data_publication_text
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
#TrackingRef '- 1-2crystaldata-new.CIF'

_publ_contact_author_name        'Christoph Janiak'
_publ_contact_author_address     
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
_publ_contact_author_email       janiak@uni-freiburg.de
_publ_contact_author_phone       +49-761-2036127
loop_
_publ_author_name
_publ_author_address
B.Gil-Hernandez
;Departamento de Qu\'imica Inorg\'anica
Universidad de La Laguna
38206 La Laguna, Tenerife
Spain
;
H.Hoppe
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
J.K.Vieth
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
J.Sanchiz
;Departamento de Qu\'imica Inorg\'anica
Universidad de La Laguna
38206 La Laguna, Tenerife
Spain
;
C.Janiak
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
_publ_section_title              
;
Spontaneous/Self-resolution upon crystallization of chiral La(III) and Gd(III)
MOFs from achiral dihydroxymalonate
;
#==============================================================================

data_2Laketo_c
_database_code_depnum_ccdc_archive 'CCDC 780266'
#TrackingRef '- 1-2crystaldata-new.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-\L-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')lanthanum(III)]
;
_chemical_name_common            
;
catena-clambda-(triaqua-1.5(mu-dihydroxymalonato-
kappaO,O'':O''',O'''')lanthanum(iii))
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H18 La2 O24'
_chemical_formula_sum            'C9 H18 La2 O24'
_chemical_formula_weight         788.05

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   9.75040(10)
_cell_length_b                   9.75040(10)
_cell_length_c                   21.2854(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1752.50(13)
_cell_formula_units_Z            3
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    87519
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      69.4

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1134
_exptl_absorpt_coefficient_mu    3.714
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3327
_exptl_absorpt_correction_T_max  0.4228
_exptl_absorpt_process_details   '(<i>ABSCOR</i>; Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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 RAXIS conversion
;
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            46805
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0077
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         4.18
_diffrn_reflns_theta_max         39.99
_reflns_number_total             2409
_reflns_number_gt                2401
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material  ?

_publ_section_references         
;
Crystal Impact (2009). <i>DIAMOND</i>. Version 3.2. Crystal Impact GbR, Bonn,
Germany.

Higashi, T. (1995). <i>ABSCOR</i>. Rigaku Corporation, Tokyo, Japan.

Rigaku (2009). <i>Spider</i> and <i>CrystalClear</i>.
Rigaku Corporation, Tokyo, Japan.

Sheldrick, G. M. (2008). <i>Acta Cryst.</i> A<b>64</b>, 112--122.
;

_publ_section_exptl_refinement   
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).

H atoms on crystal water oxygen / on nitrogen atoms have been found and
refined with U~iso~(H) = 1.5U~eq~(O).
;

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

For data set 2Laket_c the protons of the aqua ligand (HW1 and HW2) and
the C-OH group (H1) were found at a sensible position for a water ligand
molecule and C-OH group, respectively. In subsequent refinement the protons
were unstable due to their close proximity to the lanthanide atom.
Therefore the restraints
DFIX 0.9 0.02 O1 H1 OW HW1 OW HW2,
DANG 1.11 0.04 HW1 HW2 and
SADI La HW1 La HW2
were used to keep the protons of the water molecule stable.

