4) 0.9872(2) 0.0315(9) Uani 1 1 d . . .
H3A H 0.2864 0.2795 1.0132 0.038 Uiso 1 1 calc R . .
H3B H 0.3958 0.3975 1.0208 0.038 Uiso 1 1 calc R . .
C4 C 0.2298(4) 0.4836(4) 0.9700(2) 0.0229(8) Uani 1 1 d . . .
C5 C 0.7118(4) 0.6998(4) 0.7703(2) 0.0231(8) Uani 1 1 d . . .
C6 C 0.6110(4) 0.8110(4) 0.7366(3) 0.0324(10) Uani 1 1 d . . .
H6A H 0.5832 0.8905 0.7695 0.039 Uiso 1 1 calc R . .
H6B H 0.6676 0.8489 0.6836 0.039 Uiso 1 1 calc R . .
C7 C 0.3954(4) 0.8380(4) 0.6838(3) 0.0268(9) Uani 1 1 d . . .
H7A H 0.4658 0.8640 0.6320 0.032 Uiso 1 1 calc R . .
H7B H 0.3558 0.9259 0.7082 0.032 Uiso 1 1 calc R . .
C8 C 0.2650(4) 0.7547(4) 0.6753(2) 0.0205(8) Uani 1 1 d . . .
C9 C 0.2436(4) 0.2327(4) 0.7045(3) 0.0273(9) Uani 1 1 d . . .
C10 C 0.3719(5) 0.2371(4) 0.6185(3) 0.0341(10) Uani 1 1 d . . .
H10A H 0.4265 0.1449 0.6114 0.041 Uiso 1 1 calc R . .
H10B H 0.3248 0.2597 0.5763 0.041 Uiso 1 1 calc R . .
C11 C 0.6023(4) 0.3545(4) 0.5424(2) 0.0258(9) Uani 1 1 d . . .
H11A H 0.6615 0.2645 0.5373 0.031 Uiso 1 1 calc R . .
H11B H 0.5642 0.3752 0.4968 0.031 Uiso 1 1 calc R . .
C12 C 0.6978(4) 0.4749(4) 0.5487(2) 0.0251(9) Uani 1 1 d . . .
C13 C 0.1571(5) 0.8983(4) 0.8847(3) 0.0326(10) Uani 1 1 d . . .
N1 N 0.0650(5) 0.8505(4) 0.8622(3) 0.0434(10) Uani 1 1 d . . .
O1 O 0.6382(3) 0.2678(3) 0.75840(19) 0.0317(7) Uani 1 1 d . . .
O2 O 0.4493(3) 0.3377(3) 0.90554(16) 0.0281(6) Uani 1 1 d . . .
O3 O 0.2441(3) 0.5282(3) 0.89058(17) 0.0303(6) Uani 1 1 d . . .
O4 O 0.7802(4) 0.1226(3) 0.8255(2) 0.0426(8) Uani 1 1 d . . .
O5 O 0.1338(3) 0.5241(3) 1.03665(17) 0.0334(7) Uani 1 1 d . . .
O6 O 0.6583(3) 0.5771(3) 0.80007(18) 0.0286(6) Uani 1 1 d . . .
O7 O 0.4773(3) 0.7464(3) 0.73407(18) 0.0250(6) Uani 1 1 d . . .
O8 O 0.2571(3) 0.6227(3) 0.70251(17) 0.0265(6) Uani 1 1 d . . .
O9 O 0.8425(3) 0.7353(3) 0.7645(2) 0.0376(8) Uani 1 1 d . . .
O10 O 0.1731(3) 0.8233(3) 0.64066(18) 0.0308(7) Uani 1 1 d . . .
O11 O 0.2579(3) 0.3041(3) 0.76460(19) 0.0317(7) Uani 1 1 d . . .
O12 O 0.4718(3) 0.3459(3) 0.61825(16) 0.0275(6) Uani 1 1 d . . .
O13 O 0.6537(3) 0.5420(3) 0.61701(19) 0.0404(8) Uani 1 1 d . . .
