# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_year                    2010
_journal_volume                  12
_journal_page_first              774

_publ_contact_author_name        'Liya Wang'
_publ_contact_author_email       WLYA@LYNU.EDU.CN

_publ_section_title              
;
Series of anion-directed lanthanide-rigid-flexible
frameworks: syntheses, structures, luminescence and magnetic properties
;
loop_
_publ_author_name
'Xun Feng'
'Li-Ya Wang'
'Jian-She Zhao'
'Jian-Ge Wang'
'Seik Weng Ng'
'Bin Liu'
'Xin-Ge Shi'

# Attachment '3A.cif'

data_3a
_database_code_depnum_ccdc_archive 'CCDC 725360'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H34 N2 O38 Sm4'
_chemical_formula_weight         1535.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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                   8.2591(17)
_cell_length_b                   10.651(2)
_cell_length_c                   13.120(3)
_cell_angle_alpha                93.858(2)
_cell_angle_beta                 103.532(2)
_cell_angle_gamma                107.906(2)
_cell_volume                     1055.5(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    3833
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.19

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_absorpt_coefficient_mu    5.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2445
_exptl_absorpt_correction_T_max  0.4157
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7897
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3897
_reflns_number_gt                3403
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0275P)²+0.5468P] 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         3897
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0601
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
Sm1 Sm 0.72321(3) 0.320860(19) 0.104615(16) 0.01382(7) Uani 1 1 d . . .
Sm2 Sm 1.17397(3) -0.02848(2) 0.311834(17) 0.01452(7) Uani 1 1 d . . .
O1 O 0.5501(4) 0.1815(3) 0.2097(2) 0.0254(7) Uani 1 1 d . . .
O2 O 0.4605(4) 0.1436(3) 0.3563(3) 0.0293(8) Uani 1 1 d . . .
O3 O 0.9233(4) 0.5520(3) 0.1629(2) 0.0246(7) Uani 1 1 d . . .
O4 O 1.0394(4) 0.7417(3) 0.2745(3) 0.0312(8) Uani 1 1 d . . .
O5 O 0.6640(4) 0.4535(3) -0.0389(2) 0.0222(7) Uani 1 1 d . . .
O6 O 0.5207(4) 0.5896(3) -0.1057(2) 0.0231(7) Uani 1 1 d . . .
O7 O 0.7642(4) 0.0929(3) 0.0916(2) 0.0213(7) Uani 1 1 d . . .
O8 O 0.9325(4) -0.0265(3) 0.1614(2) 0.0208(7) Uani 1 1 d . . .
O9 O 0.9887(4) 0.3103(3) 0.2289(2) 0.0253(7) Uani 1 1 d . . .
O10 O 1.1330(4) 0.1839(3) 0.3105(3) 0.0347(9) Uani 1 1 d . . .
O11 O 1.2207(4) 0.0267(3) 0.5016(2) 0.0282(8) Uani 1 1 d . . .
O12 O 1.1028(4) 0.0697(3) 0.6320(2) 0.0296(8) Uani 1 1 d . . .
O13 O 0.4842(4) 0.1689(3) -0.0390(2) 0.0303(8) Uani 1 1 d . . .
H1W H 0.4162 0.0923 -0.0429 0.045 Uiso 1 1 d R . .
H2W H 0.4745 0.1951 -0.0972 0.045 Uiso 1 1 d R . .
O14 O 0.9096(4) 0.3152(3) -0.0148(3) 0.0284(8) Uani 1 1 d . . .
H3W H 0.9871 0.2806 0.0047 0.043 Uiso 1 1 d R . .
H4W H 0.9391 0.3716 -0.0535 0.043 Uiso 1 1 d R . .
O15 O 1.2846(4) -0.0592(3) 0.1621(3) 0.0349(9) Uani 1 1 d . . .
H5W H 1.2352 -0.1158 0.1083 0.052 Uiso 1 1 d R . .
H6W H 1.3743 -0.0022 0.1555 0.052 Uiso 1 1 d R . .
O16 O 1.3936(5) -0.1344(4) 0.3906(3) 0.0478(11) Uani 1 1 d . . .
H7W H 1.4139 -0.1912 0.3540 0.072 Uiso 1 1 d R . .
H8W H 1.4856 -0.0754 0.4252 0.072 Uiso 1 1 d R . .
O17 O 0.8554(4) 0.8074(3) -0.0395(3) 0.0346(8) Uani 1 1 d . . .
H10W H 0.7542 0.7530 -0.0651 0.052 Uiso 1 1 d R . .
H9W H 0.8573 0.8618 0.0095 0.052 Uiso 1 1 d R . .
O18 O 1.6534(7) 0.4584(7) 0.7240(4) 0.123(3) Uani 1 1 d . . .
H12W H 1.5994 0.5081 0.7350 0.184 Uiso 1 1 d R . .
H11W H 1.7603 0.4983 0.7333 0.184 Uiso 1 1 d R . .
O19 O 1.4147(9) 0.2419(6) 0.7683(4) 0.152(4) Uani 1 1 d . . .
H13W H 1.3106 0.2092 0.7314 0.227 Uiso 1 1 d R . .
H14W H 1.4717 0.3051 0.7431 0.227 Uiso 1 1 d R . .
N1 N 0.7524(5) 0.4268(3) 0.2925(3) 0.0175(8) Uani 1 1 d . . .
C1 C 0.6620(6) 0.3565(4) 0.3544(3) 0.0211(10) Uani 1 1 d . . .
C2 C 0.6730(7) 0.4133(5) 0.4553(4) 0.0360(13) Uani 1 1 d . . .
H2 H 0.6093 0.3636 0.4974 0.043 Uiso 1 1 calc R . .
C3 C 0.7794(8) 0.5440(5) 0.4927(4) 0.0441(15) Uani 1 1 d . . .
H3 H 0.7877 0.5837 0.5599 0.053 Uiso 1 1 calc R . .
C4 C 0.8738(7) 0.6153(5) 0.4282(4) 0.0307(12) Uani 1 1 d . . .
H4 H 0.9475 0.7031 0.4517 0.037 Uiso 1 1 calc R . .
C5 C 0.8558(6) 0.5531(4) 0.3288(3) 0.0186(9) Uani 1 1 d . . .
C6 C 0.5484(6) 0.2165(4) 0.3039(4) 0.0206(10) Uani 1 1 d . . .
C7 C 0.9472(6) 0.6214(4) 0.2493(4) 0.0202(10) Uani 1 1 d . . .
C8 C 0.5539(5) 0.5122(4) -0.0417(3) 0.0182(9) Uani 1 1 d . . .
C9 C 1.0928(6) 0.0278(4) 0.5384(3) 0.0213(10) Uani 1 1 d . . .
C11 C 0.8930(5) 0.0781(4) 0.1560(3) 0.0166(9) Uani 1 1 d . . .
C16 C 1.0159(6) 0.2024(4) 0.2385(4) 0.0215(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
Sm1 O13 2.439(3) . ?
Sm1 O9 2.445(3) . ?
Sm1 O14 2.449(3) . ?
Sm1 O3 2.455(3) . ?
Sm1 O1 2.458(3) . ?
Sm1 O5 2.476(3) . ?
Sm1 O6 2.482(3) 2_665 ?
Sm1 O7 2.553(3) . ?
Sm1 N1 2.566(4) . ?
Sm2 O4 2.319(3) 1_545 ?
Sm2 O10 2.389(3) . ?
Sm2 O15 2.395(3) . ?
Sm2 O2 2.417(3) 1_655 ?
Sm2 O11 2.431(3) . ?
Sm2 O8 2.462(3) . ?
Sm2 O16 2.484(3) . ?
Sm2 O12 2.485(3) 2_756 ?
O1 C6 1.272(5) . ?
O2 C6 1.248(5) . ?
O2 Sm2 2.417(3) 1_455 ?
O3 C7 1.250(5) . ?
O4 C7 1.248(5) . ?
O4 Sm2 2.319(3) 1_565 ?
O5 C8 1.247(5) . ?
O6 C8 1.259(5) . ?
O6 Sm1 2.482(3) 2_665 ?
O6 O17 2.905(5) . ?
O7 C11 1.253(5) . ?
O8 C11 1.255(5) . ?
O9 C16 1.246(5) . ?
O10 C16 1.257(5) . ?
O11 C9 1.262(5) . ?
O12 C9 1.254(5) . ?
O12 Sm2 2.485(3) 2_756 ?
O12 O19 2.774(6) . ?
O13 H1W 0.8270 . ?
O13 H2W 0.8243 . ?
O14 H3W 0.8314 . ?
O14 H4W 0.8297 . ?
O15 H5W 0.8278 . ?
O15 H6W 0.8282 . ?
O16 H7W 0.8286 . ?
O16 H8W 0.8274 . ?
O17 H10W 0.8319 . ?
O17 H9W 0.8298 . ?
O18 O19 2.732(8) . ?
O18 H12W 0.8156 . ?
O18 H11W 0.8291 . ?
O19 H13W 0.8327 . ?
O19 H14W 0.8320 . ?
N1 C5 1.334(5) . ?
N1 C1 1.342(5) . ?
C1 C2 1.389(6) . ?
C1 C6 1.503(6) . ?
C2 C3 1.380(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(6) . ?
C4 H4 0.9300 . ?
C5 C7 1.523(6) . ?
C8 C8 1.553(8) 2_665 ?
C9 C9 1.535(8) 2_756 ?
C11 C16 1.556(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Sm1 O9 136.30(10) . . ?
O13 Sm1 O14 85.04(11) . . ?
O9 Sm1 O14 79.09(11) . . ?
O13 Sm1 O3 144.75(11) . . ?
O9 Sm1 O3 73.52(10) . . ?
O14 Sm1 O3 83.73(10) . . ?
O13 Sm1 O1 80.57(11) . . ?
O9 Sm1 O1 87.70(11) . . ?
O14 Sm1 O1 142.35(10) . . ?
O3 Sm1 O1 126.10(10) . . ?
O13 Sm1 O5 73.35(10) . . ?
O9 Sm1 O5 135.07(10) . . ?
O14 Sm1 O5 70.03(10) . . ?
O3 Sm1 O5 71.41(10) . . ?
O1 Sm1 O5 136.10(10) . . ?
O13 Sm1 O6 78.34(11) . 2_665 ?
O9 Sm1 O6 138.63(10) . 2_665 ?
O14 Sm1 O6 135.20(10) . 2_665 ?
O3 Sm1 O6 86.49(10) . 2_665 ?
O1 Sm1 O6 75.25(10) . 2_665 ?
O5 Sm1 O6 65.40(9) . 2_665 ?
O13 Sm1 O7 71.06(10) . . ?
O9 Sm1 O7 65.31(9) . . ?
O14 Sm1 O7 71.14(10) . . ?
O3 Sm1 O7 134.75(10) . . ?
O1 Sm1 O7 71.30(10) . . ?
O5 Sm1 O7 128.66(10) . . ?
O6 Sm1 O7 137.50(10) 2_665 . ?
O13 Sm1 N1 135.77(11) . . ?
O9 Sm1 N1 69.42(11) . . ?
O14 Sm1 N1 139.18(11) . . ?
O3 Sm1 N1 63.19(10) . . ?
O1 Sm1 N1 62.92(10) . . ?
O5 Sm1 N1 116.14(10) . . ?
O6 Sm1 N1 69.25(10) 2_665 . ?
O7 Sm1 N1 115.19(10) . . ?
O4 Sm2 O10 146.25(12) 1_545 . ?
O4 Sm2 O15 83.95(12) 1_545 . ?
O10 Sm2 O15 105.58(13) . . ?
O4 Sm2 O2 141.97(12) 1_545 1_655 ?
O10 Sm2 O2 71.32(11) . 1_655 ?
O15 Sm2 O2 76.43(11) . 1_655 ?
O4 Sm2 O11 105.18(12) 1_545 . ?
O10 Sm2 O11 82.41(12) . . ?
O15 Sm2 O11 150.74(11) . . ?
O2 Sm2 O11 79.85(11) 1_655 . ?
O4 Sm2 O8 84.24(11) 1_545 . ?
O10 Sm2 O8 67.16(10) . . ?
O15 Sm2 O8 77.22(11) . . ?
O2 Sm2 O8 121.58(10) 1_655 . ?
O11 Sm2 O8 130.64(10) . . ?
O4 Sm2 O16 71.50(12) 1_545 . ?
O10 Sm2 O16 141.33(12) . . ?
O15 Sm2 O16 80.49(13) . . ?
O2 Sm2 O16 73.32(12) 1_655 . ?
O11 Sm2 O16 76.45(12) . . ?
O8 Sm2 O16 148.53(12) . . ?
O4 Sm2 O12 75.75(11) 1_545 2_756 ?
O10 Sm2 O12 77.86(12) . 2_756 ?
O15 Sm2 O12 142.91(11) . 2_756 ?
O2 Sm2 O12 136.35(11) 1_655 2_756 ?
O11 Sm2 O12 65.88(10) . 2_756 ?
O8 Sm2 O12 70.20(10) . 2_756 ?
O16 Sm2 O12 120.29(12) . 2_756 ?
C6 O1 Sm1 126.0(3) . . ?
C6 O2 Sm2 134.1(3) . 1_455 ?
C7 O3 Sm1 125.6(3) . . ?
C7 O4 Sm2 171.9(3) . 1_565 ?
C8 O5 Sm1 120.5(3) . . ?
C8 O6 Sm1 120.3(3) . 2_665 ?
C8 O6 O17 99.5(3) . . ?
Sm1 O6 O17 109.24(13) 2_665 . ?
C11 O7 Sm1 118.4(3) . . ?
C11 O8 Sm2 118.3(3) . . ?
C16 O9 Sm1 121.4(3) . . ?
C16 O10 Sm2 121.0(3) . . ?
C9 O11 Sm2 120.1(3) . . ?
C9 O12 Sm2 118.8(3) . 2_756 ?
C9 O12 O19 122.1(3) . . ?
Sm2 O12 O19 118.3(2) 2_756 . ?
Sm1 O13 H1W 132.8 . . ?
Sm1 O13 H2W 114.6 . . ?
H1W O13 H2W 112.2 . . ?
Sm1 O14 H3W 116.2 . . ?
Sm1 O14 H4W 125.8 . . ?
H3W O14 H4W 111.0 . . ?
Sm2 O15 H5W 127.6 . . ?
Sm2 O15 H6W 119.9 . . ?
H5W O15 H6W 111.8 . . ?
Sm2 O16 H7W 120.8 . . ?
Sm2 O16 H8W 108.9 . . ?
H7W O16 H8W 111.9 . . ?
O6 O17 H10W 9.4 . . ?
O6 O17 H9W 111.6 . . ?
H10W O17 H9W 111.0 . . ?
O19 O18 H12W 93.2 . . ?
O19 O18 H11W 143.9 . . ?
H12W O18 H11W 112.8 . . ?
O18 O19 O12 127.9(2) . . ?
O18 O19 H13W 122.7 . . ?
O12 O19 H13W 17.3 . . ?
O18 O19 H14W 11.8 . . ?
O12 O19 H14W 116.2 . . ?
H13W O19 H14W 111.1 . . ?
C5 N1 C1 119.5(4) . . ?
C5 N1 Sm1 120.2(3) . . ?
C1 N1 Sm1 120.3(3) . . ?
N1 C1 C2 121.1(4) . . ?
N1 C1 C6 114.3(4) . . ?
C2 C1 C6 124.6(4) . . ?
C3 C2 C1 119.4(5) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.6(4) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 122.5(4) . . ?
N1 C5 C7 113.7(4) . . ?
C4 C5 C7 123.8(4) . . ?
O2 C6 O1 124.9(4) . . ?
O2 C6 C1 118.6(4) . . ?
O1 C6 C1 116.4(4) . . ?
O4 C7 O3 124.8(4) . . ?
O4 C7 C5 118.1(4) . . ?
O3 C7 C5 117.1(4) . . ?
O5 C8 O6 126.6(4) . . ?
O5 C8 C8 117.1(5) . 2_665 ?
O6 C8 C8 116.3(5) . 2_665 ?
O12 C9 O11 126.2(4) . . ?
O12 C9 C9 116.6(5) . 2_756 ?
O11 C9 C9 117.2(5) . 2_756 ?
O7 C11 O8 126.9(4) . . ?
O7 C11 C16 116.4(4) . . ?
O8 C11 C16 116.7(4) . . ?
O9 C16 O10 125.7(4) . . ?
O9 C16 C11 117.8(4) . . ?
O10 C16 C11 116.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O13 Sm1 O1 C6 -154.7(4) . . . . ?
O9 Sm1 O1 C6 67.6(3) . . . . ?
O14 Sm1 O1 C6 136.3(3) . . . . ?
O3 Sm1 O1 C6 0.0(4) . . . . ?
O5 Sm1 O1 C6 -100.9(4) . . . . ?
O6 Sm1 O1 C6 -74.4(3) 2_665 . . . ?
O7 Sm1 O1 C6 132.2(4) . . . . ?
N1 Sm1 O1 C6 -0.4(3) . . . . ?
O13 Sm1 O3 C7 128.8(3) . . . . ?
O9 Sm1 O3 C7 -78.5(3) . . . . ?
O14 Sm1 O3 C7 -159.0(4) . . . . ?
O1 Sm1 O3 C7 -4.1(4) . . . . ?
O5 Sm1 O3 C7 130.0(4) . . . . ?
O6 Sm1 O3 C7 64.8(3) 2_665 . . . ?
O7 Sm1 O3 C7 -103.5(3) . . . . ?
N1 Sm1 O3 C7 -3.7(3) . . . . ?
O13 Sm1 O5 C8 90.1(3) . . . . ?
O9 Sm1 O5 C8 -129.7(3) . . . . ?
O14 Sm1 O5 C8 -179.2(3) . . . . ?
O3 Sm1 O5 C8 -89.2(3) . . . . ?
O1 Sm1 O5 C8 34.0(4) . . . . ?
O6 Sm1 O5 C8 5.5(3) 2_665 . . . ?
O7 Sm1 O5 C8 137.8(3) . . . . ?
N1 Sm1 O5 C8 -43.3(3) . . . . ?
O13 Sm1 O7 C11 -179.2(3) . . . . ?
O9 Sm1 O7 C11 3.2(3) . . . . ?
O14 Sm1 O7 C11 89.6(3) . . . . ?
O3 Sm1 O7 C11 29.7(4) . . . . ?
O1 Sm1 O7 C11 -93.0(3) . . . . ?
O5 Sm1 O7 C11 132.3(3) . . . . ?
O6 Sm1 O7 C11 -132.9(3) 2_665 . . . ?
N1 Sm1 O7 C11 -46.7(3) . . . . ?
O4 Sm2 O8 C11 157.9(3) 1_545 . . . ?
O10 Sm2 O8 C11 -3.8(3) . . . . ?
O15 Sm2 O8 C11 -117.0(3) . . . . ?
O2 Sm2 O8 C11 -51.9(3) 1_655 . . . ?
O11 Sm2 O8 C11 52.8(3) . . . . ?
O16 Sm2 O8 C11 -163.0(3) . . . . ?
O12 Sm2 O8 C11 81.0(3) 2_756 . . . ?
O13 Sm1 O9 C16 -10.6(4) . . . . ?
O14 Sm1 O9 C16 -81.4(4) . . . . ?
O3 Sm1 O9 C16 -168.0(4) . . . . ?
O1 Sm1 O9 C16 63.1(4) . . . . ?
O5 Sm1 O9 C16 -128.1(3) . . . . ?
O6 Sm1 O9 C16 127.6(3) 2_665 . . . ?
O7 Sm1 O9 C16 -7.3(3) . . . . ?
N1 Sm1 O9 C16 125.0(4) . . . . ?
O4 Sm2 O10 C16 -34.8(5) 1_545 . . . ?
O15 Sm2 O10 C16 67.9(4) . . . . ?
O2 Sm2 O10 C16 137.4(4) 1_655 . . . ?
O11 Sm2 O10 C16 -140.8(4) . . . . ?
O8 Sm2 O10 C16 -0.5(3) . . . . ?
O16 Sm2 O10 C16 162.2(3) . . . . ?
O12 Sm2 O10 C16 -74.0(4) 2_756 . . . ?
O4 Sm2 O11 C9 -76.1(3) 1_545 . . . ?
O10 Sm2 O11 C9 70.3(3) . . . . ?
O15 Sm2 O11 C9 178.8(3) . . . . ?
O2 Sm2 O11 C9 142.6(3) 1_655 . . . ?
O8 Sm2 O11 C9 19.4(4) . . . . ?
O16 Sm2 O11 C9 -142.3(3) . . . . ?
O12 Sm2 O11 C9 -9.8(3) 2_756 . . . ?
C9 O12 O19 O18 42.2(6) . . . . ?
Sm2 O12 O19 O18 -127.4(4) 2_756 . . . ?
O13 Sm1 N1 C5 -141.0(3) . . . . ?
O9 Sm1 N1 C5 82.8(3) . . . . ?
O14 Sm1 N1 C5 40.9(4) . . . . ?
O3 Sm1 N1 C5 1.4(3) . . . . ?
O1 Sm1 N1 C5 -178.9(3) . . . . ?
O5 Sm1 N1 C5 -48.3(3) . . . . ?
O6 Sm1 N1 C5 -95.4(3) 2_665 . . . ?
O7 Sm1 N1 C5 130.8(3) . . . . ?
O13 Sm1 N1 C1 38.0(4) . . . . ?
O9 Sm1 N1 C1 -98.1(3) . . . . ?
O14 Sm1 N1 C1 -140.1(3) . . . . ?
O3 Sm1 N1 C1 -179.5(3) . . . . ?
O1 Sm1 N1 C1 0.1(3) . . . . ?
O5 Sm1 N1 C1 130.7(3) . . . . ?
O6 Sm1 N1 C1 83.7(3) 2_665 . . . ?
O7 Sm1 N1 C1 -50.2(3) . . . . ?
C5 N1 C1 C2 0.6(7) . . . . ?
Sm1 N1 C1 C2 -178.5(4) . . . . ?
C5 N1 C1 C6 179.1(4) . . . . ?
Sm1 N1 C1 C6 0.1(5) . . . . ?
N1 C1 C2 C3 -0.3(8) . . . . ?
C6 C1 C2 C3 -178.7(5) . . . . ?
C1 C2 C3 C4 -0.4(9) . . . . ?
C2 C3 C4 C5 0.8(8) . . . . ?
C1 N1 C5 C4 -0.2(7) . . . . ?
Sm1 N1 C5 C4 178.9(4) . . . . ?
C1 N1 C5 C7 -178.8(4) . . . . ?
Sm1 N1 C5 C7 0.3(5) . . . . ?
C3 C4 C5 N1 -0.5(8) . . . . ?
C3 C4 C5 C7 178.0(5) . . . . ?
Sm2 O2 C6 O1 -34.8(7) 1_455 . . . ?
Sm2 O2 C6 C1 145.2(3) 1_455 . . . ?
Sm1 O1 C6 O2 -179.4(3) . . . . ?
Sm1 O1 C6 C1 0.6(5) . . . . ?
N1 C1 C6 O2 179.6(4) . . . . ?
C2 C1 C6 O2 -1.9(7) . . . . ?
N1 C1 C6 O1 -0.4(6) . . . . ?
C2 C1 C6 O1 178.1(5) . . . . ?
Sm2 O4 C7 O3 93(2) 1_565 . . . ?
Sm2 O4 C7 C5 -87(2) 1_565 . . . ?
Sm1 O3 C7 O4 -174.5(3) . . . . ?
Sm1 O3 C7 C5 5.2(5) . . . . ?
N1 C5 C7 O4 176.4(4) . . . . ?
C4 C5 C7 O4 -2.2(7) . . . . ?
N1 C5 C7 O3 -3.3(6) . . . . ?
C4 C5 C7 O3 178.0(4) . . . . ?
Sm1 O5 C8 O6 174.8(3) . . . . ?
Sm1 O5 C8 C8 -5.3(6) . . . 2_665 ?
Sm1 O6 C8 O5 174.8(3) 2_665 . . . ?
O17 O6 C8 O5 -66.3(5) . . . . ?
Sm1 O6 C8 C8 -5.1(6) 2_665 . . 2_665 ?
O17 O6 C8 C8 113.8(4) . . . 2_665 ?
Sm2 O12 C9 O11 -171.0(3) 2_756 . . . ?
O19 O12 C9 O11 19.5(6) . . . . ?
Sm2 O12 C9 C9 8.7(6) 2_756 . . 2_756 ?
O19 O12 C9 C9 -160.8(4) . . . 2_756 ?
Sm2 O11 C9 O12 -170.9(4) . . . . ?
Sm2 O11 C9 C9 9.4(6) . . . 2_756 ?
Sm1 O7 C11 O8 179.6(3) . . . . ?
Sm1 O7 C11 C16 0.0(5) . . . . ?
Sm2 O8 C11 O7 -172.6(3) . . . . ?
Sm2 O8 C11 C16 6.9(5) . . . . ?
Sm1 O9 C16 O10 -168.6(4) . . . . ?
Sm1 O9 C16 C11 10.2(6) . . . . ?
Sm2 O10 C16 O9 -177.3(4) . . . . ?
Sm2 O10 C16 C11 3.9(6) . . . . ?
O7 C11 C16 O9 -6.6(6) . . . . ?
O8 C11 C16 O9 173.8(4) . . . . ?
O7 C11 C16 O10 172.3(4) . . . . ?
O8 C11 C16 O10 -7.3(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H1W O7 0.83 2.02 2.832(4) 165.7 2_655
O13 H2W O19 0.82 1.86 2.680(6) 171.0 1_454
O14 H3W O17 0.83 1.82 2.648(5) 175.2 2_765
O14 H4W O3 0.83 2.09 2.847(4) 151.9 2_765
O15 H5W O14 0.83 2.20 2.982(5) 157.3 2_755
O15 H5W O7 0.83 2.65 3.239(4) 129.3 2_755
O15 H6W O1 0.83 2.01 2.731(4) 145.8 1_655
O16 H7W O19 0.83 2.51 3.241(10) 148.2 2_856
O16 H8W O11 0.83 2.27 2.982(5) 144.6 2_856
O17 H10W O6 0.83 2.09 2.905(5) 166.9 .
O17 H9W O8 0.83 2.10 2.894(5) 159.4 1_565
O18 H12W O6 0.82 2.51 3.133(7) 134.6 1_656
O18 H11W O9 0.83 2.34 3.107(6) 153.8 2_866
O19 H13W O12 0.83 1.99 2.774(6) 155.5 .
O19 H14W O18 0.83 1.92 2.732(8) 163.2 .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.135

