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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Peng Cheng'
_publ_contact_author_email       PCHENG@NANKAI.EDU.CN

_publ_section_title              
;
The 3D heterometal-organic frameworks based
on oxydiacetic acid
;
loop_
_publ_author_name
'Peng Cheng.'
'Dai-Zheng Liao.'
'Wei Shi.'
'Ying Wang.'
'Shi-Ping Yan.'

#=====================================================#

data_La-Pb
_database_code_depnum_ccdc_archive 'CCDC 289448'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H32 La2 O28 Pb1'
_chemical_formula_weight         1157.31

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'
Pb Pb -3.3944 10.1111 '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           Tetragonal
_symmetry_space_group_name_H-M   I-42d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   13.9901(7)
_cell_length_b                   13.9901(7)
_cell_length_c                   18.2013(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3562.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5087
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      26.89

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_absorpt_coefficient_mu    7.165
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5343
_exptl_absorpt_correction_T_max  0.5343
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12302
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1573
_reflns_number_gt                1446
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0394P)^2^+10.7298P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(9)
_refine_ls_number_reflns         1573
_refine_ls_number_parameters     122
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.172
_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
Pb1 Pb 0.0000 0.0000 0.0000 0.02275(17) Uani 1 4 d S . .
La1 La 0.01400(4) 0.2500 0.1250 0.02142(18) Uani 1 2 d S . .
O1 O -0.2008(4) 0.0101(4) 0.1712(4) 0.0439(16) Uani 1 1 d . . .
O2 O -0.0802(4) 0.0928(4) 0.1227(4) 0.0322(14) Uani 1 1 d . . .
O3 O -0.1779(5) 0.2500 0.1250 0.039(2) Uani 1 2 d S . .
O4 O 0.1109(4) 0.1298(4) 0.0511(3) 0.0272(14) Uani 1 1 d . . .
O5 O 0.2382(4) 0.0579(4) 0.0025(4) 0.0364(14) Uani 1 1 d . . .
O6 O 0.2098(5) 0.2500 0.1250 0.036(2) Uani 1 2 d S . .
O7 O 0.0873(5) 0.3664(4) 0.0297(4) 0.0391(16) Uani 1 1 d . . .
C1 C -0.1655(6) 0.0824(6) 0.1442(5) 0.0287(19) Uani 1 1 d . . .
C2 C -0.2328(6) 0.1659(5) 0.1325(6) 0.0331(19) Uani 1 1 d . . .
H2A H -0.2706 0.1557 0.0885 0.040 Uiso 1 1 calc R . .
H2B H -0.2758 0.1719 0.1740 0.040 Uiso 1 1 calc R . .
C3 C 0.1993(6) 0.1174(6) 0.0419(5) 0.0258(19) Uani 1 1 d . . .
C4 C 0.2645(6) 0.1844(6) 0.0843(5) 0.0323(19) Uani 1 1 d . . .
H4A H 0.3047 0.1476 0.1172 0.039 Uiso 1 1 calc R . .
H4B H 0.3055 0.2186 0.0503 0.039 Uiso 1 1 calc R . .
O8 O 0.5000 0.0000 0.0777(14) 0.091(7) Uani 0.50 2 d SPU . .
O9 O 0.4967(14) 0.8541(13) 0.2387(9) 0.084(5) Uani 0.50 1 d PU A 1
O10 O 0.493(2) 0.784(2) 0.133(2) 0.088(10) Uani 0.25 1 d PU . 2

