# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full CrystEngComm
_journal_coden_Cambridge 1350
_journal_volume ?
_journal_page_first ?
_journal_year ?
_publ_contact_author_name 'Christoph Janiak'
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
40204 D\"usseldorf
Germany
;
_publ_contact_author_email janiak@uni-duesseldorf.de
_publ_contact_author_phone +49-211-8112286
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
;
J.K.Maclaren
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
H.Hoppe
;Institut f\"ur Physik
Universit\"at Augsburg
Universit\"atsstr. 1
86159 Augsburg
Germany
;
J.Pasan
;Laboratorio de Rayos X y Materiales Moleculares
Departamento de Fisica Fundamental II
Facultad de Fisica
Universidad de La Laguna
38206 La Laguna, Tenerife
Spain
;
J.Sanchiz
;Departamento de Qu\'imica Inorg\'anica
Universidad de La Laguna
38206 La Laguna, Tenerife
Spain
;
;
C.Janiak
;
;Institut f\"ur Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
40204 D\"usseldorf
Germany
;
_publ_section_title
;
Homochiral lanthanoid(III)
mesoxalate metal-organic frameworks: synthesis,
crystal growth, chirality, magnetic and
luminescent properties
;
# Attachment '- crystaldata-all.CIF'
#TrackingRef '- crystaldata-all.CIF'
#==============================================================================
data_2Laketo_c
_database_code_depnum_ccdc_archive 'CCDC 780266'
#TrackingRef '- crystaldata-all.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 '(ABSCOR; 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). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2009). Spider and CrystalClear.
Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 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 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_spherical
_database_code_depnum_ccdc_archive 'CCDC 853393'
#TrackingRef '- crystaldata-all.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-\L-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')cerium(III)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C9 H18 Ce2 O24'
_chemical_formula_sum 'C9 H18 Ce2 O24'
_chemical_formula_weight 790.47
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'
Ce Ce -0.2486 2.6331 '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'
_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'
'y, x, -z'
'-x+y, -x, z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -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'
'y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
_cell_length_a 9.7193(14)
_cell_length_b 9.7193(14)
_cell_length_c 21.191(4)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 1733.6(5)
_cell_formula_units_Z 3
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 4.05
_cell_measurement_theta_max 27.10
_exptl_crystal_description octahedra
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.271
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1140
_exptl_absorpt_coefficient_mu 3.997
_exptl_absorpt_correction_type sphere
_exptl_absorpt_correction_T_min 0.5855
_exptl_absorpt_correction_T_max 0.5855
_exptl_absorpt_process_details
;
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'horizonally mounted graphite crystal'
_diffrn_radiation_probe x-ray
_diffrn_source 'Enraf Nonius FR590'
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type KappaCCD
_diffrn_measurement_method 'CCD rotation images, thick slices'
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 6225
_diffrn_reflns_av_R_equivalents 0.0160
_diffrn_reflns_av_sigmaI/netI 0.0163
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 4.19
_diffrn_reflns_theta_max 30.49
_reflns_number_total 1179
_reflns_number_gt 1160
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND 3.1 (Crystal Impact)'
_computing_publication_material 'PARST97 (Nardelli, 1997)'
_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.
;
_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^)+(0.0179P)^2^+1.8616P] 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 0.007(19)
_refine_ls_number_reflns 1179
_refine_ls_number_parameters 63
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0133
_refine_ls_R_factor_gt 0.0127
_refine_ls_wR_factor_ref 0.0361
_refine_ls_wR_factor_gt 0.0358
_refine_ls_goodness_of_fit_ref 1.202
_refine_ls_restrained_S_all 1.204
_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
Ce Ce 0.0000 0.0000 0.268832(6) 0.00922(5) Uani 1 3 d SD . .
O1 O -0.05818(18) -0.19988(19) 0.18025(7) 0.0147(3) Uani 1 1 d D . .
H1 H 0.004(3) -0.195(4) 0.1502(12) 0.022 Uiso 1 1 d D . .
O2 O -0.2702(2) -0.2376(2) 0.25964(8) 0.0238(3) Uani 1 1 d . . .
O3 O -0.4343(2) -0.4873(2) 0.23125(9) 0.0304(4) Uani 1 1 d . . .
C1 C -0.2044(3) -0.3333 0.1667 0.0107(5) Uani 1 2 d S . .
C2 C -0.3121(3) -0.3571(3) 0.22498(10) 0.0153(4) Uani 1 1 d . . .
OW O -0.0104(3) -0.1824(3) 0.35277(11) 0.0358(5) Uani 1 1 d D . .
H1W H 0.072(3) -0.180(4) 0.3734(16) 0.054 Uiso 1 1 d D . .
H2W H -0.091(3) -0.259(4) 0.3719(15) 0.054 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
Ce 0.00938(6) 0.00938(6) 0.00888(7) 0.000 0.000 0.00469(3)
O1 0.0088(6) 0.0138(6) 0.0160(6) -0.0036(5) 0.0025(5) 0.0016(5)
O2 0.0201(8) 0.0180(8) 0.0229(8) -0.0076(6) 0.0090(6) 0.0017(7)
O3 0.0244(8) 0.0164(8) 0.0320(10) -0.0099(6) 0.0152(6) -0.0036(7)
C1 0.0108(8) 0.0101(11) 0.0112(11) -0.0007(9) -0.0004(4) 0.0050(5)
C2 0.0138(9) 0.0131(9) 0.0155(9) -0.0014(7) 0.0014(7) 0.0041(7)
OW 0.0312(11) 0.0439(13) 0.0390(12) 0.0274(10) 0.0149(9) 0.0238(10)
_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
Ce OW 2.477(2) . ?
Ce OW 2.477(2) 2 ?
Ce OW 2.477(2) 4 ?
Ce O2 2.4903(18) 2 ?
Ce O2 2.4903(18) . ?
Ce O2 2.4903(18) 4 ?