# Attachment '4B.cif'

data_4b
_database_code_depnum_ccdc_archive 'CCDC 725876'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H17 Gd2 N O19'
_chemical_formula_weight         781.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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                   8.2119(10)
_cell_length_b                   10.5846(13)
_cell_length_c                   13.0751(16)
_cell_angle_alpha                94.0010(10)
_cell_angle_beta                 103.3020(10)
_cell_angle_gamma                107.7200(10)
_cell_volume                     1041.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    4268
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    6.409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4088
_exptl_absorpt_correction_T_max  0.5135
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7967
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3852
_reflns_number_gt                3422
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0202P)²+1.9648P] 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         3852
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0501
_refine_ls_wR_factor_gt          0.0475
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
Gd1 Gd 0.27739(2) 0.178941(18) 0.395205(15) 0.01371(6) Uani 1 1 d . . .
Gd2 Gd 0.82831(3) 0.528626(19) 0.188533(15) 0.01434(6) Uani 1 1 d . . .
O1 O 0.4521(4) 0.3186(3) 0.2924(2) 0.0247(7) Uani 1 1 d . . .
O2 O 0.5446(4) 0.3582(3) 0.1459(2) 0.0281(7) Uani 1 1 d . . .
O3 O 0.0783(4) -0.0513(3) 0.3392(2) 0.0231(7) Uani 1 1 d . . .
O4 O -0.0380(4) -0.2434(3) 0.2269(3) 0.0302(8) Uani 1 1 d . . .
O5 O 0.0143(4) 0.1892(3) 0.2717(2) 0.0244(7) Uani 1 1 d . . .
O6 O -0.1318(4) 0.3164(3) 0.1896(3) 0.0344(8) Uani 1 1 d . . .
O7 O 0.2376(4) 0.4073(3) 0.4088(2) 0.0204(6) Uani 1 1 d . . .
O8 O 0.0685(4) 0.5275(3) 0.3384(2) 0.0212(6) Uani 1 1 d . . .
O9 O 0.5197(4) 0.0893(3) 0.3932(2) 0.0222(7) Uani 1 1 d . . .
O10 O 0.6656(4) -0.0471(3) 0.4614(2) 0.0231(7) Uani 1 1 d . . .
O11 O 1.1042(4) 0.5694(3) 0.1319(2) 0.0295(7) Uani 1 1 d . . .
O12 O 1.2214(4) 0.5260(3) 0.0000(2) 0.0264(7) Uani 1 1 d . . .
N1 N 0.2493(4) 0.0735(3) 0.2089(3) 0.0171(7) Uani 1 1 d . . .
C1 C 0.3397(6) 0.1440(4) 0.1462(3) 0.0205(9) Uani 1 1 d . . .
C2 C 0.3291(7) 0.0878(5) 0.0447(4) 0.0356(12) Uani 1 1 d . . .
H2 H 0.3931 0.1378 0.0025 0.043 Uiso 1 1 calc R . .
C3 C 0.2219(8) -0.0440(5) 0.0072(4) 0.0420(14) Uani 1 1 d . . .
H3 H 0.2136 -0.0842 -0.0602 0.050 Uiso 1 1 calc R . .
C4 C 0.1271(7) -0.1150(5) 0.0722(4) 0.0326(12) Uani 1 1 d . . .
H4 H 0.0520 -0.2028 0.0481 0.039 Uiso 1 1 calc R . .
C5 C 0.1452(5) -0.0538(4) 0.1728(3) 0.0189(9) Uani 1 1 d . . .
C6 C 0.4548(5) 0.2843(4) 0.1980(3) 0.0205(9) Uani 1 1 d . . .
C7 C 0.0550(6) -0.1222(4) 0.2523(3) 0.0208(9) Uani 1 1 d . . .
C8 C -0.0131(6) 0.2981(4) 0.2611(3) 0.0211(9) Uani 1 1 d . . .
C9 C 0.1093(5) 0.4224(4) 0.3439(3) 0.0179(9) Uani 1 1 d . . .
C10 C 0.5539(5) 0.0117(4) 0.4580(3) 0.0181(9) Uani 1 1 d . . .
C11 C 1.0941(5) 0.5275(4) 0.0385(3) 0.0203(9) Uani 1 1 d . . .
O13 O 0.0912(4) 0.1850(3) 0.5131(2) 0.0272(7) Uani 1 1 d . . .
H1W H 0.0131 0.2205 0.4930 0.041 Uiso 1 1 d R . .
H2W H 0.0648 0.1380 0.5595 0.041 Uiso 1 1 d R . .
O14 O 0.5148(4) 0.3292(3) 0.5378(2) 0.0285(7) Uani 1 1 d . . .
H3W H 0.5830 0.4058 0.5391 0.043 Uiso 1 1 d R . .
H4W H 0.5287 0.3081 0.5984 0.043 Uiso 1 1 d R . .
O15 O 0.7185(4) 0.5603(3) 0.3373(3) 0.0345(8) Uani 1 1 d . . .
H5W H 0.6277 0.5026 0.3423 0.052 Uiso 1 1 d R . .
H6W H 0.7583 0.6219 0.3880 0.052 Uiso 1 1 d R . .
O16 O 0.6092(5) 0.6344(4) 0.1115(3) 0.0446(10) Uani 1 1 d . . .
H7W H 0.6515 0.6974 0.0809 0.067 Uiso 1 1 d R . .
H8W H 0.5015 0.5979 0.0850 0.067 Uiso 1 1 d R . .
O17 O 0.8546(4) 0.3091(3) 0.4595(3) 0.0339(8) Uani 1 1 d . . .
H9W H 0.8615 0.3472 0.5182 0.051 Uiso 1 1 d R . .
H10W H 0.7580 0.2499 0.4342 0.051 Uiso 1 1 d R . .
O18 O 1.4166(8) 0.7411(5) 0.2678(4) 0.147(3) Uani 1 1 d . . .
H11W H 1.5027 0.7786 0.2443 0.220 Uiso 1 1 d R . .
H12W H 1.3290 0.6952 0.2180 0.220 Uiso 1 1 d R . .
O19 O 0.6543(7) -0.0381(6) 0.2236(4) 0.120(3) Uani 1 1 d . . .
H13W H 0.6608 -0.0587 0.2853 0.180 Uiso 1 1 d R . .
H14W H 0.6858 0.0431 0.2260 0.180 Uiso 1 1 d R . .