The structure contains solvent accessible VOIDS of 42.00 \%A.
This space would be sufficient to host one crystal water molecule.
The total potential solvent area volume calculated with Platon is
234.4 \%A^3^ per unit cell volume of 1752.5 \%A^3^ [13.4%].
An electron density map of the void was generated using JANA2006 to
search for a water molecule which was not found.
SQUEEZE was only used on a trial dataset and not on the submitted dataset.
SQUEEZE was not used as the overall residue electron density total
positive electron count in Voids/Cell (taken from a trial SQUEEZE
calculation) of 26 distributed over 234.4 \%A^3^ was negligible small.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+3.5048P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(11)
_refine_ls_number_reflns         2409
_refine_ls_number_parameters     63
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0126
_refine_ls_R_factor_gt           0.0125
_refine_ls_wR_factor_ref         0.0297
_refine_ls_wR_factor_gt          0.0296
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_restrained_S_all      1.205
_refine_ls_shift/su_max          0.005
_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
La La 1.0000 1.0000 0.769562(4) 0.00553(2) Uani 1 3 d SD . .
C1 C 0.79455(15) 0.6667 0.6667 0.00660(19) Uani 1 2 d S . .
C2 C 0.68631(13) 0.64257(13) 0.72454(5) 0.00945(16) Uani 1 1 d . . .
O1 O 0.94084(10) 0.79971(10) 0.68037(4) 0.00893(12) Uani 1 1 d D . .
H1 H 1.011(2) 0.820(3) 0.6520(8) 0.013 Uiso 1 1 d D . .
O2 O 0.72774(12) 0.76096(12) 0.75950(5) 0.01595(17) Uani 1 1 d . . .
O3 O 0.56344(12) 0.51131(12) 0.73054(5) 0.01682(18) Uani 1 1 d . . .
OW O 0.99194(15) 0.81868(16) 0.85431(6) 0.0236(2) Uani 1 1 d D . .
HW2 H 0.911(2) 0.738(2) 0.8665(11) 0.035 Uiso 1 1 d D . .
HW1 H 1.071(2) 0.834(3) 0.8782(11) 0.035 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
La 0.00591(2) 0.00591(2) 0.00479(3) 0.000 0.000 0.00295(1)
C1 0.0070(3) 0.0058(5) 0.0065(5) -0.0008(4) -0.00041(19) 0.0029(2)
C2 0.0090(4) 0.0077(4) 0.0085(4) -0.0013(3) 0.0020(3) 0.0019(3)
O1 0.0059(3) 0.0079(3) 0.0095(3) -0.0020(2) 0.0015(2) 0.0009(2)
O2 0.0144(4) 0.0106(3) 0.0142(4) -0.0057(3) 0.0063(3) -0.0003(3)
O3 0.0134(3) 0.0099(3) 0.0170(4) -0.0046(3) 0.0071(3) -0.0017(3)
OW 0.0220(5) 0.0299(6) 0.0245(5) 0.0187(5) 0.0109(4) 0.0172(5)

_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
La OW 2.4994(11) . ?
La OW 2.4995(11) 3_675 ?
La OW 2.4996(11) 2_765 ?
La O2 2.5175(10) 3_675 ?
La O2 2.5175(10) 2_765 ?
La O2 2.5175(10) . ?
La O1 2.5738(8) 3_675 ?
La O1 2.5738(8) 2_765 ?
La O1 2.5739(8) . ?
C1 O1 1.3971(12) 11_566 ?
C1 O1 1.3972(12) . ?
C1 C2 1.5615(14) 11_566 ?
C1 C2 1.5616(14) . ?
C2 O3 1.2475(14) . ?
C2 O2 1.2582(14) . ?
O1 H1 0.860(15) . ?
OW HW2 0.825(16) . ?
OW HW1 0.871(15) . ?