Ce O1 2.5532(15) . ?
Ce O1 2.5532(15) 4 ?
Ce O1 2.5533(15) 2 ?
O1 C1 1.394(2) . ?
O2 C2 1.257(3) . ?
O3 C2 1.236(3) . ?
C1 O1 1.394(2) 12_445 ?
C1 C2 1.560(3) 12_445 ?
C1 C2 1.560(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
OW Ce OW 74.14(10) . 2 ?
OW Ce OW 74.14(10) . 4 ?
OW Ce OW 74.14(10) 2 4 ?
OW Ce O2 70.97(6) . 2 ?
OW Ce O2 75.27(8) 2 2 ?
OW Ce O2 138.49(7) 4 2 ?
OW Ce O2 75.27(8) . . ?
OW Ce O2 138.49(7) 2 . ?
OW Ce O2 70.98(6) 4 . ?
O2 Ce O2 119.394(11) 2 . ?
OW Ce O2 138.49(7) . 4 ?
OW Ce O2 70.97(6) 2 4 ?
OW Ce O2 75.26(8) 4 4 ?
O2 Ce O2 119.395(11) 2 4 ?
O2 Ce O2 119.394(11) . 4 ?
OW Ce O1 93.96(8) . . ?
OW Ce O1 148.51(6) 2 . ?
OW Ce O1 131.43(6) 4 . ?
O2 Ce O1 73.29(6) 2 . ?
O2 Ce O1 60.48(5) . . ?
O2 Ce O1 127.43(5) 4 . ?
OW Ce O1 148.51(6) . 4 ?
OW Ce O1 131.43(6) 2 4 ?
OW Ce O1 93.97(8) 4 4 ?
O2 Ce O1 127.43(5) 2 4 ?
O2 Ce O1 73.29(6) . 4 ?
O2 Ce O1 60.48(5) 4 4 ?
O1 Ce O1 71.89(6) . 4 ?
OW Ce O1 131.43(6) . 2 ?
OW Ce O1 93.97(8) 2 2 ?
OW Ce O1 148.51(6) 4 2 ?
O2 Ce O1 60.48(5) 2 2 ?
O2 Ce O1 127.43(5) . 2 ?
O2 Ce O1 73.29(6) 4 2 ?
O1 Ce O1 71.89(6) . 2 ?
O1 Ce O1 71.89(6) 4 2 ?
C1 O1 Ce 126.50(10) . . ?
C2 O2 Ce 127.36(14) . . ?
O1 C1 O1 112.6(2) 12_445 . ?
O1 C1 C2 105.71(10) 12_445 12_445 ?
O1 C1 C2 113.05(11) . 12_445 ?
O1 C1 C2 113.04(11) 12_445 . ?
O1 C1 C2 105.70(10) . . ?
C2 C1 C2 106.7(2) 12_445 . ?
O3 C2 O2 125.8(2) . . ?
O3 C2 C1 117.82(18) . . ?
O2 C2 C1 116.26(17) . . ?
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(18) 1.80(2) 2.604(2) 155(3) 9
OW H1W O2 0.901(17) 2.08(2) 2.938(3) 160(3) 18_545
OW H2W O3 0.866(17) 1.88(2) 2.715(3) 162(4) 17_445
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 30.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 0.798
_refine_diff_density_min -0.736
_refine_diff_density_rms 0.098
#===END
data_prketo
_database_code_depnum_ccdc_archive 'CCDC 853394'
#TrackingRef '- crystaldata-all.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-\L-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')praseodymium(III)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C9 H18 O24 Pr2'
_chemical_formula_sum 'C9 H18 O24 Pr2'
_chemical_formula_weight 792.05
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'
Pr Pr -0.2180 2.8214 '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 9.7612(4)
_cell_length_b 9.7612(4)
_cell_length_c 21.3097(9)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 1758.39(13)
_cell_formula_units_Z 3
_cell_measurement_temperature 294(2)
_cell_measurement_reflns_used 18172
_cell_measurement_theta_min 3.1
_cell_measurement_theta_max 52.2
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.244
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1146
_exptl_absorpt_coefficient_mu 4.213
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.5706
_exptl_absorpt_correction_T_max 0.6780
_exptl_absorpt_process_details 'Empirical Absorption Correction 2001 Higashi'
_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 17384
_diffrn_reflns_av_R_equivalents 0.0261
_diffrn_reflns_av_sigmaI/netI 0.0187
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_theta_min 4.18
_diffrn_reflns_theta_max 35.00
_reflns_number_total 1688
_reflns_number_gt 1642
_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 'publCIF (Westrip, 2009)'
_publ_section_references
;
Rigaku Spider and CrystalClear.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 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 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.
;
_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^)+(0.0000P)^2^+2.2541P] 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 -0.007(12)
_refine_ls_number_reflns 1688
_refine_ls_number_parameters 63
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0156
_refine_ls_R_factor_gt 0.0145
_refine_ls_wR_factor_ref 0.0276
_refine_ls_wR_factor_gt 0.0274
_refine_ls_goodness_of_fit_ref 1.176
_refine_ls_restrained_S_all 1.182
_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
Pr Pr 1.0000 1.0000 0.768197(4) 0.01074(3) Uani 1 3 d SD . .
C1 C 0.7955(2) 0.6667 0.6667 0.0121(4) Uani 1 2 d S . .
C2 C 0.68837(19) 0.6439(2) 0.72521(7) 0.0163(3) Uani 1 1 d . . .
O1 O 0.94244(13) 0.80058(14) 0.68010(5) 0.0163(2) Uani 1 1 d D . .
H1 H 1.008(2) 0.825(3) 0.6510(9) 0.025 Uiso 1 1 d D . .
O2 O 0.73075(16) 0.76361(16) 0.75991(6) 0.0242(3) Uani 1 1 d . . .
O3 O 0.56583(17) 0.51303(16) 0.73198(7) 0.0326(3) Uani 1 1 d . . .
