# 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
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Ji-Qing Xu'
_publ_contact_author_email       XJQ@MAIL.JLU.EDU.CN

_publ_section_title              
;
Two- and Three-Dimensional Networks
of Lanthanide with Mixed Dicarboxylate Ligands:
Syntheses, Crystal Structures and Photoluminescent Properties
;
loop_
_publ_author_name
'Ji-Qing Xu.'
'Tianyou Song.'
'Tie-Gang Wang.'
'Qing-Feng Yang.'
'Yang Yu.'
;
Jie-Hui Yu
;
'Xiao Zhang.'

# Attachment 'cif.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 715640'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H18 Ce2 O17'
_chemical_formula_sum            'C18 H18 Ce2 O17'
_chemical_formula_weight         786.56

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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'
'-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                   20.090(2)
_cell_length_b                   6.0758(7)
_cell_length_c                   20.626(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.267(2)
_cell_angle_gamma                90.00
_cell_volume                     2346.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2907
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      28.30

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512
_exptl_absorpt_coefficient_mu    3.916
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7558
_exptl_absorpt_correction_T_max  0.8998
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8119
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         28.30
_reflns_number_total             2907
_reflns_number_gt                2711
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0674P)²+7.7665P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2907
_refine_ls_number_parameters     188
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001

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 0.24612(9) -0.0221(3) 0.60175(9) 0.0149(4) Uani 1 1 d . . .
C2 C 0.29639(9) 0.0273(3) 0.67407(9) 0.0157(4) Uani 1 1 d . . .
C3 C 0.29584(12) -0.1220(4) 0.72523(10) 0.0245(5) Uani 1 1 d . . .
H3 H 0.2665 -0.2454 0.7130 0.029 Uiso 1 1 calc R . .
C4 C 0.33895(11) -0.0873(4) 0.79443(10) 0.0242(5) Uani 1 1 d . . .
H4 H 0.3389 -0.1887 0.8282 0.029 Uiso 1 1 calc R . .
C5 C 0.38178(12) 0.0967(4) 0.81311(11) 0.0276(5) Uani 1 1 d . . .
H5 H 0.4099 0.1206 0.8596 0.033 Uiso 1 1 calc R . .
C6 C 0.38313(11) 0.2462(4) 0.76280(10) 0.0241(5) Uani 1 1 d . . .
H6 H 0.4124 0.3696 0.7758 0.029 Uiso 1 1 calc R . .
C7 C 0.34081(10) 0.2136(3) 0.69247(9) 0.0172(4) Uani 1 1 d . . .
C8 C 0.34655(10) 0.3714(3) 0.63894(9) 0.0159(4) Uani 1 1 d . . .
C9 C 0.50068(9) -0.3880(3) 0.48230(9) 0.0153(4) Uani 1 1 d . . .
Ce1 Ce 0.362865(5) -0.330688(16) 0.533921(5) 0.01289(3) Uani 1 1 d . . .
H1 H 0.368(2) 0.074(7) 0.471(2) 0.078(12) Uiso 1 1 d . . .
H2 H 0.3051(16) 0.066(5) 0.4550(15) 0.040(8) Uiso 1 1 d . . .
H7 H 0.4559(13) 0.057(4) 0.5947(13) 0.024(6) Uiso 1 1 d . . .
H8 H 0.4693(12) -0.067(4) 0.6549(12) 0.016(5) Uiso 1 1 d . . .
H9 H 0.4622(4) 0.7098(17) 0.7342(19) 0.062(11) Uiso 1 1 d D . .
O1 O 0.26755(7) -0.1423(2) 0.56235(7) 0.0193(3) Uani 1 1 d . . .
O2 O 0.18230(7) 0.0403(2) 0.58196(7) 0.0218(3) Uani 1 1 d . . .
O3 O 0.30488(8) 0.3510(2) 0.57615(7) 0.0203(4) Uani 1 1 d . . .
O4 O 0.39255(8) 0.5228(3) 0.65694(7) 0.0273(4) Uani 1 1 d . . .
O5 O 0.45667(7) -0.2477(3) 0.48428(8) 0.0240(3) Uani 1 1 d . . .
O6 O 0.54751(7) -0.3660(2) 0.45461(8) 0.0238(3) Uani 1 1 d . . .
O7 O 0.33664(8) 0.0109(3) 0.46355(9) 0.0287(4) Uani 1 1 d . . .
O8 O 0.44272(9) -0.0480(3) 0.61296(8) 0.0299(4) Uani 1 1 d . . .
O9 O 0.5000 0.7879(4) 0.7500 0.0382(7) Uani 1 2 d SD . .


_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 O2 1.255(2) . ?
C1 O1 1.278(2) . ?
C1 C2 1.497(2) . ?
C1 Ce1 2.9967(16) 7_546 ?
C2 C3 1.395(3) . ?
C2 C7 1.406(3) . ?
C3 C4 1.391(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.387(3) . ?
C6 C7 1.404(2) . ?
C7 C8 1.498(3) . ?
C8 O4 1.260(2) . ?
C8 O3 1.268(2) . ?
C8 Ce1 2.931(2) 1_565 ?
C9 O5 1.240(2) . ?
C9 O6 1.272(3) . ?
C9 C9 1.549(4) 5_646 ?
Ce1 O1 2.4770(16) . ?
Ce1 O7 2.4772(16) . ?
Ce1 O5 2.5009(16) . ?
Ce1 O8 2.5070(15) . ?
Ce1 O6 2.5268(15) 5_646 ?
Ce1 O4 2.5474(15) 1_545 ?
Ce1 O2 2.5660(14) 7_546 ?
Ce1 O3 2.5677(15) 1_545 ?
Ce1 O1 2.6573(13) 7_546 ?
Ce1 C8 2.931(2) 1_545 ?
Ce1 C1 2.9967(16) 7_546 ?
O1 Ce1 2.6573(13) 7_546 ?
O2 Ce1 2.5660(14) 7_546 ?
O3 Ce1 2.5677(15) 1_565 ?
O4 Ce1 2.5474(15) 1_565 ?
O6 Ce1 2.5268(15) 5_646 ?

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
O2 C1 O1 120.40(15) . . ?
O2 C1 C2 120.25(17) . . ?
O1 C1 C2 119.14(15) . . ?
O2 C1 Ce1 58.14(9) . 7_546 ?
O1 C1 Ce1 62.37(8) . 7_546 ?
C2 C1 Ce1 172.05(13) . 7_546 ?
C3 C2 C7 119.86(16) . . ?
C3 C2 C1 115.84(16) . . ?
C7 C2 C1 124.26(16) . . ?
C4 C3 C2 120.3(2) . . ?
C5 C4 C3 120.2(2) . . ?
C4 C5 C6 120.14(18) . . ?
C5 C6 C7 120.8(2) . . ?
C6 C7 C2 118.67(18) . . ?
C6 C7 C8 119.44(17) . . ?
C2 C7 C8 121.83(15) . . ?
O4 C8 O3 120.97(18) . . ?
O4 C8 C7 119.60(15) . . ?
O3 C8 C7 119.43(16) . . ?
O4 C8 Ce1 60.04(10) . 1_565 ?
O3 C8 Ce1 60.99(10) . 1_565 ?
C7 C8 Ce1 177.59(14) . 1_565 ?
O5 C9 O6 126.51(18) . . ?
O5 C9 C9 117.0(2) . 5_646 ?
O6 C9 C9 116.5(2) . 5_646 ?
O1 Ce1 O7 74.52(5) . . ?
O1 Ce1 O5 139.98(5) . . ?
O7 Ce1 O5 67.85(5) . . ?
O1 Ce1 O8 84.07(5) . . ?
O7 Ce1 O8 75.93(5) . . ?
O5 Ce1 O8 74.25(6) . . ?
O1 Ce1 O6 154.25(5) . 5_646 ?
O7 Ce1 O6 131.20(6) . 5_646 ?
O5 Ce1 O6 64.41(5) . 5_646 ?
O8 Ce1 O6 99.94(5) . 5_646 ?
O1 Ce1 O4 81.23(5) . 1_545 ?
O7 Ce1 O4 143.10(5) . 1_545 ?
O5 Ce1 O4 122.64(5) . 1_545 ?
O8 Ce1 O4 74.24(5) . 1_545 ?
O6 Ce1 O4 75.55(5) 5_646 1_545 ?
O1 Ce1 O2 114.04(4) . 7_546 ?
O7 Ce1 O2 86.66(5) . 7_546 ?
O5 Ce1 O2 77.47(5) . 7_546 ?
O8 Ce1 O2 150.74(6) . 7_546 ?
O6 Ce1 O2 74.01(4) 5_646 7_546 ?
O4 Ce1 O2 129.07(5) 1_545 7_546 ?
O1 Ce1 O3 77.47(5) . 1_545 ?
O7 Ce1 O3 143.47(5) . 1_545 ?
O5 Ce1 O3 142.44(5) . 1_545 ?
O8 Ce1 O3 123.89(5) . 1_545 ?
O6 Ce1 O3 79.31(5) 5_646 1_545 ?
O4 Ce1 O3 50.94(4) 1_545 1_545 ?
O2 Ce1 O3 83.77(5) 7_546 1_545 ?
O1 Ce1 O1 64.41(5) . 7_546 ?
O7 Ce1 O1 70.82(5) . 7_546 ?
O5 Ce1 O1 113.06(5) . 7_546 ?
O8 Ce1 O1 138.87(5) . 7_546 ?
O6 Ce1 O1 120.06(4) 5_646 7_546 ?
O4 Ce1 O1 122.27(5) 1_545 7_546 ?
O2 Ce1 O1 49.73(5) 7_546 7_546 ?
O3 Ce1 O1 76.19(4) 1_545 7_546 ?
O1 Ce1 C8 78.88(5) . 1_545 ?
O7 Ce1 C8 153.29(6) . 1_545 ?
O5 Ce1 C8 136.89(5) . 1_545 ?
O8 Ce1 C8 99.17(5) . 1_545 ?
O6 Ce1 C8 75.37(5) 5_646 1_545 ?
O4 Ce1 C8 25.38(5) 1_545 1_545 ?
O2 Ce1 C8 106.58(5) 7_546 1_545 ?
O3 Ce1 C8 25.58(4) 1_545 1_545 ?
O1 Ce1 C8 99.78(5) 7_546 1_545 ?
O1 Ce1 C1 89.61(5) . 7_546 ?
O7 Ce1 C1 76.99(5) . 7_546 ?
O5 Ce1 C1 94.69(5) . 7_546 ?
O8 Ce1 C1 152.90(5) . 7_546 ?
O6 Ce1 C1 97.14(5) 5_646 7_546 ?
O4 Ce1 C1 130.81(5) 1_545 7_546 ?
O2 Ce1 C1 24.54(5) 7_546 7_546 ?
O3 Ce1 C1 79.88(5) 1_545 7_546 ?
O1 Ce1 C1 25.21(5) 7_546 7_546 ?
C8 Ce1 C1 105.43(5) 1_545 7_546 ?
C1 O1 Ce1 151.93(11) . . ?
C1 O1 Ce1 92.42(10) . 7_546 ?
Ce1 O1 Ce1 115.59(5) . 7_546 ?
C1 O2 Ce1 97.32(11) . 7_546 ?
C8 O3 Ce1 93.44(12) . 1_565 ?
C8 O4 Ce1 94.58(11) . 1_565 ?
C9 O5 Ce1 121.83(13) . . ?
C9 O6 Ce1 119.95(12) . 5_646 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.047
_refine_diff_density_min         -3.454
_refine_diff_density_rms         0.273

data_2
_database_code_depnum_ccdc_archive 'CCDC 715641'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H18 O17 Pr2'
_chemical_formula_sum            'C18 H18 O17 Pr2'
_chemical_formula_weight         788.14

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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'
'-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                   19.9212(19)
_cell_length_b                   6.0431(5)
_cell_length_c                   20.5250(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.164(3)
_cell_angle_gamma                90.00
_cell_volume                     2304.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2870
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      28.36

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    4.265
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7350
_exptl_absorpt_correction_T_max  0.8504
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8050
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         28.36
_reflns_number_total             2870
_reflns_number_gt                2557
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0357P)²+1.3034P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2870
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.002
_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 0.15326(19) 0.6277(5) 0.36181(18) 0.0176(6) Uani 1 1 d . . .
C2 C 0.15865(19) 0.7855(5) 0.30775(18) 0.0172(6) Uani 1 1 d . . .
C3 C 0.20321(17) 0.9712(5) 0.32619(16) 0.0154(6) Uani 1 1 d . . .
C4 C 0.25397(17) 1.0232(5) 0.39886(16) 0.0147(6) Uani 1 1 d . . .
C5 C 0.2038(2) 1.1208(6) 0.27496(19) 0.0231(7) Uani 1 1 d . . .
H5 H 0.2333 1.2448 0.2872 0.028 Uiso 1 1 calc R . .
C6 C 0.1605(2) 1.0865(7) 0.20557(19) 0.0269(8) Uani 1 1 d . . .
H6 H 0.1601 1.1896 0.1718 0.032 Uiso 1 1 calc R . .
C7 C 0.1180(2) 0.8996(7) 0.18664(19) 0.0274(8) Uani 1 1 d . . .
H7 H 0.0905 0.8730 0.1399 0.033 Uiso 1 1 calc R . .
C8 C 0.1165(2) 0.7515(7) 0.23791(19) 0.0234(7) Uani 1 1 d . . .
H8 H 0.0869 0.6277 0.2253 0.028 Uiso 1 1 calc R . .
C9 C 0.00079(18) 0.6135(6) 0.48234(17) 0.0166(6) Uani 1 1 d . . .
H9 H 0.033(4) 0.306(10) 0.268(4) 0.07(2) Uiso 1 1 d . . .
O1 O 0.10700(15) 0.4742(4) 0.34414(13) 0.0258(6) Uani 1 1 d . . .
O2 O 0.19489(14) 0.6496(4) 0.42478(13) 0.0189(5) Uani 1 1 d . . .
O3 O 0.31834(13) 0.9612(4) 0.41812(13) 0.0207(5) Uani 1 1 d . . .
O4 O 0.23264(14) 1.1439(4) 0.43763(13) 0.0183(5) Uani 1 1 d . . .
O5 O 0.04769(14) 0.6334(4) 0.45483(15) 0.0228(5) Uani 1 1 d . . .
O6 O -0.04352(14) 0.7537(4) 0.48389(14) 0.0230(5) Uani 1 1 d . . .
O7 O 0.05729(16) 0.0491(4) 0.38743(14) 0.0300(6) Uani 1 1 d . . .
O8 O 0.16363(14) -0.0120(4) 0.53641(14) 0.0248(5) Uani 1 1 d . . .
O9 O 0.0000 0.2093(8) 0.2500 0.0379(11) Uani 1 2 d S . .
Pr1 Pr 0.137233(9) 0.33049(3) 0.466475(8) 0.01254(8) 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 O1 1.265(4) . ?
C1 O2 1.266(4) . ?
C1 C2 1.496(5) . ?
C2 C8 1.390(5) . ?
C2 C3 1.396(5) . ?
C3 C5 1.390(5) . ?
C3 C4 1.502(4) . ?
C4 O3 1.255(4) . ?
C4 O4 1.261(4) . ?
C4 Pr1 2.965(3) 7_566 ?
C5 C6 1.388(5) . ?
C6 C7 1.381(6) . ?
C7 C8 1.390(6) . ?
C9 O6 1.232(4) . ?
C9 O5 1.260(4) . ?
C9 C9 1.557(7) 5_566 ?
O1 Pr1 2.516(2) . ?
O2 Pr1 2.546(2) . ?
O3 Pr1 2.543(2) 7_566 ?
O4 Pr1 2.459(2) 1_565 ?
O4 Pr1 2.633(3) 7_566 ?
O5 Pr1 2.506(2) . ?
O6 Pr1 2.481(3) 5_566 ?
O7 Pr1 2.489(3) . ?
O8 Pr1 2.465(2) . ?
Pr1 O4 2.459(2) 1_545 ?
Pr1 O6 2.481(3) 5_566 ?
Pr1 O3 2.543(2) 7_566 ?
Pr1 O4 2.633(3) 7_566 ?
Pr1 C4 2.965(3) 7_566 ?