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
OW La OW 73.66(5) . 3_675 ?
OW La OW 73.66(5) . 2_765 ?
OW La OW 73.65(5) 3_675 2_765 ?
OW La O2 138.52(4) . 3_675 ?
OW La O2 76.17(4) 3_675 3_675 ?
OW La O2 70.98(3) 2_765 3_675 ?
OW La O2 70.98(3) . 2_765 ?
OW La O2 138.52(4) 3_675 2_765 ?
OW La O2 76.17(4) 2_765 2_765 ?
O2 La O2 119.284(7) 3_675 2_765 ?
OW La O2 76.17(4) . . ?
OW La O2 70.98(3) 3_675 . ?
OW La O2 138.52(4) 2_765 . ?
O2 La O2 119.285(7) 3_675 . ?
O2 La O2 119.284(7) 2_765 . ?
OW La O1 149.28(4) . 3_675 ?
OW La O1 94.58(4) 3_675 3_675 ?
OW La O1 131.12(3) 2_765 3_675 ?
O2 La O1 60.15(3) 3_675 3_675 ?
O2 La O1 126.81(3) 2_765 3_675 ?
O2 La O1 73.16(3) . 3_675 ?
OW La O1 131.12(3) . 2_765 ?
OW La O1 149.28(4) 3_675 2_765 ?
OW La O1 94.58(4) 2_765 2_765 ?
O2 La O1 73.16(3) 3_675 2_765 ?
O2 La O1 60.15(3) 2_765 2_765 ?
O2 La O1 126.81(3) . 2_765 ?
O1 La O1 71.57(3) 3_675 2_765 ?
OW La O1 94.58(4) . . ?
OW La O1 131.12(3) 3_675 . ?
OW La O1 149.28(4) 2_765 . ?
O2 La O1 126.81(3) 3_675 . ?
O2 La O1 73.16(3) 2_765 . ?
O2 La O1 60.15(3) . . ?
O1 La O1 71.57(3) 3_675 . ?
O1 La O1 71.57(3) 2_765 . ?
O1 C1 O1 112.34(13) 11_566 . ?
O1 C1 C2 105.94(5) 11_566 11_566 ?
O1 C1 C2 113.22(6) . 11_566 ?
O1 C1 C2 113.21(6) 11_566 . ?
O1 C1 C2 105.93(5) . . ?
C2 C1 C2 106.18(12) 11_566 . ?
O3 C2 O2 125.73(11) . . ?
O3 C2 C1 117.72(9) . . ?
O2 C2 C1 116.46(9) . . ?
C1 O1 La 126.57(6) . . ?
C1 O1 H1 113.4(15) . . ?
La O1 H1 119.4(15) . . ?
C2 O2 La 127.30(8) . . ?
La OW HW2 125.1(15) . . ?
La OW HW1 125.9(15) . . ?
HW2 OW HW1 109(2) . . ?

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
O1 H1 O3 0.860(15) 1.755(16) 2.6038(13) 169(2) 10_556
OW HW2 O3 0.825(16) 1.974(18) 2.7153(15) 149(2) 18_656
OW HW1 O2 0.871(15) 2.073(17) 2.9095(17) 161(2) 17_666

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        39.99
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.093

#===END

data_ketb
_database_code_depnum_ccdc_archive 'CCDC 780267'
#TrackingRef '- 1-2crystaldata-new.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-\D-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')lanthanum(III)]
;
_chemical_name_common            
;
catena-cdelta-(triaqua-1.5(mu-dihydroxymalonato-
kappaO,O'':O''',O'''')lanthanum(iii))
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H18 La2 O24'
_chemical_formula_sum            'C9 H18 La2 O24'
_chemical_formula_weight         788.05

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   9.7580(3)
_cell_length_b                   9.7580(3)
_cell_length_c                   21.2982(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1756.29(15)
_cell_formula_units_Z            3
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    32425
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      69.2

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1134
_exptl_absorpt_coefficient_mu    3.706
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2072
_exptl_absorpt_correction_T_max  0.4235
_exptl_absorpt_process_details   '(<i>ABSCOR</i>; Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203(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 RAXIS conversion
;
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20627
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         39.98
_reflns_number_total             2432
_reflns_number_gt                2295
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material  ?

_publ_section_references         
;
Crystal Impact (2009). <i>DIAMOND</i>. Version 3.2. Crystal Impact GbR, Bonn,
Germany.

Higashi, T. (1995). <i>ABSCOR</i>. Rigaku Corporation, Tokyo, Japan.

Rigaku (2009). <i>Spider</i> and <i>CrystalClear</i>.
Rigaku Corporation, Tokyo, Japan.

Sheldrick, G. M. (2008). <i>Acta Cryst.</i> A<b>64</b>, 112--122.
;

_publ_section_exptl_refinement   
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).