OW O 0.98925(19) 0.8180(2) 0.85185(8) 0.0371(4) Uani 1 1 d D . .
HW1 H 0.911(2) 0.752(3) 0.8723(11) 0.056 Uiso 1 1 d D . .
HW2 H 1.074(2) 0.815(3) 0.8648(12) 0.056 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
Pr 0.01098(4) 0.01098(4) 0.01027(4) 0.000 0.000 0.00549(2)
C1 0.0120(7) 0.0104(8) 0.0133(8) -0.0010(6) -0.0005(3) 0.0052(4)
C2 0.0157(7) 0.0149(7) 0.0147(6) -0.0017(5) 0.0025(5) 0.0048(6)
O1 0.0106(5) 0.0156(5) 0.0174(5) -0.0040(4) 0.0023(3) 0.0024(4)
O2 0.0220(6) 0.0179(6) 0.0221(6) -0.0073(4) 0.0083(4) 0.0021(5)
O3 0.0251(7) 0.0187(6) 0.0350(7) -0.0091(5) 0.0154(5) -0.0033(5)
OW 0.0338(9) 0.0441(10) 0.0407(9) 0.0287(7) 0.0161(6) 0.0250(8)
_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
Pr OW 2.4813(14) . ?
Pr OW 2.4814(14) 3_675 ?
Pr OW 2.4814(14) 2_765 ?
Pr O2 2.4896(13) 3_675 ?
Pr O2 2.4897(13) . ?
Pr O2 2.4897(13) 2_765 ?
Pr O1 2.5565(11) 3_675 ?
Pr O1 2.5566(11) . ?
Pr O1 2.5566(11) 2_765 ?
C1 O1 1.4043(16) 11_566 ?
C1 O1 1.4044(16) . ?
C1 C2 1.5707(19) 11_566 ?
C1 C2 1.5709(19) . ?
C2 O3 1.247(2) . ?
C2 O2 1.265(2) . ?
O1 H1 0.836(16) . ?
OW HW1 0.836(15) . ?
OW HW2 0.893(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 Pr OW 74.09(7) . 3_675 ?
OW Pr OW 74.09(7) . 2_765 ?
OW Pr OW 74.09(7) 3_675 2_765 ?
OW Pr O2 138.04(5) . 3_675 ?
OW Pr O2 74.95(6) 3_675 3_675 ?
OW Pr O2 70.67(4) 2_765 3_675 ?
OW Pr O2 74.95(6) . . ?
OW Pr O2 70.67(5) 3_675 . ?
OW Pr O2 138.04(5) 2_765 . ?
O2 Pr O2 119.503(7) 3_675 . ?
OW Pr O2 70.66(4) . 2_765 ?
OW Pr O2 138.04(5) 3_675 2_765 ?
OW Pr O2 74.95(6) 2_765 2_765 ?
O2 Pr O2 119.503(7) 3_675 2_765 ?
O2 Pr O2 119.501(7) . 2_765 ?
OW Pr O1 148.34(5) . 3_675 ?
OW Pr O1 93.90(5) 3_675 3_675 ?
OW Pr O1 131.57(4) 2_765 3_675 ?
O2 Pr O1 60.92(4) 3_675 3_675 ?
O2 Pr O1 73.43(4) . 3_675 ?
O2 Pr O1 127.95(4) 2_765 3_675 ?
OW Pr O1 93.90(5) . . ?
OW Pr O1 131.57(4) 3_675 . ?
OW Pr O1 148.34(5) 2_765 . ?
O2 Pr O1 127.95(4) 3_675 . ?
O2 Pr O1 60.92(4) . . ?
O2 Pr O1 73.43(4) 2_765 . ?
O1 Pr O1 72.01(4) 3_675 . ?
OW Pr O1 131.57(4) . 2_765 ?
OW Pr O1 148.34(5) 3_675 2_765 ?
OW Pr O1 93.90(5) 2_765 2_765 ?
O2 Pr O1 73.43(4) 3_675 2_765 ?
O2 Pr O1 127.95(4) . 2_765 ?
O2 Pr O1 60.92(4) 2_765 2_765 ?
O1 Pr O1 72.01(4) 3_675 2_765 ?
O1 Pr O1 72.01(4) . 2_765 ?
O1 C1 O1 112.49(17) 11_566 . ?
O1 C1 C2 105.54(7) 11_566 11_566 ?
O1 C1 C2 113.18(8) . 11_566 ?
O1 C1 C2 113.17(8) 11_566 . ?
O1 C1 C2 105.53(7) . . ?
C2 C1 C2 106.96(17) 11_566 . ?
O3 C2 O2 125.58(15) . . ?
O3 C2 C1 117.82(13) . . ?
O2 C2 C1 116.51(13) . . ?
C1 O1 Pr 126.28(8) . . ?
C1 O1 H1 113.2(16) . . ?
Pr O1 H1 118.9(16) . . ?
C2 O2 Pr 127.14(11) . . ?
Pr OW HW1 128.4(16) . . ?
Pr OW HW2 122.9(15) . . ?
HW1 OW HW2 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 0.836(16) 1.799(16) 2.6223(17) 168(2) 10_556
OW HW1 O3 0.836(15) 1.912(15) 2.7313(19) 166(2) 18_656
OW HW2 O2 0.893(16) 2.123(18) 2.961(2) 156(3) 17_666
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full 35.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max 0.558
_refine_diff_density_min -0.689
_refine_diff_density_rms 0.090
#===END
data_ndketo
_database_code_depnum_ccdc_archive 'CCDC 853395'
#TrackingRef '- crystaldata-all.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-\L-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')neodymium(III)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C9 H18 Nd2 O24'
_chemical_formula_sum 'C9 H18 Nd2 O24'
_chemical_formula_weight 798.71
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 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 9.69740(10)
_cell_length_b 9.69740(10)
_cell_length_c 20.9760(5)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 1708.30(5)
_cell_formula_units_Z 3
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 9958
_cell_measurement_theta_min 3.107
_cell_measurement_theta_max 34.276
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.329
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1152
_exptl_absorpt_coefficient_mu 4.618
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.6072
_exptl_absorpt_correction_T_max 0.6813
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_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 'Bruker APEX2 CCD area detector'
_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 20229
_diffrn_reflns_av_R_equivalents 0.0307
_diffrn_reflns_av_sigmaI/netI 0.0198
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_theta_min 2.91
_diffrn_reflns_theta_max 36.12
_reflns_number_total 1783
_reflns_number_gt 1714
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
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~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
H atoms on crystal water oxygen 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.