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
Pb1 0.0193(2) 0.0193(2) 0.0296(3) 0.000 0.000 0.000
La1 0.0168(3) 0.0196(3) 0.0279(3) -0.0068(3) 0.000 0.000
O1 0.037(3) 0.024(3) 0.071(4) 0.007(3) 0.013(3) 0.001(3)
O2 0.024(3) 0.023(3) 0.050(4) -0.005(3) 0.005(3) 0.000(2)
O3 0.019(4) 0.018(4) 0.079(7) 0.005(5) 0.000 0.000
O4 0.022(3) 0.026(3) 0.034(3) -0.010(3) -0.003(3) -0.005(2)
O5 0.034(3) 0.036(3) 0.040(3) -0.023(3) 0.000(3) 0.005(3)
O6 0.017(4) 0.039(5) 0.052(6) -0.030(4) 0.000 0.000
O7 0.042(4) 0.035(4) 0.040(4) -0.006(3) 0.004(3) -0.014(3)
C1 0.030(4) 0.020(4) 0.036(5) 0.000(4) -0.001(4) 0.002(3)
C2 0.025(4) 0.027(4) 0.047(5) 0.003(4) 0.007(5) 0.001(4)
C3 0.021(4) 0.025(4) 0.031(5) -0.004(4) -0.003(3) -0.001(3)
C4 0.025(5) 0.035(4) 0.037(5) -0.016(4) 0.003(4) -0.002(4)
O8 0.091(7) 0.091(7) 0.091(7) 0.000 0.000 -0.0002(10)
O9 0.084(5) 0.084(5) 0.085(5) 0.0008(10) -0.0002(10) 0.0001(10)
O10 0.088(10) 0.088(10) 0.088(10) -0.0001(10) 0.0000(10) 0.0000(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
Pb1 O4 2.563(5) 3 ?
Pb1 O4 2.563(5) . ?
Pb1 O4 2.563(5) 2 ?
Pb1 O4 2.563(5) 4 ?
La1 O5 2.535(6) 4 ?
La1 O5 2.535(6) 15_454 ?
La1 O4 2.545(6) 14_454 ?
La1 O4 2.545(6) . ?
La1 O2 2.563(5) 14_454 ?
La1 O2 2.563(5) . ?
La1 O7 2.590(6) . ?
La1 O7 2.590(6) 14_454 ?
La1 O3 2.685(7) . ?
La1 O6 2.740(7) . ?
O1 C1 1.227(10) . ?
O2 C1 1.266(10) . ?
O3 C2 1.411(9) . ?
O3 C2 1.411(9) 14_454 ?
O4 C3 1.260(10) . ?
O5 C3 1.226(9) . ?
O5 La1 2.535(6) 3 ?
O6 C4 1.406(9) 14_454 ?
O6 C4 1.406(9) . ?
C1 C2 1.515(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.518(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O10 O10 0.99(7) 14_464 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Pb1 O4 97.57(9) 3 . ?
O4 Pb1 O4 97.58(9) 3 2 ?
O4 Pb1 O4 137.4(3) . 2 ?
O4 Pb1 O4 137.4(3) 3 4 ?
O4 Pb1 O4 97.58(9) . 4 ?
O4 Pb1 O4 97.57(9) 2 4 ?
O5 La1 O5 133.2(3) 4 15_454 ?
O5 La1 O4 137.59(19) 4 14_454 ?
O5 La1 O4 71.62(19) 15_454 14_454 ?
O5 La1 O4 71.62(19) 4 . ?
O5 La1 O4 137.59(19) 15_454 . ?
O4 La1 O4 115.6(2) 14_454 . ?
O5 La1 O2 82.4(2) 4 14_454 ?
O5 La1 O2 74.0(2) 15_454 14_454 ?
O4 La1 O2 72.43(17) 14_454 14_454 ?
O4 La1 O2 148.2(2) . 14_454 ?
O5 La1 O2 74.0(2) 4 . ?
O5 La1 O2 82.4(2) 15_454 . ?
O4 La1 O2 148.2(2) 14_454 . ?
O4 La1 O2 72.43(17) . . ?
O2 La1 O2 118.1(2) 14_454 . ?
O5 La1 O7 65.49(19) 4 . ?
O5 La1 O7 136.8(2) 15_454 . ?
O4 La1 O7 74.2(2) 14_454 . ?
O4 La1 O7 81.42(18) . . ?
O2 La1 O7 71.1(2) 14_454 . ?
O2 La1 O7 137.0(2) . . ?
O5 La1 O7 136.8(2) 4 14_454 ?
O5 La1 O7 65.49(19) 15_454 14_454 ?
O4 La1 O7 81.42(18) 14_454 14_454 ?
O4 La1 O7 74.2(2) . 14_454 ?
O2 La1 O7 137.0(2) 14_454 14_454 ?
O2 La1 O7 71.1(2) . 14_454 ?
O7 La1 O7 133.4(3) . 14_454 ?
O5 La1 O3 66.61(13) 4 . ?
O5 La1 O3 66.61(13) 15_454 . ?
O4 La1 O3 122.19(12) 14_454 . ?
O4 La1 O3 122.20(12) . . ?
O2 La1 O3 59.07(12) 14_454 . ?
O2 La1 O3 59.07(12) . . ?
O7 La1 O3 113.31(16) . . ?
O7 La1 O3 113.31(16) 14_454 . ?
O5 La1 O6 113.39(13) 4 . ?
O5 La1 O6 113.39(13) 15_454 . ?
O4 La1 O6 57.81(12) 14_454 . ?
O4 La1 O6 57.80(12) . . ?
O2 La1 O6 120.93(12) 14_454 . ?
O2 La1 O6 120.93(12) . . ?
O7 La1 O6 66.69(16) . . ?
O7 La1 O6 66.69(16) 14_454 . ?
O3 La1 O6 180.0 . . ?
C1 O2 La1 125.4(5) . . ?
C2 O3 C2 114.1(8) . 14_454 ?
C2 O3 La1 122.9(4) . . ?
C2 O3 La1 122.9(4) 14_454 . ?
C3 O4 La1 133.2(5) . . ?
C3 O4 Pb1 116.7(5) . . ?
La1 O4 Pb1 109.7(2) . . ?
C3 O5 La1 146.5(6) . 3 ?
C4 O6 C4 114.1(8) 14_454 . ?
C4 O6 La1 122.9(4) 14_454 . ?
C4 O6 La1 122.9(4) . . ?
O1 C1 O2 126.8(8) . . ?
O1 C1 C2 116.3(7) . . ?
O2 C1 C2 116.9(7) . . ?
O3 C2 C1 108.6(6) . . ?
O3 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O3 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
O5 C3 O4 127.3(8) . . ?
O5 C3 C4 116.7(7) . . ?
O4 C3 C4 115.9(7) . . ?
O6 C4 C3 110.1(7) . . ?
O6 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
O6 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 La1 O2 C1 -94.5(7) 4 . . . ?
O5 La1 O2 C1 44.7(7) 15_454 . . . ?
O4 La1 O2 C1 79.7(8) 14_454 . . . ?
O4 La1 O2 C1 -169.8(7) . . . . ?
O2 La1 O2 C1 -22.5(6) 14_454 . . . ?
O7 La1 O2 C1 -114.5(7) . . . . ?
O7 La1 O2 C1 111.4(7) 14_454 . . . ?
O3 La1 O2 C1 -22.5(6) . . . . ?
O6 La1 O2 C1 157.5(6) . . . . ?
O5 La1 O3 C2 92.5(5) 4 . . . ?
O5 La1 O3 C2 -87.5(5) 15_454 . . . ?
O4 La1 O3 C2 -134.8(5) 14_454 . . . ?
O4 La1 O3 C2 45.2(5) . . . . ?
O2 La1 O3 C2 -172.3(5) 14_454 . . . ?
O2 La1 O3 C2 7.7(5) . . . . ?
O7 La1 O3 C2 139.8(5) . . . . ?
O7 La1 O3 C2 -40.2(5) 14_454 . . . ?
O6 La1 O3 C2 0(100) . . . . ?
O5 La1 O3 C2 -87.5(5) 4 . . 14_454 ?
O5 La1 O3 C2 92.5(5) 15_454 . . 14_454 ?
O4 La1 O3 C2 45.2(5) 14_454 . . 14_454 ?
O4 La1 O3 C2 -134.8(5) . . . 14_454 ?
O2 La1 O3 C2 7.7(5) 14_454 . . 14_454 ?
O2 La1 O3 C2 -172.3(5) . . . 14_454 ?
O7 La1 O3 C2 -40.2(5) . . . 14_454 ?
O7 La1 O3 C2 139.8(5) 14_454 . . 14_454 ?
O6 La1 O3 C2 0(29) . . . 14_454 ?
O5 La1 O4 C3 133.3(8) 4 . . . ?
O5 La1 O4 C3 -91.8(8) 15_454 . . . ?
O4 La1 O4 C3 -1.5(7) 14_454 . . . ?
O2 La1 O4 C3 96.4(8) 14_454 . . . ?
O2 La1 O4 C3 -148.2(8) . . . . ?
O7 La1 O4 C3 66.3(7) . . . . ?
O7 La1 O4 C3 -73.5(7) 14_454 . . . ?
O3 La1 O4 C3 178.5(7) . . . . ?
O6 La1 O4 C3 -1.5(7) . . . . ?
O5 La1 O4 Pb1 -55.0(2) 4 . . . ?
O5 La1 O4 Pb1 79.9(3) 15_454 . . . ?
O4 La1 O4 Pb1 170.3(3) 14_454 . . . ?
O2 La1 O4 Pb1 -91.8(4) 14_454 . . . ?
O2 La1 O4 Pb1 23.5(2) . . . . ?
O7 La1 O4 Pb1 -121.9(2) . . . . ?
O7 La1 O4 Pb1 98.2(3) 14_454 . . . ?
O3 La1 O4 Pb1 -9.7(3) . . . . ?
O6 La1 O4 Pb1 170.3(3) . . . . ?
O4 Pb1 O4 C3 0.9(5) 3 . . . ?
O4 Pb1 O4 C3 110.8(6) 2 . . . ?
O4 Pb1 O4 C3 -139.2(7) 4 . . . ?
O4 Pb1 O4 La1 -172.4(3) 3 . . . ?
O4 Pb1 O4 La1 -62.44(17) 2 . . . ?
O4 Pb1 O4 La1 47.52(7) 4 . . . ?
O5 La1 O6 C4 133.0(5) 4 . . 14_454 ?
O5 La1 O6 C4 -47.0(5) 15_454 . . 14_454 ?
O4 La1 O6 C4 0.3(5) 14_454 . . 14_454 ?
O4 La1 O6 C4 -179.7(5) . . . 14_454 ?
O2 La1 O6 C4 37.8(5) 14_454 . . 14_454 ?
O2 La1 O6 C4 -142.2(5) . . . 14_454 ?
O7 La1 O6 C4 85.7(5) . . . 14_454 ?
O7 La1 O6 C4 -94.3(5) 14_454 . . 14_454 ?
O3 La1 O6 C4 0(84) . . . 14_454 ?
O5 La1 O6 C4 -47.0(5) 4 . . . ?
O5 La1 O6 C4 133.0(5) 15_454 . . . ?
O4 La1 O6 C4 -179.7(5) 14_454 . . . ?
O4 La1 O6 C4 0.3(5) . . . . ?
O2 La1 O6 C4 -142.2(5) 14_454 . . . ?
O2 La1 O6 C4 37.8(5) . . . . ?
O7 La1 O6 C4 -94.3(5) . . . . ?
O7 La1 O6 C4 85.7(5) 14_454 . . . ?
O3 La1 O6 C4 0(100) . . . . ?
La1 O2 C1 O1 -149.0(7) . . . . ?
La1 O2 C1 C2 34.1(11) . . . . ?
C2 O3 C2 C1 -176.8(9) 14_454 . . . ?
La1 O3 C2 C1 3.2(9) . . . . ?
O1 C1 C2 O3 160.8(8) . . . . ?
O2 C1 C2 O3 -22.0(11) . . . . ?
La1 O5 C3 O4 52.8(15) 3 . . . ?
La1 O5 C3 C4 -126.9(9) 3 . . . ?
La1 O4 C3 O5 -177.4(6) . . . . ?
Pb1 O4 C3 O5 11.2(12) . . . . ?
La1 O4 C3 C4 2.3(12) . . . . ?
Pb1 O4 C3 C4 -169.0(6) . . . . ?
C4 O6 C4 C3 -179.5(9) 14_454 . . . ?
La1 O6 C4 C3 0.5(9) . . . . ?
O5 C3 C4 O6 178.2(7) . . . . ?
O4 C3 C4 O6 -1.5(11) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.165
#=====================================================END