H atoms on crystal water oxygen / on nitrogen atoms have been found and
refined with U~iso~(H) = 1.5U~eq~(O)
;

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

For data set ketb the protons of the aqua ligand (HW1 and HW2) and
the C-OH group (H1) were found at a sensible position for a water ligand
molecule and C-OH group, respectively. In subsequent refinement the protons
were unstable due to their close proximity to the lanthanide atom.
Therefore the restraints
DFIX 0.9 0.02 O1 H1 OW HW1 OW HW2,
DANG 1.41 0.04 HW1 HW2 and
SADI La HW1 La HW2
were used to keep the protons of the water molecule stable.

The structure contains solvent accessible VOIDS of 43.00 \%A.
This space would be sufficient to host one crystal water molecule.
The total potential solvent area volume calculated with Platon is
240.5 \%A^3^ per unit cell volume of 1756.3 \%A^3^ [13.7%].
An electron density map of the void was generated using JANA2006 to
search for a water molecule which was not found.
SQUEEZE was only used on a trial dataset and not on the submitted dataset.
SQUEEZE was not used as the overall residue electron density total
positive electron count in Voids/Cell (taken from a trial SQUEEZE
calculation) of 28 distributed over 240.5 \%A^3^ was negligible small.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+0.6499P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_number_reflns         2432
_refine_ls_number_parameters     63
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0178
_refine_ls_wR_factor_ref         0.0381
_refine_ls_wR_factor_gt          0.0378
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.104
_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
La La 0.0000 0.0000 0.230512(4) 0.00866(3) Uani 1 3 d SD . .
C1 C 0.20519(18) 0.3333 0.3333 0.0097(3) Uani 1 2 d S . .
C2 C 0.31353(17) 0.35766(17) 0.27540(7) 0.0136(2) Uani 1 1 d . . .
O1 O 0.05915(12) 0.20025(13) 0.31960(5) 0.01288(17) Uani 1 1 d D . .
H1 H -0.002(3) 0.186(3) 0.3498(9) 0.019 Uiso 1 1 d D . .
O2 O 0.27200(15) 0.23930(15) 0.24054(6) 0.0208(2) Uani 1 1 d . . .
O3 O 0.43616(15) 0.48807(15) 0.26958(6) 0.0244(3) Uani 1 1 d . . .
OW O 0.00922(18) 0.1821(2) 0.14594(8) 0.0322(3) Uani 1 1 d D . .
HW1 H 0.094(2) 0.256(3) 0.1300(12) 0.048 Uiso 1 1 d D . .
HW2 H -0.072(2) 0.163(3) 0.1207(12) 0.048 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
La 0.00942(3) 0.00942(3) 0.00714(4) 0.000 0.000 0.00471(2)
C1 0.0106(5) 0.0091(7) 0.0090(7) -0.0021(5) -0.0010(3) 0.0046(3)
C2 0.0135(5) 0.0131(5) 0.0115(6) -0.0014(4) 0.0018(4) 0.0047(5)
O1 0.0092(4) 0.0120(4) 0.0129(4) -0.0029(3) 0.0020(3) 0.0019(3)
O2 0.0182(5) 0.0161(5) 0.0176(5) -0.0065(4) 0.0078(4) 0.0007(4)
O3 0.0204(5) 0.0151(5) 0.0240(6) -0.0069(4) 0.0102(4) -0.0014(4)
OW 0.0303(7) 0.0402(8) 0.0341(8) 0.0260(7) 0.0155(6) 0.0236(7)

_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
La OW 2.5003(13) . ?
La OW 2.5003(13) 2 ?
La OW 2.5003(13) 3 ?
La O2 2.5189(12) 3 ?
La O2 2.5189(12) 2 ?
La O2 2.5190(12) . ?
La O1 2.5737(10) . ?
La O1 2.5738(10) 2 ?
La O1 2.5738(10) 3 ?
C1 O1 1.3971(14) 17 ?
C1 O1 1.3972(14) . ?
C1 C2 1.5638(18) 17 ?
C1 C2 1.5639(18) . ?
C2 O3 1.2425(18) . ?
C2 O2 1.2574(18) . ?
O1 H1 0.838(16) . ?
OW HW1 0.851(15) . ?
OW HW2 0.900(16) . ?