;
_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^)+(0.0120P)^2^+1.7534P] 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(12)
_refine_ls_number_reflns 1783
_refine_ls_number_parameters 63
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0160
_refine_ls_R_factor_gt 0.0146
_refine_ls_wR_factor_ref 0.0296
_refine_ls_wR_factor_gt 0.0292
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_restrained_S_all 1.060
_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
Nd Nd 1.0000 1.0000 0.767796(5) 0.00817(3) Uani 1 3 d SD . .
C1 C 0.7962(2) 0.6667 0.6667 0.0092(3) Uani 1 2 d S . .
C2 C 0.68844(18) 0.64418(19) 0.72557(7) 0.0126(3) Uani 1 1 d . . .
O1 O 0.94300(13) 0.80098(13) 0.67997(5) 0.0123(2) Uani 1 1 d D . .
H1 H 1.011(2) 0.827(3) 0.6506(9) 0.018 Uiso 1 1 d D . .
O2 O 0.73092(15) 0.76466(15) 0.76025(6) 0.0184(2) Uani 1 1 d . . .
O3 O 0.56563(16) 0.51303(15) 0.73258(7) 0.0244(3) Uani 1 1 d . . .
OW O 0.98915(18) 0.81844(19) 0.85083(7) 0.0282(3) Uani 1 1 d D . .
HW1 H 0.909(2) 0.753(3) 0.8722(10) 0.042 Uiso 1 1 d D . .
HW2 H 1.077(2) 0.834(3) 0.8715(11) 0.042 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
Nd 0.00846(3) 0.00846(3) 0.00759(5) 0.000 0.000 0.00423(2)
C1 0.0092(6) 0.0089(8) 0.0093(8) -0.0007(6) -0.0003(3) 0.0044(4)
C2 0.0114(6) 0.0118(6) 0.0121(6) -0.0018(5) 0.0010(5) 0.0040(5)
O1 0.0079(4) 0.0118(5) 0.0128(5) -0.0031(4) 0.0019(3) 0.0018(4)
O2 0.0164(5) 0.0137(5) 0.0175(6) -0.0057(4) 0.0063(4) 0.0018(5)
O3 0.0195(6) 0.0146(5) 0.0257(6) -0.0069(4) 0.0105(5) -0.0016(4)
OW 0.0244(7) 0.0347(8) 0.0307(8) 0.0213(6) 0.0119(6) 0.0186(6)
_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
Nd OW 2.4412(14) . ?
Nd OW 2.4412(14) 3_675 ?
Nd OW 2.4412(14) 2_765 ?
Nd O2 2.4672(12) 3_675 ?
Nd O2 2.4673(13) . ?
Nd O2 2.4673(13) 2_765 ?
Nd O1 2.5212(11) 2_765 ?
Nd O1 2.5213(11) 3_675 ?
Nd O1 2.5213(11) . ?
C1 O1 1.3954(15) 11_566 ?
C1 O1 1.3954(15) . ?
C1 C2 1.5613(19) 11_566 ?
C1 C2 1.5614(19) . ?
C2 O3 1.2421(19) . ?
C2 O2 1.2580(19) . ?
O1 H1 0.846(16) . ?
OW HW1 0.843(15) . ?
OW HW2 0.899(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 Nd OW 74.72(6) . 3_675 ?
OW Nd OW 74.72(6) . 2_765 ?
OW Nd OW 74.72(6) 3_675 2_765 ?
OW Nd O2 138.04(5) . 3_675 ?
OW Nd O2 74.59(5) 3_675 3_675 ?
OW Nd O2 70.08(4) 2_765 3_675 ?
OW Nd O2 74.60(5) . . ?
OW Nd O2 70.08(4) 3_675 . ?
OW Nd O2 138.04(5) 2_765 . ?
O2 Nd O2 119.593(7) 3_675 . ?
OW Nd O2 70.08(4) . 2_765 ?
OW Nd O2 138.04(5) 3_675 2_765 ?
OW Nd O2 74.59(5) 2_765 2_765 ?
O2 Nd O2 119.593(7) 3_675 2_765 ?
O2 Nd O2 119.593(7) . 2_765 ?
OW Nd O1 131.33(4) . 2_765 ?
OW Nd O1 148.01(5) 3_675 2_765 ?
OW Nd O1 93.17(5) 2_765 2_765 ?
O2 Nd O1 73.44(4) 3_675 2_765 ?
O2 Nd O1 128.69(4) . 2_765 ?
O2 Nd O1 61.28(4) 2_765 2_765 ?
OW Nd O1 148.01(5) . 3_675 ?
OW Nd O1 93.17(5) 3_675 3_675 ?
OW Nd O1 131.33(4) 2_765 3_675 ?
O2 Nd O1 61.27(4) 3_675 3_675 ?
O2 Nd O1 73.44(4) . 3_675 ?
O2 Nd O1 128.69(4) 2_765 3_675 ?
O1 Nd O1 72.50(4) 2_765 3_675 ?
OW Nd O1 93.17(5) . . ?
OW Nd O1 131.33(4) 3_675 . ?
OW Nd O1 148.01(5) 2_765 . ?
O2 Nd O1 128.69(4) 3_675 . ?
O2 Nd O1 61.27(4) . . ?
O2 Nd O1 73.44(4) 2_765 . ?