O14 O 0.1330(3) 0.1599(3) 0.7106(2) 0.0482(9) Uani 1 1 d . . .
O15 O 0.8132(3) 0.5017(3) 0.48482(19) 0.0390(8) Uani 1 1 d . . .
O16 O 0.7311(4) 0.9814(3) 0.5140(2) 0.0472(8) Uani 1 1 d . . .
O17 O -0.0658(4) 0.7470(3) 0.5106(2) 0.0445(8) Uani 1 1 d . . .
O18 O -0.0522(3) 0.4347(3) 0.7385(2) 0.0463(9) Uani 1 1 d . . .
O19 O 0.8500(4) 0.1071(3) 0.6281(2) 0.0400(8) Uani 1 1 d . . .
N2 N 0.0013(4) 0.2126(4) 0.9124(2) 0.0393(9) Uani 1 1 d . . .
S1 S 0.28425(16) 0.96940(15) 0.91944(10) 0.0548(4) Uani 1 1 d . . .
Pr1 Pr 0.453829(18) 0.473221(17) 0.756330(11) 0.01729(11) Uani 1 1 d . . .
Na1 Na 0.02091(17) 0.60233(17) 0.83614(10) 0.0319(4) Uani 1 1 d . . .
Na2 Na 0.96443(16) -0.02968(16) 0.73585(12) 0.0311(4) Uani 1 1 d . . .
Na3 Na 0.02948(19) 0.62731(17) 0.62484(10) 0.0346(4) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O4 1.236(5) . ?
C1 O1 1.383(6) . ?
C1 C2 1.651(6) . ?
C2 O2 1.424(4) . ?
C3 C4 1.517(6) . ?
C3 O2 1.537(4) . ?
C4 O5 1.325(5) . ?
C4 O3 1.397(5) . ?
C5 O9 1.236(5) . ?
C5 O6 1.272(5) . ?
C5 C6 1.538(6) . ?
C6 O7 1.414(5) . ?
C7 O7 1.498(5) . ?
C7 C8 1.519(5) . ?
C8 O8 1.272(5) . ?
C8 O10 1.287(5) . ?
C8 Na3 2.931(4) . ?
C9 O14 1.228(5) . ?
C9 O11 1.360(5) . ?
C9 C10 1.627(6) . ?
C10 O12 1.408(4) . ?
C11 C12 1.501(5) . ?
C11 O12 1.512(4) . ?
C12 O15 1.315(5) . ?
C12 O13 1.368(5) . ?
C13 N1 1.165(6) . ?
C13 S1 1.672(5) . ?
N1 Na1 2.492(4) . ?
O1 Pr1 2.482(3) . ?
O2 Pr1 2.800(3) . ?
O3 Na1 2.542(3) . ?
O3 Pr1 2.659(3) . ?
O4 Na2 2.452(3) . ?
O6 Pr1 2.514(3) . ?
O7 Pr1 2.551(3) . ?
O8 Pr1 2.558(3) . ?
O8 Na1 2.695(3) . ?
O8 Na3 2.820(3) . ?
O10 Na3 2.407(3) . ?
O11 Pr1 2.427(3) . ?
O12 Pr1 2.798(3) . ?
O13 Pr1 2.647(3) . ?
O17 Na3 2.563(4) . ?
O18 Na3 2.520(4) . ?
O18 Na1 2.706(4) . ?
O19 Na2 2.626(4) . ?
Pr1 Na1 3.9587(17) . ?
Na1 Na3 3.713(3) . ?

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
O4 C1 O1 123.2(4) . . ?
O4 C1 C2 113.1(4) . . ?
O1 C1 C2 123.7(3) . . ?
O2 C2 C1 104.9(3) . . ?
C4 C3 O2 104.8(3) . . ?
O5 C4 O3 132.0(4) . . ?
O5 C4 C3 110.8(4) . . ?
O3 C4 C3 117.2(3) . . ?
O9 C5 O6 124.2(4) . . ?
O9 C5 C6 117.0(3) . . ?
O6 C5 C6 118.8(3) . . ?