# Attachment 'La_Ni.cif'

data_La_Ni
_database_code_depnum_ccdc_archive 'CCDC 289449'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 La0.33 Ni0.50 O7'
_chemical_formula_sum            'C4 H8 La0.33 Ni0.50 O7'
_chemical_formula_weight         243.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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           Hexagonal
_symmetry_space_group_name_H-M   P6/mcc

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

_cell_length_a                   15.3476(8)
_cell_length_b                   15.3476(8)
_cell_length_c                   14.9728(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3054.3(4)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3428
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      26.50

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5177
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating node'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15318
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         25.02
_reflns_number_total             951
_reflns_number_gt                740
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0612P)^2^+7.5651P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         951
_refine_ls_number_parameters     76
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.3333 0.6667 0.2500 0.0178(3) Uani 1 6 d S . .
Ni1 Ni 0.0000 0.5000 0.0000 0.0188(3) Uani 1 4 d S . .
O1 O 0.1927(2) 0.6180(3) 0.1411(2) 0.0337(8) Uani 1 1 d . . .
O2 O 0.0509(3) 0.6093(3) 0.0951(3) 0.0441(10) Uani 1 1 d . . .
O3 O -0.1307(3) 0.5100(3) 0.0000 0.0257(10) Uani 1 2 d SD . .
H3A H -0.1599 0.4711 0.0439 0.039 Uiso 1 1 d RD . .
O4 O 0.23589(17) 0.76411(17) 0.2500 0.0322(11) Uani 1 2 d S . .
C1 C 0.1290(4) 0.6465(4) 0.1408(3) 0.0326(11) Uani 1 1 d . . .
C2 C 0.1475(4) 0.7320(5) 0.2001(5) 0.064(2) Uani 1 1 d . . .
H2A H 0.1536 0.7874 0.1642 0.077 Uiso 1 1 calc R . .
H2B H 0.0909 0.7112 0.2402 0.077 Uiso 1 1 calc R . .
O5 O 0.923(3) 0.719(3) 1.0000 0.124(11) Uani 0.30 2 d SPU . .
O6 O 1.006(3) 0.765(3) 1.0000 0.082(10) Uani 0.20 2 d SPU . .
O7 O 0.822(3) 0.845(3) 0.850(3) 0.205(18) Uani 0.25 1 d PU . .

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
La1 0.0188(3) 0.0188(3) 0.0160(4) 0.000 0.000 0.00939(16)
Ni1 0.0151(6) 0.0207(6) 0.0175(6) 0.000 0.000 0.0067(5)
O1 0.0310(18) 0.0416(19) 0.0339(19) -0.0141(16) -0.0128(16) 0.0223(16)
O2 0.037(2) 0.056(2) 0.050(2) -0.0316(19) -0.0253(18) 0.0305(19)
O3 0.023(2) 0.028(2) 0.024(2) 0.000 0.000 0.011(2)
O4 0.0304(18) 0.0304(18) 0.040(3) -0.0184(19) -0.0184(19) 0.018(2)
C1 0.030(3) 0.035(3) 0.036(3) -0.012(2) -0.011(2) 0.018(2)
C2 0.056(4) 0.071(4) 0.090(5) -0.058(4) -0.054(4) 0.050(4)
O5 0.135(14) 0.106(13) 0.151(15) 0.000 0.000 0.075(10)
O6 0.096(14) 0.071(13) 0.105(15) 0.000 0.000 0.062(10)
O7 0.20(2) 0.19(2) 0.22(2) -0.002(10) -0.002(10) 0.103(13)

_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
La1 O1 2.502(3) . ?
La1 O1 2.502(3) 10_665 ?
La1 O1 2.502(3) 3_565 ?
La1 O1 2.502(3) 12_565 ?
La1 O1 2.502(3) 11 ?
La1 O1 2.502(3) 2_665 ?
La1 O4 2.590(4) . ?
La1 O4 2.590(4) 3_565 ?
La1 O4 2.590(4) 2_665 ?
Ni1 O2 2.036(3) 13_565 ?
Ni1 O2 2.036(3) . ?
Ni1 O2 2.036(3) 16 ?
Ni1 O2 2.036(3) 4_565 ?
Ni1 O3 2.087(4) 13_565 ?
Ni1 O3 2.087(4) . ?
O1 C1 1.254(5) . ?
O2 C1 1.244(6) . ?
O3 H3A 0.8501 . ?
O4 C2 1.405(5) 10_665 ?
O4 C2 1.405(5) . ?
C1 C2 1.491(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O5 O6 1.10(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O1 121.52(15) . 10_665 ?
O1 La1 O1 82.16(12) . 3_565 ?
O1 La1 O1 83.32(16) 10_665 3_565 ?
O1 La1 O1 83.32(16) . 12_565 ?
O1 La1 O1 82.16(12) 10_665 12_565 ?
O1 La1 O1 150.02(16) 3_565 12_565 ?
O1 La1 O1 150.02(16) . 11 ?
O1 La1 O1 82.16(12) 10_665 11 ?
O1 La1 O1 121.52(15) 3_565 11 ?
O1 La1 O1 82.16(12) 12_565 11 ?
O1 La1 O1 82.16(12) . 2_665 ?
O1 La1 O1 150.02(16) 10_665 2_665 ?
O1 La1 O1 82.16(12) 3_565 2_665 ?
O1 La1 O1 121.52(15) 12_565 2_665 ?
O1 La1 O1 83.32(16) 11 2_665 ?
O1 La1 O4 60.76(7) . . ?
O1 La1 O4 60.76(7) 10_665 . ?
O1 La1 O4 75.01(8) 3_565 . ?
O1 La1 O4 75.01(8) 12_565 . ?
O1 La1 O4 138.34(8) 11 . ?
O1 La1 O4 138.34(8) 2_665 . ?
O1 La1 O4 138.34(8) . 3_565 ?
O1 La1 O4 75.01(8) 10_665 3_565 ?
O1 La1 O4 60.76(7) 3_565 3_565 ?
O1 La1 O4 138.34(8) 12_565 3_565 ?
O1 La1 O4 60.76(7) 11 3_565 ?
O1 La1 O4 75.01(8) 2_665 3_565 ?
O4 La1 O4 120.000(1) . 3_565 ?
O1 La1 O4 75.01(8) . 2_665 ?
O1 La1 O4 138.34(8) 10_665 2_665 ?
O1 La1 O4 138.34(8) 3_565 2_665 ?
O1 La1 O4 60.76(7) 12_565 2_665 ?
O1 La1 O4 75.01(8) 11 2_665 ?
O1 La1 O4 60.76(7) 2_665 2_665 ?
O4 La1 O4 120.0 . 2_665 ?
O4 La1 O4 120.0 3_565 2_665 ?
O2 Ni1 O2 180.0(2) 13_565 . ?
O2 Ni1 O2 91.2(2) 13_565 16 ?
O2 Ni1 O2 88.8(2) . 16 ?
O2 Ni1 O2 88.8(2) 13_565 4_565 ?
O2 Ni1 O2 91.2(2) . 4_565 ?
O2 Ni1 O2 180.0 16 4_565 ?
O2 Ni1 O3 85.75(13) 13_565 13_565 ?
O2 Ni1 O3 94.25(13) . 13_565 ?
O2 Ni1 O3 94.25(13) 16 13_565 ?
O2 Ni1 O3 85.75(13) 4_565 13_565 ?
O2 Ni1 O3 94.25(13) 13_565 . ?
O2 Ni1 O3 85.75(13) . . ?
O2 Ni1 O3 85.75(13) 16 . ?
O2 Ni1 O3 94.25(13) 4_565 . ?
O3 Ni1 O3 180.0 13_565 . ?
C1 O1 La1 127.2(3) . . ?
C1 O2 Ni1 130.3(3) . . ?
Ni1 O3 H3A 97.9 . . ?
C2 O4 C2 115.6(5) 10_665 . ?
C2 O4 La1 122.2(3) 10_665 . ?
C2 O4 La1 122.2(3) . . ?
O2 C1 O1 125.7(5) . . ?
O2 C1 C2 116.5(4) . . ?
O1 C1 C2 117.8(4) . . ?
O4 C2 C1 110.5(4) . . ?
O4 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O4 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 La1 O1 C1 -11.4(4) 10_665 . . . ?
O1 La1 O1 C1 -88.6(5) 3_565 . . . ?
O1 La1 O1 C1 65.1(4) 12_565 . . . ?
O1 La1 O1 C1 126.6(4) 11 . . . ?
O1 La1 O1 C1 -171.7(4) 2_665 . . . ?
O4 La1 O1 C1 -11.4(4) . . . . ?
O4 La1 O1 C1 -114.9(4) 3_565 . . . ?
O4 La1 O1 C1 126.6(4) 2_665 . . . ?
O2 Ni1 O2 C1 -169(100) 13_565 . . . ?
O2 Ni1 O2 C1 -100.3(5) 16 . . . ?
O2 Ni1 O2 C1 79.7(5) 4_565 . . . ?
O3 Ni1 O2 C1 -6.1(5) 13_565 . . . ?
O3 Ni1 O2 C1 173.9(5) . . . . ?
O1 La1 O4 C2 -170.7(4) . . . 10_665 ?
O1 La1 O4 C2 9.3(4) 10_665 . . 10_665 ?
O1 La1 O4 C2 -81.3(4) 3_565 . . 10_665 ?
O1 La1 O4 C2 98.7(4) 12_565 . . 10_665 ?
O1 La1 O4 C2 39.5(4) 11 . . 10_665 ?
O1 La1 O4 C2 -140.5(4) 2_665 . . 10_665 ?
O4 La1 O4 C2 -38.9(4) 3_565 . . 10_665 ?
O4 La1 O4 C2 141.1(4) 2_665 . . 10_665 ?
O1 La1 O4 C2 9.3(4) . . . . ?
O1 La1 O4 C2 -170.7(4) 10_665 . . . ?
O1 La1 O4 C2 98.7(4) 3_565 . . . ?
O1 La1 O4 C2 -81.3(4) 12_565 . . . ?
O1 La1 O4 C2 -140.5(4) 11 . . . ?
O1 La1 O4 C2 39.5(4) 2_665 . . . ?
O4 La1 O4 C2 141.1(4) 3_565 . . . ?
O4 La1 O4 C2 -38.9(4) 2_665 . . . ?
Ni1 O2 C1 O1 -4.9(9) . . . . ?
Ni1 O2 C1 C2 175.3(4) . . . . ?
La1 O1 C1 O2 -167.8(4) . . . . ?
La1 O1 C1 C2 12.0(7) . . . . ?
C2 O4 C2 C1 172.2(7) 10_665 . . . ?
La1 O4 C2 C1 -7.8(7) . . . . ?
O2 C1 C2 O4 177.8(5) . . . . ?
O1 C1 C2 O4 -2.0(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.118