_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
Gd1 O14 2.415(3) . ?
Gd1 O5 2.419(3) . ?
Gd1 O13 2.419(3) . ?
Gd1 O3 2.433(3) . ?
Gd1 O1 2.435(3) . ?
Gd1 O9 2.455(3) . ?
Gd1 O10 2.458(3) 2_656 ?
Gd1 O7 2.536(3) . ?
Gd1 N1 2.538(3) . ?
Gd2 O4 2.290(3) 1_665 ?
Gd2 O6 2.367(3) 1_655 ?
Gd2 O15 2.368(3) . ?
Gd2 O2 2.387(3) . ?
Gd2 O12 2.402(3) 2_765 ?
Gd2 O8 2.443(3) 1_655 ?
Gd2 O16 2.460(3) . ?
Gd2 O11 2.468(3) . ?
O1 C6 1.269(5) . ?
O2 C6 1.255(5) . ?
O3 C7 1.259(5) . ?
O4 C7 1.253(5) . ?
O4 Gd2 2.290(3) 1_445 ?
O5 C8 1.250(5) . ?
O6 C8 1.258(5) . ?
O6 Gd2 2.367(3) 1_455 ?
O7 C9 1.251(5) . ?
O8 C9 1.258(5) . ?
O8 Gd2 2.443(3) 1_455 ?
O9 C10 1.265(5) . ?
O9 O17 2.908(4) . ?
O10 C10 1.250(5) . ?
O10 Gd1 2.458(3) 2_656 ?
O10 O19 3.098(6) . ?
O11 C11 1.244(5) . ?
O11 O18 2.766(5) . ?
O12 C11 1.265(5) . ?
O12 Gd2 2.402(3) 2_765 ?
N1 C5 1.339(5) . ?
N1 C1 1.344(5) . ?
C1 C2 1.389(6) . ?
C1 C6 1.505(6) . ?
C2 C3 1.385(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(6) . ?
C4 H4 0.9300 . ?
C5 C7 1.511(6) . ?
C8 C9 1.552(6) . ?
C10 C10 1.550(8) 2_656 ?
C11 C11 1.547(8) 2_765 ?
O13 H1W 0.8393 . ?
O13 H2W 0.8360 . ?
O14 H3W 0.8296 . ?
O14 H4W 0.8305 . ?
O15 H5W 0.8275 . ?
O15 H6W 0.8264 . ?
O16 H7W 0.8286 . ?
O16 H8W 0.8271 . ?
O17 H9W 0.8238 . ?
O17 H10W 0.8246 . ?
O18 H11W 0.8354 . ?
O18 H12W 0.8391 . ?
O19 H13W 0.8437 . ?
O19 H14W 0.8141 . ?

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
O14 Gd1 O5 136.71(10) . . ?
O14 Gd1 O13 85.25(11) . . ?
O5 Gd1 O13 79.10(10) . . ?
O14 Gd1 O3 144.13(10) . . ?
O5 Gd1 O3 73.62(10) . . ?
O13 Gd1 O3 83.18(10) . . ?
O14 Gd1 O1 80.06(10) . . ?
O5 Gd1 O1 88.06(10) . . ?
O13 Gd1 O1 142.12(10) . . ?
O3 Gd1 O1 127.19(10) . . ?
O14 Gd1 O9 78.27(10) . . ?
O5 Gd1 O9 138.24(10) . . ?
O13 Gd1 O9 135.51(10) . . ?
O3 Gd1 O9 86.60(10) . . ?
O1 Gd1 O9 75.02(10) . . ?
O14 Gd1 O10 73.14(10) . 2_656 ?
O5 Gd1 O10 134.83(10) . 2_656 ?
O13 Gd1 O10 69.71(10) . 2_656 ?
O3 Gd1 O10 71.00(10) . 2_656 ?
O1 Gd1 O10 136.10(10) . 2_656 ?
O9 Gd1 O10 66.01(9) . 2_656 ?
O14 Gd1 O7 71.04(9) . . ?
O5 Gd1 O7 65.73(9) . . ?
O13 Gd1 O7 71.18(10) . . ?
O3 Gd1 O7 134.97(10) . . ?
O1 Gd1 O7 71.04(10) . . ?
O9 Gd1 O7 137.27(9) . . ?
O10 Gd1 O7 128.21(9) 2_656 . ?
O14 Gd1 N1 135.70(11) . . ?
O5 Gd1 N1 69.18(10) . . ?
O13 Gd1 N1 139.04(11) . . ?
O3 Gd1 N1 63.79(10) . . ?
O1 Gd1 N1 63.40(10) . . ?
O9 Gd1 N1 69.10(10) . . ?
O10 Gd1 N1 116.53(10) 2_656 . ?
O7 Gd1 N1 115.25(10) . . ?
O4 Gd2 O6 146.28(12) 1_665 1_655 ?
O4 Gd2 O15 83.46(11) 1_665 . ?
O6 Gd2 O15 105.64(12) 1_655 . ?
O4 Gd2 O2 142.04(11) 1_665 . ?
O6 Gd2 O2 71.09(11) 1_655 . ?
O15 Gd2 O2 76.30(11) . . ?
O4 Gd2 O12 105.61(11) 1_665 2_765 ?
O6 Gd2 O12 82.82(11) 1_655 2_765 ?
O15 Gd2 O12 150.05(11) . 2_765 ?
O2 Gd2 O12 79.67(10) . 2_765 ?
O4 Gd2 O8 83.63(11) 1_665 1_655 ?
O6 Gd2 O8 67.61(10) 1_655 1_655 ?
O15 Gd2 O8 76.98(11) . 1_655 ?
O2 Gd2 O8 121.44(10) . 1_655 ?
O12 Gd2 O8 131.68(10) 2_765 1_655 ?
O4 Gd2 O16 71.79(12) 1_665 . ?
O6 Gd2 O16 141.15(11) 1_655 . ?
O15 Gd2 O16 80.16(12) . . ?
O2 Gd2 O16 73.31(12) . . ?
O12 Gd2 O16 75.99(12) 2_765 . ?
O8 Gd2 O16 148.05(11) 1_655 . ?
O4 Gd2 O11 75.81(11) 1_665 . ?
O6 Gd2 O11 78.15(12) 1_655 . ?
O15 Gd2 O11 142.88(10) . . ?
O2 Gd2 O11 136.58(10) . . ?
O12 Gd2 O11 66.51(10) 2_765 . ?
O8 Gd2 O11 70.47(10) 1_655 . ?
O16 Gd2 O11 120.42(12) . . ?
C6 O1 Gd1 125.9(3) . . ?
C6 O2 Gd2 135.0(3) . . ?
C7 O3 Gd1 125.2(3) . . ?
C7 O4 Gd2 172.0(3) . 1_445 ?
C8 O5 Gd1 121.5(3) . . ?
C8 O6 Gd2 120.8(3) . 1_455 ?
C9 O7 Gd1 118.0(3) . . ?
C9 O8 Gd2 118.2(3) . 1_455 ?
C10 O9 Gd1 120.2(3) . . ?
C10 O9 O17 99.3(2) . . ?
Gd1 O9 O17 108.89(12) . . ?
C10 O10 Gd1 120.2(3) . 2_656 ?
C10 O10 O19 92.9(3) . . ?
Gd1 O10 O19 141.98(18) 2_656 . ?
C11 O11 Gd2 118.7(3) . . ?
C11 O11 O18 122.1(3) . . ?
Gd2 O11 O18 118.4(2) . . ?
C11 O12 Gd2 120.2(3) . 2_765 ?
C5 N1 C1 119.6(4) . . ?
C5 N1 Gd1 119.9(3) . . ?
C1 N1 Gd1 120.5(3) . . ?
N1 C1 C2 121.6(4) . . ?
N1 C1 C6 113.9(4) . . ?
C2 C1 C6 124.5(4) . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 118.8(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 121.6(4) . . ?
N1 C5 C7 114.1(4) . . ?
C4 C5 C7 124.3(4) . . ?
O2 C6 O1 124.9(4) . . ?
O2 C6 C1 118.7(4) . . ?
O1 C6 C1 116.4(4) . . ?
O4 C7 O3 125.0(4) . . ?
O4 C7 C5 118.2(4) . . ?
O3 C7 C5 116.8(4) . . ?
O5 C8 O6 126.0(4) . . ?
O5 C8 C9 117.3(4) . . ?
O6 C8 C9 116.6(4) . . ?
O7 C9 O8 127.1(4) . . ?
O7 C9 C8 116.6(4) . . ?
O8 C9 C8 116.3(4) . . ?
O10 C10 O9 126.8(4) . . ?
O10 C10 C10 117.0(4) . 2_656 ?
O9 C10 C10 116.2(4) . 2_656 ?
O11 C11 O12 126.8(4) . . ?
O11 C11 C11 116.5(5) . 2_765 ?
O12 C11 C11 116.7(5) . 2_765 ?
Gd1 O13 H1W 115.8 . . ?
Gd1 O13 H2W 131.8 . . ?
H1W O13 H2W 108.9 . . ?
Gd1 O14 H3W 130.7 . . ?
Gd1 O14 H4W 118.6 . . ?
H3W O14 H4W 110.4 . . ?
Gd2 O15 H5W 118.4 . . ?
Gd2 O15 H6W 129.6 . . ?
H5W O15 H6W 112.0 . . ?
Gd2 O16 H7W 112.1 . . ?
Gd2 O16 H8W 127.9 . . ?
H7W O16 H8W 111.8 . . ?
O9 O17 H9W 107.8 . . ?
O9 O17 H10W 6.5 . . ?
H9W O17 H10W 112.1 . . ?
O11 O18 H11W 120.5 . . ?
O11 O18 H12W 10.1 . . ?
H11W O18 H12W 110.7 . . ?
O10 O19 H13W 14.0 . . ?
O10 O19 H14W 98.0 . . ?
H13W O19 H14W 110.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O14 Gd1 O1 C6 154.8(3) . . . . ?
O5 Gd1 O1 C6 -67.1(3) . . . . ?
O13 Gd1 O1 C6 -136.5(3) . . . . ?
O3 Gd1 O1 C6 0.6(4) . . . . ?
O9 Gd1 O1 C6 74.4(3) . . . . ?
O10 Gd1 O1 C6 102.1(3) 2_656 . . . ?
O7 Gd1 O1 C6 -132.0(3) . . . . ?
N1 Gd1 O1 C6 0.6(3) . . . . ?
O4 Gd2 O2 C6 -95.9(4) 1_665 . . . ?
O6 Gd2 O2 C6 76.1(4) 1_655 . . . ?
O15 Gd2 O2 C6 -36.1(4) . . . . ?
O12 Gd2 O2 C6 161.9(4) 2_765 . . . ?
O8 Gd2 O2 C6 29.0(4) 1_655 . . . ?
O16 Gd2 O2 C6 -119.7(4) . . . . ?
O11 Gd2 O2 C6 123.4(4) . . . . ?
O14 Gd1 O3 C7 -128.8(3) . . . . ?
O5 Gd1 O3 C7 78.5(3) . . . . ?
O13 Gd1 O3 C7 159.1(3) . . . . ?
O1 Gd1 O3 C7 4.0(4) . . . . ?
O9 Gd1 O3 C7 -64.3(3) . . . . ?
O10 Gd1 O3 C7 -130.0(3) 2_656 . . . ?
O7 Gd1 O3 C7 104.5(3) . . . . ?
N1 Gd1 O3 C7 4.1(3) . . . . ?
O14 Gd1 O5 C8 11.0(4) . . . . ?
O13 Gd1 O5 C8 81.9(3) . . . . ?
O3 Gd1 O5 C8 167.9(3) . . . . ?
O1 Gd1 O5 C8 -62.2(3) . . . . ?
O9 Gd1 O5 C8 -127.0(3) . . . . ?
O10 Gd1 O5 C8 128.4(3) 2_656 . . . ?
O7 Gd1 O5 C8 7.8(3) . . . . ?
N1 Gd1 O5 C8 -124.4(3) . . . . ?
O14 Gd1 O7 C9 178.9(3) . . . . ?
O5 Gd1 O7 C9 -3.5(3) . . . . ?
O13 Gd1 O7 C9 -89.7(3) . . . . ?
O3 Gd1 O7 C9 -30.9(3) . . . . ?
O1 Gd1 O7 C9 93.2(3) . . . . ?
O9 Gd1 O7 C9 132.4(3) . . . . ?
O10 Gd1 O7 C9 -132.5(3) 2_656 . . . ?
N1 Gd1 O7 C9 46.4(3) . . . . ?
O14 Gd1 O9 C10 81.7(3) . . . . ?
O5 Gd1 O9 C10 -126.2(3) . . . . ?
O13 Gd1 O9 C10 11.1(4) . . . . ?
O3 Gd1 O9 C10 -65.5(3) . . . . ?
O1 Gd1 O9 C10 164.5(3) . . . . ?
O10 Gd1 O9 C10 5.2(3) 2_656 . . . ?
O7 Gd1 O9 C10 126.2(3) . . . . ?
N1 Gd1 O9 C10 -128.7(3) . . . . ?
O14 Gd1 O9 O17 -31.68(12) . . . . ?
O5 Gd1 O9 O17 120.41(15) . . . . ?
O13 Gd1 O9 O17 -102.28(16) . . . . ?
O3 Gd1 O9 O17 -178.97(13) . . . . ?
O1 Gd1 O9 O17 51.03(12) . . . . ?
O10 Gd1 O9 O17 -108.27(14) 2_656 . . . ?
O7 Gd1 O9 O17 12.78(19) . . . . ?
N1 Gd1 O9 O17 117.83(14) . . . . ?
O4 Gd2 O11 C11 -124.2(3) 1_665 . . . ?
O6 Gd2 O11 C11 77.4(3) 1_655 . . . ?
O15 Gd2 O11 C11 177.8(3) . . . . ?
O2 Gd2 O11 C11 32.1(4) . . . . ?
O12 Gd2 O11 C11 -9.8(3) 2_765 . . . ?
O8 Gd2 O11 C11 147.6(3) 1_655 . . . ?
O16 Gd2 O11 C11 -65.7(4) . . . . ?
O4 Gd2 O11 O18 46.01(19) 1_665 . . . ?
O6 Gd2 O11 O18 -112.38(19) 1_655 . . . ?
O15 Gd2 O11 O18 -12.1(3) . . . . ?
O2 Gd2 O11 O18 -157.67(18) . . . . ?
O12 Gd2 O11 O18 160.4(2) 2_765 . . . ?
O8 Gd2 O11 O18 -42.17(18) 1_655 . . . ?
O16 Gd2 O11 O18 104.5(2) . . . . ?
O14 Gd1 N1 C5 140.7(3) . . . . ?
O5 Gd1 N1 C5 -82.8(3) . . . . ?
O13 Gd1 N1 C5 -41.1(4) . . . . ?
O3 Gd1 N1 C5 -1.4(3) . . . . ?
O1 Gd1 N1 C5 178.6(3) . . . . ?
O9 Gd1 N1 C5 95.4(3) . . . . ?
O10 Gd1 N1 C5 48.0(3) 2_656 . . . ?
O7 Gd1 N1 C5 -131.1(3) . . . . ?
O14 Gd1 N1 C1 -38.6(4) . . . . ?
O5 Gd1 N1 C1 97.9(3) . . . . ?
O13 Gd1 N1 C1 139.6(3) . . . . ?
O3 Gd1 N1 C1 179.3(3) . . . . ?
O1 Gd1 N1 C1 -0.7(3) . . . . ?
O9 Gd1 N1 C1 -83.9(3) . . . . ?
O10 Gd1 N1 C1 -131.3(3) 2_656 . . . ?
O7 Gd1 N1 C1 49.6(3) . . . . ?
C5 N1 C1 C2 -0.5(6) . . . . ?
Gd1 N1 C1 C2 178.8(3) . . . . ?
C5 N1 C1 C6 -178.5(4) . . . . ?
Gd1 N1 C1 C6 0.8(5) . . . . ?
N1 C1 C2 C3 0.4(8) . . . . ?
C6 C1 C2 C3 178.1(5) . . . . ?
C1 C2 C3 C4 0.7(8) . . . . ?
C2 C3 C4 C5 -1.6(8) . . . . ?
C1 N1 C5 C4 -0.4(6) . . . . ?
Gd1 N1 C5 C4 -179.7(3) . . . . ?
C1 N1 C5 C7 178.6(4) . . . . ?
Gd1 N1 C5 C7 -0.7(4) . . . . ?
C3 C4 C5 N1 1.4(7) . . . . ?
C3 C4 C5 C7 -177.4(4) . . . . ?
Gd2 O2 C6 O1 34.8(7) . . . . ?
Gd2 O2 C6 C1 -145.6(3) . . . . ?
Gd1 O1 C6 O2 179.3(3) . . . . ?
Gd1 O1 C6 C1 -0.4(5) . . . . ?
N1 C1 C6 O2 180.0(4) . . . . ?
C2 C1 C6 O2 2.1(7) . . . . ?
N1 C1 C6 O1 -0.3(5) . . . . ?
C2 C1 C6 O1 -178.2(4) . . . . ?
Gd2 O4 C7 O3 -96(2) 1_445 . . . ?
Gd2 O4 C7 C5 85(2) 1_445 . . . ?
Gd1 O3 C7 O4 174.7(3) . . . . ?
Gd1 O3 C7 C5 -6.0(5) . . . . ?
N1 C5 C7 O4 -176.6(4) . . . . ?
C4 C5 C7 O4 2.4(6) . . . . ?
N1 C5 C7 O3 4.1(5) . . . . ?
C4 C5 C7 O3 -176.9(4) . . . . ?
Gd1 O5 C8 O6 169.6(4) . . . . ?
Gd1 O5 C8 C9 -10.8(5) . . . . ?
Gd2 O6 C8 O5 176.8(3) 1_455 . . . ?
Gd2 O6 C8 C9 -2.9(5) 1_455 . . . ?
Gd1 O7 C9 O8 180.0(3) . . . . ?
Gd1 O7 C9 C8 0.0(5) . . . . ?
Gd2 O8 C9 O7 173.1(3) 1_455 . . . ?
Gd2 O8 C9 C8 -6.9(5) 1_455 . . . ?
O5 C8 C9 O7 7.0(6) . . . . ?
O6 C8 C9 O7 -173.4(4) . . . . ?
O5 C8 C9 O8 -173.0(4) . . . . ?
O6 C8 C9 O8 6.6(6) . . . . ?
Gd1 O10 C10 O9 175.1(3) 2_656 . . . ?
O19 O10 C10 O9 -24.5(5) . . . . ?
Gd1 O10 C10 C10 -4.5(6) 2_656 . . 2_656 ?
O19 O10 C10 C10 155.9(4) . . . 2_656 ?
Gd1 O9 C10 O10 175.4(3) . . . . ?
O17 O9 C10 O10 -66.2(5) . . . . ?
Gd1 O9 C10 C10 -5.0(6) . . . 2_656 ?
O17 O9 C10 C10 113.4(4) . . . 2_656 ?
Gd2 O11 C11 O12 -171.2(3) . . . . ?
O18 O11 C11 O12 19.0(6) . . . . ?
Gd2 O11 C11 C11 9.2(6) . . . 2_765 ?
O18 O11 C11 C11 -160.6(4) . . . 2_765 ?
Gd2 O12 C11 O11 -170.6(4) 2_765 . . . ?
Gd2 O12 C11 C11 9.0(6) 2_765 . . 2_765 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H1W O17 0.84 1.82 2.654(4) 174.9 1_455
O13 H2W O3 0.84 2.05 2.844(4) 158.1 2_556
O14 H3W O7 0.83 2.03 2.832(4) 162.3 2_666
O14 H4W O18 0.83 1.86 2.682(6) 173.6 2_766
O15 H5W O1 0.83 1.99 2.733(4) 148.2 .
O15 H6W O13 0.83 2.17 2.971(5) 161.7 2_666
O16 H8W O12 0.83 2.18 2.998(4) 171.2 1_455
O17 H9W O8 0.82 2.07 2.882(4) 167.0 2_666
O17 H10W O9 0.82 2.09 2.908(4) 171.0 .
O18 H11W O19 0.84 2.04 2.745(7) 142.3 1_665
O18 H12W O11 0.84 1.95 2.766(5) 165.5 .
O19 H13W O10 0.84 2.29 3.098(6) 160.9 .
O19 H14W O5 0.81 2.57 3.087(6) 122.5 1_655