O1 Nd O1 72.50(4) 2_765 . ?
O1 Nd O1 72.50(4) 3_675 . ?
O1 C1 O1 112.76(16) 11_566 . ?
O1 C1 C2 105.75(7) 11_566 11_566 ?
O1 C1 C2 113.10(8) . 11_566 ?
O1 C1 C2 113.10(8) 11_566 . ?
O1 C1 C2 105.74(7) . . ?
C2 C1 C2 106.36(16) 11_566 . ?
O3 C2 O2 125.70(15) . . ?
O3 C2 C1 117.95(13) . . ?
O2 C2 C1 116.26(12) . . ?
C1 O1 Nd 126.26(8) . . ?
C1 O1 H1 114.6(16) . . ?
Nd O1 H1 117.6(16) . . ?
C2 O2 Nd 126.86(10) . . ?
Nd OW HW1 127.6(16) . . ?
Nd OW HW2 121.7(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 0.846(16) 1.762(16) 2.5985(17) 169(2) 10_556
OW HW1 O3 0.843(15) 1.882(15) 2.7079(19) 166(2) 18_656
OW HW2 O2 0.899(15) 2.051(16) 2.939(2) 170(2) 17_666
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full 36.12
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max 0.915
_refine_diff_density_min -0.723
_refine_diff_density_rms 0.094
#===END
data_gdketo
_database_code_depnum_ccdc_archive 'CCDC 853396'
#TrackingRef '- crystaldata-all.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 ?
_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 bloc
_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 ' Empirical Absorption Correction 2001 Higashi'
_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 10169
_diffrn_reflns_av_R_equivalents 0.0346
_diffrn_reflns_av_sigmaI/netI 0.0310
_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 4.23
_diffrn_reflns_theta_max 33.14
_reflns_number_total 1425
_reflns_number_gt 1389
_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 'publCIF (Westrip, 2009)'
_publ_section_references
;
Rigaku Spider and CrystalClear.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 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 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^)+(0.0073P)^2^+2.2130P] 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 -0.027(16)
_refine_ls_number_reflns 1425
_refine_ls_number_parameters 63
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0187
_refine_ls_R_factor_gt 0.0179
_refine_ls_wR_factor_ref 0.0394
_refine_ls_wR_factor_gt 0.0391
_refine_ls_goodness_of_fit_ref 1.190
_refine_ls_restrained_S_all 1.192
_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) 0.00883(5) Uani 1 3 d SD . .
C1 C 0.7977(3) 0.6667 0.6667 0.0102(6) Uani 1 2 d S . .
C2 C 0.6902(3) 0.6461(3) 0.72650(12) 0.0140(5) Uani 1 1 d . . .
O1 O 0.9449(2) 0.8022(2) 0.67977(9) 0.0140(4) Uani 1 1 d D . .
H1 H 1.011(3) 0.809(4) 0.6505(13) 0.021 Uiso 1 1 d D . .
O2 O 0.7335(3) 0.7682(3) 0.76080(10) 0.0204(4) Uani 1 1 d . . .
O3 O 0.5680(3) 0.5140(3) 0.73449(11) 0.0307(6) Uani 1 1 d . . .
OW O 0.9859(3) 0.8185(3) 0.84797(12) 0.0316(6) Uani 1 1 d D . .
HW1 H 0.901(3) 0.736(3) 0.8621(16) 0.047 Uiso 1 1 d D . .
HW2 H 1.070(3) 0.825(4) 0.8684(16) 0.047 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 0.00916(6) 0.00916(6) 0.00816(8) 0.000 0.000 0.00458(3)
C1 0.0103(12) 0.0104(14) 0.0100(14) -0.0001(11) 0.0000(5) 0.0052(7)
C2 0.0128(12) 0.0152(12) 0.0121(12) -0.0019(9) 0.0018(8) 0.0056(10)
O1 0.0076(8) 0.0138(8) 0.0156(8) -0.0030(7) 0.0028(6) 0.0017(7)
O2 0.0163(10) 0.0164(10) 0.0199(10) -0.0056(7) 0.0071(7) 0.0017(8)
O3 0.0233(11) 0.0162(10) 0.0343(12) -0.0095(8) 0.0159(8) -0.0038(9)
OW 0.0256(13) 0.0379(14) 0.0358(14) 0.0239(11) 0.0129(10) 0.0193(11)
_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 2.392(2) 2_765 ?
Gd OW 2.392(2) . ?
Gd OW 2.392(2) 3_675 ?
Gd O2 2.422(2) 3_675 ?
Gd O2 2.422(2) 2_765 ?
Gd O2 2.422(2) . ?
Gd O1 2.4730(19) 2_765 ?
Gd O1 2.4730(19) 3_675 ?
Gd O1 2.4730(19) . ?
C1 O1 1.393(2) 11_566 ?
C1 O1 1.393(2) . ?
C1 C2 1.564(3) 11_566 ?
C1 C2 1.564(3) . ?
C2 O3 1.240(3) . ?
C2 O2 1.255(3) . ?
O1 H1 0.859(18) . ?
OW HW1 0.861(17) . ?
OW HW2 0.889(17) . ?
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 75.23(11) 2_765 . ?
OW Gd OW 75.23(11) 2_765 3_675 ?
OW Gd OW 75.23(11) . 3_675 ?
OW Gd O2 69.54(7) 2_765 3_675 ?
OW Gd O2 137.37(9) . 3_675 ?
OW Gd O2 73.23(8) 3_675 3_675 ?
OW Gd O2 73.23(9) 2_765 2_765 ?
OW Gd O2 69.54(7) . 2_765 ?
OW Gd O2 137.37(9) 3_675 2_765 ?
O2 Gd O2 119.792(8) 3_675 2_765 ?
OW Gd O2 137.37(9) 2_765 . ?
OW Gd O2 73.23(9) . . ?
OW Gd O2 69.54(7) 3_675 . ?