# Attachment 'data.cif'

data_La_Zn
_database_code_depnum_ccdc_archive 'CCDC 289450'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 La2 O36 Zn3'
_chemical_formula_weight         1362.42

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'
Zn Zn 0.2839 1.4301 '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           Hexagonal
_symmetry_space_group_name_H-M   P6/mcc

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

_cell_length_a                   15.3708(10)
_cell_length_b                   15.3708(10)
_cell_length_c                   15.118(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3093.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5568
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.88

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      None
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1404
_exptl_absorpt_coefficient_mu    2.583
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6003
_exptl_absorpt_correction_T_max  0.7822
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19215
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0115
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         27.95
_reflns_number_total             1299
_reflns_number_gt                1032
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II CCD area detector'
_computing_cell_refinement       'APEX II CCD area detector'
_computing_data_reduction        'APEX II CCD area detector'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0556P)^2^+1.6805P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1299
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.6667 0.3333 0.2500 0.01962(14) Uani 1 6 d S . .
Zn1 Zn 0.5000 0.0000 0.0000 0.02273(17) Uani 1 4 d S . .
O1 O 0.61795(15) 0.19285(15) 0.14196(13) 0.0360(4) Uani 1 1 d . . .
O2 O 0.61082(18) 0.05201(16) 0.09595(16) 0.0542(7) Uani 1 1 d . . .
O3 O 0.76391(10) 0.23609(10) 0.2500 0.0351(7) Uani 1 2 d S . .
O4 O 0.50806(19) -0.13505(18) 0.0000 0.0308(6) Uani 1 2 d S . .
C1 C 0.6470(2) 0.1297(2) 0.1416(2) 0.0368(6) Uani 1 1 d . . .
C2 C 0.7331(3) 0.1487(3) 0.2001(3) 0.0686(13) Uani 1 1 d . . .
H2A H 0.7130 0.0919 0.2394 0.082 Uiso 1 1 calc R . .
H2B H 0.7887 0.1559 0.1642 0.082 Uiso 1 1 calc R . .

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
La1 0.02041(16) 0.02041(16) 0.0180(2) 0.000 0.000 0.01020(8)
Zn1 0.0243(3) 0.0178(3) 0.0220(3) 0.000 0.000 0.0076(2)
O1 0.0425(10) 0.0335(10) 0.0371(10) -0.0151(9) -0.0161(9) 0.0228(9)
O2 0.0646(15) 0.0457(13) 0.0669(15) -0.0364(12) -0.0418(12) 0.0385(12)
O3 0.0338(11) 0.0338(11) 0.0441(16) -0.0206(10) -0.0206(10) 0.0218(12)
O4 0.0344(13) 0.0248(12) 0.0321(13) 0.000 0.000 0.0140(11)
C1 0.0411(15) 0.0327(14) 0.0403(15) -0.0140(12) -0.0166(13) 0.0211(12)
C2 0.079(3) 0.058(2) 0.095(3) -0.057(2) -0.060(2) 0.054(2)