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.121


# Attachment '2A.cif'

data_2a
_database_code_depnum_ccdc_archive 'CCDC 727551'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H14 Gd N2 O9'
_chemical_formula_weight         451.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)/c

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

_cell_length_a                   8.8003(8)
_cell_length_b                   14.0615(13)
_cell_length_c                   11.8535(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0240(10)
_cell_angle_gamma                90.00
_cell_volume                     1464.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9310
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.28

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    4.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6332
_exptl_absorpt_correction_T_max  0.7112
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10941
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2715
_reflns_number_gt                2598
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0350P)²+1.6343P] 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         2715
_refine_ls_number_parameters     202
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C6 C 0.6059(4) 0.3340(4) 1.0400(3) 0.0531(2) Uani 0.693(3) 1 d PDU A 1
H6A H 0.6087 0.3986 1.0685 0.064 Uiso 0.693(3) 1 calc PR A 1
H6B H 0.5425 0.2964 1.0875 0.064 Uiso 0.693(3) 1 calc PR A 1
C7 C 0.7643(4) 0.2935(4) 1.0440(3) 0.0539(2) Uani 0.693(3) 1 d PDU A 1
H7A H 0.8283 0.3335 0.9997 0.065 Uiso 0.693(3) 1 calc PR A 1
H7B H 0.7614 0.2307 1.0099 0.065 Uiso 0.693(3) 1 calc PR A 1
C8 C 0.8339(5) 0.2862(4) 1.1637(3) 0.0583(6) Uani 0.693(3) 1 d PDU A 1
H8A H 0.8537 0.3488 1.1931 0.087 Uiso 0.693(3) 1 calc PR A 1
H8B H 0.9275 0.2511 1.1633 0.087 Uiso 0.693(3) 1 calc PR A 1
H8C H 0.7645 0.2539 1.2105 0.087 Uiso 0.693(3) 1 calc PR A 1
C6' C 0.6272(10) 0.3189(5) 1.0315(4) 0.0531(2) Uani 0.307(3) 1 d PDU A 2
H6'1 H 0.5923 0.2610 1.0663 0.064 Uiso 0.307(3) 1 calc PR A 2
H6'2 H 0.7341 0.3108 1.0177 0.064 Uiso 0.307(3) 1 calc PR A 2
C7' C 0.6106(10) 0.3998(5) 1.1119(4) 0.0539(2) Uani 0.307(3) 1 d PDU A 2
H7'1 H 0.5043 0.4075 1.1278 0.065 Uiso 0.307(3) 1 calc PR A 2
H7'2 H 0.6450 0.4582 1.0779 0.065 Uiso 0.307(3) 1 calc PR A 2
C8' C 0.7053(11) 0.3804(7) 1.2228(5) 0.0583(6) Uani 0.307(3) 1 d PDU A 2
H8'1 H 0.6695 0.3233 1.2570 0.087 Uiso 0.307(3) 1 calc PR A 2
H8'2 H 0.6948 0.4329 1.2736 0.087 Uiso 0.307(3) 1 calc PR A 2
H8'3 H 0.8104 0.3730 1.2068 0.087 Uiso 0.307(3) 1 calc PR A 2
Gd1 Gd 0.270917(10) 0.133323(6) 0.938191(7) 0.01423(3) Uani 1 1 d . . .
O1 O 0.6401(2) 0.49570(12) 0.65307(14) 0.0354(4) Uani 1 1 d . . .
O2 O 0.49302(17) 0.40100(11) 0.54265(12) 0.0240(4) Uani 1 1 d . . .
O3 O 0.26921(18) 0.26104(11) 0.59196(12) 0.0251(4) Uani 1 1 d . . .
O4 O 0.25327(19) 0.16835(11) 0.74078(12) 0.0283(4) Uani 1 1 d . A .
O5 O 0.15040(18) 0.04638(12) 1.08603(13) 0.0307(4) Uani 1 1 d . . .
O6 O -0.04142(18) -0.04927(12) 1.12995(13) 0.0321(4) Uani 1 1 d . . .
N1 N 0.4353(2) 0.27397(13) 0.87582(14) 0.0244(4) Uani 1 1 d . A .
N2 N 0.5850(2) 0.39448(15) 0.84113(16) 0.0304(5) Uani 1 1 d . A .
H2 H 0.6520 0.4385 0.8522 0.036 Uiso 1 1 calc R . .
C1 C 0.5394(3) 0.33320(18) 0.92031(18) 0.0327(6) Uani 1 1 d D . .
C2 C 0.5075(3) 0.37547(14) 0.74016(19) 0.0225(5) Uani 1 1 d . . .
C3 C 0.4133(2) 0.30016(15) 0.76317(16) 0.0187(4) Uani 1 1 d . A .
C4 C 0.5469(2) 0.42867(15) 0.63692(18) 0.0216(5) Uani 1 1 d . A .
C5 C 0.3042(2) 0.24098(14) 0.69246(16) 0.0182(4) Uani 1 1 d . . .
C9 C 0.0312(2) -0.00119(15) 1.06233(17) 0.0229(5) Uani 1 1 d . . .
O7 O 0.0590(2) 0.24586(14) 0.90445(17) 0.0490(5) Uani 1 1 d . . .
H1W H -0.0150 0.2191 0.8729 0.074 Uiso 1 1 d R . .
H2W H 0.0758 0.2987 0.8769 0.074 Uiso 1 1 d R . .
O8 O 0.0947(3) 0.43298(18) 0.8486(2) 0.0693(7) Uani 1 1 d . . .
H3W H 0.0181 0.4586 0.8734 0.104 Uiso 1 1 d R . .
H4W H 0.1012 0.4439 0.7803 0.104 Uiso 1 1 d R . .
O9 O 0.1729(2) 0.02523(13) 0.59289(17) 0.0444(5) Uani 1 1 d . . .
H5W H 0.1865 0.0705 0.6367 0.067 Uiso 1 1 d R A .
H6W H 0.2000 0.0378 0.5287 0.067 Uiso 1 1 d R . .