O2 Gd O2 119.792(8) 3_675 . ?
O2 Gd O2 119.791(8) 2_765 . ?
OW Gd O1 92.20(9) 2_765 2_765 ?
OW Gd O1 131.83(7) . 2_765 ?
OW Gd O1 146.81(7) 3_675 2_765 ?
O2 Gd O1 73.60(7) 3_675 2_765 ?
O2 Gd O1 62.32(6) 2_765 2_765 ?
O2 Gd O1 130.32(7) . 2_765 ?
OW Gd O1 131.83(7) 2_765 3_675 ?
OW Gd O1 146.81(8) . 3_675 ?
OW Gd O1 92.19(8) 3_675 3_675 ?
O2 Gd O1 62.32(6) 3_675 3_675 ?
O2 Gd O1 130.33(7) 2_765 3_675 ?
O2 Gd O1 73.60(7) . 3_675 ?
O1 Gd O1 73.29(7) 2_765 3_675 ?
OW Gd O1 146.81(7) 2_765 . ?
OW Gd O1 92.20(9) . . ?
OW Gd O1 131.83(7) 3_675 . ?
O2 Gd O1 130.32(7) 3_675 . ?
O2 Gd O1 73.60(7) 2_765 . ?
O2 Gd O1 62.32(6) . . ?
O1 Gd O1 73.29(7) 2_765 . ?
O1 Gd O1 73.29(7) 3_675 . ?
O1 C1 O1 113.3(3) 11_566 . ?
O1 C1 C2 105.28(13) 11_566 11_566 ?
O1 C1 C2 113.27(14) . 11_566 ?
O1 C1 C2 113.26(13) 11_566 . ?
O1 C1 C2 105.27(13) . . ?
C2 C1 C2 106.4(3) 11_566 . ?
O3 C2 O2 125.9(3) . . ?
O3 C2 C1 117.7(2) . . ?
O2 C2 C1 116.3(2) . . ?
C1 O1 Gd 126.15(13) . . ?
C1 O1 H1 108(2) . . ?
Gd O1 H1 126(2) . . ?
C2 O2 Gd 126.39(18) . . ?
Gd OW HW1 127(2) . . ?
Gd OW HW2 125(2) . . ?
HW1 OW HW2 109(3) . . ?
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 0.859(18) 1.78(2) 2.593(3) 158(3) 10_556
OW HW1 O3 0.861(17) 1.92(2) 2.700(3) 151(3) 18_656
OW HW2 O2 0.889(17) 2.097(19) 2.967(3) 166(3) 17_666
OW HW2 OW 0.889(17) 2.40(4) 2.836(5) 110(3) 16_546
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 33.14
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.834
_refine_diff_density_min -0.959
_refine_diff_density_rms 0.125
#===END
data_erketo
_database_code_depnum_ccdc_archive 'CCDC 853397'
#TrackingRef '- crystaldata-all.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-\D-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')erbium(III)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C9 H18 Er2 O24'
_chemical_formula_sum 'C9 H18 Er2 O24'
_chemical_formula_weight 844.75
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'
Er Er -0.2586 4.9576 '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 9.5813(2)
_cell_length_b 9.5813(2)
_cell_length_c 20.4715(6)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 1627.53(7)
_cell_formula_units_Z 3
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 9935
_cell_measurement_theta_min 2.65
_cell_measurement_theta_max 34.14
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.11
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.586
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1200
_exptl_absorpt_coefficient_mu 7.796
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.1893
_exptl_absorpt_correction_T_max 0.4809
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_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 'Bruker APEX2 CCD area detector'
_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 13137
_diffrn_reflns_av_R_equivalents 0.0255
_diffrn_reflns_av_sigmaI/netI 0.0163
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_theta_min 2.65
_diffrn_reflns_theta_max 34.49
_reflns_number_total 1480
_reflns_number_gt 1473
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
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~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
;
_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.
;
_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^)+(0.0148P)^2^+3.8931P] 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 0.012(12)
_refine_ls_number_reflns 1480
_refine_ls_number_parameters 63
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0133
_refine_ls_R_factor_gt 0.0132
_refine_ls_wR_factor_ref 0.0357
_refine_ls_wR_factor_gt 0.0357
_refine_ls_goodness_of_fit_ref 1.230
_refine_ls_restrained_S_all 1.246
_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
Er Er 0.0000 0.0000 0.234896(5) 0.00601(4) Uani 1 3 d SD . .
C1 C 0.2015(3) 0.3333 0.3333 0.0068(5) Uani 1 2 d S . .
C2 C 0.3081(3) 0.3526(3) 0.27295(11) 0.0097(4) Uani 1 1 d . . .
O1 O 0.05312(19) 0.19662(19) 0.32032(8) 0.0095(3) Uani 1 1 d D . .
H1 H -0.018(3) 0.186(4) 0.3498(14) 0.014 Uiso 1 1 d D . .
O2 O 0.2651(2) 0.2278(2) 0.23892(9) 0.0133(3) Uani 1 1 d . . .
O3 O 0.4313(2) 0.4861(2) 0.26372(10) 0.0210(4) Uani 1 1 d . . .
OW O 0.0153(2) 0.1800(3) 0.15447(10) 0.0206(4) Uani 1 1 d D . .
HW1 H 0.102(3) 0.259(3) 0.1369(15) 0.031 Uiso 1 1 d D . .
HW2 H -0.073(3) 0.158(4) 0.1276(15) 0.031 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
Er 0.00646(4) 0.00646(4) 0.00509(6) 0.000 0.000 0.00323(2)
C1 0.0069(8) 0.0063(10) 0.0068(11) -0.0009(8) -0.0005(4) 0.0032(5)
C2 0.0090(9) 0.0100(9) 0.0082(9) -0.0021(7) 0.0002(6) 0.0033(7)
O1 0.0050(6) 0.0088(6) 0.0105(7) -0.0021(5) 0.0018(5) 0.0005(5)
O2 0.0129(7) 0.0105(7) 0.0123(8) -0.0037(6) 0.0047(6) 0.0028(6)
O3 0.0169(8) 0.0113(7) 0.0219(9) -0.0056(6) 0.0113(7) -0.0026(6)
OW 0.0157(8) 0.0239(10) 0.0235(9) 0.0155(8) 0.0075(7) 0.0109(8)
_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
Er OW 2.3357(19) 2 ?