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
O1 C1 O2 120.7(3) . . ?
O1 C1 C2 119.7(3) . . ?
O2 C1 C2 119.7(3) . . ?
C8 C2 C3 119.1(3) . . ?
C8 C2 C1 119.5(3) . . ?
C3 C2 C1 121.4(3) . . ?
C5 C3 C2 119.7(3) . . ?
C5 C3 C4 115.4(3) . . ?
C2 C3 C4 124.9(3) . . ?
O3 C4 O4 120.8(3) . . ?
O3 C4 C3 119.7(3) . . ?
O4 C4 C3 119.2(3) . . ?
O3 C4 Pr1 58.37(16) . 7_566 ?
O4 C4 Pr1 62.53(17) . 7_566 ?
C3 C4 Pr1 172.4(2) . 7_566 ?
C6 C5 C3 120.5(3) . . ?
C7 C6 C5 120.1(3) . . ?
C6 C7 C8 119.5(3) . . ?
C2 C8 C7 121.0(4) . . ?
O6 C9 O5 126.9(3) . . ?
O6 C9 C9 117.3(4) . 5_566 ?
O5 C9 C9 115.8(4) . 5_566 ?
C1 O1 Pr1 94.6(2) . . ?
C1 O2 Pr1 93.2(2) . . ?
C4 O3 Pr1 96.78(19) . 7_566 ?
C4 O4 Pr1 152.0(2) . 1_565 ?
C4 O4 Pr1 92.3(2) . 7_566 ?
Pr1 O4 Pr1 115.53(9) 1_565 7_566 ?
C9 O5 Pr1 120.4(2) . . ?
C9 O6 Pr1 121.5(2) . 5_566 ?
O4 Pr1 O8 74.59(9) 1_545 . ?
O4 Pr1 O6 140.04(8) 1_545 5_566 ?
O8 Pr1 O6 67.84(9) . 5_566 ?
O4 Pr1 O7 84.15(9) 1_545 . ?
O8 Pr1 O7 75.98(9) . . ?
O6 Pr1 O7 74.24(10) 5_566 . ?
O4 Pr1 O5 153.80(8) 1_545 . ?
O8 Pr1 O5 131.57(8) . . ?
O6 Pr1 O5 64.76(8) 5_566 . ?
O7 Pr1 O5 99.84(10) . . ?
O4 Pr1 O1 81.10(9) 1_545 . ?
O8 Pr1 O1 142.65(9) . . ?
O6 Pr1 O1 122.42(9) 5_566 . ?
O7 Pr1 O1 73.69(9) . . ?
O5 Pr1 O1 75.35(9) . . ?
O4 Pr1 O3 114.33(8) 1_545 7_566 ?
O8 Pr1 O3 86.78(9) . 7_566 ?
O6 Pr1 O3 77.26(9) 5_566 7_566 ?
O7 Pr1 O3 150.59(9) . 7_566 ?
O5 Pr1 O3 73.96(9) . 7_566 ?
O1 Pr1 O3 129.51(9) . 7_566 ?
O4 Pr1 O2 77.56(8) 1_545 . ?
O8 Pr1 O2 143.57(9) . . ?
O6 Pr1 O2 142.28(9) 5_566 . ?
O7 Pr1 O2 123.96(8) . . ?
O5 Pr1 O2 78.85(8) . . ?
O1 Pr1 O2 51.50(8) . . ?
O3 Pr1 O2 83.71(8) 7_566 . ?
O4 Pr1 O4 64.47(9) 1_545 7_566 ?
O8 Pr1 O4 70.64(8) . 7_566 ?
O6 Pr1 O4 112.88(8) 5_566 7_566 ?
O7 Pr1 O4 138.84(9) . 7_566 ?
O5 Pr1 O4 120.21(8) . 7_566 ?
O1 Pr1 O4 122.82(9) . 7_566 ?
O3 Pr1 O4 49.98(7) 7_566 7_566 ?
O2 Pr1 O4 76.40(8) . 7_566 ?
O4 Pr1 C4 89.59(9) 1_545 7_566 ?
O8 Pr1 C4 77.12(9) . 7_566 ?
O6 Pr1 C4 94.79(9) 5_566 7_566 ?
O7 Pr1 C4 153.08(9) . 7_566 ?
O5 Pr1 C4 97.27(9) . 7_566 ?
O1 Pr1 C4 131.17(8) . 7_566 ?
O3 Pr1 C4 24.85(8) 7_566 7_566 ?
O2 Pr1 C4 79.68(8) . 7_566 ?
O4 Pr1 C4 25.15(8) 7_566 7_566 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.228

data_3
_database_code_depnum_ccdc_archive 'CCDC 715642'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H18 Nd2 O17'
_chemical_formula_sum            'C18 H18 Nd2 O17'
_chemical_formula_weight         794.80

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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'
'-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                   19.8310(18)
_cell_length_b                   6.0329(5)
_cell_length_c                   20.4964(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.096(2)
_cell_angle_gamma                90.00
_cell_volume                     2287.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2840
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      28.34

_exptl_crystal_description       rod
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    4.576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4140
_exptl_absorpt_correction_T_max  0.6358
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7989
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         28.34
_reflns_number_total             2840
_reflns_number_gt                2499
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0253P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2840
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0509
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

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 0.15353(15) 0.8744(4) 0.86240(15) 0.0165(5) Uani 1 1 d . . .
C2 C 0.15868(16) 0.7170(4) 0.80834(15) 0.0171(6) Uani 1 1 d . . .
C3 C 0.11628(17) 0.7506(5) 0.73837(16) 0.0225(6) Uani 1 1 d . . .
H3 H 0.0865 0.8745 0.7257 0.027 Uiso 1 1 calc R . .
C4 C 0.11784(17) 0.6021(6) 0.68734(16) 0.0263(7) Uani 1 1 d . . .
H4 H 0.0899 0.6281 0.6407 0.032 Uiso 1 1 calc R . .
C5 C 0.16061(18) 0.4167(6) 0.70561(15) 0.0260(7) Uani 1 1 d . . .
H5 H 0.1608 0.3153 0.6715 0.031 Uiso 1 1 calc R . .
C6 C 0.20355(17) 0.3804(5) 0.77501(16) 0.0222(6) Uani 1 1 d . . .
H6 H 0.2326 0.2548 0.7871 0.027 Uiso 1 1 calc R . .
C7 C 0.20359(14) 0.5297(4) 0.82657(13) 0.0157(5) Uani 1 1 d . . .
C8 C 0.25401(14) 0.4768(4) 0.89930(13) 0.0139(5) Uani 1 1 d . . .
C9 C -0.00083(14) 1.1128(4) 1.01762(14) 0.0151(5) Uani 1 1 d . . .
H1 H 0.199(2) 1.558(7) 1.041(2) 0.031(11) Uiso 1 1 d . . .
H2 H 0.139(3) 1.580(10) 1.036(3) 0.08(2) Uiso 1 1 d . . .
H7 H 0.044(2) 1.577(8) 0.906(2) 0.059(14) Uiso 1 1 d . . .
H8 H 0.034(2) 1.432(7) 0.854(2) 0.040(13) Uiso 1 1 d . . .
H9 H 0.036(3) 0.791(7) 0.267(3) 0.061(15) Uiso 1 1 d . . .
Nd1 Nd 0.137328(7) 1.16956(2) 0.966874(7) 0.01264(5) Uani 1 1 d . . .
O1 O 0.19462(11) 0.8516(3) 0.92564(10) 0.0188(4) Uani 1 1 d . . .
O2 O 0.10733(12) 1.0288(4) 0.84477(10) 0.0252(5) Uani 1 1 d . . .
O3 O 0.31860(10) 0.5396(3) 0.91877(10) 0.0203(4) Uani 1 1 d . . .
O4 O 0.23263(11) 0.3560(3) 0.93846(10) 0.0184(4) Uani 1 1 d . . .
O5 O 0.04383(11) 1.2534(3) 1.01632(12) 0.0225(5) Uani 1 1 d . . .
O6 O -0.04827(11) 1.1338(3) 1.04522(12) 0.0228(5) Uani 1 1 d . . .
O7 O 0.16341(15) 1.5088(4) 1.03623(13) 0.0262(5) Uani 1 1 d . . .
O8 O 0.05788(14) 1.4487(4) 0.88850(13) 0.0296(6) Uani 1 1 d . . .
O9 O 0.0000 0.7068(7) 0.2500 0.0365(9) Uani 1 2 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 O2 1.265(3) . ?
C1 O1 1.266(3) . ?
C1 C2 1.490(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.404(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.372(5) . ?
C5 C6 1.387(4) . ?
C6 C7 1.388(4) . ?
C7 C8 1.500(4) . ?
C8 O3 1.255(3) . ?
C8 O4 1.265(3) . ?
C8 Nd1 2.948(3) 7_567 ?
C9 O5 1.234(3) . ?
C9 O6 1.267(3) . ?
C9 C9 1.547(5) 5_577 ?
Nd1 O7 2.439(2) . ?
Nd1 O4 2.443(2) 1_565 ?
Nd1 O5 2.464(2) . ?
Nd1 O8 2.465(2) . ?
Nd1 O6 2.493(2) 5_577 ?
Nd1 O2 2.503(2) . ?
Nd1 O3 2.5249(19) 7_567 ?
Nd1 O1 2.5252(19) . ?
Nd1 O4 2.615(2) 7_567 ?
Nd1 C8 2.948(3) 7_567 ?
O3 Nd1 2.5249(19) 7_567 ?
O4 Nd1 2.4430(19) 1_545 ?
O4 Nd1 2.615(2) 7_567 ?
O6 Nd1 2.493(2) 5_577 ?

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
O2 C1 O1 120.4(3) . . ?
O2 C1 C2 119.6(2) . . ?
O1 C1 C2 120.1(2) . . ?
C3 C2 C7 118.8(3) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 121.4(2) . . ?
C4 C3 C2 120.9(3) . . ?
C5 C4 C3 120.0(3) . . ?
C4 C5 C6 120.0(3) . . ?
C5 C6 C7 120.7(3) . . ?
C6 C7 C2 119.5(3) . . ?
C6 C7 C8 115.9(2) . . ?
C2 C7 C8 124.6(2) . . ?
O3 C8 O4 120.6(2) . . ?
O3 C8 C7 119.4(2) . . ?
O4 C8 C7 119.8(2) . . ?
O3 C8 Nd1 58.27(13) . 7_567 ?
O4 C8 Nd1 62.41(14) . 7_567 ?
C7 C8 Nd1 172.17(18) . 7_567 ?
O5 C9 O6 126.5(3) . . ?
O5 C9 C9 117.3(3) . 5_577 ?
O6 C9 C9 116.2(3) . 5_577 ?
O7 Nd1 O4 74.49(8) . 1_565 ?
O7 Nd1 O5 67.74(8) . . ?
O4 Nd1 O5 139.87(6) 1_565 . ?
O7 Nd1 O8 76.01(9) . . ?
O4 Nd1 O8 84.14(8) 1_565 . ?
O5 Nd1 O8 74.26(8) . . ?
O7 Nd1 O6 131.92(8) . 5_577 ?
O4 Nd1 O6 153.56(7) 1_565 5_577 ?
O5 Nd1 O6 65.21(7) . 5_577 ?
O8 Nd1 O6 99.96(8) . 5_577 ?
O7 Nd1 O2 142.34(8) . . ?
O4 Nd1 O2 81.01(7) 1_565 . ?
O5 Nd1 O2 122.51(7) . . ?
O8 Nd1 O2 73.39(8) . . ?
O6 Nd1 O2 75.32(7) 5_577 . ?
O7 Nd1 O3 87.04(8) . 7_567 ?
O4 Nd1 O3 114.36(6) 1_565 7_567 ?
O5 Nd1 O3 77.36(7) . 7_567 ?
O8 Nd1 O3 150.79(8) . 7_567 ?
O6 Nd1 O3 73.83(7) 5_577 7_567 ?
O2 Nd1 O3 129.56(7) . 7_567 ?
O7 Nd1 O1 143.71(8) . . ?
O4 Nd1 O1 77.88(6) 1_565 . ?
O5 Nd1 O1 142.13(7) . . ?
O8 Nd1 O1 124.05(8) . . ?
O6 Nd1 O1 78.28(7) 5_577 . ?
O2 Nd1 O1 51.78(6) . . ?
O3 Nd1 O1 83.34(7) 7_567 . ?
O7 Nd1 O4 70.81(8) . 7_567 ?
O4 Nd1 O4 64.09(7) 1_565 7_567 ?
O5 Nd1 O4 113.21(7) . 7_567 ?
O8 Nd1 O4 138.78(8) . 7_567 ?
O6 Nd1 O4 120.31(7) 5_577 7_567 ?
O2 Nd1 O4 122.54(7) . 7_567 ?
O3 Nd1 O4 50.38(6) 7_567 7_567 ?
O1 Nd1 O4 76.18(6) . 7_567 ?
O7 Nd1 C8 77.20(8) . 7_567 ?
O4 Nd1 C8 89.46(7) 1_565 7_567 ?
O5 Nd1 C8 94.88(7) . 7_567 ?
O8 Nd1 C8 153.20(8) . 7_567 ?
O6 Nd1 C8 97.29(7) 5_577 7_567 ?
O2 Nd1 C8 131.27(7) . 7_567 ?
O3 Nd1 C8 25.01(7) 7_567 7_567 ?
O1 Nd1 C8 79.49(7) . 7_567 ?
O4 Nd1 C8 25.39(6) 7_567 7_567 ?
C1 O1 Nd1 93.37(16) . . ?
C1 O2 Nd1 94.43(16) . . ?
C8 O3 Nd1 96.72(16) . 7_567 ?
C8 O4 Nd1 151.80(18) . 1_545 ?
C8 O4 Nd1 92.20(16) . 7_567 ?
Nd1 O4 Nd1 115.91(7) 1_545 7_567 ?
C9 O5 Nd1 121.32(18) . . ?
C9 O6 Nd1 119.69(17) . 5_577 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.641
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.189

data_4
_database_code_depnum_ccdc_archive 'CCDC 715643'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H18 O17 Sm2'
_chemical_formula_sum            'C18 H18 O17 Sm2'
_chemical_formula_weight         807.02

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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'
'-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                   19.697(4)
_cell_length_b                   6.0193(12)
_cell_length_c                   20.472(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.89(3)
_cell_angle_gamma                90.00
_cell_volume                     2267.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2585
_cell_measurement_theta_min      3.56
_cell_measurement_theta_max      27.42

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544
_exptl_absorpt_coefficient_mu    5.216
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4383
_exptl_absorpt_correction_T_max  0.5000
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10452
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.56
_diffrn_reflns_theta_max         27.42
_reflns_number_total             2585
_reflns_number_gt                2338
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0248P)²+22.1488P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2585
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_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 0.2972(2) -0.0312(7) 0.6728(2) 0.0133(8) Uani 1 1 d . . .
C2 C 0.3414(2) -0.2186(7) 0.6903(2) 0.0144(8) Uani 1 1 d . . .
C3 C 0.3841(3) -0.2563(9) 0.7611(2) 0.0223(10) Uani 1 1 d . . .
H3 H 0.4135 -0.3817 0.7737 0.027 Uiso 1 1 calc R . .
C4 C 0.3823(3) -0.1066(9) 0.8118(2) 0.0229(10) Uani 1 1 d . . .
H4 H 0.4102 -0.1333 0.8584 0.028 Uiso 1 1 calc R . .
C5 C 0.3397(3) 0.0812(9) 0.7940(2) 0.0247(10) Uani 1 1 d . . .
H5 H 0.3399 0.1827 0.8283 0.030 Uiso 1 1 calc R . .
C6 C 0.2963(3) 0.1186(8) 0.7245(2) 0.0200(9) Uani 1 1 d . . .
H6 H 0.2667 0.2437 0.7125 0.024 Uiso 1 1 calc R . .
C7 C 0.2461(2) 0.0239(7) 0.6002(2) 0.0121(8) Uani 1 1 d . . .
C8 C 0.3470(2) -0.3773(7) 0.6363(2) 0.0133(8) Uani 1 1 d . . .
C9 C -0.0008(2) 0.1125(7) 0.5178(2) 0.0136(8) Uani 1 1 d . . .
H1 H 0.198(3) 0.568(10) 0.545(3) 0.017(14) Uiso 1 1 d . . .
H2 H 0.134(5) 0.588(16) 0.530(5) 0.08(3) Uiso 1 1 d . . .
H7 H 0.044(4) 0.543(15) 0.407(4) 0.06(3) Uiso 1 1 d . . .
H8 H 0.037(4) 0.423(11) 0.354(4) 0.04(2) Uiso 1 1 d . . .
H9 H 0.035(4) 0.218(12) 0.270(4) 0.06(2) Uiso 1 1 d . . .
O1 O 0.18105(16) -0.0390(5) 0.57999(16) 0.0182(6) Uani 1 1 d . . .
O2 O 0.26818(16) 0.1447(5) 0.56137(15) 0.0164(6) Uani 1 1 d . . .
O3 O 0.30592(16) -0.3532(5) 0.57283(15) 0.0155(6) Uani 1 1 d . . .
O4 O 0.39285(17) -0.5337(6) 0.65384(16) 0.0228(7) Uani 1 1 d . . .
O5 O 0.04436(17) 0.2539(5) 0.51702(17) 0.0202(7) Uani 1 1 d . . .
O6 O -0.04850(17) 0.1319(5) 0.54564(17) 0.0208(7) Uani 1 1 d . . .
O7 O 0.1637(2) 0.5055(6) 0.5366(2) 0.0228(7) Uani 1 1 d . . .
O8 O 0.0581(2) 0.4460(7) 0.3900(2) 0.0286(9) Uani 1 1 d . . .
O9 O 0.0000 0.2970(10) 0.2500 0.0359(14) Uani 1 2 d S . .
Sm1 Sm 0.137333(10) 0.17003(3) 0.467527(10) 0.00999(7) 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 C2 1.393(6) . ?
C1 C6 1.396(6) . ?
C1 C7 1.504(5) . ?
C2 C3 1.411(6) . ?
C2 C8 1.494(6) . ?
C3 C4 1.385(7) . ?
C4 C5 1.378(7) . ?
C5 C6 1.393(6) . ?
C7 O1 1.255(5) . ?
C7 O2 1.264(5) . ?
C8 O4 1.265(5) . ?
C8 O3 1.270(5) . ?
C8 Sm1 2.861(4) 7_546 ?
C9 O5 1.235(5) . ?
C9 O6 1.267(5) . ?
C9 C9 1.543(8) 5_556 ?
O1 Sm1 2.492(3) . ?
O2 Sm1 2.417(3) 7_556 ?
O2 Sm1 2.612(3) . ?
O3 Sm1 2.496(3) 7_546 ?
O4 Sm1 2.479(3) 7_546 ?
O5 Sm1 2.441(3) . ?
O6 Sm1 2.470(3) 5_556 ?
O7 Sm1 2.413(3) . ?
O8 Sm1 2.439(4) . ?
Sm1 O2 2.417(3) 7_556 ?
Sm1 O6 2.470(3) 5_556 ?
Sm1 O4 2.479(3) 7_546 ?
Sm1 O3 2.496(3) 7_546 ?
Sm1 C8 2.861(4) 7_546 ?