O7 C6 C5 110.3(3) . . ?
O7 C7 C8 109.3(3) . . ?
O8 C8 O10 125.7(4) . . ?
O8 C8 C7 117.0(3) . . ?
O10 C8 C7 117.3(3) . . ?
O8 C8 Na3 72.4(2) . . ?
O10 C8 Na3 53.8(2) . . ?
C7 C8 Na3 167.7(3) . . ?
O14 C9 O11 123.0(4) . . ?
O14 C9 C10 114.4(4) . . ?
O11 C9 C10 122.6(3) . . ?
O12 C10 C9 105.6(3) . . ?
C12 C11 O12 105.4(3) . . ?
O15 C12 O13 129.3(4) . . ?
O15 C12 C11 113.0(3) . . ?
O13 C12 C11 117.6(3) . . ?
N1 C13 S1 178.0(4) . . ?
C13 N1 Na1 133.0(4) . . ?
C13 N1 Na2 125.4(4) . 1_465 ?
Na1 N1 Na2 91.40(15) . 1_465 ?
C1 O1 Pr1 123.7(2) . . ?
C2 O2 C3 108.5(3) . . ?
C2 O2 Pr1 122.3(2) . . ?
C3 O2 Pr1 128.9(2) . . ?
C4 O3 Na1 124.4(2) . . ?
C4 O3 Pr1 132.7(2) . . ?
Na1 O3 Pr1 99.10(11) . . ?
C1 O4 Na2 140.0(3) . . ?
C4 O5 Na1 135.5(3) . 2_567 ?
C5 O6 Pr1 120.9(3) . . ?
C6 O7 C7 112.1(3) . . ?
C6 O7 Pr1 120.5(2) . . ?
C7 O7 Pr1 121.7(2) . . ?
C8 O8 Pr1 127.0(2) . . ?
C8 O8 Na1 107.2(2) . . ?
Pr1 O8 Na1 97.77(10) . . ?
C8 O8 Na3 82.1(2) . . ?
Pr1 O8 Na3 147.44(11) . . ?
Na1 O8 Na3 84.59(9) . . ?
C5 O9 Na2 132.4(3) . 1_565 ?
C5 O9 Na1 125.4(3) . 1_655 ?
Na2 O9 Na1 97.87(12) 1_565 1_655 ?
C5 O9 Na3 105.4(3) . 1_655 ?
Na2 O9 Na3 94.07(12) 1_565 1_655 ?
Na1 O9 Na3 87.56(10) 1_655 1_655 ?
C8 O10 Na3 100.6(2) . . ?
C8 O10 Na2 112.2(2) . 1_465 ?
Na3 O10 Na2 101.53(11) . 1_465 ?
C9 O11 Pr1 126.4(2) . . ?
C10 O12 C11 110.5(3) . . ?
C10 O12 Pr1 121.2(2) . . ?
C11 O12 Pr1 126.8(2) . . ?
C12 O13 Pr1 131.8(2) . . ?
C9 O14 Na2 163.6(3) . 1_455 ?
C12 O15 Na3 137.8(2) . 2_666 ?
Na3 O18 Na1 90.47(11) . . ?
O11 Pr1 O1 89.43(10) . . ?
O11 Pr1 O6 155.06(11) . . ?
O1 Pr1 O6 76.36(10) . . ?
O11 Pr1 O7 135.96(9) . . ?
O1 Pr1 O7 134.07(9) . . ?
O6 Pr1 O7 63.26(9) . . ?
O11 Pr1 O8 75.66(9) . . ?
O1 Pr1 O8 153.86(10) . . ?
O6 Pr1 O8 124.61(9) . . ?
O7 Pr1 O8 61.55(8) . . ?
O11 Pr1 O13 118.74(10) . . ?
O1 Pr1 O13 81.92(11) . . ?
O6 Pr1 O13 79.94(10) . . ?
O7 Pr1 O13 70.78(9) . . ?
O8 Pr1 O13 86.58(10) . . ?
O11 Pr1 O3 77.74(10) . . ?