_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
La1 O1 2.5049(18) 12 ?
La1 O1 2.5049(18) . ?
La1 O1 2.5049(18) 11_655 ?
La1 O1 2.5049(18) 2_655 ?
La1 O1 2.5049(18) 10_665 ?
La1 O1 2.5049(18) 3_665 ?
La1 O3 2.589(3) 3_665 ?
La1 O3 2.589(3) . ?
La1 O3 2.589(3) 2_655 ?
Zn1 O2 2.070(2) . ?
Zn1 O2 2.070(2) 13_655 ?
Zn1 O2 2.070(2) 4_655 ?
Zn1 O2 2.070(2) 16 ?
Zn1 O4 2.140(2) 13_655 ?
Zn1 O4 2.140(2) . ?
O1 C1 1.255(3) . ?
O2 C1 1.244(3) . ?
O3 C2 1.401(3) 10_665 ?
O3 C2 1.401(3) . ?
C1 C2 1.494(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O1 149.99(9) 12 . ?
O1 La1 O1 82.08(7) 12 11_655 ?
O1 La1 O1 83.41(10) . 11_655 ?
O1 La1 O1 121.63(9) 12 2_655 ?
O1 La1 O1 82.08(7) . 2_655 ?
O1 La1 O1 149.99(9) 11_655 2_655 ?
O1 La1 O1 82.08(7) 12 10_665 ?
O1 La1 O1 121.62(9) . 10_665 ?
O1 La1 O1 82.08(7) 11_655 10_665 ?
O1 La1 O1 83.41(10) 2_655 10_665 ?
O1 La1 O1 83.41(10) 12 3_665 ?
O1 La1 O1 82.08(7) . 3_665 ?
O1 La1 O1 121.62(9) 11_655 3_665 ?
O1 La1 O1 82.08(7) 2_655 3_665 ?
O1 La1 O1 149.99(9) 10_665 3_665 ?
O1 La1 O3 75.00(5) 12 3_665 ?
O1 La1 O3 75.00(5) . 3_665 ?
O1 La1 O3 60.81(4) 11_655 3_665 ?
O1 La1 O3 138.29(5) 2_655 3_665 ?
O1 La1 O3 138.29(5) 10_665 3_665 ?
O1 La1 O3 60.81(4) 3_665 3_665 ?
O1 La1 O3 138.29(5) 12 . ?
O1 La1 O3 60.81(4) . . ?
O1 La1 O3 75.00(5) 11_655 . ?
O1 La1 O3 74.99(5) 2_655 . ?
O1 La1 O3 60.81(4) 10_665 . ?
O1 La1 O3 138.29(5) 3_665 . ?
O3 La1 O3 120.0 3_665 . ?
O1 La1 O3 60.81(4) 12 2_655 ?
O1 La1 O3 138.29(5) . 2_655 ?
O1 La1 O3 138.29(5) 11_655 2_655 ?
O1 La1 O3 60.81(4) 2_655 2_655 ?
O1 La1 O3 75.00(5) 10_665 2_655 ?
O1 La1 O3 75.00(5) 3_665 2_655 ?
O3 La1 O3 120.0 3_665 2_655 ?
O3 La1 O3 120.0 . 2_655 ?
O2 Zn1 O2 180.0 . 13_655 ?
O2 Zn1 O2 90.99(15) . 4_655 ?
O2 Zn1 O2 89.01(15) 13_655 4_655 ?
O2 Zn1 O2 89.01(15) . 16 ?
O2 Zn1 O2 90.99(15) 13_655 16 ?
O2 Zn1 O2 180.00(10) 4_655 16 ?
O2 Zn1 O4 93.49(7) . 13_655 ?
O2 Zn1 O4 86.51(7) 13_655 13_655 ?
O2 Zn1 O4 86.51(7) 4_655 13_655 ?
O2 Zn1 O4 93.49(7) 16 13_655 ?
O2 Zn1 O4 86.51(7) . . ?
O2 Zn1 O4 93.49(7) 13_655 . ?
O2 Zn1 O4 93.49(7) 4_655 . ?
O2 Zn1 O4 86.50(7) 16 . ?
O4 Zn1 O4 180.0 13_655 . ?
C1 O1 La1 126.95(17) . . ?
C1 O2 Zn1 130.26(18) . . ?
C2 O3 C2 114.9(3) 10_665 . ?
C2 O3 La1 122.54(16) 10_665 . ?
C2 O3 La1 122.54(16) . . ?
O2 C1 O1 125.7(3) . . ?
O2 C1 C2 116.3(2) . . ?
O1 C1 C2 118.0(2) . . ?
O3 C2 C1 110.3(2) . . ?
O3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
O3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 La1 O1 C1 -126.9(3) 12 . . . ?
O1 La1 O1 C1 -65.5(2) 11_655 . . . ?
O1 La1 O1 C1 88.2(3) 2_655 . . . ?
O1 La1 O1 C1 11.0(2) 10_665 . . . ?
O1 La1 O1 C1 171.2(3) 3_665 . . . ?
O3 La1 O1 C1 -126.9(3) 3_665 . . . ?
O3 La1 O1 C1 11.0(2) . . . . ?
O3 La1 O1 C1 114.5(2) 2_655 . . . ?
O2 Zn1 O2 C1 -23(12) 13_655 . . . ?
O2 Zn1 O2 C1 -79.3(3) 4_655 . . . ?
O2 Zn1 O2 C1 100.7(3) 16 . . . ?
O4 Zn1 O2 C1 7.3(3) 13_655 . . . ?
O4 Zn1 O2 C1 -172.7(3) . . . . ?
O1 La1 O3 C2 -38.8(2) 12 . . 10_665 ?
O1 La1 O3 C2 171.4(2) . . . 10_665 ?
O1 La1 O3 C2 -97.8(2) 11_655 . . 10_665 ?
O1 La1 O3 C2 82.2(2) 2_655 . . 10_665 ?
O1 La1 O3 C2 -8.6(2) 10_665 . . 10_665 ?
O1 La1 O3 C2 141.2(2) 3_665 . . 10_665 ?
O3 La1 O3 C2 -140.3(2) 3_665 . . 10_665 ?
O3 La1 O3 C2 39.7(2) 2_655 . . 10_665 ?
O1 La1 O3 C2 141.2(2) 12 . . . ?
O1 La1 O3 C2 -8.6(2) . . . . ?
O1 La1 O3 C2 82.2(2) 11_655 . . . ?
O1 La1 O3 C2 -97.8(2) 2_655 . . . ?
O1 La1 O3 C2 171.4(2) 10_665 . . . ?
O1 La1 O3 C2 -38.8(2) 3_665 . . . ?
O3 La1 O3 C2 39.7(2) 3_665 . . . ?
O3 La1 O3 C2 -140.3(2) 2_655 . . . ?
Zn1 O2 C1 O1 4.5(5) . . . . ?
Zn1 O2 C1 C2 -175.0(3) . . . . ?
La1 O1 C1 O2 168.5(3) . . . . ?
La1 O1 C1 C2 -12.0(4) . . . . ?
C2 O3 C2 C1 -173.3(4) 10_665 . . . ?
La1 O3 C2 C1 6.7(4) . . . . ?
O2 C1 C2 O3 -177.7(3) . . . . ?
O1 C1 C2 O3 2.8(5) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.024 1058 138 ' '
_platon_squeeze_details          
;
;
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.95
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.105

# Attachment 'La_Co.cif'

data_La_Co
_database_code_depnum_ccdc_archive 'CCDC 289451'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H7.50 Co0.50 La0.33 O6.75'
_chemical_formula_sum            'C4 H7.50 Co0.50 La0.33 O6.75'
_chemical_formula_weight         239.37

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'
Co Co 0.3494 0.9721 '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           Hexagonal
_symmetry_space_group_name_H-M   P6/mcc

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

_cell_length_a                   15.371(3)
_cell_length_b                   15.371(3)
_cell_length_c                   15.127(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3095.4(10)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6203
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.86

_exptl_crystal_description       PRISM
_exptl_crystal_colour            PURPLE
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    2.226
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6171
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating node'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18968
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         27.85
_reflns_number_total             1284
_reflns_number_gt                1068
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0818P)^2^+3.9566P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0012(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1284
_refine_ls_number_parameters     72
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.1263
_refine_ls_wR_factor_gt          0.1181
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.6667 0.3333 0.2500 0.0201(2) Uani 1 6 d S . .
Co1 Co 0.5000 0.0000 0.0000 0.0212(3) Uani 1 4 d S . .
O1 O 0.6102(2) 0.0517(2) 0.09620(19) 0.0529(8) Uani 1 1 d . . .
O2 O 0.6181(2) 0.19291(18) 0.14199(16) 0.0367(5) Uani 1 1 d . . .
O3 O 0.76402(13) 0.23598(13) 0.2500 0.0348(8) Uani 1 2 d S . .
O4 O 0.5090(2) -0.1347(2) 0.0000 0.0308(7) Uani 1 2 d SD . .
H4A H 0.4725 -0.1640 -0.0447 0.046 Uiso 1 1 d RD . .
C1 C 0.6472(3) 0.1297(3) 0.1415(2) 0.0365(7) Uani 1 1 d . . .
C2 C 0.7333(4) 0.1488(3) 0.2000(3) 0.0683(16) Uani 1 1 d . . .
H2A H 0.7133 0.0920 0.2392 0.082 Uiso 1 1 calc R . .
H2B H 0.7889 0.1562 0.1642 0.082 Uiso 1 1 calc R . .
O5 O 0.841(4) 1.0000 0.2500 0.230(17) Uani 0.25 2 d SPU . .
O6 O 0.720(3) 0.920(3) 1.0000 0.144(12) Uani 0.25 2 d SPU A 1
O6' O 0.768(3) 1.003(3) 1.0000 0.113(10) Uani 0.25 2 d SPU B 2