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
C2 C1 C6 120.3(4) . . ?
C2 C1 C7 124.7(4) . . ?
C6 C1 C7 115.0(4) . . ?
C1 C2 C3 118.9(4) . . ?
C1 C2 C8 122.2(4) . . ?
C3 C2 C8 118.9(4) . . ?
C4 C3 C2 120.1(4) . . ?
C5 C4 C3 120.8(4) . . ?
C4 C5 C6 119.8(4) . . ?
C5 C6 C1 120.1(4) . . ?
O1 C7 O2 120.4(4) . . ?
O1 C7 C1 120.2(4) . . ?
O2 C7 C1 119.2(4) . . ?
O4 C8 O3 120.4(4) . . ?
O4 C8 C2 119.9(4) . . ?
O3 C8 C2 119.7(4) . . ?
O4 C8 Sm1 59.8(2) . 7_546 ?
O3 C8 Sm1 60.6(2) . 7_546 ?
C2 C8 Sm1 177.5(3) . 7_546 ?
O5 C9 O6 126.5(4) . . ?
O5 C9 C9 117.7(4) . 5_556 ?
O6 C9 C9 115.8(4) . 5_556 ?
C7 O1 Sm1 97.4(2) . . ?
C7 O2 Sm1 152.6(3) . 7_556 ?
C7 O2 Sm1 91.4(2) . . ?
Sm1 O2 Sm1 115.90(11) 7_556 . ?
C8 O3 Sm1 93.1(2) . 7_546 ?
C8 O4 Sm1 94.0(2) . 7_546 ?
C9 O5 Sm1 120.8(3) . . ?
C9 O6 Sm1 119.6(3) . 5_556 ?
O7 Sm1 O2 74.53(12) . 7_556 ?
O7 Sm1 O8 76.44(14) . . ?
O2 Sm1 O8 84.07(12) 7_556 . ?
O7 Sm1 O5 67.70(12) . . ?
O2 Sm1 O5 139.74(11) 7_556 . ?
O8 Sm1 O5 74.22(13) . . ?
O7 Sm1 O6 132.54(12) . 5_556 ?
O2 Sm1 O6 152.89(10) 7_556 5_556 ?
O8 Sm1 O6 99.55(13) . 5_556 ?
O5 Sm1 O6 65.82(10) . 5_556 ?
O7 Sm1 O4 142.07(12) . 7_546 ?
O2 Sm1 O4 80.67(11) 7_556 7_546 ?
O8 Sm1 O4 72.81(13) . 7_546 ?
O5 Sm1 O4 122.49(11) . 7_546 ?
O6 Sm1 O4 74.91(11) 5_556 7_546 ?
O7 Sm1 O1 87.13(12) . . ?
O2 Sm1 O1 114.62(10) 7_556 . ?
O8 Sm1 O1 151.04(12) . . ?
O5 Sm1 O1 77.54(11) . . ?
O6 Sm1 O1 74.17(11) 5_556 . ?
O4 Sm1 O1 129.72(11) 7_546 . ?
O7 Sm1 O3 143.61(12) . 7_546 ?
O2 Sm1 O3 78.28(10) 7_556 7_546 ?
O8 Sm1 O3 124.31(12) . 7_546 ?
O5 Sm1 O3 141.85(10) . 7_546 ?
O6 Sm1 O3 77.59(10) 5_556 7_546 ?
O4 Sm1 O3 52.47(10) 7_546 7_546 ?
O1 Sm1 O3 82.65(10) . 7_546 ?
O7 Sm1 O2 70.61(12) . . ?
O2 Sm1 O2 64.10(11) 7_556 . ?
O8 Sm1 O2 138.86(12) . . ?
O5 Sm1 O2 113.35(10) . . ?
O6 Sm1 O2 120.79(10) 5_556 . ?
O4 Sm1 O2 122.59(10) 7_546 . ?
O1 Sm1 O2 50.65(10) . . ?
O3 Sm1 O2 75.99(9) 7_546 . ?
O7 Sm1 C8 153.23(12) . 7_546 ?
O2 Sm1 C8 78.81(11) 7_556 7_546 ?
O8 Sm1 C8 98.62(13) . 7_546 ?
O5 Sm1 C8 137.01(11) . 7_546 ?
O6 Sm1 C8 74.08(11) 5_556 7_546 ?
O4 Sm1 C8 26.17(11) 7_546 7_546 ?
O1 Sm1 C8 106.38(11) . 7_546 ?
O3 Sm1 C8 26.32(11) 7_546 7_546 ?
O2 Sm1 C8 99.83(11) . 7_546 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.726
_refine_diff_density_min         -2.663
_refine_diff_density_rms         0.149

data_5
_database_code_depnum_ccdc_archive 'CCDC 715644'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H18 Eu2 O17'
_chemical_formula_sum            'C18 H18 Eu2 O17'
_chemical_formula_weight         810.24

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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'
'-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                   19.6326(12)
_cell_length_b                   6.0048(4)
_cell_length_c                   20.4684(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.895(4)
_cell_angle_gamma                90.00
_cell_volume                     2254.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2176
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      25.82

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    5.602
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3760
_exptl_absorpt_correction_T_max  0.5710
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6436
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.82
_reflns_number_total             2176
_reflns_number_gt                1941
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0567P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2176
_refine_ls_number_parameters     188
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_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 0.2463(3) 0.4774(8) 0.5999(2) 0.0130(10) Uani 1 1 d . . .
C2 C 0.2969(3) 0.5312(8) 0.6724(3) 0.0152(10) Uani 1 1 d . . .
C3 C 0.2970(3) 0.3821(9) 0.7247(3) 0.0221(12) Uani 1 1 d . . .
H3 H 0.2681 0.2551 0.7129 0.027 Uiso 1 1 calc R . .
C4 C 0.3397(3) 0.4205(10) 0.7940(3) 0.0236(12) Uani 1 1 d . . .
H4 H 0.3396 0.3195 0.8284 0.028 Uiso 1 1 calc R . .
C5 C 0.3824(3) 0.6096(11) 0.8117(3) 0.0259(13) Uani 1 1 d . . .
H5 H 0.4104 0.6379 0.8582 0.031 Uiso 1 1 calc R . .
C6 C 0.3836(3) 0.7563(10) 0.7602(3) 0.0212(12) Uani 1 1 d . . .
H6 H 0.4131 0.8818 0.7727 0.025 Uiso 1 1 calc R . .
C7 C 0.3417(3) 0.7217(9) 0.6902(3) 0.0173(11) Uani 1 1 d . . .
C8 C 0.3467(3) 0.8779(8) 0.6357(3) 0.0152(10) Uani 1 1 d . . .
C9 C -0.0007(3) 0.3867(9) 0.5177(3) 0.0162(11) Uani 1 1 d . . .
Eu1 Eu 0.137337(12) 0.32964(4) 0.467693(12) 0.01198(13) Uani 1 1 d . . .
H1 H 0.136(4) -0.097(10) 0.545(4) 0.04(2) Uiso 1 1 d D . .
H2 H 0.193(5) -0.060(18) 0.575(3) 0.09(3) Uiso 1 1 d D . .
H7 H 0.045(5) -0.062(9) 0.405(5) 0.07(3) Uiso 1 1 d D . .
H8 H 0.037(4) 0.083(13) 0.345(4) 0.04(2) Uiso 1 1 d . . .
H9 H 0.033(4) 0.256(13) 0.268(4) 0.03(2) Uiso 1 1 d . . .
O1 O 0.18095(19) 0.5384(6) 0.5800(2) 0.0198(8) Uani 1 1 d . . .
O2 O 0.2680(2) 0.3546(6) 0.5610(2) 0.0162(8) Uani 1 1 d . . .
O3 O 0.3063(2) 0.8537(5) 0.5722(2) 0.0165(8) Uani 1 1 d . . .
O4 O 0.3930(2) 1.0361(6) 0.6531(2) 0.0255(9) Uani 1 1 d . . .
O5 O 0.0444(2) 0.2464(6) 0.5170(2) 0.0215(8) Uani 1 1 d . . .
O6 O -0.0488(2) 0.3689(6) 0.5455(2) 0.0217(9) Uani 1 1 d . . .
O7 O 0.1641(2) -0.0049(7) 0.5364(2) 0.0233(8) Uani 1 1 d D . .
O8 O 0.0574(2) 0.0562(7) 0.3898(2) 0.0279(10) Uani 1 1 d D . .
O9 O 0.0000 0.1989(12) 0.2500 0.0364(18) Uani 1 2 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 O1 1.254(6) . ?
C1 O2 1.265(6) . ?
C1 C2 1.498(7) . ?
C2 C3 1.394(8) . ?
C2 C7 1.410(7) . ?
C3 C4 1.385(8) . ?
C4 C5 1.381(9) . ?
C5 C6 1.379(9) . ?
C6 C7 1.390(8) . ?
C7 C8 1.489(8) . ?
C8 O3 1.267(6) . ?
C8 O4 1.274(6) . ?
C8 Eu1 2.851(5) 7_566 ?
C9 O5 1.226(7) . ?
C9 O6 1.268(7) . ?
C9 C9 1.548(10) 5_566 ?
Eu1 O7 2.401(4) . ?
Eu1 O2 2.409(4) 7_556 ?
Eu1 O8 2.432(4) . ?
Eu1 O5 2.432(4) . ?
Eu1 O6 2.457(4) 5_566 ?
Eu1 O4 2.463(4) 7_566 ?
Eu1 O3 2.480(4) 7_566 ?
Eu1 O1 2.487(4) . ?
Eu1 O2 2.599(4) . ?
Eu1 C8 2.851(5) 7_566 ?
Eu1 Eu1 4.2497(5) 7_556 ?
O2 Eu1 2.409(4) 7_556 ?
O3 Eu1 2.480(4) 7_566 ?
O4 Eu1 2.463(4) 7_566 ?
O6 Eu1 2.457(4) 5_566 ?

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
O1 C1 O2 120.1(4) . . ?
O1 C1 C2 119.9(5) . . ?
O2 C1 C2 119.8(4) . . ?
C3 C2 C7 119.5(5) . . ?
C3 C2 C1 116.2(5) . . ?
C7 C2 C1 124.3(5) . . ?
C4 C3 C2 120.9(5) . . ?
C3 C4 C5 119.6(5) . . ?
C6 C5 C4 119.9(5) . . ?
C5 C6 C7 121.8(5) . . ?
C6 C7 C2 118.2(5) . . ?
C6 C7 C8 120.4(5) . . ?
C2 C7 C8 121.3(5) . . ?
O3 C8 O4 119.7(5) . . ?
O3 C8 C7 120.8(5) . . ?
O4 C8 C7 119.4(5) . . ?
O3 C8 Eu1 60.2(3) . 7_566 ?
O4 C8 Eu1 59.5(3) . 7_566 ?
C7 C8 Eu1 177.6(4) . 7_566 ?
O5 C9 O6 127.1(5) . . ?
O5 C9 C9 117.7(6) . 5_566 ?
O6 C9 C9 115.2(6) . 5_566 ?
O7 Eu1 O2 74.46(13) . 7_556 ?
O7 Eu1 O8 76.93(14) . . ?
O2 Eu1 O8 84.47(14) 7_556 . ?
O7 Eu1 O5 67.94(13) . . ?
O2 Eu1 O5 139.95(12) 7_556 . ?
O8 Eu1 O5 74.27(15) . . ?
O7 Eu1 O6 132.79(14) . 5_566 ?
O2 Eu1 O6 152.71(13) 7_556 5_566 ?
O8 Eu1 O6 99.20(15) . 5_566 ?
O5 Eu1 O6 65.85(13) . 5_566 ?
O7 Eu1 O4 141.81(14) . 7_566 ?
O2 Eu1 O4 80.61(14) 7_556 7_566 ?
O8 Eu1 O4 72.22(14) . 7_566 ?
O5 Eu1 O4 122.37(14) . 7_566 ?
O6 Eu1 O4 74.94(14) 5_566 7_566 ?
O7 Eu1 O3 143.55(13) . 7_566 ?
O2 Eu1 O3 78.35(12) 7_556 7_566 ?
O8 Eu1 O3 124.16(14) . 7_566 ?
O5 Eu1 O3 141.56(13) . 7_566 ?
O6 Eu1 O3 77.30(12) 5_566 7_566 ?
O4 Eu1 O3 52.80(12) 7_566 7_566 ?
O7 Eu1 O1 87.08(13) . . ?
O2 Eu1 O1 114.55(12) 7_556 . ?
O8 Eu1 O1 151.05(15) . . ?
O5 Eu1 O1 77.41(14) . . ?
O6 Eu1 O1 74.16(13) 5_566 . ?
O4 Eu1 O1 130.03(13) 7_566 . ?
O3 Eu1 O1 82.57(13) 7_566 . ?
O7 Eu1 O2 70.46(12) . . ?
O2 Eu1 O2 63.93(14) 7_556 . ?
O8 Eu1 O2 139.23(13) . . ?
O5 Eu1 O2 113.38(13) . . ?
O6 Eu1 O2 120.82(12) 5_566 . ?
O4 Eu1 O2 122.73(13) 7_566 . ?
O3 Eu1 O2 76.01(12) 7_566 . ?
O1 Eu1 O2 50.76(12) . . ?
O7 Eu1 C8 153.04(15) . 7_566 ?
O2 Eu1 C8 78.68(14) 7_556 7_566 ?
O8 Eu1 C8 98.37(15) . 7_566 ?
O5 Eu1 C8 137.03(14) . 7_566 ?
O6 Eu1 C8 74.04(14) 5_566 7_566 ?
O4 Eu1 C8 26.47(13) 7_566 7_566 ?
O3 Eu1 C8 26.33(13) 7_566 7_566 ?
O1 Eu1 C8 106.42(14) . 7_566 ?
O2 Eu1 C8 99.74(13) . 7_566 ?
O7 Eu1 Eu1 69.12(9) . 7_556 ?
O2 Eu1 Eu1 33.32(9) 7_556 7_556 ?
O8 Eu1 Eu1 114.11(11) . 7_556 ?
O5 Eu1 Eu1 132.58(9) . 7_556 ?
O6 Eu1 Eu1 144.79(9) 5_566 7_556 ?
O4 Eu1 Eu1 103.78(10) 7_566 7_556 ?
O3 Eu1 Eu1 74.79(8) 7_566 7_556 ?
O1 Eu1 Eu1 81.30(8) . 7_556 ?
O2 Eu1 Eu1 30.61(8) . 7_556 ?
C8 Eu1 Eu1 89.55(10) 7_566 7_556 ?
C1 O1 Eu1 97.3(3) . . ?
C1 O2 Eu1 152.0(3) . 7_556 ?
C1 O2 Eu1 91.8(3) . . ?
Eu1 O2 Eu1 116.07(14) 7_556 . ?
C8 O3 Eu1 93.4(3) . 7_566 ?
C8 O4 Eu1 94.0(3) . 7_566 ?
C9 O5 Eu1 121.0(3) . . ?
C9 O6 Eu1 119.9(3) . 5_566 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.82
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.527
_refine_diff_density_min         -1.800
_refine_diff_density_rms         0.232

data_6
_database_code_depnum_ccdc_archive 'CCDC 715645'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C18 H18 Gd2 O17'
_chemical_formula_sum            'C18 H18 Gd2 O17'
_chemical_formula_weight         820.82