_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
C6 C7 1.504(5) . ?
C6 C1 1.505(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.520(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C6' C7' 1.495(7) . ?
C6' C1 1.506(6) . ?
C6' H6'1 0.9700 . ?
C6' H6'2 0.9700 . ?
C7' C8' 1.544(7) . ?
C7' H7'1 0.9700 . ?
C7' H7'2 0.9700 . ?
C8' H8'1 0.9600 . ?
C8' H8'2 0.9600 . ?
C8' H8'3 0.9600 . ?
Gd1 O2 2.3089(15) 4_566 ?
Gd1 O3 2.3520(14) 4_566 ?
Gd1 O1 2.3701(16) 2_646 ?
Gd1 O4 2.3883(15) . ?
Gd1 O5 2.4262(16) . ?
Gd1 O6 2.4405(16) 3_557 ?
Gd1 O7 2.4625(19) . ?
Gd1 N1 2.5814(18) . ?
O1 C4 1.258(3) . ?
O1 Gd1 2.3701(16) 2_656 ?
O2 C4 1.253(3) . ?
O2 Gd1 2.3089(15) 4_565 ?
O3 C5 1.247(2) . ?
O3 Gd1 2.3520(14) 4_565 ?
O4 C5 1.265(3) . ?
O4 O9 2.737(2) . ?
O5 C9 1.263(3) . ?
O6 C9 1.250(3) . ?
O6 Gd1 2.4405(16) 3_557 ?
N1 C1 1.327(3) . ?
N1 C3 1.389(3) . ?
N2 C1 1.351(3) . ?
N2 C2 1.372(3) . ?
N2 H2 0.8600 . ?
C2 C3 1.381(3) . ?
C2 C4 1.491(3) . ?
C3 C5 1.494(3) . ?
C9 C9 1.550(4) 3_557 ?
O7 O8 2.735(3) . ?
O7 H1W 0.8243 . ?
O7 H2W 0.8281 . ?
O8 H3W 0.8313 . ?
O8 H4W 0.8289 . ?
O9 H5W 0.8260 . ?
O9 H6W 0.8286 . ?

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
C7 C6 C1 109.9(3) . . ?
C7 C6 H6A 109.7 . . ?
C1 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
C1 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C6 C7 C8 112.5(3) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C7' C6' C1 113.1(5) . . ?
C7' C6' H6'1 109.0 . . ?
C1 C6' H6'1 109.0 . . ?
C7' C6' H6'2 109.0 . . ?
C1 C6' H6'2 109.0 . . ?
H6'1 C6' H6'2 107.8 . . ?
C6' C7' C8' 110.0(6) . . ?
C6' C7' H7'1 109.7 . . ?
C8' C7' H7'1 109.7 . . ?
C6' C7' H7'2 109.7 . . ?
C8' C7' H7'2 109.7 . . ?
H7'1 C7' H7'2 108.2 . . ?
C7' C8' H8'1 109.5 . . ?
C7' C8' H8'2 109.5 . . ?
H8'1 C8' H8'2 109.5 . . ?
C7' C8' H8'3 109.5 . . ?
H8'1 C8' H8'3 109.5 . . ?
H8'2 C8' H8'3 109.5 . . ?
O2 Gd1 O3 75.89(5) 4_566 4_566 ?
O2 Gd1 O1 77.49(5) 4_566 2_646 ?
O3 Gd1 O1 152.27(5) 4_566 2_646 ?
O2 Gd1 O4 125.31(6) 4_566 . ?
O3 Gd1 O4 128.78(5) 4_566 . ?
O1 Gd1 O4 74.17(6) 2_646 . ?
O2 Gd1 O5 84.10(5) 4_566 . ?
O3 Gd1 O5 74.79(6) 4_566 . ?
O1 Gd1 O5 94.92(6) 2_646 . ?
O4 Gd1 O5 143.45(5) . . ?
O2 Gd1 O6 137.61(6) 4_566 3_557 ?
O3 Gd1 O6 121.56(6) 4_566 3_557 ?
O1 Gd1 O6 74.99(6) 2_646 3_557 ?
O4 Gd1 O6 76.45(5) . 3_557 ?
O5 Gd1 O6 67.01(5) . 3_557 ?
O2 Gd1 O7 146.50(6) 4_566 . ?
O3 Gd1 O7 71.59(6) 4_566 . ?
O1 Gd1 O7 135.74(6) 2_646 . ?
O4 Gd1 O7 72.47(6) . . ?
O5 Gd1 O7 94.87(6) . . ?
O6 Gd1 O7 69.57(6) 3_557 . ?
O2 Gd1 N1 80.93(6) 4_566 . ?
O3 Gd1 N1 76.39(6) 4_566 . ?
O1 Gd1 N1 106.93(6) 2_646 . ?
O4 Gd1 N1 64.53(5) . . ?
O5 Gd1 N1 149.98(5) . . ?
O6 Gd1 N1 137.97(5) 3_557 . ?
O7 Gd1 N1 83.82(7) . . ?
C4 O1 Gd1 140.45(14) . 2_656 ?
C4 O2 Gd1 144.40(14) . 4_565 ?
C5 O3 Gd1 150.67(14) . 4_565 ?
C5 O4 Gd1 127.15(13) . . ?
C5 O4 O9 112.93(13) . . ?
Gd1 O4 O9 118.50(7) . . ?
C9 O5 Gd1 119.71(13) . . ?
C9 O6 Gd1 119.48(13) . 3_557 ?
C1 N1 C3 105.90(18) . . ?
C1 N1 Gd1 138.84(14) . . ?
C3 N1 Gd1 115.26(13) . . ?
C1 N2 C2 109.24(19) . . ?
C1 N2 H2 125.4 . . ?
C2 N2 H2 125.4 . . ?
N1 C1 N2 110.40(19) . . ?
N1 C1 C6 127.2(3) . . ?
N2 C1 C6 122.4(3) . . ?
N1 C1 C6' 125.1(4) . . ?
N2 C1 C6' 122.4(4) . . ?
C6 C1 C6' 11.6(4) . . ?
N2 C2 C3 104.66(18) . . ?
N2 C2 C4 119.47(19) . . ?
C3 C2 C4 135.6(2) . . ?
C2 C3 N1 109.80(18) . . ?
C2 C3 C5 133.71(18) . . ?
N1 C3 C5 116.40(17) . . ?
O2 C4 O1 125.6(2) . . ?
O2 C4 C2 118.90(19) . . ?
O1 C4 C2 115.42(18) . . ?
O3 C5 O4 122.65(18) . . ?
O3 C5 C3 121.95(18) . . ?
O4 C5 C3 115.37(17) . . ?
O6 C9 O5 126.2(2) . . ?
O6 C9 C9 117.1(2) . 3_557 ?
O5 C9 C9 116.7(2) . 3_557 ?
Gd1 O7 O8 124.18(10) . . ?
Gd1 O7 H1W 110.7 . . ?
O8 O7 H1W 115.3 . . ?
Gd1 O7 H2W 119.4 . . ?
O8 O7 H2W 10.3 . . ?
H1W O7 H2W 112.6 . . ?
O7 O8 H3W 103.0 . . ?
O7 O8 H4W 115.4 . . ?
H3W O8 H4W 111.4 . . ?
O4 O9 H5W 6.8 . . ?
O4 O9 H6W 110.8 . . ?
H5W O9 H6W 112.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C6 C7 C8 -176.2(4) . . . . ?
C1 C6' C7' C8' -179.3(7) . . . . ?
O2 Gd1 O4 C5 -67.60(19) 4_566 . . . ?
O3 Gd1 O4 C5 33.1(2) 4_566 . . . ?
O1 Gd1 O4 C5 -129.13(18) 2_646 . . . ?
O5 Gd1 O4 C5 154.34(16) . . . . ?
O6 Gd1 O4 C5 152.91(18) 3_557 . . . ?
O7 Gd1 O4 C5 80.39(18) . . . . ?
N1 Gd1 O4 C5 -11.07(17) . . . . ?
O2 Gd1 O4 O9 97.76(9) 4_566 . . . ?
O3 Gd1 O4 O9 -161.53(7) 4_566 . . . ?
O1 Gd1 O4 O9 36.23(8) 2_646 . . . ?
O5 Gd1 O4 O9 -40.31(14) . . . . ?
O6 Gd1 O4 O9 -41.74(8) 3_557 . . . ?
O7 Gd1 O4 O9 -114.26(10) . . . . ?
N1 Gd1 O4 O9 154.29(10) . . . . ?
O2 Gd1 O5 C9 -147.55(17) 4_566 . . . ?
O3 Gd1 O5 C9 135.50(17) 4_566 . . . ?
O1 Gd1 O5 C9 -70.69(17) 2_646 . . . ?
O4 Gd1 O5 C9 -0.8(2) . . . . ?
O6 Gd1 O5 C9 0.71(16) 3_557 . . . ?
O7 Gd1 O5 C9 66.09(17) . . . . ?
N1 Gd1 O5 C9 152.16(16) . . . . ?
O2 Gd1 N1 C1 -38.3(2) 4_566 . . . ?
O3 Gd1 N1 C1 39.3(2) 4_566 . . . ?
O1 Gd1 N1 C1 -112.1(2) 2_646 . . . ?
O4 Gd1 N1 C1 -174.7(3) . . . . ?
O5 Gd1 N1 C1 22.8(3) . . . . ?
O6 Gd1 N1 C1 161.7(2) 3_557 . . . ?
O7 Gd1 N1 C1 111.8(3) . . . . ?
O2 Gd1 N1 C3 142.59(15) 4_566 . . . ?
O3 Gd1 N1 C3 -139.84(15) 4_566 . . . ?
O1 Gd1 N1 C3 68.73(15) 2_646 . . . ?
O4 Gd1 N1 C3 6.17(14) . . . . ?
O5 Gd1 N1 C3 -156.37(13) . . . . ?
O6 Gd1 N1 C3 -17.46(19) 3_557 . . . ?
O7 Gd1 N1 C3 -67.33(15) . . . . ?
C3 N1 C1 N2 -0.7(3) . . . . ?
Gd1 N1 C1 N2 -179.87(17) . . . . ?
C3 N1 C1 C6 -178.8(3) . . . . ?
Gd1 N1 C1 C6 2.0(5) . . . . ?
C3 N1 C1 C6' -164.7(4) . . . . ?
Gd1 N1 C1 C6' 16.1(5) . . . . ?
C2 N2 C1 N1 0.3(3) . . . . ?
C2 N2 C1 C6 178.5(3) . . . . ?
C2 N2 C1 C6' 164.8(4) . . . . ?
C7 C6 C1 N1 104.6(4) . . . . ?
C7 C6 C1 N2 -73.3(5) . . . . ?
C7 C6 C1 C6' 21(2) . . . . ?
C7' C6' C1 N1 -123.6(6) . . . . ?
C7' C6' C1 N2 74.2(8) . . . . ?
C7' C6' C1 C6 -19.2(17) . . . . ?
C1 N2 C2 C3 0.2(3) . . . . ?
C1 N2 C2 C4 -175.1(2) . . . . ?
N2 C2 C3 N1 -0.6(2) . . . . ?
C4 C2 C3 N1 173.5(2) . . . . ?
N2 C2 C3 C5 -176.7(2) . . . . ?
C4 C2 C3 C5 -2.6(4) . . . . ?
C1 N1 C3 C2 0.8(3) . . . . ?
Gd1 N1 C3 C2 -179.79(14) . . . . ?
C1 N1 C3 C5 177.67(19) . . . . ?
Gd1 N1 C3 C5 -2.9(2) . . . . ?
Gd1 O2 C4 O1 -128.1(2) 4_565 . . . ?
Gd1 O2 C4 C2 56.1(3) 4_565 . . . ?
Gd1 O1 C4 O2 21.0(4) 2_656 . . . ?
Gd1 O1 C4 C2 -163.06(17) 2_656 . . . ?
N2 C2 C4 O2 169.0(2) . . . . ?
C3 C2 C4 O2 -4.5(4) . . . . ?
N2 C2 C4 O1 -7.2(3) . . . . ?
C3 C2 C4 O1 179.3(2) . . . . ?
Gd1 O3 C5 O4 171.15(19) 4_565 . . . ?
Gd1 O3 C5 C3 -10.6(4) 4_565 . . . ?
Gd1 O4 C5 O3 -168.17(15) . . . . ?
O9 O4 C5 O3 25.8(3) . . . . ?
Gd1 O4 C5 C3 13.5(3) . . . . ?
O9 O4 C5 C3 -152.57(14) . . . . ?
C2 C3 C5 O3 -8.1(4) . . . . ?
N1 C3 C5 O3 175.91(19) . . . . ?
C2 C3 C5 O4 170.2(2) . . . . ?
N1 C3 C5 O4 -5.7(3) . . . . ?
Gd1 O6 C9 O5 179.29(18) 3_557 . . . ?
Gd1 O6 C9 C9 -0.1(3) 3_557 . . 3_557 ?
Gd1 O5 C9 O6 179.66(18) . . . . ?
Gd1 O5 C9 C9 -0.9(3) . . . 3_557 ?
O2 Gd1 O7 O8 57.93(17) 4_566 . . . ?
O3 Gd1 O7 O8 72.42(11) 4_566 . . . ?
O1 Gd1 O7 O8 -113.23(12) 2_646 . . . ?
O4 Gd1 O7 O8 -70.46(11) . . . . ?
O5 Gd1 O7 O8 144.60(11) . . . . ?
O6 Gd1 O7 O8 -152.15(12) 3_557 . . . ?
N1 Gd1 O7 O8 -5.26(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H2W O8 0.83 1.93 2.735(3) 165.2 .
O8 H4W O6 0.83 2.59 3.240(3) 136.2 4_565
O8 H4W O5 0.83 2.37 3.190(3) 170.2 4_565
O9 H5W O4 0.83 1.92 2.737(2) 170.3 .
O8 H3W O9 0.83 1.98 2.807(3) 170.8 2_556
O9 H6W O8 0.83 2.32 2.999(3) 139.7 4_565
N2 H2 O9 0.86 2.04 2.890(3) 167.7 2_656

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.791
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.146