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
OW La OW 73.83(7) . 2 ?
OW La OW 73.83(7) . 3 ?
OW La OW 73.83(7) 2 3 ?
OW La O2 138.65(5) . 3 ?
OW La O2 71.17(4) 2 3 ?
OW La O2 75.85(5) 3 3 ?
OW La O2 71.17(4) . 2 ?
OW La O2 75.85(5) 2 2 ?
OW La O2 138.65(5) 3 2 ?
O2 La O2 119.287(8) 3 2 ?
OW La O2 75.84(5) . . ?
OW La O2 138.65(5) 2 . ?
OW La O2 71.17(4) 3 . ?
O2 La O2 119.288(8) 3 . ?
O2 La O2 119.288(8) 2 . ?
OW La O1 94.40(5) . . ?
OW La O1 149.03(5) 2 . ?
OW La O1 131.24(4) 3 . ?
O2 La O1 126.84(4) 3 . ?
O2 La O1 73.23(4) 2 . ?
O2 La O1 60.09(3) . . ?
OW La O1 131.24(4) . 2 ?
OW La O1 94.40(5) 2 2 ?
OW La O1 149.02(5) 3 2 ?
O2 La O1 73.23(4) 3 2 ?
O2 La O1 60.08(3) 2 2 ?
O2 La O1 126.84(4) . 2 ?
O1 La O1 71.62(4) . 2 ?
OW La O1 149.03(5) . 3 ?
OW La O1 131.24(4) 2 3 ?
OW La O1 94.40(5) 3 3 ?
O2 La O1 60.08(3) 3 3 ?
O2 La O1 126.84(4) 2 3 ?
O2 La O1 73.23(4) . 3 ?
O1 La O1 71.62(4) . 3 ?
O1 La O1 71.62(4) 2 3 ?
O1 C1 O1 112.55(15) 17 . ?
O1 C1 C2 105.90(7) 17 17 ?
O1 C1 C2 113.11(7) . 17 ?
O1 C1 C2 113.11(7) 17 . ?
O1 C1 C2 105.89(7) . . ?
C2 C1 C2 106.24(15) 17 . ?
O3 C2 O2 125.80(14) . . ?
O3 C2 C1 117.77(12) . . ?
O2 C2 C1 116.32(11) . . ?
C1 O1 La 126.68(7) . . ?
C1 O1 H1 107.4(16) . . ?
La O1 H1 124.8(16) . . ?
C2 O2 La 127.43(10) . . ?
La OW HW1 124.6(16) . . ?
La OW HW2 124.9(15) . . ?
HW1 OW HW2 108(2) . . ?

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
O1 H1 O3 0.838(16) 1.804(17) 2.6083(16) 160(2) 16_445
OW HW1 O3 0.851(15) 1.916(17) 2.7158(18) 156(2) 12
OW HW2 O2 0.900(16) 2.066(18) 2.926(2) 160(2) 11_455

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        39.98
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.964
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.107

#===END

data_gdketo
_database_code_depnum_ccdc_archive 'CCDC 780268'
#TrackingRef '- 1-2crystaldata-new.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-\L-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')gadolinium(III)]
;
_chemical_name_common            
;
catena-clambda-(triaqua-1.5(mu-dihydroxymalonato-
kappaO,O'':O''',O'''')gadolinium(iii))
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H18 Gd2 O24'
_chemical_formula_sum            'C9 H18 Gd2 O24'
_chemical_formula_weight         824.73

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   9.6396(8)
_cell_length_b                   9.6396(8)
_cell_length_c                   20.7433(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1669.3(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    9845
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      40.3

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    6.020
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3942
_exptl_absorpt_correction_T_max  0.6445
_exptl_absorpt_process_details   '(<i>ABSCOR</i>; Higashi, 1995)'

_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  
;
Rigaku RAXIS conversion
;

_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10186
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         33.14
_reflns_number_total             1427
_reflns_number_gt                1391
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material  ?

_publ_section_references         
;
Crystal Impact (2009). <i>DIAMOND</i>. Version 3.2. Crystal Impact GbR, Bonn,
Germany.

Higashi, T. (1995). <i>ABSCOR</i>. Rigaku Corporation, Tokyo, Japan.