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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'
'-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                   19.556(4)
_cell_length_b                   5.9957(12)
_cell_length_c                   20.412(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.82(3)
_cell_angle_gamma                90.00
_cell_volume                     2237.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2559
_cell_measurement_theta_min      3.58
_cell_measurement_theta_max      27.46

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    5.967
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3927
_exptl_absorpt_correction_T_max  0.5000
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10565
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         27.46
_reflns_number_total             2559
_reflns_number_gt                2418
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0317P)²+22.8529P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2559
_refine_ls_number_parameters     188
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0193
_refine_ls_wR_factor_ref         0.0599
_refine_ls_wR_factor_gt          0.0478
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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 0.7970(2) 0.4684(6) 0.17249(19) 0.0136(7) Uani 1 1 d . . .
C2 C 0.8420(2) 0.2796(7) 0.1902(2) 0.0153(7) Uani 1 1 d . . .
C3 C 0.8842(2) 0.2411(7) 0.2606(2) 0.0193(8) Uani 1 1 d . . .
H3 H 0.9135 0.1147 0.2730 0.023 Uiso 1 1 calc R . .
C4 C 0.8826(2) 0.3896(8) 0.3120(2) 0.0245(9) Uani 1 1 d . . .
H4 H 0.9102 0.3612 0.3587 0.029 Uiso 1 1 calc R . .
C5 C 0.8399(2) 0.5806(8) 0.2941(2) 0.0220(9) Uani 1 1 d . . .
H5 H 0.8400 0.6826 0.3284 0.026 Uiso 1 1 calc R . .
C6 C 0.7970(2) 0.6180(7) 0.2240(2) 0.0210(8) Uani 1 1 d . . .
H6 H 0.7679 0.7451 0.2118 0.025 Uiso 1 1 calc R . .
C7 C 0.7461(2) 0.5223(6) 0.09970(18) 0.0129(7) Uani 1 1 d . . .
C8 C 0.8472(2) 0.1209(6) 0.1356(2) 0.0141(7) Uani 1 1 d . . .
C9 C 0.49899(19) 0.6118(6) 0.01800(18) 0.0108(7) Uani 1 1 d . . .
Gd1 Gd 0.637328(9) 0.67065(3) -0.032106(8) 0.01000(7) Uani 1 1 d . . .
H1 H 0.636(5) 1.101(14) 0.037(4) 0.07(2) Uiso 1 1 d . . .
H2 H 0.699(3) 1.068(10) 0.040(3) 0.032(16) Uiso 1 1 d . . .
H7 H 0.535(3) 0.911(10) -0.146(3) 0.025(14) Uiso 1 1 d . . .
H8 H 0.546(4) 1.069(7) -0.096(4) 0.08(3) Uiso 1 1 d D . .
H9 H 0.038(3) 0.772(12) 0.269(4) 0.05(2) Uiso 1 1 d . . .
O1 O 0.68058(15) 0.4626(5) 0.07966(15) 0.0178(6) Uani 1 1 d . . .
O2 O 0.89310(16) -0.0373(5) 0.15292(15) 0.0222(6) Uani 1 1 d . . .
O3 O 0.80621(15) 0.1454(4) 0.07186(14) 0.0150(5) Uani 1 1 d . . .
O4 O 0.54435(15) 0.7551(5) 0.01714(16) 0.0191(6) Uani 1 1 d . . .
O5 O 0.45085(16) 0.6323(5) 0.04569(16) 0.0200(6) Uani 1 1 d . . .
O6 O 0.66404(18) 1.0031(5) 0.03649(17) 0.0219(6) Uani 1 1 d . . .
O7 O 0.76824(15) 0.6467(4) 0.06073(14) 0.0155(5) Uani 1 1 d . . .
O8 O 0.55844(19) 0.9445(5) -0.10854(17) 0.0253(7) Uani 1 1 d D . .
O9 O 0.0000 0.7000(9) 0.2500 0.0336(11) Uani 1 2 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 C6 1.383(6) . ?
C1 C2 1.400(5) . ?
C1 C7 1.501(5) . ?
C2 C3 1.399(5) . ?
C2 C8 1.496(5) . ?
C3 C4 1.384(6) . ?
C4 C5 1.387(7) . ?
C5 C6 1.395(6) . ?
C7 O1 1.251(5) . ?
C7 O7 1.273(4) . ?
C8 O2 1.266(5) . ?
C8 O3 1.271(5) . ?
C8 Gd1 2.839(4) 7_655 ?
C9 O4 1.239(5) . ?
C9 O5 1.265(4) . ?
C9 C9 1.536(7) 5_665 ?
Gd1 O6 2.385(3) . ?
Gd1 O7 2.391(3) 7_665 ?
Gd1 O8 2.408(3) . ?
Gd1 O4 2.423(3) . ?
Gd1 O5 2.451(3) 5_665 ?
Gd1 O2 2.456(3) 7_655 ?
Gd1 O1 2.471(3) . ?
Gd1 O3 2.471(3) 7_655 ?
Gd1 O7 2.592(3) . ?
Gd1 C8 2.839(4) 7_655 ?
O2 Gd1 2.456(3) 7_655 ?
O3 Gd1 2.471(3) 7_655 ?
O5 Gd1 2.451(3) 5_665 ?
O7 Gd1 2.391(3) 7_665 ?

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
C6 C1 C2 119.9(4) . . ?
C6 C1 C7 115.7(3) . . ?
C2 C1 C7 124.4(3) . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 C8 119.3(4) . . ?
C1 C2 C8 121.7(3) . . ?
C4 C3 C2 120.5(4) . . ?
C3 C4 C5 120.4(4) . . ?
C4 C5 C6 119.3(4) . . ?
C1 C6 C5 120.8(4) . . ?
O1 C7 O7 120.0(3) . . ?
O1 C7 C1 120.3(3) . . ?
O7 C7 C1 119.4(3) . . ?
O2 C8 O3 119.9(3) . . ?
O2 C8 C2 119.8(3) . . ?
O3 C8 C2 120.2(3) . . ?
O2 C8 Gd1 59.6(2) . 7_655 ?
O3 C8 Gd1 60.33(19) . 7_655 ?
C2 C8 Gd1 177.5(3) . 7_655 ?
O4 C9 O5 126.1(3) . . ?
O4 C9 C9 117.2(4) . 5_665 ?
O5 C9 C9 116.6(4) . 5_665 ?
O6 Gd1 O7 74.55(10) . 7_665 ?
O6 Gd1 O8 76.51(12) . . ?
O7 Gd1 O8 84.38(11) 7_665 . ?
O6 Gd1 O4 67.78(11) . . ?
O7 Gd1 O4 139.84(9) 7_665 . ?
O8 Gd1 O4 73.98(11) . . ?
O6 Gd1 O5 133.17(10) . 5_665 ?
O7 Gd1 O5 152.25(9) 7_665 5_665 ?
O8 Gd1 O5 99.73(12) . 5_665 ?
O4 Gd1 O5 66.44(9) . 5_665 ?
O6 Gd1 O2 141.81(11) . 7_655 ?
O7 Gd1 O2 80.58(10) 7_665 7_655 ?
O8 Gd1 O2 72.58(11) . 7_655 ?
O4 Gd1 O2 122.33(10) . 7_655 ?
O5 Gd1 O2 74.67(10) 5_665 7_655 ?
O6 Gd1 O1 87.03(11) . . ?
O7 Gd1 O1 114.60(9) 7_665 . ?
O8 Gd1 O1 150.77(10) . . ?
O4 Gd1 O1 77.49(10) . . ?
O5 Gd1 O1 74.13(10) 5_665 . ?
O2 Gd1 O1 130.10(10) 7_655 . ?
O6 Gd1 O3 143.48(10) . 7_655 ?
O7 Gd1 O3 78.28(9) 7_665 7_655 ?
O8 Gd1 O3 124.63(10) . 7_655 ?
O4 Gd1 O3 141.74(9) . 7_655 ?
O5 Gd1 O3 76.89(9) 5_665 7_655 ?
O2 Gd1 O3 52.96(9) 7_655 7_655 ?
O1 Gd1 O3 82.52(9) . 7_655 ?
O6 Gd1 O7 70.35(10) . . ?
O7 Gd1 O7 63.64(11) 7_665 . ?
O8 Gd1 O7 138.62(11) . . ?
O4 Gd1 O7 113.59(9) . . ?
O5 Gd1 O7 120.93(10) 5_665 . ?
O2 Gd1 O7 122.68(9) 7_655 . ?
O1 Gd1 O7 51.09(9) . . ?
O3 Gd1 O7 75.93(9) 7_655 . ?
O6 Gd1 C8 153.17(11) . 7_655 ?
O7 Gd1 C8 78.73(10) 7_665 7_655 ?
O8 Gd1 C8 98.67(11) . 7_655 ?
O4 Gd1 C8 136.98(10) . 7_655 ?
O5 Gd1 C8 73.52(10) 5_665 7_655 ?
O2 Gd1 C8 26.42(10) 7_655 7_655 ?
O1 Gd1 C8 106.51(10) . 7_655 ?
O3 Gd1 C8 26.55(10) 7_655 7_655 ?
O7 Gd1 C8 99.86(10) . 7_655 ?
C7 O1 Gd1 97.6(2) . . ?
C8 O2 Gd1 93.9(2) . 7_655 ?
C8 O3 Gd1 93.1(2) . 7_655 ?
C9 O4 Gd1 120.5(2) . . ?
C9 O5 Gd1 118.9(2) . 5_665 ?
C7 O7 Gd1 152.2(2) . 7_665 ?
C7 O7 Gd1 91.3(2) . . ?
Gd1 O7 Gd1 116.36(11) 7_665 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.804
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.171

data_7
_database_code_depnum_ccdc_archive 'CCDC 715646'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C7 H3 K O9 Tb'
_chemical_formula_sum            'C7 H3 K O9 Tb'
_chemical_formula_weight         429.11

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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

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

_cell_length_a                   6.6743(4)
_cell_length_b                   7.6033(5)
_cell_length_c                   11.0030(6)
_cell_angle_alpha                100.210(4)
_cell_angle_beta                 103.892(4)
_cell_angle_gamma                106.921(4)
_cell_volume                     499.87(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1901
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      25.76

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             402
_exptl_absorpt_coefficient_mu    7.532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4885
_exptl_absorpt_correction_T_max  0.5627
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2997
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.76
_reflns_number_total             1901
_reflns_number_gt                1783
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0362P)²+0.2181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1901
_refine_ls_number_parameters     171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.004
_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 0.8999(8) 0.4863(7) 0.3697(4) 0.0132(9) Uani 1 1 d . . .
C2 C 0.9359(7) 0.3268(7) 0.4062(4) 0.0125(9) Uani 1 1 d . . .
C3 C 1.0347(8) 0.3440(7) 0.5358(5) 0.0142(10) Uani 1 1 d . . .
H3 H 1.0577 0.2386 0.5600 0.017 Uiso 1 1 calc R . .
C4 C 0.7919(8) 0.4784(7) 0.2288(5) 0.0160(10) Uani 1 1 d . . .
C5 C 0.8668(8) 0.1356(7) 0.3098(5) 0.0147(10) Uani 1 1 d . . .
C6 C 0.5310(7) 0.4378(7) 0.5448(4) 0.0128(10) Uani 1 1 d . . .
C7 C 0.0158(8) -0.0975(7) -0.0070(4) 0.0155(10) Uani 1 1 d . . .
H1 H 0.150(11) -0.205(9) 0.291(6) 0.021(15) Uiso 1 1 d . . .
H2 H 0.372(12) -0.157(9) 0.376(6) 0.031(18) Uiso 1 1 d . . .
K1 K 0.3649(3) 0.6253(2) 0.10294(13) 0.0382(3) Uani 1 1 d . . .
O1 O 0.8873(7) 0.6005(6) 0.1819(4) 0.0382(11) Uani 1 1 d . . .
O2 O 0.6076(6) 0.3473(5) 0.1668(3) 0.0218(8) Uani 1 1 d . . .
O3 O 0.6626(6) 0.0394(5) 0.2635(4) 0.0233(8) Uani 1 1 d . . .
O4 O 1.0140(6) 0.0800(5) 0.2863(4) 0.0219(8) Uani 1 1 d . . .
O5 O 0.5063(6) 0.2700(5) 0.4893(3) 0.0156(7) Uani 1 1 d . . .
O6 O 0.3979(6) 0.4855(5) 0.3362(3) 0.0176(7) Uani 1 1 d . . .
O7 O 0.1891(6) -0.1001(5) 0.0671(3) 0.0184(7) Uani 1 1 d . . .
O8 O 0.1325(6) 0.2372(5) 0.0896(3) 0.0230(8) Uani 1 1 d . . .
O9 O 0.2861(7) -0.1331(6) 0.3188(4) 0.0215(8) Uani 1 1 d . . .
Tb1 Tb 0.36549(3) 0.15624(3) 0.256321(19) 0.01101(10) 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 C3 1.384(7) 2_766 ?
C1 C2 1.409(7) . ?
C1 C4 1.527(6) . ?
C2 C3 1.385(7) . ?
C2 C5 1.510(7) . ?
C3 C1 1.384(7) 2_766 ?
C4 O1 1.232(6) . ?
C4 O2 1.270(6) . ?
C4 K1 3.421(5) 2_665 ?
C5 O4 1.239(6) . ?
C5 O3 1.267(6) . ?
C6 O6 1.244(6) 2_666 ?
C6 O5 1.257(6) . ?
C6 C6 1.550(9) 2_666 ?
C7 O8 1.244(6) 2 ?
C7 O7 1.253(6) . ?
C7 C7 1.544(10) 2 ?
K1 O7 2.718(4) 1_565 ?
K1 O8 2.865(4) . ?
K1 O6 2.932(4) . ?
K1 O9 2.985(4) 1_565 ?
K1 O2 3.057(4) 2_665 ?
K1 O1 3.079(4) 2_665 ?
K1 O2 3.092(4) . ?
K1 O3 3.112(4) 1_565 ?
K1 C4 3.421(5) 2_665 ?
K1 K1 3.801(3) 2_665 ?
K1 Tb1 4.0886(14) 1_565 ?
K1 K1 4.501(3) 2_565 ?
O1 K1 3.079(4) 2_665 ?
O2 Tb1 2.366(3) . ?
O2 K1 3.057(4) 2_665 ?
O3 Tb1 2.388(4) . ?
O3 K1 3.112(4) 1_545 ?
O4 Tb1 2.366(3) 1_655 ?
O5 Tb1 2.406(3) . ?
O6 C6 1.244(6) 2_666 ?
O6 Tb1 2.429(3) . ?
O7 Tb1 2.359(3) . ?
O7 K1 2.718(4) 1_545 ?
O8 C7 1.244(6) 2 ?
O8 Tb1 2.397(4) . ?
O9 Tb1 2.372(4) . ?
O9 K1 2.985(4) 1_545 ?
Tb1 O4 2.366(3) 1_455 ?
Tb1 K1 4.0886(14) 1_545 ?