O1 Pr1 O3 118.88(9) . . ?
O6 Pr1 O3 91.16(9) . . ?
O7 Pr1 O3 84.31(9) . . ?
O8 Pr1 O3 79.30(9) . . ?
O13 Pr1 O3 154.98(9) . . ?
O11 Pr1 O12 63.24(9) . . ?
O1 Pr1 O12 76.66(10) . . ?
O6 Pr1 O12 130.50(8) . . ?
O7 Pr1 O12 113.31(9) . . ?
O8 Pr1 O12 77.46(9) . . ?
O13 Pr1 O12 55.72(8) . . ?
O3 Pr1 O12 138.31(8) . . ?
O11 Pr1 O2 83.95(10) . . ?
O1 Pr1 O2 63.52(9) . . ?
O6 Pr1 O2 71.42(9) . . ?
O7 Pr1 O2 117.92(9) . . ?
O8 Pr1 O2 133.86(8) . . ?
O13 Pr1 O2 139.03(10) . . ?
O3 Pr1 O2 55.88(8) . . ?
O12 Pr1 O2 128.32(8) . . ?
O11 Pr1 Na1 61.78(7) . . ?
O1 Pr1 Na1 144.52(7) . . ?
O6 Pr1 Na1 121.18(7) . . ?
O7 Pr1 Na1 78.90(6) . . ?
O8 Pr1 Na1 42.43(7) . . ?
O13 Pr1 Na1 128.85(9) . . ?
O3 Pr1 Na1 39.34(7) . . ?
O12 Pr1 Na1 104.66(6) . . ?
O2 Pr1 Na1 91.47(6) . . ?
N1 Na1 O5 107.87(14) . 2_567 ?
N1 Na1 O3 84.95(13) . . ?
O5 Na1 O3 83.86(11) 2_567 . ?
N1 Na1 O9 82.90(13) . 1_455 ?
O5 Na1 O9 109.30(12) 2_567 1_455 ?
O3 Na1 O9 164.32(12) . 1_455 ?
N1 Na1 O8 90.34(13) . . ?
O5 Na1 O8 153.69(11) 2_567 . ?
O3 Na1 O8 78.91(10) . . ?
O9 Na1 O8 91.27(11) 1_455 . ?
N1 Na1 O18 147.01(15) . . ?
O5 Na1 O18 96.92(11) 2_567 . ?
O3 Na1 O18 119.81(11) . . ?
O9 Na1 O18 68.28(11) 1_455 . ?
O8 Na1 O18 75.12(10) . . ?
N1 Na1 Na3 105.83(12) . . ?
O5 Na1 Na3 136.45(10) 2_567 . ?
O3 Na1 Na3 126.07(8) . . ?
O9 Na1 Na3 49.20(9) 1_455 . ?
O8 Na1 Na3 49.13(7) . . ?
O18 Na1 Na3 42.74(8) . . ?
N1 Na1 Na2 47.30(11) . 1_465 ?
O5 Na1 Na2 130.60(9) 2_567 1_465 ?
O3 Na1 Na2 124.54(9) . 1_465 ?
O9 Na1 Na2 40.21(7) 1_455 1_465 ?
O8 Na1 Na2 75.71(7) . 1_465 ?
O18 Na1 Na2 99.91(9) . 1_465 ?
Na3 Na1 Na2 62.16(5) . 1_465 ?
N1 Na1 Pr1 97.83(11) . . ?
O5 Na1 Pr1 116.78(9) 2_567 . ?
O3 Na1 Pr1 41.55(6) . . ?
O9 Na1 Pr1 130.91(9) 1_455 . ?
O8 Na1 Pr1 39.80(6) . . ?
O18 Na1 Pr1 89.72(8) . . ?
Na3 Na1 Pr1 84.53(4) . . ?
Na2 Na1 Pr1 109.42(5) 1_465 . ?
O14 Na2 O4 86.66(13) 1_655 . ?
O14 Na2 O9 166.05(13) 1_655 1_545 ?