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
La1 0.0213(2) 0.0213(2) 0.0176(3) 0.000 0.000 0.01067(12)
Co1 0.0232(4) 0.0174(4) 0.0192(4) 0.000 0.000 0.0074(3)
O1 0.0658(17) 0.0451(15) 0.0616(17) -0.0333(13) -0.0383(14) 0.0380(14)
O2 0.0443(13) 0.0342(12) 0.0366(12) -0.0151(10) -0.0157(11) 0.0234(11)
O3 0.0325(13) 0.0325(13) 0.0448(19) -0.0202(11) -0.0202(11) 0.0204(15)
O4 0.0363(16) 0.0273(15) 0.0265(14) 0.000 0.000 0.0141(13)
C1 0.0404(17) 0.0321(16) 0.0394(17) -0.0137(14) -0.0153(15) 0.0199(14)
C2 0.078(3) 0.059(3) 0.093(4) -0.054(3) -0.060(3) 0.053(3)
O5 0.217(19) 0.231(17) 0.25(2) 0.008(9) 0.004(5) 0.115(8)
O6 0.134(15) 0.150(15) 0.161(16) 0.000 0.000 0.081(10)
O6' 0.106(13) 0.129(14) 0.131(14) 0.000 0.000 0.080(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
La1 O2 2.505(2) 10_665 ?
La1 O2 2.505(2) . ?
La1 O2 2.505(2) 11_655 ?
La1 O2 2.505(2) 2_655 ?
La1 O2 2.505(2) 3_665 ?
La1 O2 2.505(2) 12 ?
La1 O3 2.592(3) . ?
La1 O3 2.592(3) 3_665 ?
La1 O3 2.592(3) 2_655 ?
Co1 O1 2.067(2) 13_655 ?
Co1 O1 2.067(2) . ?
Co1 O1 2.067(2) 16 ?
Co1 O1 2.067(2) 4_655 ?
Co1 O4 2.142(3) . ?
Co1 O4 2.142(3) 13_655 ?
O1 C1 1.245(4) . ?
O2 C1 1.256(4) . ?
O3 C2 1.399(4) 10_665 ?
O3 C2 1.399(4) . ?
O4 H4A 0.8499 . ?
C1 C2 1.494(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 La1 O2 121.56(11) 10_665 . ?
O2 La1 O2 82.06(9) 10_665 11_655 ?
O2 La1 O2 83.46(13) . 11_655 ?
O2 La1 O2 83.46(13) 10_665 2_655 ?
O2 La1 O2 82.06(9) . 2_655 ?
O2 La1 O2 150.09(12) 11_655 2_655 ?
O2 La1 O2 150.09(12) 10_665 3_665 ?
O2 La1 O2 82.06(9) . 3_665 ?
O2 La1 O2 121.56(11) 11_655 3_665 ?
O2 La1 O2 82.06(9) 2_655 3_665 ?
O2 La1 O2 82.06(9) 10_665 12 ?
O2 La1 O2 150.09(12) . 12 ?
O2 La1 O2 82.06(9) 11_655 12 ?
O2 La1 O2 121.56(11) 2_655 12 ?
O2 La1 O2 83.46(12) 3_665 12 ?
O2 La1 O3 60.78(5) 10_665 . ?
O2 La1 O3 60.78(5) . . ?
O2 La1 O3 75.04(6) 11_655 . ?
O2 La1 O3 75.04(6) 2_655 . ?
O2 La1 O3 138.27(6) 3_665 . ?
O2 La1 O3 138.27(6) 12 . ?
O2 La1 O3 138.27(6) 10_665 3_665 ?
O2 La1 O3 75.04(6) . 3_665 ?
O2 La1 O3 60.78(5) 11_655 3_665 ?
O2 La1 O3 138.27(6) 2_655 3_665 ?
O2 La1 O3 60.78(5) 3_665 3_665 ?
O2 La1 O3 75.04(6) 12 3_665 ?
O3 La1 O3 120.0 . 3_665 ?
O2 La1 O3 75.04(6) 10_665 2_655 ?
O2 La1 O3 138.27(6) . 2_655 ?
O2 La1 O3 138.27(6) 11_655 2_655 ?
O2 La1 O3 60.78(5) 2_655 2_655 ?
O2 La1 O3 75.04(6) 3_665 2_655 ?
O2 La1 O3 60.78(5) 12 2_655 ?
O3 La1 O3 120.0 . 2_655 ?
O3 La1 O3 120.0 3_665 2_655 ?
O1 Co1 O1 180.00(18) 13_655 . ?
O1 Co1 O1 90.47(19) 13_655 16 ?
O1 Co1 O1 89.53(19) . 16 ?
O1 Co1 O1 89.53(19) 13_655 4_655 ?
O1 Co1 O1 90.47(19) . 4_655 ?
O1 Co1 O1 180.00(15) 16 4_655 ?
O1 Co1 O4 93.71(9) 13_655 . ?
O1 Co1 O4 86.29(9) . . ?
O1 Co1 O4 86.29(9) 16 . ?
O1 Co1 O4 93.71(9) 4_655 . ?
O1 Co1 O4 86.29(9) 13_655 13_655 ?
O1 Co1 O4 93.71(9) . 13_655 ?
O1 Co1 O4 93.71(9) 16 13_655 ?
O1 Co1 O4 86.29(9) 4_655 13_655 ?
O4 Co1 O4 180.00(17) . 13_655 ?
C1 O1 Co1 130.6(2) . . ?
C1 O2 La1 127.0(2) . . ?
C2 O3 C2 115.1(4) 10_665 . ?
C2 O3 La1 122.4(2) 10_665 . ?
C2 O3 La1 122.4(2) . . ?
Co1 O4 H4A 99.7 . . ?
O1 C1 O2 125.5(3) . . ?
O1 C1 C2 116.7(3) . . ?
O2 C1 C2 117.9(3) . . ?
O3 C2 C1 110.5(3) . . ?
O3 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O3 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Co1 O1 C1 -12(100) 13_655 . . . ?
O1 Co1 O1 C1 99.9(4) 16 . . . ?
O1 Co1 O1 C1 -80.1(4) 4_655 . . . ?
O4 Co1 O1 C1 -173.8(4) . . . . ?
O4 Co1 O1 C1 6.2(4) 13_655 . . . ?
O2 La1 O2 C1 11.0(3) 10_665 . . . ?
O2 La1 O2 C1 -65.5(3) 11_655 . . . ?
O2 La1 O2 C1 88.2(4) 2_655 . . . ?
O2 La1 O2 C1 171.3(3) 3_665 . . . ?
O2 La1 O2 C1 -126.9(3) 12 . . . ?
O3 La1 O2 C1 11.0(3) . . . . ?
O3 La1 O2 C1 -126.9(3) 3_665 . . . ?
O3 La1 O2 C1 114.5(3) 2_655 . . . ?
O2 La1 O3 C2 -8.5(3) 10_665 . . 10_665 ?
O2 La1 O3 C2 171.5(3) . . . 10_665 ?
O2 La1 O3 C2 -97.7(3) 11_655 . . 10_665 ?
O2 La1 O3 C2 82.3(3) 2_655 . . 10_665 ?
O2 La1 O3 C2 141.4(3) 3_665 . . 10_665 ?
O2 La1 O3 C2 -38.6(3) 12 . . 10_665 ?
O3 La1 O3 C2 -140.1(3) 3_665 . . 10_665 ?
O3 La1 O3 C2 39.9(3) 2_655 . . 10_665 ?
O2 La1 O3 C2 171.5(3) 10_665 . . . ?
O2 La1 O3 C2 -8.5(3) . . . . ?
O2 La1 O3 C2 82.3(3) 11_655 . . . ?
O2 La1 O3 C2 -97.7(3) 2_655 . . . ?
O2 La1 O3 C2 -38.6(3) 3_665 . . . ?
O2 La1 O3 C2 141.4(3) 12 . . . ?
O3 La1 O3 C2 39.9(3) 3_665 . . . ?
O3 La1 O3 C2 -140.1(3) 2_655 . . . ?
Co1 O1 C1 O2 5.6(7) . . . . ?
Co1 O1 C1 C2 -174.5(3) . . . . ?
La1 O2 C1 O1 167.9(3) . . . . ?
La1 O2 C1 C2 -12.1(5) . . . . ?
C2 O3 C2 C1 -173.4(5) 10_665 . . . ?
La1 O3 C2 C1 6.6(5) . . . . ?
O1 C1 C2 O3 -177.1(4) . . . . ?
O2 C1 C2 O3 2.8(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.85
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.129