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
C3 C1 C2 119.1(4) 2_766 . ?
C3 C1 C4 118.8(4) 2_766 . ?
C2 C1 C4 122.1(4) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 C5 118.3(4) . . ?
C1 C2 C5 122.6(4) . . ?
C1 C3 C2 121.9(5) 2_766 . ?
O1 C4 O2 123.6(5) . . ?
O1 C4 C1 118.2(4) . . ?
O2 C4 C1 118.2(4) . . ?
O1 C4 K1 63.7(3) . 2_665 ?
O2 C4 K1 62.8(3) . 2_665 ?
C1 C4 K1 163.2(3) . 2_665 ?
O4 C5 O3 124.6(5) . . ?
O4 C5 C2 117.7(4) . . ?
O3 C5 C2 117.6(4) . . ?
O6 C6 O5 126.8(4) 2_666 . ?
O6 C6 C6 116.9(5) 2_666 2_666 ?
O5 C6 C6 116.3(5) . 2_666 ?
O8 C7 O7 126.1(5) 2 . ?
O8 C7 C7 117.4(5) 2 2 ?
O7 C7 C7 116.5(5) . 2 ?
O7 K1 O8 127.02(12) 1_565 . ?
O7 K1 O6 122.37(11) 1_565 . ?
O8 K1 O6 58.35(10) . . ?
O7 K1 O9 57.72(10) 1_565 1_565 ?
O8 K1 O9 106.43(11) . 1_565 ?
O6 K1 O9 66.02(10) . 1_565 ?
O7 K1 O2 78.59(11) 1_565 2_665 ?
O8 K1 O2 109.05(11) . 2_665 ?
O6 K1 O2 158.95(11) . 2_665 ?
O9 K1 O2 134.81(11) 1_565 2_665 ?
O7 K1 O1 89.59(12) 1_565 2_665 ?
O8 K1 O1 70.08(11) . 2_665 ?
O6 K1 O1 128.38(11) . 2_665 ?
O9 K1 O1 137.43(14) 1_565 2_665 ?
O2 K1 O1 42.13(10) 2_665 2_665 ?
O7 K1 O2 173.77(11) 1_565 . ?
O8 K1 O2 58.03(10) . . ?
O6 K1 O2 55.74(10) . . ?
O9 K1 O2 118.68(10) 1_565 . ?
O2 K1 O2 103.65(9) 2_665 . ?
O1 K1 O2 95.94(12) 2_665 . ?
O7 K1 O3 64.32(10) 1_565 1_565 ?
O8 K1 O3 150.64(11) . 1_565 ?
O6 K1 O3 92.39(11) . 1_565 ?
O9 K1 O3 53.36(10) 1_565 1_565 ?
O2 K1 O3 99.58(11) 2_665 1_565 ?
O1 K1 O3 139.23(12) 2_665 1_565 ?
O2 K1 O3 109.48(10) . 1_565 ?
O7 K1 C4 80.37(11) 1_565 2_665 ?
O8 K1 C4 90.56(11) . 2_665 ?
O6 K1 C4 148.19(12) . 2_665 ?
O9 K1 C4 137.03(12) 1_565 2_665 ?
O2 K1 C4 21.69(10) 2_665 2_665 ?
O1 K1 C4 21.01(11) 2_665 2_665 ?
O2 K1 C4 103.90(11) . 2_665 ?
O3 K1 C4 118.78(12) 1_565 2_665 ?
O7 K1 K1 130.51(10) 1_565 2_665 ?
O8 K1 K1 80.31(9) . 2_665 ?
O6 K1 K1 107.02(9) . 2_665 ?
O9 K1 K1 163.20(11) 1_565 2_665 ?
O2 K1 K1 52.24(8) 2_665 2_665 ?
O1 K1 K1 59.18(10) 2_665 2_665 ?
O2 K1 K1 51.41(7) . 2_665 ?
O3 K1 K1 113.90(10) 1_565 2_665 ?
C4 K1 K1 56.49(9) 2_665 2_665 ?
O7 K1 Tb1 33.48(7) 1_565 1_565 ?
O8 K1 Tb1 138.13(9) . 1_565 ?
O6 K1 Tb1 98.77(7) . 1_565 ?
O9 K1 Tb1 34.97(7) 1_565 1_565 ?
O2 K1 Tb1 101.04(8) 2_665 1_565 ?
O1 K1 Tb1 122.72(10) 2_665 1_565 ?
O2 K1 Tb1 140.60(8) . 1_565 ?
O3 K1 Tb1 35.58(7) 1_565 1_565 ?
C4 K1 Tb1 110.25(9) 2_665 1_565 ?
K1 K1 Tb1 141.51(7) 2_665 1_565 ?
O7 K1 K1 68.19(8) 1_565 2_565 ?
O8 K1 K1 61.18(8) . 2_565 ?
O6 K1 K1 101.73(9) . 2_565 ?
O9 K1 K1 89.89(9) 1_565 2_565 ?
O2 K1 K1 83.57(8) 2_665 2_565 ?
O1 K1 K1 50.18(9) 2_665 2_565 ?
O2 K1 K1 117.67(8) . 2_565 ?
O3 K1 K1 130.56(8) 1_565 2_565 ?
C4 K1 K1 63.86(9) 2_665 2_565 ?
K1 K1 K1 106.72(6) 2_665 2_565 ?
Tb1 K1 K1 95.12(4) 1_565 2_565 ?
C4 O1 K1 95.3(3) . 2_665 ?
C4 O2 Tb1 126.8(3) . . ?
C4 O2 K1 95.5(3) . 2_665 ?
Tb1 O2 K1 137.61(14) . 2_665 ?
C4 O2 K1 94.5(3) . . ?
Tb1 O2 K1 100.04(13) . . ?
K1 O2 K1 76.35(9) 2_665 . ?
C5 O3 Tb1 127.1(3) . . ?
C5 O3 K1 137.5(3) . 1_545 ?
Tb1 O3 K1 95.14(11) . 1_545 ?
C5 O4 Tb1 148.3(3) . 1_655 ?
C6 O5 Tb1 120.2(3) . . ?
C6 O6 Tb1 119.6(3) 2_666 . ?
C6 O6 K1 134.8(3) 2_666 . ?
Tb1 O6 K1 103.02(11) . . ?
C7 O7 Tb1 115.9(3) . . ?
C7 O7 K1 134.7(3) . 1_545 ?
Tb1 O7 K1 107.05(12) . 1_545 ?
C7 O8 Tb1 114.3(3) 2 . ?
C7 O8 K1 136.7(3) 2 . ?
Tb1 O8 K1 105.84(13) . . ?
Tb1 O9 K1 98.85(12) . 1_545 ?
O7 Tb1 O2 95.60(12) . . ?
O7 Tb1 O4 84.90(12) . 1_455 ?
O2 Tb1 O4 144.61(13) . 1_455 ?
O7 Tb1 O9 71.46(13) . . ?
O2 Tb1 O9 142.04(14) . . ?
O4 Tb1 O9 71.48(13) 1_455 . ?
O7 Tb1 O3 82.19(12) . . ?
O2 Tb1 O3 72.71(13) . . ?
O4 Tb1 O3 141.74(13) 1_455 . ?
O9 Tb1 O3 70.28(13) . . ?
O7 Tb1 O8 68.46(12) . . ?
O2 Tb1 O8 74.89(13) . . ?
O4 Tb1 O8 72.45(13) 1_455 . ?
O9 Tb1 O8 127.46(13) . . ?
O3 Tb1 O8 133.30(13) . . ?
O7 Tb1 O5 149.70(12) . . ?
O2 Tb1 O5 108.81(12) . . ?
O4 Tb1 O5 85.25(12) 1_455 . ?
O9 Tb1 O5 78.24(13) . . ?
O3 Tb1 O5 88.07(12) . . ?
O8 Tb1 O5 134.39(12) . . ?
O7 Tb1 O6 140.13(12) . . ?
O2 Tb1 O6 72.03(13) . . ?
O4 Tb1 O6 85.01(12) 1_455 . ?
O9 Tb1 O6 139.46(12) . . ?
O3 Tb1 O6 126.30(12) . . ?
O8 Tb1 O6 71.71(12) . . ?
O5 Tb1 O6 67.04(11) . . ?
O7 Tb1 K1 39.46(9) . 1_545 ?
O2 Tb1 K1 101.48(10) . 1_545 ?
O4 Tb1 K1 101.05(9) 1_455 1_545 ?
O9 Tb1 K1 46.17(10) . 1_545 ?
O3 Tb1 K1 49.29(9) . 1_545 ?
O8 Tb1 K1 107.63(9) . 1_545 ?
O5 Tb1 K1 115.54(8) . 1_545 ?
O6 Tb1 K1 173.48(9) . 1_545 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.76
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.165

data_8
_database_code_depnum_ccdc_archive 'CCDC 715647'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C7 H3 Dy K O9'
_chemical_formula_sum            'C7 H3 Dy K O9'
_chemical_formula_weight         432.69

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.6560(2)
_cell_length_b                   7.5778(3)
_cell_length_c                   10.9904(3)
_cell_angle_alpha                100.325(2)
_cell_angle_beta                 103.827(2)
_cell_angle_gamma                106.904(2)
_cell_volume                     496.21(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2446
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             404
_exptl_absorpt_coefficient_mu    7.990
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4453
_exptl_absorpt_correction_T_max  0.5754
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3649
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         28.29
_reflns_number_total             2446
_reflns_number_gt                2218
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0265P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2446
_refine_ls_number_parameters     171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0568
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.1008(7) 0.5145(6) 0.6312(4) 0.0131(8) Uani 1 1 d . . .
C2 C 0.0639(7) 0.6733(6) 0.5942(4) 0.0131(8) Uani 1 1 d . . .
C3 C -0.0352(7) 0.6575(6) 0.4648(4) 0.0149(8) Uani 1 1 d . . .
H3 H -0.0586 0.7634 0.4411 0.018 Uiso 1 1 calc R . .
C4 C 0.2101(8) 0.5222(6) 0.7705(4) 0.0161(9) Uani 1 1 d . . .
C5 C 0.1358(7) 0.8651(6) 0.6914(4) 0.0130(8) Uani 1 1 d . . .
C6 C 0.4679(7) 0.5622(6) 0.4552(4) 0.0133(8) Uani 1 1 d . . .
C7 C 0.9831(8) 1.0981(6) 1.0067(4) 0.0159(9) Uani 1 1 d . . .
H1 H 0.839(10) 1.195(9) 0.696(6) 0.030(17) Uiso 1 1 d . . .
H2 H 0.654(9) 1.168(7) 0.632(5) 0.012(14) Uiso 1 1 d . . .
K1 K 0.6340(2) 0.37423(18) 0.89687(12) 0.0356(3) Uani 1 1 d . . .
O1 O 0.1157(7) 0.3973(5) 0.8179(3) 0.0351(10) Uani 1 1 d . . .
O2 O 0.3939(5) 0.6537(5) 0.8330(3) 0.0207(7) Uani 1 1 d . . .
O3 O 0.3388(5) 0.9606(5) 0.7373(3) 0.0213(7) Uani 1 1 d . . .
O4 O -0.0129(5) 0.9217(5) 0.7152(3) 0.0220(7) Uani 1 1 d . . .
O5 O 0.4945(5) 0.7309(4) 0.5114(3) 0.0160(6) Uani 1 1 d . . .
O6 O 0.6048(5) 0.5145(4) 0.6638(3) 0.0175(7) Uani 1 1 d . . .
O7 O 0.8091(5) 1.0985(5) 0.9318(3) 0.0184(7) Uani 1 1 d . . .
O8 O 0.8679(6) 0.7628(5) 0.9092(3) 0.0216(7) Uani 1 1 d . . .
O9 O 0.7150(6) 1.1331(5) 0.6822(4) 0.0210(7) Uani 1 1 d . . .
Dy1 Dy 0.63606(3) 0.84399(3) 0.743752(19) 0.01073(7) 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 C3 1.399(6) 2_566 ?
C1 C2 1.405(6) . ?
C1 C4 1.512(6) . ?
C2 C3 1.384(6) . ?
C2 C5 1.509(6) . ?
C3 C1 1.399(6) 2_566 ?
C4 O1 1.245(5) . ?
C4 O2 1.267(5) . ?
C4 K1 3.427(5) 2_667 ?
C5 O4 1.250(5) . ?
C5 O3 1.257(5) . ?
C6 O6 1.242(5) 2_666 ?
C6 O5 1.258(5) . ?
C6 C6 1.552(8) 2_666 ?
C7 O8 1.246(6) 2_777 ?
C7 O7 1.252(5) . ?
C7 C7 1.554(9) 2_777 ?
K1 O7 2.713(3) 1_545 ?
K1 O8 2.864(4) . ?
K1 O6 2.930(3) . ?
K1 O9 2.972(4) 1_545 ?
K1 O2 3.059(3) 2_667 ?
K1 O1 3.079(4) 2_667 ?
K1 O2 3.082(4) . ?
K1 O3 3.092(4) 1_545 ?
K1 O1 3.415(5) . ?
K1 C4 3.427(5) 2_667 ?
K1 K1 3.784(2) 2_667 ?
K1 Dy1 4.0738(12) 1_545 ?
O1 K1 3.079(4) 2_667 ?
O2 Dy1 2.356(3) . ?
O2 K1 3.059(3) 2_667 ?
O3 Dy1 2.382(3) . ?
O3 K1 3.092(3) 1_565 ?
O4 Dy1 2.350(3) 1_455 ?
O5 Dy1 2.396(3) . ?
O6 C6 1.242(5) 2_666 ?
O6 Dy1 2.424(3) . ?
O7 Dy1 2.336(3) . ?
O7 K1 2.713(3) 1_565 ?
O8 C7 1.246(6) 2_777 ?
O8 Dy1 2.383(3) . ?
O9 Dy1 2.359(3) . ?
O9 K1 2.972(4) 1_565 ?
Dy1 O4 2.350(3) 1_655 ?
Dy1 K1 4.0738(12) 1_565 ?