Er OW 2.3357(19) . ?
Er OW 2.3357(19) 3 ?
Er O2 2.3831(18) 3 ?
Er O2 2.3831(18) . ?
Er O2 2.3832(18) 2 ?
Er O1 2.4305(16) . ?
Er O1 2.4305(16) 3 ?
Er O1 2.4305(16) 2 ?
C1 O1 1.395(2) 17 ?
C1 O1 1.395(2) . ?
C1 C2 1.555(3) . ?
C1 C2 1.555(3) 17 ?
C2 O3 1.247(3) . ?
C2 O2 1.262(3) . ?
O1 H1 0.879(18) . ?
OW HW1 0.877(17) . ?
OW HW2 0.939(17) . ?
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 Er OW 75.80(9) 2 . ?
OW Er OW 75.80(9) 2 3 ?
OW Er OW 75.80(9) . 3 ?
OW Er O2 68.74(6) 2 3 ?
OW Er O2 137.07(7) . 3 ?
OW Er O2 72.76(7) 3 3 ?
OW Er O2 137.07(7) 2 . ?
OW Er O2 72.75(7) . . ?
OW Er O2 68.74(6) 3 . ?
O2 Er O2 119.882(5) 3 . ?
OW Er O2 72.76(7) 2 2 ?
OW Er O2 68.74(6) . 2 ?
OW Er O2 137.07(7) 3 2 ?
O2 Er O2 119.881(5) 3 2 ?
O2 Er O2 119.881(5) . 2 ?
OW Er O1 145.97(6) 2 . ?
OW Er O1 91.33(7) . . ?
OW Er O1 132.04(6) 3 . ?
O2 Er O1 131.53(6) 3 . ?
O2 Er O1 63.33(5) . . ?
O2 Er O1 73.22(6) 2 . ?
OW Er O1 132.04(6) 2 3 ?
OW Er O1 145.97(6) . 3 ?
OW Er O1 91.33(7) 3 3 ?
O2 Er O1 63.33(5) 3 3 ?
O2 Er O1 73.22(6) . 3 ?
O2 Er O1 131.53(6) 2 3 ?
O1 Er O1 73.94(6) . 3 ?
OW Er O1 91.33(7) 2 2 ?
OW Er O1 132.04(6) . 2 ?
OW Er O1 145.97(6) 3 2 ?
O2 Er O1 73.22(6) 3 2 ?
O2 Er O1 131.53(6) . 2 ?
O2 Er O1 63.33(5) 2 2 ?
O1 Er O1 73.95(6) . 2 ?
O1 Er O1 73.94(6) 3 2 ?
O1 C1 O1 113.3(2) 17 . ?
O1 C1 C2 113.37(11) 17 . ?
O1 C1 C2 105.09(11) . . ?
O1 C1 C2 105.09(10) 17 17 ?
O1 C1 C2 113.37(11) . 17 ?
C2 C1 C2 106.6(2) . 17 ?
O3 C2 O2 125.6(2) . . ?
O3 C2 C1 118.09(18) . . ?
O2 C2 C1 116.26(18) . . ?
C1 O1 Er 125.83(12) . . ?
C1 O1 H1 110(2) . . ?
Er O1 H1 124(2) . . ?
C2 O2 Er 125.48(15) . . ?
Er OW HW1 128(2) . . ?
Er OW HW2 122.2(18) . . ?
HW1 OW HW2 108(3) . . ?
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 0.879(18) 1.73(2) 2.579(2) 161(3) 16_445
OW HW1 O3 0.877(17) 1.86(2) 2.690(3) 157(3) 12
OW HW2 O2 0.939(17) 2.05(2) 2.964(3) 164(3) 11_455
_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full 34.49
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max 1.679
_refine_diff_density_min -2.219
_refine_diff_density_rms 0.138
#===END
data_ybketo_2
_database_code_depnum_ccdc_archive 'CCDC 853398'
#TrackingRef '- crystaldata-all.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-\D-[triaqua-1.5(\m-dihydroxymalonato-
\kO,O'':O''',O'''')ytterbium(III)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C9 H18 O24 Yb2'
_chemical_formula_sum 'C9 H18 O24 Yb2'
_chemical_formula_weight 856.31
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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 9.55480(10)
_cell_length_b 9.55480(10)
_cell_length_c 20.4006(4)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 1612.93(4)
_cell_formula_units_Z 3
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 9863
_cell_measurement_theta_min 3.17
_cell_measurement_theta_max 35.99
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.11
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.645
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1212
_exptl_absorpt_coefficient_mu 8.759
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.1659
_exptl_absorpt_correction_T_max 0.4458
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_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 'Bruker APEX2 CCD area detector'
_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 21721
_diffrn_reflns_av_R_equivalents 0.0252
_diffrn_reflns_av_sigmaI/netI 0.0165
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_theta_min 2.66
_diffrn_reflns_theta_max 36.25
_reflns_number_total 1696
_reflns_number_gt 1662
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material 'publCIF (Westrip, 2009)'
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
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~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
;
_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.
;
_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^)+(0.0183P)^2^+0.6634P] 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 0.010(11)
_refine_ls_number_reflns 1696
_refine_ls_number_parameters 63
_refine_ls_number_restraints 4
_refine_ls_R_factor_all 0.0137
_refine_ls_R_factor_gt 0.0132
_refine_ls_wR_factor_ref 0.0367
_refine_ls_wR_factor_gt 0.0366
_refine_ls_goodness_of_fit_ref 1.276
_refine_ls_restrained_S_all 1.325
_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
YB Yb 0.0000 0.0000 0.235333(5) 0.00632(4) Uani 1 3 d S . .