# Attachment 'E.cif'

data_e1
_database_code_depnum_ccdc_archive 'CCDC 737323'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H20 Ce2 N2 O19 S'
_chemical_formula_weight         832.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   18.8558(19)
_cell_length_b                   6.5831(7)
_cell_length_c                   18.7543(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2328.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4666
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    4.049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2876
_exptl_absorpt_correction_T_max  0.4310
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11356
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         25.49
_reflns_number_total             4230
_reflns_number_gt                3935
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0230P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         4230
_refine_ls_number_parameters     343
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0520
_refine_ls_wR_factor_gt          0.0502
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Ce1 Ce 0.522249(14) 0.13660(4) 0.761263(16) 0.01604(8) Uani 1 1 d . . .
Ce2 Ce 0.755806(13) 0.13751(4) 0.721065(14) 0.01243(7) Uani 1 1 d . . .
S1 S 0.75929(6) 0.63599(16) 0.72195(9) 0.0143(2) Uani 1 1 d . . .
O1 O 0.4894(3) 0.8473(7) 0.5351(3) 0.0576(16) Uani 1 1 d . . .
H1W H 0.4789 0.9045 0.4971 0.086 Uiso 1 1 d R . .
H2W H 0.4703 0.7335 0.5378 0.086 Uiso 1 1 d R . .
O2 O 0.0090(2) 0.8447(7) 0.9217(3) 0.0504(13) Uani 1 1 d . . .
H3W H 0.0338 0.7544 0.9400 0.076 Uiso 1 1 d R . .
H4W H -0.0084 0.9199 0.9526 0.076 Uiso 1 1 d R . .
O3 O 0.49023(17) 0.4529(5) 0.69028(19) 0.0216(8) Uani 1 1 d . . .
H5W H 0.5167 0.4358 0.6554 0.032 Uiso 1 1 d R . .
H6W H 0.4508 0.4957 0.6775 0.032 Uiso 1 1 d R . .
O4 O 0.5839(2) 0.4363(6) 0.8196(2) 0.0291(10) Uani 1 1 d . . .
H7W H 0.6150 0.5050 0.7996 0.044 Uiso 1 1 d R . .
H8W H 0.5563 0.5100 0.8425 0.044 Uiso 1 1 d R . .
O5 O 0.56523(18) -0.1913(6) 0.7118(3) 0.0394(11) Uani 1 1 d . . .
H9W H 0.6064 -0.2250 0.7004 0.059 Uiso 1 1 d R . .
H10W H 0.5381 -0.2910 0.7088 0.059 Uiso 1 1 d R . .
O6 O 0.4452(2) -0.1463(6) 0.8103(2) 0.0337(10) Uani 1 1 d . . .
H11W H 0.4532 -0.2249 0.8437 0.051 Uiso 1 1 d R . .
H12W H 0.4066 -0.1723 0.7908 0.051 Uiso 1 1 d R . .
O7 O 0.44600(19) 0.0247(6) 0.66041(19) 0.0282(9) Uani 1 1 d . . .
H13W H 0.4646 -0.0589 0.6332 0.042 Uiso 1 1 d R . .
H14W H 0.4046 -0.0075 0.6702 0.042 Uiso 1 1 d R . .
O8 O 0.5607(2) 0.3178(7) 0.5782(2) 0.0420(12) Uani 1 1 d . . .
O9 O 0.62757(18) 0.2133(6) 0.67046(19) 0.0207(8) Uani 1 1 d . . .
O10 O 0.9115(2) 0.0080(7) 0.5390(2) 0.0392(11) Uani 1 1 d . . .
O11 O 0.85532(19) 0.0415(6) 0.6433(2) 0.0240(9) Uani 1 1 d . . .
O12 O 0.95198(19) 0.2287(6) 0.8676(2) 0.0276(9) Uani 1 1 d . . .
O13 O 0.87468(18) 0.2315(6) 0.77942(17) 0.0210(8) Uani 1 1 d . . .
O14 O 0.65075(17) 0.0556(6) 0.7976(2) 0.0190(8) Uani 1 1 d . . .
O15 O 0.58673(18) 0.0264(6) 0.8956(2) 0.0271(9) Uani 1 1 d . . .
O16 O 0.79617(17) 0.4996(5) 0.67133(19) 0.0198(8) Uani 1 1 d . . .
O17 O 0.72073(18) 0.4998(5) 0.77141(19) 0.0196(8) Uani 1 1 d . . .
O18 O 0.70995(17) 0.7746(5) 0.68437(19) 0.0182(8) Uani 1 1 d . . .
O19 O 0.80889(16) 0.7689(5) 0.7609(2) 0.0207(7) Uani 1 1 d . . .
N1 N 0.7356(2) 0.1380(6) 0.5807(3) 0.0171(10) Uani 1 1 d . . .
N2 N 0.7684(2) 0.1269(6) 0.8644(2) 0.0143(10) Uani 1 1 d . . .
C1 C 0.8902(3) 0.2104(9) 0.8447(3) 0.0168(11) Uani 1 1 d . . .
C2 C 0.8313(3) 0.1648(8) 0.8961(3) 0.0148(11) Uani 1 1 d . . .
C3 C 0.8394(3) 0.1679(8) 0.9691(3) 0.0185(12) Uani 1 1 d . . .
H3 H 0.8836 0.1925 0.9893 0.022 Uiso 1 1 calc R . .
C4 C 0.7811(3) 0.1340(8) 1.0115(3) 0.0221(13) Uani 1 1 d . . .
H4 H 0.7855 0.1373 1.0609 0.027 Uiso 1 1 calc R . .
C5 C 0.7158(3) 0.0948(9) 0.9804(3) 0.0217(13) Uani 1 1 d . . .
H5 H 0.6758 0.0724 1.0084 0.026 Uiso 1 1 calc R . .
C6 C 0.7118(3) 0.0899(8) 0.9069(3) 0.0160(11) Uani 1 1 d . . .
C7 C 0.6444(3) 0.0536(8) 0.8656(3) 0.0165(12) Uani 1 1 d . . .
C8 C 0.8577(3) 0.0445(9) 0.5755(3) 0.0202(12) Uani 1 1 d . . .
C9 C 0.7896(3) 0.0952(8) 0.5378(3) 0.0169(12) Uani 1 1 d . . .
C10 C 0.7828(3) 0.0942(8) 0.4635(3) 0.0221(13) Uani 1 1 d . . .
H10 H 0.8219 0.0698 0.4345 0.026 Uiso 1 1 calc R . .
C11 C 0.7170(3) 0.1301(8) 0.4343(3) 0.0233(13) Uani 1 1 d . . .
H11 H 0.7106 0.1249 0.3851 0.028 Uiso 1 1 calc R . .
C12 C 0.6605(3) 0.1742(8) 0.4789(3) 0.0211(12) Uani 1 1 d . . .
H12 H 0.6156 0.1995 0.4602 0.025 Uiso 1 1 calc R . .
C13 C 0.6722(3) 0.1797(8) 0.5522(3) 0.0182(12) Uani 1 1 d . . .
C14 C 0.6149(3) 0.2421(8) 0.6035(3) 0.0197(12) 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
Ce1 O5 2.485(4) . ?
Ce1 O7 2.488(4) . ?
Ce1 O6 2.535(4) . ?
Ce1 O4 2.538(4) . ?
Ce1 O3 2.544(4) . ?
Ce1 O12 2.553(4) 3_455 ?
Ce1 O14 2.573(3) . ?
Ce1 O9 2.664(4) . ?
Ce1 O15 2.891(4) . ?
Ce1 O13 2.935(3) 3_455 ?
Ce1 C7 3.071(5) . ?
Ce2 O11 2.459(4) . ?
Ce2 O14 2.504(3) . ?
Ce2 O13 2.570(4) . ?
Ce2 O18 2.632(3) 1_545 ?
Ce2 O9 2.645(3) . ?
Ce2 O17 2.649(3) . ?
Ce2 N1 2.661(5) . ?
Ce2 O16 2.670(4) . ?
Ce2 N2 2.700(4) . ?
Ce2 O19 2.729(3) 1_545 ?
Ce2 S1 3.2823(11) . ?
Ce2 S1 3.3022(11) 1_545 ?
S1 O19 1.475(4) . ?
S1 O16 1.480(4) . ?
S1 O17 1.481(4) . ?
S1 O18 1.482(3) . ?
S1 Ce2 3.3022(11) 1_565 ?
O1 H1W 0.8309 . ?
O1 H2W 0.8323 . ?
O2 H3W 0.8310 . ?
O2 H4W 0.8301 . ?
O3 H5W 0.8307 . ?
O3 H6W 0.8306 . ?
O4 H7W 0.8304 . ?
O4 H8W 0.8309 . ?
O5 H9W 0.8352 . ?
O5 H10W 0.8346 . ?
O6 H11W 0.8277 . ?
O6 H12W 0.8318 . ?
O7 H13W 0.8284 . ?
O7 H14W 0.8300 . ?
O8 C14 1.232(6) . ?
O9 C14 1.292(6) . ?
O10 C8 1.246(6) . ?
O11 C8 1.274(7) . ?
O12 C1 1.247(6) . ?
O12 Ce1 2.553(4) 3 ?
O13 C1 1.266(6) . ?
O13 Ce1 2.935(3) 3 ?
O14 C7 1.281(7) . ?
O15 C7 1.237(6) . ?
O18 Ce2 2.632(3) 1_565 ?
O19 Ce2 2.729(3) 1_565 ?
N1 C9 1.327(7) . ?
N1 C13 1.338(7) . ?
N2 C2 1.350(7) . ?
N2 C6 1.353(7) . ?
C1 C2 1.500(7) . ?
C2 C3 1.377(8) . ?
C3 C4 1.375(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.508(7) . ?
C8 C9 1.503(8) . ?
C9 C10 1.399(8) . ?
C10 C11 1.377(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.394(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.503(7) . ?