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
C3 C1 C2 118.7(4) 2_566 . ?
C3 C1 C4 118.6(4) 2_566 . ?
C2 C1 C4 122.7(4) . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 C5 118.3(4) . . ?
C1 C2 C5 121.8(4) . . ?
C2 C3 C1 121.4(4) . 2_566 ?
O1 C4 O2 123.1(4) . . ?
O1 C4 C1 118.2(4) . . ?
O2 C4 C1 118.7(4) . . ?
O1 C4 K1 63.5(2) . 2_667 ?
O2 C4 K1 62.6(2) . 2_667 ?
C1 C4 K1 162.6(3) . 2_667 ?
O4 C5 O3 124.6(4) . . ?
O4 C5 C2 117.1(4) . . ?
O3 C5 C2 118.1(4) . . ?
O6 C6 O5 126.8(4) 2_666 . ?
O6 C6 C6 117.1(5) 2_666 2_666 ?
O5 C6 C6 116.0(5) . 2_666 ?
O8 C7 O7 127.4(4) 2_777 . ?
O8 C7 C7 116.4(5) 2_777 2_777 ?
O7 C7 C7 116.3(5) . 2_777 ?
O7 K1 O8 126.95(11) 1_545 . ?
O7 K1 O6 121.97(10) 1_545 . ?
O8 K1 O6 57.98(9) . . ?
O7 K1 O9 57.47(10) 1_545 1_545 ?
O8 K1 O9 106.00(10) . 1_545 ?
O6 K1 O9 65.88(10) . 1_545 ?
O7 K1 O2 78.59(10) 1_545 2_667 ?
O8 K1 O2 109.43(10) . 2_667 ?
O6 K1 O2 159.32(10) . 2_667 ?
O9 K1 O2 134.64(10) 1_545 2_667 ?
O7 K1 O1 90.13(11) 1_545 2_667 ?
O8 K1 O1 70.18(10) . 2_667 ?
O6 K1 O1 128.10(10) . 2_667 ?
O9 K1 O1 137.58(13) 1_545 2_667 ?
O2 K1 O1 42.17(9) 2_667 2_667 ?
O7 K1 O2 173.79(11) 1_545 . ?
O8 K1 O2 57.87(9) . . ?
O6 K1 O2 55.87(9) . . ?
O9 K1 O2 118.72(10) 1_545 . ?
O2 K1 O2 103.94(8) 2_667 . ?
O1 K1 O2 95.52(11) 2_667 . ?
O7 K1 O3 63.97(10) 1_545 1_545 ?
O8 K1 O3 150.49(10) . 1_545 ?
O6 K1 O3 92.63(10) . 1_545 ?
O9 K1 O3 53.46(9) 1_545 1_545 ?
O2 K1 O3 99.43(10) 2_667 1_545 ?
O1 K1 O3 139.26(10) 2_667 1_545 ?
O2 K1 O3 109.88(9) . 1_545 ?
O7 K1 O1 135.90(11) 1_545 . ?
O8 K1 O1 97.11(10) . . ?
O6 K1 O1 77.01(9) . . ?
O9 K1 O1 113.43(11) 1_545 . ?
O2 K1 O1 89.42(9) 2_667 . ?
O1 K1 O1 108.93(9) 2_667 . ?
O2 K1 O1 39.32(8) . . ?
O3 K1 O1 76.73(9) 1_545 . ?
O7 K1 C4 80.47(10) 1_545 2_667 ?
O8 K1 C4 90.96(11) . 2_667 ?
O6 K1 C4 148.26(11) . 2_667 ?
O9 K1 C4 136.85(11) 1_545 2_667 ?
O2 K1 C4 21.58(9) 2_667 2_667 ?
O1 K1 C4 21.21(10) 2_667 2_667 ?
O2 K1 C4 104.00(10) . 2_667 ?
O3 K1 C4 118.54(11) 1_545 2_667 ?
O1 K1 C4 103.06(10) . 2_667 ?
O7 K1 K1 130.53(9) 1_545 2_667 ?
O8 K1 K1 80.55(8) . 2_667 ?
O6 K1 K1 107.42(8) . 2_667 ?
O9 K1 K1 163.64(10) 1_545 2_667 ?
O2 K1 K1 52.24(7) 2_667 2_667 ?
O1 K1 K1 58.60(9) 2_667 2_667 ?
O2 K1 K1 51.70(6) . 2_667 ?
O3 K1 K1 114.17(8) 1_545 2_667 ?
O1 K1 K1 50.33(7) . 2_667 ?
C4 K1 K1 56.31(8) 2_667 2_667 ?
O7 K1 Dy1 33.19(7) 1_545 1_545 ?
O8 K1 Dy1 137.63(8) . 1_545 ?
O6 K1 Dy1 98.61(7) . 1_545 ?
O9 K1 Dy1 34.89(7) 1_545 1_545 ?
O2 K1 Dy1 100.98(7) 2_667 1_545 ?
O1 K1 Dy1 122.99(9) 2_667 1_545 ?
O2 K1 Dy1 140.83(7) . 1_545 ?
O3 K1 Dy1 35.61(6) 1_545 1_545 ?
O1 K1 Dy1 112.29(8) . 1_545 ?
C4 K1 Dy1 110.14(8) 2_667 1_545 ?
K1 K1 Dy1 141.76(6) 2_667 1_545 ?
C4 O1 K1 95.3(3) . 2_667 ?
C4 O1 K1 79.6(3) . . ?
K1 O1 K1 71.07(9) 2_667 . ?
C4 O2 Dy1 126.5(3) . . ?
C4 O2 K1 95.8(3) . 2_667 ?
Dy1 O2 K1 137.70(13) . 2_667 ?
C4 O2 K1 94.2(3) . . ?
Dy1 O2 K1 100.24(11) . . ?
K1 O2 K1 76.06(8) 2_667 . ?
C5 O3 Dy1 127.2(3) . . ?
C5 O3 K1 137.2(3) . 1_565 ?
Dy1 O3 K1 95.30(10) . 1_565 ?
C5 O4 Dy1 147.9(3) . 1_455 ?
C6 O5 Dy1 120.3(3) . . ?
C6 O6 Dy1 119.2(3) 2_666 . ?
C6 O6 K1 134.9(3) 2_666 . ?
Dy1 O6 K1 102.90(10) . . ?
C7 O7 Dy1 116.4(3) . . ?
C7 O7 K1 133.8(3) . 1_565 ?
Dy1 O7 K1 107.34(12) . 1_565 ?
C7 O8 Dy1 115.0(3) 2_777 . ?
C7 O8 K1 135.8(3) 2_777 . ?
Dy1 O8 K1 105.96(12) . . ?
Dy1 O9 K1 99.02(12) . 1_565 ?
O7 Dy1 O4 84.85(11) . 1_655 ?
O7 Dy1 O2 95.23(11) . . ?
O4 Dy1 O2 144.76(12) 1_655 . ?
O7 Dy1 O9 71.46(12) . . ?
O4 Dy1 O9 71.45(13) 1_655 . ?
O2 Dy1 O9 141.77(13) . . ?
O7 Dy1 O3 81.86(11) . . ?
O4 Dy1 O3 141.72(12) 1_655 . ?
O2 Dy1 O3 72.43(12) . . ?
O9 Dy1 O3 70.30(12) . . ?
O7 Dy1 O8 68.67(11) . . ?
O4 Dy1 O8 72.33(12) 1_655 . ?
O2 Dy1 O8 74.94(12) . . ?
O9 Dy1 O8 127.53(13) . . ?
O3 Dy1 O8 133.21(12) . . ?
O7 Dy1 O5 149.67(11) . . ?
O4 Dy1 O5 85.78(11) 1_655 . ?
O2 Dy1 O5 108.80(11) . . ?
O9 Dy1 O5 78.21(12) . . ?
O3 Dy1 O5 87.91(11) . . ?
O8 Dy1 O5 134.57(11) . . ?
O7 Dy1 O6 140.12(11) . . ?
O4 Dy1 O6 85.18(11) 1_655 . ?
O2 Dy1 O6 72.29(11) . . ?
O9 Dy1 O6 139.56(12) . . ?
O3 Dy1 O6 126.43(11) . . ?
O8 Dy1 O6 71.51(11) . . ?
O5 Dy1 O6 67.30(10) . . ?
O7 Dy1 K1 39.47(8) . 1_565 ?
O4 Dy1 K1 100.92(8) 1_655 1_565 ?
O2 Dy1 K1 101.19(9) . 1_565 ?
O9 Dy1 K1 46.10(9) . 1_565 ?
O3 Dy1 K1 49.09(8) . 1_565 ?
O8 Dy1 K1 107.86(8) . 1_565 ?
O5 Dy1 K1 115.24(7) . 1_565 ?
O6 Dy1 K1 173.44(8) . 1_565 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.200
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.181

data_9
_database_code_depnum_ccdc_archive 'CCDC 715648'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C25 H18 Ce2 K O17'
_chemical_formula_sum            'C25 H18 Ce2 K O17'
_chemical_formula_weight         909.73

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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

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

_cell_length_a                   10.4541(7)
_cell_length_b                   11.7756(8)
_cell_length_c                   12.3649(9)
_cell_angle_alpha                93.8060(10)
_cell_angle_beta                 112.6500(10)
_cell_angle_gamma                98.5580(10)
_cell_volume                     1376.30(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6809
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      28.32

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             878
_exptl_absorpt_coefficient_mu    3.502
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3610
_exptl_absorpt_correction_T_max  0.5910
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10149
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         28.32
_reflns_number_total             6809
_reflns_number_gt                6081
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0698P)²+0.9064P] 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         6809
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.1072
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.002
_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 0.4637(4) 0.6879(3) 0.4085(3) 0.0172(7) Uani 1 1 d . . .
C2 C 0.5361(4) 0.8063(3) 0.4086(3) 0.0203(7) Uani 1 1 d . . .
C3 C 0.5367(4) 0.8410(3) 0.3028(3) 0.0207(8) Uani 1 1 d . . .
H3 H 0.4945 0.7889 0.2335 0.025 Uiso 1 1 calc R . .
C4 C 0.5994(5) 0.9518(3) 0.3006(4) 0.0224(8) Uani 1 1 d . . .
C5 C 0.6683(6) 1.0280(4) 0.4059(4) 0.0367(12) Uani 1 1 d . . .
H5 H 0.7113 1.1027 0.4049 0.044 Uiso 1 1 calc R . .
C6 C 0.6729(7) 0.9931(5) 0.5112(4) 0.0456(15) Uani 1 1 d . . .
H6 H 0.7217 1.0433 0.5814 0.055 Uiso 1 1 calc R . .
C7 C 0.6052(6) 0.8835(4) 0.5126(4) 0.0340(11) Uani 1 1 d . . .
H7 H 0.6058 0.8612 0.5835 0.041 Uiso 1 1 calc R . .
C8 C 0.5918(4) 0.9903(3) 0.1852(3) 0.0181(7) Uani 1 1 d . . .
C9 C 0.8860(4) 0.7766(3) 1.0988(3) 0.0180(7) Uani 1 1 d . . .
C10 C 0.9628(4) 0.8974(3) 1.1570(3) 0.0186(7) Uani 1 1 d . . .
C11 C 1.0760(4) 0.9508(3) 1.1331(3) 0.0186(7) Uani 1 1 d . . .
H11 H 1.1090 0.9094 1.0859 0.022 Uiso 1 1 calc R . .
C12 C 1.1398(4) 1.0663(3) 1.1799(3) 0.0193(7) Uani 1 1 d . . .
C13 C 1.0917(5) 1.1261(4) 1.2532(4) 0.0282(9) Uani 1 1 d . . .
H13 H 1.1330 1.2031 1.2841 0.034 Uiso 1 1 calc R . .
C14 C 0.9827(5) 1.0719(4) 1.2803(5) 0.0349(11) Uani 1 1 d . . .
H14 H 0.9526 1.1121 1.3306 0.042 Uiso 1 1 calc R . .
C15 C 0.9189(5) 0.9585(4) 1.2328(4) 0.0282(9) Uani 1 1 d . . .
H15 H 0.8460 0.9225 1.2514 0.034 Uiso 1 1 calc R . .
C16 C 1.2598(4) 1.1222(3) 1.1508(3) 0.0176(7) Uani 1 1 d . . .
C17 C 0.2793(4) 0.6668(3) 0.7110(3) 0.0155(7) Uani 1 1 d . . .
C18 C 0.1525(4) 0.6598(3) 0.5998(3) 0.0154(7) Uani 1 1 d . . .
C19 C 0.0180(4) 0.6332(3) 0.6006(3) 0.0154(7) Uani 1 1 d . . .
H19 H 0.0087 0.6205 0.6709 0.018 Uiso 1 1 calc R . .
C20 C -0.1016(4) 0.6257(3) 0.4974(3) 0.0174(7) Uani 1 1 d . . .
C21 C -0.0873(4) 0.6482(4) 0.3924(4) 0.0235(8) Uani 1 1 d . . .
H21 H -0.1673 0.6431 0.3230 0.028 Uiso 1 1 calc R . .
C22 C 0.0449(4) 0.6778(4) 0.3915(4) 0.0259(9) Uani 1 1 d . . .
H22 H 0.0541 0.6955 0.3224 0.031 Uiso 1 1 calc R . .
C23 C 0.1643(4) 0.6810(4) 0.4941(4) 0.0208(8) Uani 1 1 d . . .
H23 H 0.2532 0.6976 0.4922 0.025 Uiso 1 1 calc R . .
C24 C -0.2434(4) 0.5866(3) 0.5000(3) 0.0159(7) Uani 1 1 d . . .
C25 C 0.5252(4) 0.4808(3) 0.9507(3) 0.0134(6) Uani 1 1 d . . .
Ce1 Ce 0.578686(19) 0.575448(16) 0.688348(16) 0.01174(8) Uani 1 1 d . . .
Ce2 Ce 0.52108(2) 0.771246(16) 0.939807(16) 0.01344(8) Uani 1 1 d . . .
K1 K 0.79029(10) 0.33869(9) 0.90276(9) 0.0297(2) Uani 1 1 d . . .
O1 O 0.4816(3) 0.6515(3) 0.5051(3) 0.0251(6) Uani 1 1 d . . .
O2 O 0.3859(3) 0.6274(2) 0.3089(3) 0.0214(6) Uani 1 1 d . . .
O3 O 0.5619(4) 0.9124(3) 0.1002(3) 0.0261(6) Uani 1 1 d . . .
O4 O 0.6158(3) 1.0964(2) 0.1800(3) 0.0247(6) Uani 1 1 d . . .
O5 O 0.7574(3) 0.7493(3) 1.0794(3) 0.0248(6) Uani 1 1 d . . .
O6 O 0.9555(3) 0.7077(3) 1.0723(3) 0.0301(7) Uani 1 1 d . . .
O7 O 1.3134(3) 1.2298(2) 1.1893(3) 0.0239(6) Uani 1 1 d . . .
O8 O 1.3026(3) 1.0665(3) 1.0873(3) 0.0264(6) Uani 1 1 d . . .
O9 O 0.2668(3) 0.6574(3) 0.8073(2) 0.0210(6) Uani 1 1 d . . .
O10 O 0.4020(3) 0.6872(2) 0.7087(2) 0.0181(5) Uani 1 1 d . . .
O11 O -0.2512(3) 0.5897(3) 0.5987(3) 0.0224(6) Uani 1 1 d . . .
O12 O -0.3460(3) 0.5498(2) 0.4013(3) 0.0203(6) Uani 1 1 d . . .
O13 O 0.5444(3) 0.5572(2) 0.8889(2) 0.0171(5) Uani 1 1 d . . .
O14 O 0.4572(3) 0.6213(2) 1.0581(2) 0.0190(5) Uani 1 1 d . . .
O1W O 0.8191(3) 0.5682(3) 0.8539(3) 0.0241(6) Uani 1 1 d . . .
O2W O 0.9174(4) 0.4749(3) 1.1205(3) 0.0334(7) Uani 1 1 d . . .
O3W O 0.7331(5) 0.1723(3) 1.0186(3) 0.0427(9) 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 O1 1.251(5) . ?
C1 O2 1.275(5) . ?
C1 C2 1.484(5) . ?
C2 C7 1.391(6) . ?
C2 C3 1.398(5) . ?
C3 C4 1.378(5) . ?
C4 C5 1.396(6) . ?
C4 C8 1.503(5) . ?
C5 C6 1.376(7) . ?
C6 C7 1.381(7) . ?
C8 O4 1.249(5) . ?
C8 O3 1.256(5) . ?
C9 O5 1.257(5) . ?
C9 O6 1.272(5) . ?
C9 C10 1.506(5) . ?
C10 C15 1.395(6) . ?
C10 C11 1.398(5) . ?
C11 C12 1.398(5) . ?
C12 C13 1.394(6) . ?
C12 C16 1.507(5) . ?
C13 C14 1.388(6) . ?
C14 C15 1.379(6) . ?
C16 O8 1.239(5) . ?
C16 O7 1.284(5) . ?
C16 Ce2 3.064(4) 2_777 ?
C17 O9 1.257(5) . ?
C17 O10 1.282(4) . ?
C17 C18 1.484(5) . ?
C18 C23 1.395(5) . ?
C18 C19 1.398(5) . ?
C19 C20 1.387(5) . ?
C20 C21 1.401(5) . ?
C20 C24 1.498(5) . ?
C21 C22 1.378(6) . ?
C22 C23 1.388(6) . ?
C24 O11 1.252(5) . ?
C24 O12 1.269(4) . ?
C25 O14 1.247(4) 2_667 ?
C25 O13 1.262(4) . ?
C25 C25 1.569(7) 2_667 ?
Ce1 O1 2.395(3) . ?
Ce1 O11 2.424(3) 1_655 ?
Ce1 O12 2.441(3) 2_566 ?
Ce1 O2 2.472(3) 2_666 ?
Ce1 O10 2.499(3) . ?
Ce1 O7 2.505(3) 2_777 ?
Ce1 O1W 2.577(3) . ?
Ce1 O13 2.656(3) . ?
Ce2 O3 2.362(3) 1_556 ?
Ce2 O4 2.451(3) 2_676 ?
Ce2 O5 2.472(3) . ?
Ce2 O14 2.540(3) . ?
Ce2 O8 2.583(3) 2_777 ?
Ce2 O9 2.616(3) . ?
Ce2 O13 2.626(3) . ?
Ce2 O10 2.686(3) . ?
Ce2 O7 2.771(3) 2_777 ?
Ce2 C16 3.064(4) 2_777 ?
Ce2 K1 4.4746(11) 2_667 ?
K1 O3W 2.632(4) . ?
K1 O2 2.655(3) 2_666 ?
K1 O6 2.698(3) 2_767 ?
K1 O2W 2.761(4) . ?
K1 O1W 2.806(3) . ?
K1 O14 2.906(3) 2_667 ?
K1 Ce2 4.4746(10) 2_667 ?
K1 K1 5.015(2) 2_767 ?
O2 Ce1 2.472(3) 2_666 ?
O2 K1 2.655(3) 2_666 ?
O3 Ce2 2.362(3) 1_554 ?
O4 Ce2 2.451(3) 2_676 ?
O6 K1 2.698(3) 2_767 ?
O7 Ce1 2.505(3) 2_777 ?
O7 Ce2 2.771(3) 2_777 ?
O8 Ce2 2.583(3) 2_777 ?
O11 Ce1 2.424(3) 1_455 ?
O12 Ce1 2.441(3) 2_566 ?
O14 C25 1.247(4) 2_667 ?
O14 K1 2.906(3) 2_667 ?