C1 C 0.2013(3) 0.3333 0.3333 0.0072(4) Uani 1 2 d S . .
C2 C 0.3081(3) 0.3524(3) 0.27281(10) 0.0097(3) Uani 1 1 d . . .
O1 O 0.05263(18) 0.19596(19) 0.32047(8) 0.0099(3) Uani 1 1 d D . .
H1 H -0.022(3) 0.186(4) 0.3499(14) 0.015 Uiso 1 1 d D . .
O2 O 0.2647(2) 0.2264(2) 0.23910(8) 0.0133(3) Uani 1 1 d . . .
O3 O 0.4309(2) 0.4859(2) 0.26318(9) 0.0214(4) Uani 1 1 d . . .
OW O 0.0165(2) 0.1800(3) 0.15556(10) 0.0199(4) Uani 1 1 d D . .
HW1 H 0.106(3) 0.256(4) 0.1359(15) 0.030 Uiso 1 1 d D . .
HW2 H -0.071(3) 0.162(5) 0.1261(15) 0.030 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
YB 0.00650(4) 0.00650(4) 0.00598(5) 0.000 0.000 0.00325(2)
C1 0.0070(8) 0.0067(10) 0.0077(10) -0.0005(8) -0.0003(4) 0.0033(5)
C2 0.0094(8) 0.0096(8) 0.0083(8) -0.0016(6) 0.0009(6) 0.0034(7)
O1 0.0053(5) 0.0092(6) 0.0114(6) -0.0021(5) 0.0013(5) 0.0008(5)
O2 0.0128(7) 0.0099(7) 0.0134(7) -0.0034(5) 0.0040(5) 0.0028(6)
O3 0.0174(8) 0.0114(7) 0.0234(8) -0.0056(6) 0.0116(6) -0.0017(6)
OW 0.0144(8) 0.0236(9) 0.0228(9) 0.0147(7) 0.0073(6) 0.0103(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
YB OW 2.3153(18) . ?
YB OW 2.3153(18) 2 ?
YB OW 2.3153(18) 3 ?
YB O2 2.3686(17) 3 ?
YB O2 2.3687(17) . ?
YB O2 2.3687(17) 2 ?
YB O1 2.4152(15) 3 ?
YB O1 2.4152(15) 2 ?
YB O1 2.4152(15) . ?
C1 O1 1.395(2) 17 ?
C1 O1 1.395(2) . ?
C1 C2 1.554(3) . ?
C1 C2 1.554(3) 17 ?
C2 O3 1.243(3) . ?
C2 O2 1.263(3) . ?
O1 H1 0.897(18) . ?
OW HW1 0.894(18) . ?
OW HW2 0.974(18) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
OW YB OW 76.05(8) . 2 ?
OW YB OW 76.05(8) . 3 ?
OW YB OW 76.05(8) 2 3 ?
OW YB O2 137.12(7) . 3 ?
OW YB O2 68.66(6) 2 3 ?
OW YB O2 72.51(7) 3 3 ?
OW YB O2 72.51(7) . . ?
OW YB O2 137.12(7) 2 . ?
OW YB O2 68.66(6) 3 . ?
O2 YB O2 119.896(5) 3 . ?
OW YB O2 68.66(6) . 2 ?
OW YB O2 72.51(7) 2 2 ?
OW YB O2 137.12(7) 3 2 ?
O2 YB O2 119.896(4) 3 2 ?
O2 YB O2 119.896(5) . 2 ?
OW YB O1 145.60(6) . 3 ?
OW YB O1 132.23(6) 2 3 ?
OW YB O1 91.09(7) 3 3 ?
O2 YB O1 63.60(5) 3 3 ?
O2 YB O1 73.09(6) . 3 ?
O2 YB O1 131.73(6) 2 3 ?
OW YB O1 132.23(6) . 2 ?
OW YB O1 91.09(7) 2 2 ?
OW YB O1 145.60(6) 3 2 ?
O2 YB O1 73.09(6) 3 2 ?
O2 YB O1 131.72(6) . 2 ?
O2 YB O1 63.60(5) 2 2 ?
O1 YB O1 74.00(6) 3 2 ?
OW YB O1 91.09(7) . . ?
OW YB O1 145.60(6) 2 . ?
OW YB O1 132.23(6) 3 . ?
O2 YB O1 131.73(6) 3 . ?
O2 YB O1 63.60(5) . . ?
O2 YB O1 73.09(6) 2 . ?
O1 YB O1 74.00(6) 3 . ?
O1 YB O1 74.00(6) 2 . ?
O1 C1 O1 113.6(2) 17 . ?
O1 C1 C2 113.25(11) 17 . ?
O1 C1 C2 105.13(10) . . ?
O1 C1 C2 105.14(10) 17 17 ?
O1 C1 C2 113.25(11) . 17 ?
C2 C1 C2 106.5(2) . 17 ?
O3 C2 O2 125.7(2) . . ?
O3 C2 C1 118.25(17) . . ?
O2 C2 C1 115.94(17) . . ?
C1 O1 YB 125.75(11) . . ?
C1 O1 H1 111(2) . . ?
YB O1 H1 123(2) . . ?
C2 O2 YB 125.46(14) . . ?
YB OW HW1 127(2) . . ?
YB OW HW2 125(2) . . ?
HW1 OW HW2 105(3) . . ?
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 0.897(18) 1.71(2) 2.575(2) 160(3) 16_445
OW HW1 O3 0.894(18) 1.83(2) 2.687(3) 159(3) 12
OW HW2 O2 0.974(18) 2.04(2) 2.972(3) 160(3) 11_455
_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full 36.25
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max 1.607
_refine_diff_density_min -2.094
_refine_diff_density_rms 0.201
#===END