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
O5 Ce1 O7 69.36(13) . . ?
O5 Ce1 O6 71.58(14) . . ?
O7 Ce1 O6 74.13(12) . . ?
O5 Ce1 O4 133.37(12) . . ?
O7 Ce1 O4 145.38(12) . . ?
O6 Ce1 O4 132.64(13) . . ?
O5 Ce1 O3 126.37(14) . . ?
O7 Ce1 O3 72.98(11) . . ?
O6 Ce1 O3 130.92(12) . . ?
O4 Ce1 O3 72.44(12) . . ?
O5 Ce1 O12 139.68(14) . 3_455 ?
O7 Ce1 O12 113.37(12) . 3_455 ?
O6 Ce1 O12 71.01(13) . 3_455 ?
O4 Ce1 O12 68.34(13) . 3_455 ?
O3 Ce1 O12 90.06(12) . 3_455 ?
O5 Ce1 O14 67.15(12) . . ?
O7 Ce1 O14 133.17(12) . . ?
O6 Ce1 O14 106.97(12) . . ?
O4 Ce1 O14 67.39(13) . . ?
O3 Ce1 O14 122.11(11) . . ?
O12 Ce1 O14 110.75(12) 3_455 . ?
O5 Ce1 O9 71.52(13) . . ?
O7 Ce1 O9 90.05(11) . . ?
O6 Ce1 O9 142.96(13) . . ?
O4 Ce1 O9 77.70(12) . . ?
O3 Ce1 O9 71.78(11) . . ?
O12 Ce1 O9 145.11(13) 3_455 . ?
O14 Ce1 O9 60.42(11) . . ?
O5 Ce1 O15 88.29(14) . . ?
O7 Ce1 O15 146.27(12) . . ?
O6 Ce1 O15 74.97(11) . . ?
O4 Ce1 O15 68.07(12) . . ?
O3 Ce1 O15 139.60(11) . . ?
O12 Ce1 O15 67.96(11) 3_455 . ?
O14 Ce1 O15 47.25(11) . . ?
O9 Ce1 O15 106.93(10) . . ?
O5 Ce1 O13 127.55(11) . 3_455 ?
O7 Ce1 O13 68.15(11) . 3_455 ?
O6 Ce1 O13 68.39(12) . 3_455 ?
O4 Ce1 O13 98.87(11) . 3_455 ?
O3 Ce1 O13 66.02(10) . 3_455 ?
O12 Ce1 O13 46.72(11) 3_455 3_455 ?
O14 Ce1 O13 157.46(11) . 3_455 ?
O9 Ce1 O13 136.46(11) . 3_455 ?
O15 Ce1 O13 111.83(9) . 3_455 ?
O5 Ce1 C7 80.72(14) . . ?
O7 Ce1 C7 149.91(13) . . ?
O6 Ce1 C7 93.91(14) . . ?
O4 Ce1 C7 61.32(13) . . ?
O3 Ce1 C7 131.07(13) . . ?
O12 Ce1 C7 87.33(13) 3_455 . ?
O14 Ce1 C7 24.25(13) . . ?
O9 Ce1 C7 83.22(12) . . ?
O15 Ce1 C7 23.71(11) . . ?
O13 Ce1 C7 133.61(11) 3_455 . ?
O11 Ce2 O14 152.61(12) . . ?
O11 Ce2 O13 69.43(12) . . ?
O14 Ce2 O13 119.85(11) . . ?
O11 Ce2 O18 82.09(12) . 1_545 ?
O14 Ce2 O18 72.22(11) . 1_545 ?
O13 Ce2 O18 128.05(11) . 1_545 ?
O11 Ce2 O9 122.24(12) . . ?
O14 Ce2 O9 61.51(12) . . ?
O13 Ce2 O9 154.78(11) . . ?
O18 Ce2 O9 77.12(11) 1_545 . ?
O11 Ce2 O17 129.30(13) . . ?
O14 Ce2 O17 78.00(12) . . ?
O13 Ce2 O17 81.33(11) . . ?
O18 Ce2 O17 145.93(10) 1_545 . ?
O9 Ce2 O17 74.33(11) . . ?
O11 Ce2 N1 61.51(13) . . ?
O14 Ce2 N1 116.99(13) . . ?
O13 Ce2 N1 123.10(12) . . ?
O18 Ce2 N1 72.26(12) 1_545 . ?
O9 Ce2 N1 60.90(12) . . ?
O17 Ce2 N1 108.41(12) . . ?
O11 Ce2 O16 78.75(12) . . ?
O14 Ce2 O16 128.14(11) . . ?
O13 Ce2 O16 71.65(11) . . ?
O18 Ce2 O16 144.34(12) 1_545 . ?
O9 Ce2 O16 88.11(11) . . ?
O17 Ce2 O16 52.55(9) . . ?
N1 Ce2 O16 72.18(12) . . ?
O11 Ce2 N2 121.09(13) . . ?
O14 Ce2 N2 59.58(12) . . ?
O13 Ce2 N2 60.36(11) . . ?
O18 Ce2 N2 105.41(12) 1_545 . ?
O9 Ce2 N2 116.27(12) . . ?
O17 Ce2 N2 71.97(12) . . ?
N1 Ce2 N2 176.51(14) . . ?
O16 Ce2 N2 110.24(12) . . ?
O11 Ce2 O19 69.76(13) . 1_545 ?
O14 Ce2 O19 86.66(11) . 1_545 ?
O13 Ce2 O19 77.15(11) . 1_545 ?
O18 Ce2 O19 52.06(10) 1_545 1_545 ?
O9 Ce2 O19 126.96(11) . 1_545 ?
O17 Ce2 O19 142.59(12) . 1_545 ?
N1 Ce2 O19 108.96(13) . 1_545 ?
O16 Ce2 O19 141.70(9) . 1_545 ?
N2 Ce2 O19 70.84(13) . 1_545 ?
O11 Ce2 S1 104.17(10) . . ?
O14 Ce2 S1 103.18(9) . . ?
O13 Ce2 S1 74.91(9) . . ?
O18 Ce2 S1 156.25(8) 1_545 . ?
O9 Ce2 S1 80.30(9) . . ?
O17 Ce2 S1 26.24(8) . . ?
N1 Ce2 S1 90.38(10) . . ?
O16 Ce2 S1 26.32(8) . . ?
N2 Ce2 S1 91.10(9) . . ?
O19 Ce2 S1 151.66(8) 1_545 . ?
O11 Ce2 S1 74.38(10) . 1_545 ?
O14 Ce2 S1 78.33(9) . 1_545 ?
O13 Ce2 S1 102.78(9) . 1_545 ?
O18 Ce2 S1 25.90(7) 1_545 1_545 ?
O9 Ce2 S1 102.03(9) . 1_545 ?
O17 Ce2 S1 154.60(8) . 1_545 ?
N1 Ce2 S1 90.52(9) . 1_545 ?
O16 Ce2 S1 152.69(8) . 1_545 ?
N2 Ce2 S1 88.12(9) . 1_545 ?
O19 Ce2 S1 26.16(8) 1_545 1_545 ?
S1 Ce2 S1 177.64(4) . 1_545 ?
O19 S1 O16 112.3(2) . . ?
O19 S1 O17 111.1(2) . . ?
O16 S1 O17 105.37(18) . . ?
O19 S1 O18 105.58(18) . . ?
O16 S1 O18 111.3(2) . . ?
O17 S1 O18 111.3(2) . . ?
O19 S1 Ce2 127.48(14) . . ?
O16 S1 Ce2 53.11(14) . . ?
O17 S1 Ce2 52.27(14) . . ?
O18 S1 Ce2 126.93(15) . . ?
O19 S1 Ce2 54.68(13) . 1_565 ?
O16 S1 Ce2 127.78(16) . 1_565 ?
O17 S1 Ce2 126.78(15) . 1_565 ?
O18 S1 Ce2 50.89(14) . 1_565 ?
Ce2 S1 Ce2 177.64(4) . 1_565 ?
H1W O1 H2W 110.9 . . ?
H3W O2 H4W 111.1 . . ?
Ce1 O3 H5W 99.1 . . ?
Ce1 O3 H6W 129.9 . . ?
H5W O3 H6W 111.0 . . ?
Ce1 O4 H7W 123.5 . . ?
Ce1 O4 H8W 113.0 . . ?
H7W O4 H8W 110.9 . . ?
Ce1 O5 H9W 129.0 . . ?
Ce1 O5 H10W 120.6 . . ?
H9W O5 H10W 110.1 . . ?
Ce1 O6 H11W 129.0 . . ?
Ce1 O6 H12W 119.6 . . ?
H11W O6 H12W 111.3 . . ?
Ce1 O7 H13W 114.9 . . ?
Ce1 O7 H14W 116.8 . . ?
H13W O7 H14W 111.4 . . ?
C14 O9 Ce2 123.0(3) . . ?
C14 O9 Ce1 120.8(3) . . ?
Ce2 O9 Ce1 114.61(13) . . ?
C8 O11 Ce2 128.0(3) . . ?
C1 O12 Ce1 104.5(3) . 3 ?
C1 O13 Ce2 125.9(3) . . ?
C1 O13 Ce1 85.7(3) . 3 ?
Ce2 O13 Ce1 148.08(13) . 3 ?
C7 O14 Ce2 130.3(3) . . ?
C7 O14 Ce1 100.2(3) . . ?
Ce2 O14 Ce1 123.28(15) . . ?
C7 O15 Ce1 86.3(3) . . ?
S1 O16 Ce2 100.58(17) . . ?
S1 O17 Ce2 101.50(18) . . ?
S1 O18 Ce2 103.21(17) . 1_565 ?
S1 O19 Ce2 99.16(17) . 1_565 ?
C9 N1 C13 119.2(5) . . ?
C9 N1 Ce2 119.2(4) . . ?
C13 N1 Ce2 121.5(3) . . ?
C2 N2 C6 117.9(5) . . ?
C2 N2 Ce2 120.7(3) . . ?
C6 N2 Ce2 121.4(3) . . ?
O12 C1 O13 122.5(5) . . ?
O12 C1 C2 119.3(5) . . ?
O13 C1 C2 118.2(4) . . ?
N2 C2 C3 122.4(5) . . ?
N2 C2 C1 113.9(4) . . ?
C3 C2 C1 123.6(5) . . ?
C4 C3 C2 119.0(5) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.8(5) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 118.2(6) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
N2 C6 C5 122.6(5) . . ?
N2 C6 C7 113.0(5) . . ?
C5 C6 C7 124.2(5) . . ?
O15 C7 O14 122.5(5) . . ?
O15 C7 C6 122.0(5) . . ?
O14 C7 C6 115.5(4) . . ?
O15 C7 Ce1 70.0(3) . . ?
O14 C7 Ce1 55.5(3) . . ?
C6 C7 Ce1 158.7(4) . . ?
O10 C8 O11 125.0(5) . . ?
O10 C8 C9 118.7(5) . . ?
O11 C8 C9 116.3(5) . . ?
N1 C9 C10 122.2(5) . . ?
N1 C9 C8 114.7(5) . . ?
C10 C9 C8 123.0(5) . . ?
C11 C10 C9 118.6(6) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 119.2(5) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C13 118.7(5) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
N1 C13 C12 122.0(5) . . ?
N1 C13 C14 116.3(5) . . ?
C12 C13 C14 121.7(5) . . ?
O8 C14 O9 125.9(5) . . ?
O8 C14 C13 117.4(5) . . ?
O9 C14 C13 116.7(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O11 Ce2 S1 O19 -76.0(2) . . . . ?
O14 Ce2 S1 O19 105.5(2) . . . . ?
O13 Ce2 S1 O19 -12.3(2) . . . . ?
O18 Ce2 S1 O19 -178.8(3) 1_545 . . . ?
O9 Ce2 S1 O19 163.0(2) . . . . ?
O17 Ce2 S1 O19 88.9(3) . . . . ?
N1 Ce2 S1 O19 -136.6(2) . . . . ?
O16 Ce2 S1 O19 -91.3(3) . . . . ?
N2 Ce2 S1 O19 46.5(2) . . . . ?
O19 Ce2 S1 O19 -2.46(15) 1_545 . . . ?
S1 Ce2 S1 O19 -24.2(16) 1_545 . . . ?
O11 Ce2 S1 O16 15.3(2) . . . . ?
O14 Ce2 S1 O16 -163.18(19) . . . . ?
O13 Ce2 S1 O16 79.03(19) . . . . ?
O18 Ce2 S1 O16 -87.4(3) 1_545 . . . ?
O9 Ce2 S1 O16 -105.65(19) . . . . ?
O17 Ce2 S1 O16 -179.8(3) . . . . ?
N1 Ce2 S1 O16 -45.3(2) . . . . ?
N2 Ce2 S1 O16 137.9(2) . . . . ?
O19 Ce2 S1 O16 88.9(3) 1_545 . . . ?
S1 Ce2 S1 O16 67.2(15) 1_545 . . . ?
O11 Ce2 S1 O17 -164.9(2) . . . . ?
O14 Ce2 S1 O17 16.6(2) . . . . ?
O13 Ce2 S1 O17 -101.17(19) . . . . ?
O18 Ce2 S1 O17 92.4(3) 1_545 . . . ?
O9 Ce2 S1 O17 74.14(19) . . . . ?
N1 Ce2 S1 O17 134.5(2) . . . . ?
O16 Ce2 S1 O17 179.8(3) . . . . ?
N2 Ce2 S1 O17 -42.3(2) . . . . ?
O19 Ce2 S1 O17 -91.3(3) 1_545 . . . ?
S1 Ce2 S1 O17 -113.0(15) 1_545 . . . ?
O11 Ce2 S1 O18 105.6(2) . . . . ?
O14 Ce2 S1 O18 -72.9(2) . . . . ?
O13 Ce2 S1 O18 169.3(2) . . . . ?
O18 Ce2 S1 O18 2.82(16) 1_545 . . . ?
O9 Ce2 S1 O18 -15.4(2) . . . . ?
O17 Ce2 S1 O18 -89.5(3) . . . . ?
N1 Ce2 S1 O18 45.0(2) . . . . ?
O16 Ce2 S1 O18 90.3(3) . . . . ?
N2 Ce2 S1 O18 -131.9(2) . . . . ?
O19 Ce2 S1 O18 179.1(3) 1_545 . . . ?
S1 Ce2 S1 O18 157.4(14) 1_545 . . . ?
O11 Ce2 S1 Ce2 128.2(15) . . . 1_565 ?
O14 Ce2 S1 Ce2 -50.4(15) . . . 1_565 ?
O13 Ce2 S1 Ce2 -168.1(15) . . . 1_565 ?
O18 Ce2 S1 Ce2 25.4(16) 1_545 . . 1_565 ?
O9 Ce2 S1 Ce2 7.2(15) . . . 1_565 ?
O17 Ce2 S1 Ce2 -67.0(15) . . . 1_565 ?
N1 Ce2 S1 Ce2 67.5(15) . . . 1_565 ?
O16 Ce2 S1 Ce2 112.8(15) . . . 1_565 ?
N2 Ce2 S1 Ce2 -109.3(15) . . . 1_565 ?
O19 Ce2 S1 Ce2 -158.3(14) 1_545 . . 1_565 ?
S1 Ce2 S1 Ce2 180.00(2) 1_545 . . 1_565 ?
O11 Ce2 O9 C14 -13.9(5) . . . . ?
O14 Ce2 O9 C14 -162.4(5) . . . . ?
O13 Ce2 O9 C14 97.4(5) . . . . ?
O18 Ce2 O9 C14 -85.8(4) 1_545 . . . ?
O17 Ce2 O9 C14 113.0(4) . . . . ?
N1 Ce2 O9 C14 -9.1(4) . . . . ?
O16 Ce2 O9 C14 61.5(4) . . . . ?
N2 Ce2 O9 C14 173.2(4) . . . . ?
O19 Ce2 O9 C14 -101.8(4) 1_545 . . . ?
S1 Ce2 O9 C14 86.8(4) . . . . ?
S1 Ce2 O9 C14 -92.9(4) 1_545 . . . ?
O11 Ce2 O9 Ce1 151.68(15) . . . . ?
O14 Ce2 O9 Ce1 3.24(13) . . . . ?
O13 Ce2 O9 Ce1 -96.9(3) . . . . ?
O18 Ce2 O9 Ce1 79.81(15) 1_545 . . . ?
O17 Ce2 O9 Ce1 -81.40(15) . . . . ?
N1 Ce2 O9 Ce1 156.5(2) . . . . ?
O16 Ce2 O9 Ce1 -132.90(15) . . . . ?
N2 Ce2 O9 Ce1 -21.2(2) . . . . ?
O19 Ce2 O9 Ce1 63.8(2) 1_545 . . . ?
S1 Ce2 O9 Ce1 -107.61(14) . . . . ?
S1 Ce2 O9 Ce1 72.69(14) 1_545 . . . ?
O5 Ce1 O9 C14 89.1(4) . . . . ?
O7 Ce1 O9 C14 21.0(4) . . . . ?
O6 Ce1 O9 C14 84.0(4) . . . . ?
O4 Ce1 O9 C14 -126.4(4) . . . . ?
O3 Ce1 O9 C14 -51.1(4) . . . . ?
O12 Ce1 O9 C14 -113.1(4) 3_455 . . . ?
O14 Ce1 O9 C14 162.8(4) . . . . ?
O15 Ce1 O9 C14 171.4(4) . . . . ?
O13 Ce1 O9 C14 -36.4(5) 3_455 . . . ?
C7 Ce1 O9 C14 171.6(4) . . . . ?
O5 Ce1 O9 Ce2 -76.86(17) . . . . ?
O7 Ce1 O9 Ce2 -145.02(16) . . . . ?
O6 Ce1 O9 Ce2 -81.9(2) . . . . ?
O4 Ce1 O9 Ce2 67.63(15) . . . . ?
O3 Ce1 O9 Ce2 142.94(18) . . . . ?
O12 Ce1 O9 Ce2 81.0(2) 3_455 . . . ?
O14 Ce1 O9 Ce2 -3.19(13) . . . . ?
O15 Ce1 O9 Ce2 5.40(18) . . . . ?
O13 Ce1 O9 Ce2 157.61(11) 3_455 . . . ?
C7 Ce1 O9 Ce2 5.58(16) . . . . ?
O14 Ce2 O11 C8 99.1(5) . . . . ?