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
O1 C1 O2 122.8(4) . . ?
O1 C1 C2 119.1(4) . . ?
O2 C1 C2 118.0(3) . . ?
C7 C2 C3 119.1(4) . . ?
C7 C2 C1 121.2(4) . . ?
C3 C2 C1 119.7(3) . . ?
C4 C3 C2 120.4(4) . . ?
C3 C4 C5 119.5(4) . . ?
C3 C4 C8 119.9(3) . . ?
C5 C4 C8 120.5(4) . . ?
C6 C5 C4 120.4(4) . . ?
C5 C6 C7 120.0(4) . . ?
C6 C7 C2 120.4(4) . . ?
O4 C8 O3 124.4(4) . . ?
O4 C8 C4 118.4(3) . . ?
O3 C8 C4 117.1(3) . . ?
O5 C9 O6 123.7(4) . . ?
O5 C9 C10 118.5(4) . . ?
O6 C9 C10 117.8(3) . . ?
C15 C10 C11 119.3(4) . . ?
C15 C10 C9 120.1(3) . . ?
C11 C10 C9 120.5(3) . . ?
C10 C11 C12 120.3(4) . . ?
C13 C12 C11 119.1(4) . . ?
C13 C12 C16 121.7(3) . . ?
C11 C12 C16 119.1(3) . . ?
C14 C13 C12 120.6(4) . . ?
C15 C14 C13 120.1(4) . . ?
C14 C15 C10 120.5(4) . . ?
O8 C16 O7 120.6(4) . . ?
O8 C16 C12 120.6(3) . . ?
O7 C16 C12 118.8(3) . . ?
O8 C16 Ce2 56.0(2) . 2_777 ?
O7 C16 Ce2 64.7(2) . 2_777 ?
C12 C16 Ce2 173.1(3) . 2_777 ?
O9 C17 O10 120.2(3) . . ?
O9 C17 C18 120.4(3) . . ?
O10 C17 C18 119.3(3) . . ?
C23 C18 C19 118.9(3) . . ?
C23 C18 C17 121.4(3) . . ?
C19 C18 C17 119.7(3) . . ?
C20 C19 C18 120.5(3) . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 C24 118.7(3) . . ?
C21 C20 C24 121.6(3) . . ?
C22 C21 C20 120.3(4) . . ?
C21 C22 C23 119.9(4) . . ?
C22 C23 C18 120.8(4) . . ?
O11 C24 O12 125.1(3) . . ?
O11 C24 C20 118.0(3) . . ?
O12 C24 C20 116.9(3) . . ?
O14 C25 O13 126.8(3) 2_667 . ?
O14 C25 C25 117.1(4) 2_667 2_667 ?
O13 C25 C25 116.1(4) . 2_667 ?
O1 Ce1 O11 71.35(10) . 1_655 ?
O1 Ce1 O12 79.67(10) . 2_566 ?
O11 Ce1 O12 123.55(10) 1_655 2_566 ?
O1 Ce1 O2 120.75(10) . 2_666 ?
O11 Ce1 O2 82.31(10) 1_655 2_666 ?
O12 Ce1 O2 72.46(10) 2_566 2_666 ?
O1 Ce1 O10 74.51(10) . . ?
O11 Ce1 O10 138.15(10) 1_655 . ?
O12 Ce1 O10 71.72(9) 2_566 . ?
O2 Ce1 O10 137.09(9) 2_666 . ?
O1 Ce1 O7 94.71(11) . 2_777 ?
O11 Ce1 O7 93.05(11) 1_655 2_777 ?
O12 Ce1 O7 137.52(10) 2_566 2_777 ?
O2 Ce1 O7 139.82(10) 2_666 2_777 ?
O10 Ce1 O7 66.26(9) . 2_777 ?
O1 Ce1 O1W 140.41(10) . . ?
O11 Ce1 O1W 73.37(10) 1_655 . ?
O12 Ce1 O1W 136.34(10) 2_566 . ?
O2 Ce1 O1W 70.72(10) 2_666 . ?
O10 Ce1 O1W 125.30(9) . . ?
O7 Ce1 O1W 69.73(10) 2_777 . ?
O1 Ce1 O13 141.17(9) . . ?
O11 Ce1 O13 144.66(9) 1_655 . ?
O12 Ce1 O13 83.97(9) 2_566 . ?
O2 Ce1 O13 86.57(9) 2_666 . ?
O10 Ce1 O13 66.94(9) . . ?
O7 Ce1 O13 74.41(9) 2_777 . ?
O1W Ce1 O13 71.29(9) . . ?
O3 Ce2 O4 84.13(10) 1_556 2_676 ?
O3 Ce2 O5 78.87(11) 1_556 . ?
O4 Ce2 O5 145.02(10) 2_676 . ?
O3 Ce2 O14 87.14(10) 1_556 . ?
O4 Ce2 O14 130.99(10) 2_676 . ?
O5 Ce2 O14 78.67(10) . . ?
O3 Ce2 O8 79.11(10) 1_556 2_777 ?
O4 Ce2 O8 72.50(11) 2_676 2_777 ?
O5 Ce2 O8 74.38(10) . 2_777 ?
O14 Ce2 O8 151.60(10) . 2_777 ?
O3 Ce2 O9 121.34(10) 1_556 . ?
O4 Ce2 O9 70.97(10) 2_676 . ?
O5 Ce2 O9 143.62(10) . . ?
O14 Ce2 O9 73.12(9) . . ?
O8 Ce2 O9 135.16(10) 2_777 . ?
O3 Ce2 O13 142.43(10) 1_556 . ?
O4 Ce2 O13 132.24(9) 2_676 . ?
O5 Ce2 O13 73.75(9) . . ?
O14 Ce2 O13 62.79(8) . . ?
O8 Ce2 O13 116.51(9) 2_777 . ?
O9 Ce2 O13 73.14(9) . . ?
O3 Ce2 O10 152.13(10) 1_556 . ?
O4 Ce2 O10 68.03(9) 2_676 . ?
O5 Ce2 O10 125.17(9) . . ?
O14 Ce2 O10 109.71(9) . . ?
O8 Ce2 O10 93.24(9) 2_777 . ?
O9 Ce2 O10 49.05(8) . . ?
O13 Ce2 O10 64.77(8) . . ?
O3 Ce2 O7 125.04(10) 1_556 2_777 ?
O4 Ce2 O7 92.23(10) 2_676 2_777 ?
O5 Ce2 O7 73.58(10) . 2_777 ?
O14 Ce2 O7 130.70(9) . 2_777 ?
O8 Ce2 O7 48.18(9) 2_777 2_777 ?
O9 Ce2 O7 108.62(9) . 2_777 ?
O13 Ce2 O7 70.65(8) . 2_777 ?
O10 Ce2 O7 60.13(8) . 2_777 ?
O3 Ce2 C16 101.25(11) 1_556 2_777 ?
O4 Ce2 C16 82.34(10) 2_676 2_777 ?
O5 Ce2 C16 71.46(10) . 2_777 ?
O14 Ce2 C16 146.54(10) . 2_777 ?
O8 Ce2 C16 23.43(10) 2_777 2_777 ?
O9 Ce2 C16 125.45(9) . 2_777 ?
O13 Ce2 C16 93.97(9) . 2_777 ?
O10 Ce2 C16 77.17(9) . 2_777 ?
O7 Ce2 C16 24.78(9) 2_777 2_777 ?
O3 Ce2 K1 71.65(8) 1_556 2_667 ?
O4 Ce2 K1 94.58(8) 2_676 2_667 ?
O5 Ce2 K1 108.46(8) . 2_667 ?
O14 Ce2 K1 37.51(6) . 2_667 ?
O8 Ce2 K1 149.16(7) 2_777 2_667 ?
O9 Ce2 K1 59.10(6) . 2_667 ?
O13 Ce2 K1 93.09(6) . 2_667 ?
O10 Ce2 K1 108.02(6) . 2_667 ?
O7 Ce2 K1 162.63(6) 2_777 2_667 ?
C16 Ce2 K1 172.58(7) 2_777 2_667 ?
O3W K1 O2 123.89(12) . 2_666 ?
O3W K1 O6 95.27(13) . 2_767 ?
O2 K1 O6 118.64(11) 2_666 2_767 ?
O3W K1 O2W 85.80(12) . . ?
O2 K1 O2W 133.40(10) 2_666 . ?
O6 K1 O2W 89.15(10) 2_767 . ?
O3W K1 O1W 154.25(11) . . ?
O2 K1 O1W 64.65(9) 2_666 . ?
O6 K1 O1W 100.65(10) 2_767 . ?
O2W K1 O1W 74.42(10) . . ?
O3W K1 O14 73.61(11) . 2_667 ?
O2 K1 O14 76.70(9) 2_666 2_667 ?
O6 K1 O14 164.63(10) 2_767 2_667 ?
O2W K1 O14 79.63(9) . 2_667 ?
O1W K1 O14 86.52(9) . 2_667 ?
O3W K1 Ce2 41.49(10) . 2_667 ?
O2 K1 Ce2 99.47(7) 2_666 2_667 ?
O6 K1 Ce2 135.46(8) 2_767 2_667 ?
O2W K1 Ce2 79.39(7) . 2_667 ?
O1W K1 Ce2 116.86(7) . 2_667 ?
O14 K1 Ce2 32.16(5) 2_667 2_667 ?
O3W K1 K1 121.60(10) . 2_767 ?
O2 K1 K1 113.70(7) 2_666 2_767 ?
O6 K1 K1 62.72(7) 2_767 2_767 ?
O2W K1 K1 44.45(7) . 2_767 ?
O1W K1 K1 52.00(6) . 2_767 ?
O14 K1 K1 113.68(7) 2_667 2_767 ?
Ce2 K1 K1 123.49(3) 2_667 2_767 ?
C1 O1 Ce1 163.7(3) . . ?
C1 O2 Ce1 110.5(2) . 2_666 ?
C1 O2 K1 137.7(2) . 2_666 ?
Ce1 O2 K1 111.64(10) 2_666 2_666 ?
C8 O3 Ce2 176.0(3) . 1_554 ?
C8 O4 Ce2 134.1(3) . 2_676 ?
C9 O5 Ce2 141.5(3) . . ?
C9 O6 K1 147.9(3) . 2_767 ?
C16 O7 Ce1 166.0(3) . 2_777 ?
C16 O7 Ce2 90.5(2) . 2_777 ?
Ce1 O7 Ce2 99.53(9) 2_777 2_777 ?
C16 O8 Ce2 100.6(2) . 2_777 ?
C17 O9 Ce2 95.1(2) . . ?
C17 O10 Ce1 138.3(2) . . ?
C17 O10 Ce2 91.3(2) . . ?
Ce1 O10 Ce2 102.01(9) . . ?
C24 O11 Ce1 141.6(2) . 1_455 ?
C24 O12 Ce1 142.4(3) . 2_566 ?
C25 O13 Ce2 120.2(2) . . ?
C25 O13 Ce1 139.9(2) . . ?
Ce2 O13 Ce1 99.49(9) . . ?
C25 O14 Ce2 123.3(2) 2_667 . ?
C25 O14 K1 117.5(2) 2_667 2_667 ?
Ce2 O14 K1 110.33(10) . 2_667 ?
Ce1 O1W K1 103.94(10) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.080
_refine_diff_density_min         -2.218
_refine_diff_density_rms         0.245

data_10
_database_code_depnum_ccdc_archive 'CCDC 715649'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C25 H18 K O17 Pr2'
_chemical_formula_sum            'C25 H18 K O17 Pr2'
_chemical_formula_weight         911.31

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.3647(7)
_cell_length_b                   11.5338(8)
_cell_length_c                   12.2664(8)
_cell_angle_alpha                82.0820(10)
_cell_angle_beta                 65.0190(10)
_cell_angle_gamma                84.3190(10)
_cell_volume                     1315.16(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6512
_cell_measurement_theta_min      1.78
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             882
_exptl_absorpt_coefficient_mu    3.908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4130
_exptl_absorpt_correction_T_max  0.6770
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens Smart CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9690
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         28.29
_reflns_number_total             6512
_reflns_number_gt                5876
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_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)+(0.0416P)²+7.4554P] 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         6512
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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 0.3975(5) 0.6265(4) 0.3449(4) 0.0167(8) Uani 1 1 d . . .
C2 C 0.5405(5) 0.5670(4) 0.3177(4) 0.0174(8) Uani 1 1 d . . .
C3 C 0.6651(5) 0.6254(4) 0.2484(5) 0.0248(10) Uani 1 1 d . . .
H3 H 0.6606 0.7038 0.2192 0.030 Uiso 1 1 calc R . .
C4 C 0.7975(6) 0.5658(5) 0.2226(5) 0.0310(11) Uani 1 1 d . . .
H4 H 0.8810 0.6036 0.1732 0.037 Uiso 1 1 calc R . .
C5 C 0.8043(5) 0.4504(4) 0.2705(5) 0.0244(10) Uani 1 1 d . . .
H5 H 0.8925 0.4116 0.2538 0.029 Uiso 1 1 calc R . .
C6 C 0.6803(5) 0.3921(4) 0.3436(4) 0.0180(8) Uani 1 1 d . . .
C7 C 0.6869(5) 0.2697(4) 0.4029(4) 0.0188(8) Uani 1 1 d . . .
C8 C 0.5483(5) 0.4500(4) 0.3647(4) 0.0186(8) Uani 1 1 d . . .
H8 H 0.4650 0.4105 0.4104 0.022 Uiso 1 1 calc R . .
C9 C 0.0829(5) 0.4887(4) 0.3169(4) 0.0171(8) Uani 1 1 d . . .
C10 C 0.1952(5) 0.4504(4) 0.2026(4) 0.0196(8) Uani 1 1 d . . .
C11 C 0.2348(6) 0.5229(4) 0.0938(5) 0.0294(11) Uani 1 1 d . . .
H11 H 0.1909 0.5971 0.0924 0.035 Uiso 1 1 calc R . .
C12 C 0.3379(7) 0.4858(5) -0.0110(5) 0.0339(12) Uani 1 1 d . . .
H12 H 0.3601 0.5335 -0.0835 0.041 Uiso 1 1 calc R . .
C13 C 0.4097(6) 0.3771(4) -0.0099(4) 0.0282(11) Uani 1 1 d . . .
H13 H 0.4813 0.3531 -0.0808 0.034 Uiso 1 1 calc R . .
C14 C 0.3729(5) 0.3048(4) 0.0987(4) 0.0182(8) Uani 1 1 d . . .
C15 C 0.2642(5) 0.3407(4) 0.2045(4) 0.0189(8) Uani 1 1 d . . .
H15 H 0.2377 0.2913 0.2763 0.023 Uiso 1 1 calc R . .
C16 C 0.4449(4) 0.1875(4) 0.1042(4) 0.0156(8) Uani 1 1 d . . .
C17 C 0.0782(4) 0.8288(3) 0.2091(4) 0.0140(7) Uani 1 1 d . . .
C18 C 0.0567(4) 0.8366(4) 0.0951(4) 0.0154(8) Uani 1 1 d . . .
C19 C 0.1710(5) 0.8180(4) -0.0143(4) 0.0183(8) Uani 1 1 d . . .
H19 H 0.2618 0.8009 -0.0170 0.022 Uiso 1 1 calc R . .
C20 C 0.1498(5) 0.8249(5) -0.1194(4) 0.0242(9) Uani 1 1 d . . .
H20 H 0.2260 0.8096 -0.1917 0.029 Uiso 1 1 calc R . .
C21 C 0.0160(5) 0.8545(4) -0.1174(4) 0.0212(9) Uani 1 1 d . . .
H21 H 0.0027 0.8616 -0.1885 0.025 Uiso 1 1 calc R . .
C22 C -0.0996(4) 0.8738(4) -0.0071(4) 0.0150(8) Uani 1 1 d . . .
C23 C -0.2428(4) 0.9156(4) -0.0041(4) 0.0155(8) Uani 1 1 d . . .
C24 C -0.0789(4) 0.8636(4) 0.0976(4) 0.0150(8) Uani 1 1 d . . .
H24 H -0.1559 0.8748 0.1707 0.018 Uiso 1 1 calc R . .
C25 C -0.0726(4) 0.9777(4) 0.5503(4) 0.0136(7) Uani 1 1 d . . .
K1 K 0.3734(2) 1.15344(19) 0.41305(19) 0.0687(5) Uani 1 1 d . . .
O1 O 0.2875(4) 0.5708(3) 0.4051(3) 0.0245(7) Uani 1 1 d . . .
O2 O 0.3882(4) 0.7352(3) 0.3077(3) 0.0220(7) Uani 1 1 d . . .
O3 O 0.7964(4) 0.2376(3) 0.4217(3) 0.0250(7) Uani 1 1 d . . .
O4 O 0.5854(4) 0.2055(3) 0.4307(4) 0.0297(8) Uani 1 1 d . . .
O5 O 0.0514(4) 0.5959(3) 0.3237(3) 0.0211(6) Uani 1 1 d . . .
O6 O 0.0240(4) 0.4100(3) 0.4012(3) 0.0258(7) Uani 1 1 d . . .
O7 O 0.2017(3) 0.8070(3) 0.2057(3) 0.0163(6) Uani 1 1 d . . .
O8 O -0.0276(3) 0.8391(3) 0.3080(3) 0.0194(6) Uani 1 1 d . . .
O9 O 0.4232(4) 0.1325(3) 0.2072(3) 0.0199(6) Uani 1 1 d . . .
O10 O 0.5220(3) 0.1429(3) 0.0077(3) 0.0222(7) Uani 1 1 d . . .
O11 O -0.2483(3) 0.9536(3) -0.1028(3) 0.0186(6) Uani 1 1 d . . .
O12 O -0.3467(3) 0.9109(3) 0.0989(3) 0.0222(7) Uani 1 1 d . . .
O13 O -0.0911(4) 0.8710(3) 0.5648(3) 0.0219(7) Uani 1 1 d . . .
O14 O -0.1617(3) 1.0552(3) 0.6073(3) 0.0164(6) Uani 1 1 d . . .
O15 O 0.4732(4) 0.9469(3) 0.3587(3) 0.0220(7) Uani 1 1 d . . .
O16 O 0.2786(4) 1.0352(3) 0.6058(3) 0.0308(8) Uani 1 1 d . . .
O17 O 0.2262(5) 1.3166(4) 0.5066(4) 0.0356(9) Uani 1 1 d . . .
Pr1 Pr 0.39826(2) 0.927130(18) 0.186756(19) 0.01171(7) Uani 1 1 d . . .
Pr2 Pr 0.09399(2) 0.730313(18) 0.440322(19) 0.01398(7) 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 O1 1.249(6) . ?
C1 O2 1.282(5) . ?
C1 C2 1.492(6) . ?
C2 C3 1.390(7) . ?
C2 C8 1.402(6) . ?
C3 C4 1.401(7) . ?
C4 C5 1.387(7) . ?
C5 C6 1.392(7) . ?
C6 C8 1.397(6) . ?
C6 C7 1.505(6) . ?
C7 O4 1.247(6) . ?
C7 O3 1.262(6) . ?
C9 O5 1.252(5) . ?
C9 O6 1.259(5) . ?
C9 C10 1.485(6) . ?
C10 C15 1.392(6) . ?
C10 C11 1.395(6) . ?
C11 C12 1.371(7) . ?
C12 C13 1.395(7) . ?
C13 C14 1.393(6) . ?
C14 C15 1.395(6) . ?
C14 C16 1.486(6) . ?
C16 O10 1.262(5) . ?
C16 O9 1.272(5) . ?
C16 Pr1 3.052(4) 1_545 ?
C16 K1 3.512(5) 1_545 ?
C17 O8 1.257(5) . ?
C17 O7 1.264(5) . ?
C17 C18 1.496(6) . ?
C18 C19 1.392(6) . ?
C18 C24 1.398(6) . ?
C19 C20 1.386(6) . ?
C20 C21 1.387(7) . ?
C21 C22 1.406(6) . ?
C22 C24 1.376(6) . ?
C22 C23 1.502(6) . ?
C23 O11 1.251(5) . ?
C23 O12 1.266(5) . ?
C25 O13 1.240(5) . ?
C25 O14 1.267(5) . ?
C25 C25 1.569(8) 2_576 ?
C25 K1 3.431(5) 2_576 ?
K1 O17 2.395(4) . ?
K1 O9 2.397(4) 1_565 ?
K1 O16 2.414(4) . ?
K1 O4 2.436(4) 1_565 ?
K1 O15 2.561(4) . ?
K1 O13 2.861(4) 2_576 ?
K1 C25 3.431(5) 2_576 ?
K1 C16 3.512(5) 1_565 ?
K1 Pr2 4.530(2) 2_576 ?
K1 K1 4.978(4) 2_676 ?
O1 Pr2 2.520(3) . ?
O2 Pr1 2.474(3) . ?
O2 Pr2 2.787(4) . ?
O3 Pr2 2.484(3) 2_666 ?
O4 K1 2.436(4) 1_545 ?
O5 Pr2 2.434(3) . ?
O6 Pr2 2.326(3) 2_566 ?
O7 Pr1 2.489(3) . ?
O7 Pr2 2.663(3) . ?
O8 Pr2 2.579(3) . ?
O9 K1 2.397(4) 1_545 ?
O9 Pr1 2.465(3) 1_545 ?
O10 Pr1 2.400(3) 2_665 ?
O11 Pr1 2.431(3) 2_575 ?
O12 Pr1 2.395(3) 1_455 ?
O13 Pr2 2.498(3) . ?
O13 K1 2.861(4) 2_576 ?
O14 Pr2 2.560(3) 2_576 ?
O14 Pr1 2.692(3) 2_576 ?
O15 Pr1 2.580(3) . ?
Pr1 O12 2.395(3) 1_655 ?
Pr1 O10 2.400(3) 2_665 ?
Pr1 O11 2.431(3) 2_575 ?
Pr1 O9 2.465(3) 1_565 ?
Pr1 O14 2.692(3) 2_576 ?
Pr1 C16 3.052(4) 1_565 ?
Pr2 O6 2.326(3) 2_566 ?
Pr2 O3 2.484(4) 2_666 ?
Pr2 O14 2.560(3) 2_576 ?
Pr2 K1 4.530(2) 2_576 ?