Rigaku (2009). <i>Spider</i> and <i>CrystalClear</i>.
Rigaku Corporation, Tokyo, Japan.

Sheldrick, G. M. (2008). <i>Acta Cryst.</i> A<b>64</b>, 112--122.
;

_publ_section_exptl_refinement   
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).

H atoms on crystal water oxygen / on nitrogen atoms have been found and
refined with U~iso~(H) = 1.5U~eq~(O)
;

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

For data set gdketo the protons of the aqua ligand (HW1 and HW2) and
the C-OH group (H1) were found at a sensible position for a water ligand
molecule and C-OH group, respectively. In subsequent refinement the protons
were unstable due to their close proximity to the lanthanide atom.
Therefore the restraints
DFIX 0.9 0.02 O1 H1 OW HW1 OW HW2,
DANG 1.46 0.04 HW1 HW2 and
SADI Gd HW1 Gd HW2
were used to keep the protons of the water molecule stable.

The structure contains solvent accessible VOIDS of 45.00 \%A.
This space would be sufficient to host one crystal water molecule.
The total potential solvent area volume calculated with Platon is
240.7 \%A^3^ per unit cell volume of 1669.3 \%A^3^ [14.4%].
An electron density map of the void was generated using JANA2006 to
search for a water molecule which was not found.
SQUEEZE was only used on a trial dataset and not on the submitted dataset.
SQUEEZE was not used as the overall residue electron density total
positive electron count in Voids/Cell (taken from a trial SQUEEZE
calculation) of 35 distributed over 240.5 \%A^3^ was negligible small.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0102P)^2^+1.7470P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_number_reflns         1427
_refine_ls_number_parameters     63
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0411
_refine_ls_wR_factor_gt          0.0408
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.213
_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
Gd Gd 1.0000 1.0000 0.766162(7) 0.00878(5) Uani 1 3 d SD . .
C1 C 0.7975(3) 0.6667 0.6667 0.0102(7) Uani 1 2 d S . .
C2 C 0.6902(3) 0.6461(3) 0.72650(13) 0.0139(5) Uani 1 1 d . . .
O1 O 0.9450(2) 0.8022(2) 0.67979(9) 0.0140(4) Uani 1 1 d D . .
H1 H 1.005(4) 0.808(4) 0.6532(16) 0.021 Uiso 1 1 d D . .
O2 O 0.7335(3) 0.7681(3) 0.76079(10) 0.0203(4) Uani 1 1 d . . .
O3 O 0.5680(3) 0.5140(3) 0.73445(12) 0.0306(6) Uani 1 1 d . . .
OW O 0.9858(3) 0.8185(3) 0.84797(13) 0.0318(6) Uani 1 1 d D . .
HW1 H 0.907(3) 0.742(4) 0.8603(18) 0.048 Uiso 1 1 d D . .
HW2 H 1.060(3) 0.823(5) 0.8671(18) 0.048 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd 0.00912(6) 0.00912(6) 0.00811(8) 0.000 0.000 0.00456(3)
C1 0.0104(12) 0.0104(15) 0.0099(14) 0.0000(11) 0.0000(6) 0.0052(7)
C2 0.0128(12) 0.0153(13) 0.0120(12) -0.0019(9) 0.0017(9) 0.0057(10)
O1 0.0076(8) 0.0138(9) 0.0155(8) -0.0030(7) 0.0029(6) 0.0016(7)
O2 0.0163(10) 0.0163(10) 0.0196(10) -0.0055(8) 0.0071(8) 0.0016(9)
O3 0.0232(11) 0.0162(11) 0.0341(13) -0.0094(8) 0.0156(9) -0.0038(9)
OW 0.0256(13) 0.0381(15) 0.0363(14) 0.0242(12) 0.0129(10) 0.0193(12)

_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
Gd OW 2.391(2) . ?
Gd OW 2.391(2) 2_765 ?
Gd OW 2.391(2) 3_675 ?
Gd O2 2.422(2) 2_765 ?
Gd O2 2.422(2) 3_675 ?
Gd O2 2.422(2) . ?
Gd O1 2.473(2) 2_765 ?
Gd O1 2.4727(19) 3_675 ?
Gd O1 2.4727(19) . ?
C1 O1 1.395(3) 11_566 ?
C1 O1 1.395(3) . ?
C1 C2 1.564(3) 11_566 ?
C1 C2 1.564(3) . ?
C2 O3 1.240(3) . ?
C2 O2 1.254(3) . ?
O1 H1 0.78(3) . ?
OW HW1 0.79(2) . ?
OW HW2 0.80(2) . ?