#=====================================================#

data_La_Mn
_database_code_depnum_ccdc_archive 'CCDC 289452'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 La4 Mn6 O78'
_chemical_formula_weight         2782.34

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'
Mn Mn 0.3368 0.7283 '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           Cubic
_symmetry_space_group_name_H-M   Fd-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+3/4, z+1/2'
'-x+3/4, y+1/2, -z+1/4'
'x+1/2, -y+1/4, -z+3/4'
'z, x, y'
'z+1/2, -x+1/4, -y+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+3/4, x+1/2, -y+1/4'
'y, z, x'
'-y+3/4, z+1/2, -x+1/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'y+3/4, x+1/4, -z'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/4, -x, z+3/4'
'-y, x+3/4, z+1/4'
'x+3/4, z+1/4, -y'
'-x, z+3/4, y+1/4'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/4, -z, y+3/4'
'z+3/4, y+1/4, -x'
'z+1/4, -y, x+3/4'
'-z, y+3/4, x+1/4'
'-z+1/2, -y+1/2, -x+1/2'
'x, y+1/2, z+1/2'
'-x+1/4, -y+5/4, z+1'
'-x+3/4, y+1, -z+3/4'
'x+1/2, -y+3/4, -z+5/4'
'z, x+1/2, y+1/2'
'z+1/2, -x+3/4, -y+5/4'
'-z+1/4, -x+5/4, y+1'
'-z+3/4, x+1, -y+3/4'
'y, z+1/2, x+1/2'
'-y+3/4, z+1, -x+3/4'
'y+1/2, -z+3/4, -x+5/4'
'-y+1/4, -z+5/4, x+1'
'y+3/4, x+3/4, -z+1/2'
'-y+1/2, -x+1, -z+1'
'y+1/4, -x+1/2, z+5/4'
'-y, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+1/2'
'-x, z+5/4, y+3/4'
'-x+1/2, -z+1, -y+1'
'x+1/4, -z+1/2, y+5/4'
'z+3/4, y+3/4, -x+1/2'
'z+1/4, -y+1/2, x+5/4'
'-z, y+5/4, x+3/4'
'-z+1/2, -y+1, -x+1'
'x+1/2, y, z+1/2'
'-x+3/4, -y+3/4, z+1'
'-x+5/4, y+1/2, -z+3/4'
'x+1, -y+1/4, -z+5/4'
'z+1/2, x, y+1/2'
'z+1, -x+1/4, -y+5/4'
'-z+3/4, -x+3/4, y+1'
'-z+5/4, x+1/2, -y+3/4'
'y+1/2, z, x+1/2'
'-y+5/4, z+1/2, -x+3/4'
'y+1, -z+1/4, -x+5/4'
'-y+3/4, -z+3/4, x+1'
'y+5/4, x+1/4, -z+1/2'
'-y+1, -x+1/2, -z+1'
'y+3/4, -x, z+5/4'
'-y+1/2, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+1/2'
'-x+1/2, z+3/4, y+3/4'
'-x+1, -z+1/2, -y+1'
'x+3/4, -z, y+5/4'
'z+5/4, y+1/4, -x+1/2'
'z+3/4, -y, x+5/4'
'-z+1/2, y+3/4, x+3/4'
'-z+1, -y+1/2, -x+1'
'x+1/2, y+1/2, z'
'-x+3/4, -y+5/4, z+1/2'
'-x+5/4, y+1, -z+1/4'
'x+1, -y+3/4, -z+3/4'
'z+1/2, x+1/2, y'
'z+1, -x+3/4, -y+3/4'
'-z+3/4, -x+5/4, y+1/2'
'-z+5/4, x+1, -y+1/4'
'y+1/2, z+1/2, x'
'-y+5/4, z+1, -x+1/4'
'y+1, -z+3/4, -x+3/4'
'-y+3/4, -z+5/4, x+1/2'
'y+5/4, x+3/4, -z'
'-y+1, -x+1, -z+1/2'
'y+3/4, -x+1/2, z+3/4'
'-y+1/2, x+5/4, z+1/4'
'x+5/4, z+3/4, -y'
'-x+1/2, z+5/4, y+1/4'
'-x+1, -z+1, -y+1/2'
'x+3/4, -z+1/2, y+3/4'
'z+5/4, y+3/4, -x'
'z+3/4, -y+1/2, x+3/4'
'-z+1/2, y+5/4, x+1/4'
'-z+1, -y+1, -x+1/2'
'-x, -y, -z'
'x-1/4, y-3/4, -z-1/2'
'x-3/4, -y-1/2, z-1/4'
'-x-1/2, y-1/4, z-3/4'
'-z, -x, -y'
'-z-1/2, x-1/4, y-3/4'
'z-1/4, x-3/4, -y-1/2'
'z-3/4, -x-1/2, y-1/4'
'-y, -z, -x'
'y-3/4, -z-1/2, x-1/4'
'-y-1/2, z-1/4, x-3/4'
'y-1/4, z-3/4, -x-1/2'
'-y-3/4, -x-1/4, z'
'y-1/2, x-1/2, z-1/2'
'-y-1/4, x, -z-3/4'
'y, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y'
'x, -z-3/4, -y-1/4'
'x-1/2, z-1/2, y-1/2'
'-x-1/4, z, -y-3/4'
'-z-3/4, -y-1/4, x'
'-z-1/4, y, -x-3/4'
'z, -y-3/4, -x-1/4'
'z-1/2, y-1/2, x-1/2'
'-x, -y+1/2, -z+1/2'
'x-1/4, y-1/4, -z'
'x-3/4, -y, z+1/4'
'-x-1/2, y+1/4, z-1/4'
'-z, -x+1/2, -y+1/2'
'-z-1/2, x+1/4, y-1/4'
'z-1/4, x-1/4, -y'
'z-3/4, -x, y+1/4'
'-y, -z+1/2, -x+1/2'
'y-3/4, -z, x+1/4'
'-y-1/2, z+1/4, x-1/4'
'y-1/4, z-1/4, -x'
'-y-3/4, -x+1/4, z+1/2'
'y-1/2, x, z'
'-y-1/4, x+1/2, -z-1/4'
'y, -x-1/4, -z+1/4'
'-x-3/4, -z+1/4, y+1/2'
'x, -z-1/4, -y+1/4'
'x-1/2, z, y'
'-x-1/4, z+1/2, -y-1/4'
'-z-3/4, -y+1/4, x+1/2'
'-z-1/4, y+1/2, -x-1/4'
'z, -y-1/4, -x+1/4'
'z-1/2, y, x'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-3/4, -z'
'x-1/4, -y-1/2, z+1/4'
'-x, y-1/4, z-1/4'
'-z+1/2, -x, -y+1/2'
'-z, x-1/4, y-1/4'
'z+1/4, x-3/4, -y'
'z-1/4, -x-1/2, y+1/4'
'-y+1/2, -z, -x+1/2'
'y-1/4, -z-1/2, x+1/4'
'-y, z-1/4, x-1/4'
'y+1/4, z-3/4, -x'
'-y-1/4, -x-1/4, z+1/2'
'y, x-1/2, z'
'-y+1/4, x, -z-1/4'
'y+1/2, -x-3/4, -z+1/4'
'-x-1/4, -z-1/4, y+1/2'
'x+1/2, -z-3/4, -y+1/4'
'x, z-1/2, y'
'-x+1/4, z, -y-1/4'
'-z-1/4, -y-1/4, x+1/2'
'-z+1/4, y, -x-1/4'
'z+1/2, -y-3/4, -x+1/4'
'z, y-1/2, x'
'-x+1/2, -y+1/2, -z'
'x+1/4, y-1/4, -z-1/2'
'x-1/4, -y, z-1/4'
'-x, y+1/4, z-3/4'
'-z+1/2, -x+1/2, -y'
'-z, x+1/4, y-3/4'
'z+1/4, x-1/4, -y-1/2'
'z-1/4, -x, y-1/4'
'-y+1/2, -z+1/2, -x'
'y-1/4, -z, x-1/4'
'-y, z+1/4, x-3/4'
'y+1/4, z-1/4, -x-1/2'
'-y-1/4, -x+1/4, z'
'y, x, z-1/2'
'-y+1/4, x+1/2, -z-3/4'
'y+1/2, -x-1/4, -z-1/4'
'-x-1/4, -z+1/4, y'
'x+1/2, -z-1/4, -y-1/4'
'x, z, y-1/2'
'-x+1/4, z+1/2, -y-3/4'
'-z-1/4, -y+1/4, x'
'-z+1/4, y+1/2, -x-3/4'
'z+1/2, -y-1/4, -x-1/4'
'z, y, x-1/2'