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
O1 C1 O2 120.4(4) . . ?
O1 C1 C2 119.9(4) . . ?
O2 C1 C2 119.7(4) . . ?
C3 C2 C8 119.7(4) . . ?
C3 C2 C1 121.5(4) . . ?
C8 C2 C1 118.8(4) . . ?
C2 C3 C4 119.8(4) . . ?
C5 C4 C3 120.0(5) . . ?
C4 C5 C6 120.7(4) . . ?
C5 C6 C8 119.1(4) . . ?
C5 C6 C7 120.9(4) . . ?
C8 C6 C7 119.9(4) . . ?
O4 C7 O3 123.4(4) . . ?
O4 C7 C6 119.0(4) . . ?
O3 C7 C6 117.6(4) . . ?
C6 C8 C2 120.5(4) . . ?
O5 C9 O6 124.0(4) . . ?
O5 C9 C10 118.8(4) . . ?
O6 C9 C10 117.2(4) . . ?
C15 C10 C11 119.3(4) . . ?
C15 C10 C9 119.3(4) . . ?
C11 C10 C9 121.3(4) . . ?
C12 C11 C10 120.6(5) . . ?
C11 C12 C13 120.6(5) . . ?
C14 C13 C12 119.3(5) . . ?
C13 C14 C15 120.1(4) . . ?
C13 C14 C16 121.2(4) . . ?
C15 C14 C16 118.6(4) . . ?
C10 C15 C14 120.1(4) . . ?
O10 C16 O9 121.3(4) . . ?
O10 C16 C14 119.9(4) . . ?
O9 C16 C14 118.8(4) . . ?
O10 C16 Pr1 78.8(3) . 1_545 ?
O9 C16 Pr1 51.3(2) . 1_545 ?
C14 C16 Pr1 144.7(3) . 1_545 ?
O10 C16 K1 140.6(3) . 1_545 ?
O9 C16 K1 23.27(19) . 1_545 ?
C14 C16 K1 98.4(3) . 1_545 ?
Pr1 C16 K1 74.28(10) 1_545 1_545 ?
O8 C17 O7 120.6(4) . . ?
O8 C17 C18 119.6(4) . . ?
O7 C17 C18 119.7(4) . . ?
C19 C18 C24 119.3(4) . . ?
C19 C18 C17 120.6(4) . . ?
C24 C18 C17 120.0(4) . . ?
C20 C19 C18 120.2(4) . . ?
C19 C20 C21 120.5(4) . . ?
C20 C21 C22 119.4(4) . . ?
C24 C22 C21 119.9(4) . . ?
C24 C22 C23 119.5(4) . . ?
C21 C22 C23 120.4(4) . . ?
O11 C23 O12 126.1(4) . . ?
O11 C23 C22 117.4(4) . . ?
O12 C23 C22 116.5(4) . . ?
C22 C24 C18 120.6(4) . . ?
O13 C25 O14 126.1(4) . . ?
O13 C25 C25 117.6(4) . 2_576 ?
O14 C25 C25 116.3(4) . 2_576 ?
O13 C25 K1 53.0(2) . 2_576 ?
O14 C25 K1 83.2(2) . 2_576 ?
C25 C25 K1 141.5(3) 2_576 2_576 ?
O17 K1 O9 119.49(16) . 1_565 ?
O17 K1 O16 89.34(15) . . ?
O9 K1 O16 137.05(16) 1_565 . ?
O17 K1 O4 95.68(16) . 1_565 ?
O9 K1 O4 110.98(15) 1_565 1_565 ?
O16 K1 O4 95.47(15) . 1_565 ?
O17 K1 O15 163.95(16) . . ?
O9 K1 O15 68.51(12) 1_565 . ?
O16 K1 O15 76.84(13) . . ?
O4 K1 O15 93.75(14) 1_565 . ?
O17 K1 O13 71.51(14) . 2_576 ?
O9 K1 O13 79.96(12) 1_565 2_576 ?
O16 K1 O13 80.45(13) . 2_576 ?
O4 K1 O13 166.49(15) 1_565 2_576 ?
O15 K1 O13 97.81(12) . 2_576 ?
O17 K1 C25 88.96(14) . 2_576 ?
O9 K1 C25 79.13(12) 1_565 2_576 ?
O16 K1 C25 69.67(13) . 2_576 ?
O4 K1 C25 164.44(14) 1_565 2_576 ?
O15 K1 C25 78.70(12) . 2_576 ?
O13 K1 C25 20.25(10) 2_576 2_576 ?
O17 K1 C16 109.31(14) . 1_565 ?
O9 K1 C16 12.10(10) 1_565 1_565 ?
O16 K1 C16 148.24(15) . 1_565 ?
O4 K1 C16 107.51(14) 1_565 1_565 ?
O15 K1 C16 80.00(11) . 1_565 ?
O13 K1 C16 81.50(11) 2_576 1_565 ?
C25 K1 C16 84.76(11) 2_576 1_565 ?
O17 K1 Pr2 42.14(11) . 2_576 ?
O9 K1 Pr2 101.43(10) 1_565 2_576 ?
O16 K1 Pr2 78.28(10) . 2_576 ?
O4 K1 Pr2 136.71(12) 1_565 2_576 ?
O15 K1 Pr2 125.22(11) . 2_576 ?
O13 K1 Pr2 29.92(7) 2_576 2_576 ?
C25 K1 Pr2 46.91(7) 2_576 2_576 ?
C16 K1 Pr2 98.16(8) 1_565 2_576 ?
O17 K1 K1 127.78(14) . 2_676 ?
O9 K1 K1 112.64(11) 1_565 2_676 ?
O16 K1 K1 51.60(10) . 2_676 ?
O4 K1 K1 61.54(10) 1_565 2_676 ?
O15 K1 K1 47.78(8) . 2_676 ?
O13 K1 K1 122.72(11) 2_576 2_676 ?
C25 K1 K1 104.05(10) 2_576 2_676 ?
C16 K1 K1 121.97(10) 1_565 2_676 ?
Pr2 K1 K1 129.79(7) 2_576 2_676 ?
C1 O1 Pr2 102.1(3) . . ?
C1 O2 Pr1 166.0(3) . . ?
C1 O2 Pr2 88.5(3) . . ?
Pr1 O2 Pr2 98.65(11) . . ?
C7 O3 Pr2 139.7(3) . 2_666 ?
C7 O4 K1 152.0(3) . 1_545 ?
C9 O5 Pr2 130.4(3) . . ?
C9 O6 Pr2 177.5(3) . 2_566 ?
C17 O7 Pr1 135.2(3) . . ?
C17 O7 Pr2 91.2(2) . . ?
Pr1 O7 Pr2 101.64(10) . . ?
C17 O8 Pr2 95.3(2) . . ?
C16 O9 K1 144.6(3) . 1_545 ?
C16 O9 Pr1 105.0(3) . 1_545 ?
K1 O9 Pr1 109.90(13) 1_545 1_545 ?
C16 O10 Pr1 161.8(3) . 2_665 ?
C23 O11 Pr1 141.8(3) . 2_575 ?
C23 O12 Pr1 139.8(3) . 1_455 ?
C25 O13 Pr2 122.0(3) . . ?
C25 O13 K1 106.7(3) . 2_576 ?
Pr2 O13 K1 115.24(13) . 2_576 ?
C25 O14 Pr2 119.4(3) . 2_576 ?
C25 O14 Pr1 139.6(3) . 2_576 ?
Pr2 O14 Pr1 99.01(10) 2_576 2_576 ?
K1 O15 Pr1 101.46(12) . . ?
O12 Pr1 O10 71.51(11) 1_655 2_665 ?
O12 Pr1 O11 126.80(11) 1_655 2_575 ?
O10 Pr1 O11 78.46(11) 2_665 2_575 ?
O12 Pr1 O9 86.23(12) 1_655 1_565 ?
O10 Pr1 O9 121.64(11) 2_665 1_565 ?
O11 Pr1 O9 73.48(11) 2_575 1_565 ?
O12 Pr1 O2 90.42(12) 1_655 . ?
O10 Pr1 O2 97.99(12) 2_665 . ?
O11 Pr1 O2 137.28(11) 2_575 . ?
O9 Pr1 O2 136.43(11) 1_565 . ?
O12 Pr1 O7 136.36(11) 1_655 . ?
O10 Pr1 O7 75.51(11) 2_665 . ?
O11 Pr1 O7 71.40(10) 2_575 . ?
O9 Pr1 O7 136.16(11) 1_565 . ?
O2 Pr1 O7 66.60(11) . . ?
O12 Pr1 O15 74.08(11) 1_655 . ?
O10 Pr1 O15 143.44(11) 2_665 . ?
O11 Pr1 O15 133.94(11) 2_575 . ?
O9 Pr1 O15 67.20(11) 1_565 . ?
O2 Pr1 O15 70.13(11) . . ?
O7 Pr1 O15 125.12(10) . . ?
O12 Pr1 O14 145.33(10) 1_655 2_576 ?
O10 Pr1 O14 140.72(10) 2_665 2_576 ?
O11 Pr1 O14 81.38(10) 2_575 2_576 ?
O9 Pr1 O14 83.42(10) 1_565 2_576 ?
O2 Pr1 O14 75.10(10) . 2_576 ?
O7 Pr1 O14 66.20(10) . 2_576 ?
O15 Pr1 O14 71.40(10) . 2_576 ?
O12 Pr1 C16 83.62(12) 1_655 1_565 ?
O10 Pr1 C16 98.78(12) 2_665 1_565 ?
O11 Pr1 C16 58.60(11) 2_575 1_565 ?
O9 Pr1 C16 23.74(11) 1_565 1_565 ?
O2 Pr1 C16 159.38(11) . 1_565 ?
O7 Pr1 C16 129.64(11) . 1_565 ?
O15 Pr1 C16 89.25(11) . 1_565 ?
O14 Pr1 C16 98.90(10) 2_576 1_565 ?
O6 Pr2 O5 81.80(12) 2_566 . ?
O6 Pr2 O3 81.50(13) 2_566 2_666 ?
O5 Pr2 O3 147.92(11) . 2_666 ?
O6 Pr2 O13 84.78(11) 2_566 . ?
O5 Pr2 O13 124.02(12) . . ?
O3 Pr2 O13 81.32(12) 2_666 . ?
O6 Pr2 O1 79.60(12) 2_566 . ?
O5 Pr2 O1 74.12(12) . . ?
O3 Pr2 O1 76.05(12) 2_666 . ?
O13 Pr2 O1 154.09(12) . . ?
O6 Pr2 O14 142.73(11) 2_566 2_576 ?
O5 Pr2 O14 132.43(11) . 2_576 ?
O3 Pr2 O14 73.58(11) 2_666 2_576 ?
O13 Pr2 O14 64.66(10) . 2_576 ?
O1 Pr2 O14 119.22(11) . 2_576 ?
O6 Pr2 O8 121.03(12) 2_566 . ?
O5 Pr2 O8 69.13(11) . . ?
O3 Pr2 O8 142.60(11) 2_666 . ?
O13 Pr2 O8 72.49(11) . . ?
O1 Pr2 O8 133.40(11) . . ?
O14 Pr2 O8 71.26(10) 2_576 . ?
O6 Pr2 O7 150.57(11) 2_566 . ?
O5 Pr2 O7 68.79(10) . . ?
O3 Pr2 O7 123.58(11) 2_666 . ?
O13 Pr2 O7 112.04(10) . . ?
O1 Pr2 O7 91.17(11) . . ?
O14 Pr2 O7 65.70(10) 2_576 . ?
O8 Pr2 O7 49.36(9) . . ?
O6 Pr2 O2 125.43(11) 2_566 . ?
O5 Pr2 O2 96.61(11) . . ?
O3 Pr2 O2 71.66(11) 2_666 . ?
O13 Pr2 O2 133.93(10) . . ?
O1 Pr2 O2 48.59(10) . . ?
O14 Pr2 O2 72.14(9) 2_576 . ?
O8 Pr2 O2 108.48(10) . . ?
O7 Pr2 O2 59.95(9) . . ?
O6 Pr2 K1 73.92(10) 2_566 2_576 ?
O5 Pr2 K1 89.39(9) . 2_576 ?
O3 Pr2 K1 111.82(9) 2_666 2_576 ?
O13 Pr2 K1 34.85(9) . 2_576 ?
O1 Pr2 K1 150.55(8) . 2_576 ?
O14 Pr2 K1 89.97(7) 2_576 2_576 ?
O8 Pr2 K1 56.35(7) . 2_576 ?
O7 Pr2 K1 105.64(7) . 2_576 ?
O2 Pr2 K1 160.31(7) . 2_576 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.049
_refine_diff_density_min         -2.474
_refine_diff_density_rms         0.194