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
OW Gd OW 75.21(11) . 2_765 ?
OW Gd OW 75.21(11) . 3_675 ?
OW Gd OW 75.20(11) 2_765 3_675 ?
OW Gd O2 69.59(8) . 2_765 ?
OW Gd O2 73.20(9) 2_765 2_765 ?
OW Gd O2 137.36(9) 3_675 2_765 ?
OW Gd O2 137.36(9) . 3_675 ?
OW Gd O2 69.60(8) 2_765 3_675 ?
OW Gd O2 73.20(9) 3_675 3_675 ?
O2 Gd O2 119.789(9) 2_765 3_675 ?
OW Gd O2 73.20(9) . . ?
OW Gd O2 137.36(9) 2_765 . ?
OW Gd O2 69.60(8) 3_675 . ?
O2 Gd O2 119.791(9) 2_765 . ?
O2 Gd O2 119.790(9) 3_675 . ?
OW Gd O1 131.87(7) . 2_765 ?
OW Gd O1 92.21(9) 2_765 2_765 ?
OW Gd O1 146.78(8) 3_675 2_765 ?
O2 Gd O1 62.31(6) 2_765 2_765 ?
O2 Gd O1 73.60(7) 3_675 2_765 ?
O2 Gd O1 130.32(7) . 2_765 ?
OW Gd O1 146.78(8) . 3_675 ?
OW Gd O1 131.87(7) 2_765 3_675 ?
OW Gd O1 92.21(9) 3_675 3_675 ?
O2 Gd O1 130.32(7) 2_765 3_675 ?
O2 Gd O1 62.31(6) 3_675 3_675 ?
O2 Gd O1 73.60(7) . 3_675 ?
O1 Gd O1 73.29(8) 2_765 3_675 ?
OW Gd O1 92.21(9) . . ?
OW Gd O1 146.78(8) 2_765 . ?
OW Gd O1 131.87(7) 3_675 . ?
O2 Gd O1 73.60(7) 2_765 . ?
O2 Gd O1 130.32(7) 3_675 . ?
O2 Gd O1 62.31(6) . . ?
O1 Gd O1 73.29(8) 2_765 . ?
O1 Gd O1 73.29(8) 3_675 . ?
O1 C1 O1 113.2(3) 11_566 . ?
O1 C1 C2 105.29(13) 11_566 11_566 ?
O1 C1 C2 113.29(14) . 11_566 ?
O1 C1 C2 113.28(14) 11_566 . ?
O1 C1 C2 105.28(13) . . ?
C2 C1 C2 106.5(3) 11_566 . ?
O3 C2 O2 126.0(3) . . ?
O3 C2 C1 117.7(2) . . ?
O2 C2 C1 116.2(2) . . ?
C1 O1 Gd 126.09(13) . . ?
C1 O1 H1 108(3) . . ?
Gd O1 H1 126(3) . . ?
C2 O2 Gd 126.46(18) . . ?
Gd OW HW1 126(2) . . ?
Gd OW HW2 126(3) . . ?
HW1 OW HW2 108(4) . . ?

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
O1 H1 O3 0.78(3) 1.85(3) 2.592(3) 159(4) 10_556
OW HW1 O3 0.79(2) 1.98(3) 2.700(3) 150(4) 18_656
OW HW2 O2 0.80(2) 2.19(3) 2.969(3) 165(3) 17_666
OW HW2 OW 0.80(2) 2.44(4) 2.839(5) 112(4) 16_546

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        33.14
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.141

#===END