O13 Ce2 O11 C8 -145.3(5) . . . . ?
O18 Ce2 O11 C8 78.9(5) 1_545 . . . ?
O9 Ce2 O11 C8 9.6(5) . . . . ?
O17 Ce2 O11 C8 -86.4(5) . . . . ?
N1 Ce2 O11 C8 4.8(4) . . . . ?
O16 Ce2 O11 C8 -70.9(5) . . . . ?
N2 Ce2 O11 C8 -177.9(4) . . . . ?
O19 Ce2 O11 C8 131.3(5) 1_545 . . . ?
S1 Ce2 O11 C8 -77.8(5) . . . . ?
S1 Ce2 O11 C8 104.2(5) 1_545 . . . ?
O11 Ce2 O13 C1 -139.3(5) . . . . ?
O14 Ce2 O13 C1 12.1(5) . . . . ?
O18 Ce2 O13 C1 -78.0(4) 1_545 . . . ?
O9 Ce2 O13 C1 98.0(5) . . . . ?
O17 Ce2 O13 C1 82.9(4) . . . . ?
N1 Ce2 O13 C1 -170.8(4) . . . . ?
O16 Ce2 O13 C1 136.2(4) . . . . ?
N2 Ce2 O13 C1 8.7(4) . . . . ?
O19 Ce2 O13 C1 -66.3(4) 1_545 . . . ?
S1 Ce2 O13 C1 108.9(4) . . . . ?
S1 Ce2 O13 C1 -71.6(4) 1_545 . . . ?
O11 Ce2 O13 Ce1 32.4(3) . . . 3 ?
O14 Ce2 O13 Ce1 -176.2(3) . . . 3 ?
O18 Ce2 O13 Ce1 93.6(3) 1_545 . . 3 ?
O9 Ce2 O13 Ce1 -90.4(4) . . . 3 ?
O17 Ce2 O13 Ce1 -105.5(3) . . . 3 ?
N1 Ce2 O13 Ce1 0.9(3) . . . 3 ?
O16 Ce2 O13 Ce1 -52.2(3) . . . 3 ?
N2 Ce2 O13 Ce1 -179.6(3) . . . 3 ?
O19 Ce2 O13 Ce1 105.3(3) 1_545 . . 3 ?
S1 Ce2 O13 Ce1 -79.5(3) . . . 3 ?
S1 Ce2 O13 Ce1 100.0(3) 1_545 . . 3 ?
O11 Ce2 O14 C7 104.0(5) . . . . ?
O13 Ce2 O14 C7 0.9(5) . . . . ?
O18 Ce2 O14 C7 125.1(5) 1_545 . . . ?
O9 Ce2 O14 C7 -150.2(5) . . . . ?
O17 Ce2 O14 C7 -71.7(4) . . . . ?
N1 Ce2 O14 C7 -176.4(4) . . . . ?
O16 Ce2 O14 C7 -88.5(5) . . . . ?
N2 Ce2 O14 C7 4.3(4) . . . . ?
O19 Ce2 O14 C7 74.0(4) 1_545 . . . ?
S1 Ce2 O14 C7 -79.1(4) . . . . ?
S1 Ce2 O14 C7 99.0(4) 1_545 . . . ?
O11 Ce2 O14 Ce1 -109.4(3) . . . . ?
O13 Ce2 O14 Ce1 147.44(15) . . . . ?
O18 Ce2 O14 Ce1 -88.35(17) 1_545 . . . ?
O9 Ce2 O14 Ce1 -3.65(15) . . . . ?
O17 Ce2 O14 Ce1 74.88(17) . . . . ?
N1 Ce2 O14 Ce1 -29.8(2) . . . . ?
O16 Ce2 O14 Ce1 58.1(2) . . . . ?
N2 Ce2 O14 Ce1 150.9(2) . . . . ?
O19 Ce2 O14 Ce1 -139.44(18) 1_545 . . . ?
S1 Ce2 O14 Ce1 67.45(17) . . . . ?
S1 Ce2 O14 Ce1 -114.40(16) 1_545 . . . ?
O5 Ce1 O14 C7 -120.6(3) . . . . ?
O7 Ce1 O14 C7 -143.7(3) . . . . ?
O6 Ce1 O14 C7 -59.8(3) . . . . ?
O4 Ce1 O14 C7 70.0(3) . . . . ?
O3 Ce1 O14 C7 119.7(3) . . . . ?
O12 Ce1 O14 C7 15.9(3) 3_455 . . . ?
O9 Ce1 O14 C7 158.4(4) . . . . ?
O15 Ce1 O14 C7 -10.4(3) . . . . ?
O13 Ce1 O14 C7 14.6(5) 3_455 . . . ?
O5 Ce1 O14 Ce2 84.67(19) . . . . ?
O7 Ce1 O14 Ce2 61.6(2) . . . . ?
O6 Ce1 O14 Ce2 145.52(16) . . . . ?
O4 Ce1 O14 Ce2 -84.69(18) . . . . ?
O3 Ce1 O14 Ce2 -35.0(2) . . . . ?
O12 Ce1 O14 Ce2 -138.86(17) 3_455 . . . ?
O9 Ce1 O14 Ce2 3.66(15) . . . . ?
O15 Ce1 O14 Ce2 -165.1(3) . . . . ?
O13 Ce1 O14 Ce2 -140.1(2) 3_455 . . . ?
C7 Ce1 O14 Ce2 -154.7(4) . . . . ?
O5 Ce1 O15 C7 70.5(3) . . . . ?
O7 Ce1 O15 C7 117.7(3) . . . . ?
O6 Ce1 O15 C7 141.9(3) . . . . ?
O4 Ce1 O15 C7 -68.3(3) . . . . ?
O3 Ce1 O15 C7 -81.1(3) . . . . ?
O12 Ce1 O15 C7 -142.8(3) 3_455 . . . ?
O14 Ce1 O15 C7 10.6(3) . . . . ?
O9 Ce1 O15 C7 0.5(3) . . . . ?
O13 Ce1 O15 C7 -159.3(3) 3_455 . . . ?
O19 S1 O16 Ce2 120.9(2) . . . . ?
O17 S1 O16 Ce2 -0.2(2) . . . . ?
O18 S1 O16 Ce2 -120.90(18) . . . . ?
Ce2 S1 O16 Ce2 -177.25(6) 1_565 . . . ?
O11 Ce2 O16 S1 -164.83(19) . . . . ?
O14 Ce2 O16 S1 21.0(2) . . . . ?
O13 Ce2 O16 S1 -92.97(18) . . . . ?
O18 Ce2 O16 S1 136.36(17) 1_545 . . . ?
O9 Ce2 O16 S1 71.75(18) . . . . ?
O17 Ce2 O16 S1 0.11(15) . . . . ?
N1 Ce2 O16 S1 131.7(2) . . . . ?
N2 Ce2 O16 S1 -45.6(2) . . . . ?
O19 Ce2 O16 S1 -130.02(19) 1_545 . . . ?
S1 Ce2 O16 S1 -175.26(11) 1_545 . . . ?
O19 S1 O17 Ce2 -121.74(17) . . . . ?
O16 S1 O17 Ce2 0.2(2) . . . . ?
O18 S1 O17 Ce2 120.94(18) . . . . ?
Ce2 S1 O17 Ce2 177.29(6) 1_565 . . . ?
O11 Ce2 O17 S1 19.1(2) . . . . ?
O14 Ce2 O17 S1 -163.5(2) . . . . ?
O13 Ce2 O17 S1 73.37(18) . . . . ?
O18 Ce2 O17 S1 -134.09(19) 1_545 . . . ?
O9 Ce2 O17 S1 -99.99(19) . . . . ?
N1 Ce2 O17 S1 -48.7(2) . . . . ?
O16 Ce2 O17 S1 -0.11(15) . . . . ?
N2 Ce2 O17 S1 134.9(2) . . . . ?
O19 Ce2 O17 S1 128.63(17) 1_545 . . . ?
S1 Ce2 O17 S1 174.94(11) 1_545 . . . ?
O19 S1 O18 Ce2 0.1(3) . . . 1_565 ?
O16 S1 O18 Ce2 -122.02(18) . . . 1_565 ?
O17 S1 O18 Ce2 120.77(19) . . . 1_565 ?
Ce2 S1 O18 Ce2 178.83(7) . . . 1_565 ?
O16 S1 O19 Ce2 121.37(18) . . . 1_565 ?
O17 S1 O19 Ce2 -120.87(18) . . . 1_565 ?
O18 S1 O19 Ce2 -0.1(2) . . . 1_565 ?
Ce2 S1 O19 Ce2 -178.82(7) . . . 1_565 ?
O11 Ce2 N1 C9 -2.9(4) . . . . ?
O14 Ce2 N1 C9 -151.9(4) . . . . ?
O13 Ce2 N1 C9 30.9(4) . . . . ?
O18 Ce2 N1 C9 -93.4(4) 1_545 . . . ?
O9 Ce2 N1 C9 -178.3(4) . . . . ?
O17 Ce2 N1 C9 122.4(4) . . . . ?
O16 Ce2 N1 C9 83.7(4) . . . . ?
N2 Ce2 N1 C9 -141.9(19) . . . . ?
O19 Ce2 N1 C9 -55.9(4) 1_545 . . . ?
S1 Ce2 N1 C9 103.0(4) . . . . ?
S1 Ce2 N1 C9 -74.8(4) 1_545 . . . ?
O11 Ce2 N1 C13 176.8(4) . . . . ?
O14 Ce2 N1 C13 27.8(4) . . . . ?
O13 Ce2 N1 C13 -149.4(4) . . . . ?
O18 Ce2 N1 C13 86.3(4) 1_545 . . . ?
O9 Ce2 N1 C13 1.5(4) . . . . ?
O17 Ce2 N1 C13 -57.8(4) . . . . ?
O16 Ce2 N1 C13 -96.5(4) . . . . ?
N2 Ce2 N1 C13 38(2) . . . . ?
O19 Ce2 N1 C13 123.9(4) 1_545 . . . ?
S1 Ce2 N1 C13 -77.2(4) . . . . ?
S1 Ce2 N1 C13 105.0(4) 1_545 . . . ?
O11 Ce2 N2 C2 31.7(4) . . . . ?
O14 Ce2 N2 C2 179.8(4) . . . . ?
O13 Ce2 N2 C2 -3.6(3) . . . . ?
O18 Ce2 N2 C2 121.7(4) 1_545 . . . ?
O9 Ce2 N2 C2 -155.3(4) . . . . ?
O17 Ce2 N2 C2 -93.8(4) . . . . ?
N1 Ce2 N2 C2 169.4(18) . . . . ?
O16 Ce2 N2 C2 -57.1(4) . . . . ?
O19 Ce2 N2 C2 82.2(4) 1_545 . . . ?
S1 Ce2 N2 C2 -75.6(4) . . . . ?
S1 Ce2 N2 C2 102.2(4) 1_545 . . . ?
O11 Ce2 N2 C6 -150.4(3) . . . . ?
O14 Ce2 N2 C6 -2.3(3) . . . . ?
O13 Ce2 N2 C6 174.3(4) . . . . ?
O18 Ce2 N2 C6 -60.4(4) 1_545 . . . ?
O9 Ce2 N2 C6 22.6(4) . . . . ?
O17 Ce2 N2 C6 84.1(4) . . . . ?
N1 Ce2 N2 C6 -13(2) . . . . ?
O16 Ce2 N2 C6 120.8(3) . . . . ?
O19 Ce2 N2 C6 -99.9(4) 1_545 . . . ?
S1 Ce2 N2 C6 102.3(4) . . . . ?
S1 Ce2 N2 C6 -79.9(4) 1_545 . . . ?
Ce1 O12 C1 O13 8.5(7) 3 . . . ?
Ce1 O12 C1 C2 -170.5(4) 3 . . . ?
Ce2 O13 C1 O12 168.4(4) . . . . ?
Ce1 O13 C1 O12 -7.2(5) 3 . . . ?
Ce2 O13 C1 C2 -12.5(7) . . . . ?
Ce1 O13 C1 C2 171.9(5) 3 . . . ?
C6 N2 C2 C3 -0.3(8) . . . . ?
Ce2 N2 C2 C3 177.7(4) . . . . ?
C6 N2 C2 C1 -178.1(4) . . . . ?
Ce2 N2 C2 C1 -0.2(6) . . . . ?
O12 C1 C2 N2 -173.3(5) . . . . ?
O13 C1 C2 N2 7.7(7) . . . . ?
O12 C1 C2 C3 9.0(8) . . . . ?
O13 C1 C2 C3 -170.1(5) . . . . ?
N2 C2 C3 C4 -0.9(8) . . . . ?
C1 C2 C3 C4 176.7(5) . . . . ?
C2 C3 C4 C5 0.8(8) . . . . ?
C3 C4 C5 C6 0.4(8) . . . . ?
C2 N2 C6 C5 1.7(7) . . . . ?
Ce2 N2 C6 C5 -176.3(4) . . . . ?
C2 N2 C6 C7 178.9(4) . . . . ?
Ce2 N2 C6 C7 1.0(6) . . . . ?
C4 C5 C6 N2 -1.7(8) . . . . ?
C4 C5 C6 C7 -178.7(5) . . . . ?
Ce1 O15 C7 O14 -18.8(5) . . . . ?
Ce1 O15 C7 C6 160.2(5) . . . . ?
Ce2 O14 C7 O15 173.6(4) . . . . ?
Ce1 O14 C7 O15 21.6(6) . . . . ?
Ce2 O14 C7 C6 -5.5(7) . . . . ?
Ce1 O14 C7 C6 -157.6(4) . . . . ?
Ce2 O14 C7 Ce1 152.1(4) . . . . ?
N2 C6 C7 O15 -176.7(5) . . . . ?
C5 C6 C7 O15 0.4(8) . . . . ?
N2 C6 C7 O14 2.4(7) . . . . ?
C5 C6 C7 O14 179.6(5) . . . . ?
N2 C6 C7 Ce1 -57.5(11) . . . . ?
C5 C6 C7 Ce1 119.7(9) . . . . ?
O5 Ce1 C7 O15 -107.3(3) . . . . ?
O7 Ce1 C7 O15 -101.3(4) . . . . ?
O6 Ce1 C7 O15 -36.7(3) . . . . ?
O4 Ce1 C7 O15 100.8(3) . . . . ?
O3 Ce1 C7 O15 121.8(3) . . . . ?
O12 Ce1 C7 O15 34.1(3) 3_455 . . . ?
O14 Ce1 C7 O15 -160.7(5) . . . . ?
O9 Ce1 C7 O15 -179.6(3) . . . . ?
O13 Ce1 C7 O15 26.9(4) 3_455 . . . ?
O5 Ce1 C7 O14 53.5(3) . . . . ?
O7 Ce1 C7 O14 59.4(4) . . . . ?
O6 Ce1 C7 O14 124.1(3) . . . . ?
O4 Ce1 C7 O14 -98.5(3) . . . . ?
O3 Ce1 C7 O14 -77.4(4) . . . . ?
O12 Ce1 C7 O14 -165.2(3) 3_455 . . . ?
O9 Ce1 C7 O14 -18.8(3) . . . . ?
O15 Ce1 C7 O14 160.7(5) . . . . ?
O13 Ce1 C7 O14 -172.3(3) 3_455 . . . ?
O5 Ce1 C7 C6 124.7(10) . . . . ?
O7 Ce1 C7 C6 130.7(9) . . . . ?
O6 Ce1 C7 C6 -164.7(10) . . . . ?
O4 Ce1 C7 C6 -27.2(9) . . . . ?
O3 Ce1 C7 C6 -6.2(11) . . . . ?
O12 Ce1 C7 C6 -93.9(10) 3_455 . . . ?
O14 Ce1 C7 C6 71.2(10) . . . . ?
O9 Ce1 C7 C6 52.4(10) . . . . ?
O15 Ce1 C7 C6 -128.0(11) . . . . ?
O13 Ce1 C7 C6 -101.1(10) 3_455 . . . ?
Ce2 O11 C8 O10 174.5(4) . . . . ?
Ce2 O11 C8 C9 -5.9(7) . . . . ?
C13 N1 C9 C10 0.7(8) . . . . ?
Ce2 N1 C9 C10 -179.5(4) . . . . ?
C13 N1 C9 C8 -178.2(5) . . . . ?
Ce2 N1 C9 C8 1.5(6) . . . . ?
O10 C8 C9 N1 -178.0(5) . . . . ?
O11 C8 C9 N1 2.3(7) . . . . ?
O10 C8 C9 C10 3.0(8) . . . . ?
O11 C8 C9 C10 -176.6(5) . . . . ?
N1 C9 C10 C11 -2.9(8) . . . . ?
C8 C9 C10 C11 175.9(5) . . . . ?
C9 C10 C11 C12 2.6(8) . . . . ?
C10 C11 C12 C13 -0.3(8) . . . . ?
C9 N1 C13 C12 1.8(8) . . . . ?
Ce2 N1 C13 C12 -178.0(4) . . . . ?
C9 N1 C13 C14 -175.5(5) . . . . ?
Ce2 N1 C13 C14 4.7(6) . . . . ?
C11 C12 C13 N1 -2.0(8) . . . . ?
C11 C12 C13 C14 175.2(5) . . . . ?
Ce2 O9 C14 O8 -164.1(5) . . . . ?
Ce1 O9 C14 O8 31.1(8) . . . . ?
Ce2 O9 C14 C13 15.1(7) . . . . ?
Ce1 O9 C14 C13 -149.7(4) . . . . ?
N1 C13 C14 O8 166.6(5) . . . . ?
C12 C13 C14 O8 -10.8(8) . . . . ?
N1 C13 C14 O9 -12.7(7) . . . . ?
C12 C13 C14 O9 169.9(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H14W S1 0.83 3.03 3.853(4) 173.8 3_455
O7 H14W O16 0.83 2.04 2.837(5) 159.5 3_455
O7 H13W O1 0.83 2.00 2.748(6) 150.8 1_545
O6 H12W O19 0.83 2.03 2.848(5) 168.7 3_455
O6 H11W O2 0.83 1.97 2.743(6) 155.9 3
O5 H10W O3 0.83 1.94 2.766(5) 168.4 1_545
O5 H9W O18 0.84 1.98 2.786(5) 163.3 1_545
O4 H8W O2 0.83 1.98 2.782(6) 162.3 3_565
O4 H7W O17 0.83 2.06 2.766(5) 142.1 .
O3 H6W O11 0.83 1.93 2.692(5) 152.8 3_455
O3 H5W O9 0.83 2.57 3.055(5) 118.7 .
O3 H5W O8 0.83 1.84 2.640(5) 161.3 .
O2 H4W O8 0.83 2.64 3.221(6) 128.2 4
O2 H3W O15 0.83 2.26 2.891(6) 133.0 3_455
O1 H2W O10 0.83 1.94 2.763(6) 170.3 3_455
O1 H1W O15 0.83 2.31 3.097(7) 157.2 2_664

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.117