O4 Na2 O9 103.19(13) . 1_545 ?
O14 Na2 O10 89.28(12) 1_655 1_645 ?
O4 Na2 O10 175.89(12) . 1_645 ?
O9 Na2 O10 80.69(10) 1_545 1_645 ?
O14 Na2 O19 86.88(13) 1_655 . ?
O4 Na2 O19 83.74(12) . . ?
O9 Na2 O19 103.81(12) 1_545 . ?
O10 Na2 O19 96.73(12) 1_645 . ?
O14 Na2 N1 91.53(15) 1_655 1_645 ?
O4 Na2 N1 89.26(14) . 1_645 ?
O9 Na2 N1 78.91(13) 1_545 1_645 ?
O10 Na2 N1 90.17(12) 1_645 1_645 ?
O19 Na2 N1 172.90(12) . 1_645 ?
O14 Na2 Na1 125.22(11) 1_655 1_645 ?
O4 Na2 Na1 112.13(11) . 1_645 ?
O9 Na2 Na1 41.93(8) 1_545 1_645 ?
O10 Na2 Na1 69.80(8) 1_645 1_645 ?
O19 Na2 Na1 143.48(9) . 1_645 ?
N1 Na2 Na1 41.30(9) 1_645 1_645 ?
O14 Na2 Na3 125.95(11) 1_655 1_645 ?
O4 Na2 Na3 146.51(10) . 1_645 ?
O9 Na2 Na3 46.54(9) 1_545 1_645 ?
O10 Na2 Na3 37.60(7) 1_645 1_645 ?
O19 Na2 Na3 90.09(9) . 1_645 ?
N1 Na2 Na3 96.43(10) 1_645 1_645 ?
Na1 Na2 Na3 58.14(4) 1_645 1_645 ?
O10 Na3 O15 108.38(12) . 2_666 ?
O10 Na3 O18 118.23(14) . . ?
O15 Na3 O18 104.47(12) 2_666 . ?
O10 Na3 O17 98.58(12) . . ?
O15 Na3 O17 79.17(13) 2_666 . ?
O18 Na3 O17 138.47(13) . . ?
O10 Na3 O9 77.00(10) . 1_455 ?
O15 Na3 O9 171.40(12) 2_666 1_455 ?
O18 Na3 O9 66.92(11) . 1_455 ?
O17 Na3 O9 107.03(12) . 1_455 ?
O10 Na3 O8 50.90(9) . . ?
O15 Na3 O8 94.76(11) 2_666 . ?
O18 Na3 O8 75.91(11) . . ?
O17 Na3 O8 145.60(11) . . ?
O9 Na3 O8 83.43(10) 1_455 . ?
O10 Na3 C8 25.57(10) . . ?
O15 Na3 C8 100.90(12) 2_666 . ?
O18 Na3 C8 98.28(13) . . ?
O17 Na3 C8 122.01(12) . . ?
O9 Na3 C8 81.06(10) 1_455 . ?
O8 Na3 C8 25.46(9) . . ?
O10 Na3 Na1 72.42(9) . . ?
O15 Na3 Na1 131.04(11) 2_666 . ?
O18 Na3 Na1 46.79(10) . . ?
O17 Na3 Na1 149.74(10) . . ?
O9 Na3 Na1 43.24(7) 1_455 . ?
O8 Na3 Na1 46.28(7) . . ?
C8 Na3 Na1 58.21(8) . . ?
O10 Na3 Na2 40.87(7) . 1_465 ?
O15 Na3 Na2 147.75(9) 2_666 1_465 ?
O18 Na3 Na2 101.22(10) . 1_465 ?
O17 Na3 Na2 94.25(9) . 1_465 ?
O9 Na3 Na2 39.39(7) 1_455 1_465 ?
O8 Na3 Na2 72.91(7) . 1_465 ?
C8 Na3 Na2 55.92(8) . 1_465 ?
Na1 Na3 Na2 59.70(5) . 1_465 ?

_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.904
_refine_diff_density_max         1.103
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.111
_diffrn_ambient_pressure         105