_cell_length_a                   25.9723(6)
_cell_length_b                   25.9723(6)
_cell_length_c                   25.9723(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17519.9(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1782
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      23.15

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10992
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5975
_exptl_absorpt_correction_T_max  0.6894
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating node'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26085
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.93
_reflns_number_total             888
_reflns_number_gt                433
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of 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^)+(0.0882P)^2^+398.4311P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         888
_refine_ls_number_parameters     57
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1881
_refine_ls_wR_factor_gt          0.1279
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.083
_refine_ls_shift/su_mean         0.008

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
La1 La 0.0000 0.0000 0.7500 0.0309(4) Uani 1 6 d S . .
Mn1 Mn 0.0000 0.0000 1.0000 0.0360(7) Uani 1 6 d S . .
Mn2 Mn 0.6250 0.6250 0.1250 0.0793(17) Uani 1 12 d S . .
O1 O -0.0298(2) 0.0086(2) 0.8365(2) 0.0602(16) Uani 1 1 d . . .
O2 O -0.0199(2) 0.0138(2) 0.9203(2) 0.0603(16) Uani 1 1 d . . .
O3 O 0.0662(2) 0.0000 0.8162(2) 0.052(2) Uani 1 2 d S . .
O4 O 0.7077(4) 0.6250 0.1250 0.099(3) Uani 1 2 d SD . .
H4A H 0.7339 0.6141 0.1083 0.119 Uiso 1 1 d RD . .
C1 C -0.0014(3) 0.0088(3) 0.8760(4) 0.051(3) Uani 1 1 d . . .
C2 C 0.0556(3) 0.0032(4) 0.8697(3) 0.071(3) Uani 1 1 d . . .
H2A H 0.0732 0.0326 0.8846 0.085 Uiso 1 1 calc R . .
H2B H 0.0675 -0.0277 0.8870 0.085 Uiso 1 1 calc R . .
O5 O 0.6250 0.3256(10) 0.1250 0.113(8) Uani 0.50 2 d SP . .

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
La1 0.0309(4) 0.0309(4) 0.0309(4) -0.0110(2) -0.0110(2) 0.0110(2)
Mn1 0.0360(7) 0.0360(7) 0.0360(7) 0.0031(5) 0.0031(5) 0.0031(5)
Mn2 0.0793(17) 0.0793(17) 0.0793(17) 0.000 0.000 0.000
O1 0.053(4) 0.078(4) 0.049(4) -0.012(3) -0.009(3) 0.010(3)
O2 0.064(4) 0.065(4) 0.053(4) -0.005(3) -0.002(3) 0.009(3)
O3 0.042(3) 0.071(6) 0.042(3) -0.012(3) -0.008(3) 0.012(3)
O4 0.069(6) 0.145(10) 0.083(7) -0.015(6) 0.000 0.000
C1 0.061(6) 0.043(5) 0.049(6) -0.010(3) -0.011(4) 0.010(4)
C2 0.060(6) 0.096(8) 0.056(6) -0.012(5) -0.010(4) 0.017(5)
O5 0.15(2) 0.12(2) 0.066(13) 0.000 0.024(14) 0.000

_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
La1 O1 2.388(6) 32_545 ?
La1 O1 2.388(6) 86_446 ?
La1 O1 2.388(6) 42_535 ?
La1 O1 2.388(6) . ?
La1 O1 2.388(6) 83_455 ?
La1 O1 2.388(6) 22_455 ?
La1 O3 2.432(7) 32_545 ?
La1 O3 2.432(7) . ?
La1 O3 2.432(7) 83_455 ?
Mn1 O2 2.163(7) 5_456 ?
Mn1 O2 2.163(7) 105_566 ?
Mn1 O2 2.163(7) . ?
Mn1 O2 2.163(7) 9_546 ?
Mn1 O2 2.163(7) 101_656 ?
Mn1 O2 2.163(7) 97_557 ?
Mn2 O4 2.147(10) 58 ?
Mn2 O4 2.147(10) . ?
Mn2 O4 2.147(10) 26_654 ?
Mn2 O4 2.147(10) 53_554 ?
Mn2 O4 2.147(10) 6_565 ?
Mn2 O4 2.147(10) 33_554 ?
O1 C1 1.262(9) . ?
O2 C1 1.253(10) . ?
O3 C2 1.419(9) . ?
O3 C2 1.419(10) 22_455 ?
O4 H4A 0.8547 . ?
C1 C2 1.498(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O1 86.0(3) 32_545 86_446 ?
O1 La1 O1 128.3(3) 32_545 42_535 ?
O1 La1 O1 79.2(2) 86_446 42_535 ?
O1 La1 O1 79.2(2) 32_545 . ?
O1 La1 O1 145.7(3) 86_446 . ?
O1 La1 O1 86.0(3) 42_535 . ?
O1 La1 O1 79.2(2) 32_545 83_455 ?
O1 La1 O1 128.3(3) 86_446 83_455 ?
O1 La1 O1 145.7(3) 42_535 83_455 ?
O1 La1 O1 79.2(2) . 83_455 ?
O1 La1 O1 145.7(3) 32_545 22_455 ?
O1 La1 O1 79.2(2) 86_446 22_455 ?
O1 La1 O1 79.2(2) 42_535 22_455 ?
O1 La1 O1 128.3(3) . 22_455 ?
O1 La1 O1 86.0(3) 83_455 22_455 ?
O1 La1 O3 64.13(14) 32_545 32_545 ?
O1 La1 O3 72.84(14) 86_446 32_545 ?
O1 La1 O3 64.13(14) 42_535 32_545 ?
O1 La1 O3 72.84(14) . 32_545 ?
O1 La1 O3 137.01(14) 83_455 32_545 ?
O1 La1 O3 137.01(14) 22_455 32_545 ?
O1 La1 O3 137.01(14) 32_545 . ?
O1 La1 O3 137.01(14) 86_446 . ?
O1 La1 O3 72.84(14) 42_535 . ?
O1 La1 O3 64.13(14) . . ?
O1 La1 O3 72.84(14) 83_455 . ?
O1 La1 O3 64.13(14) 22_455 . ?
O3 La1 O3 120.0 32_545 . ?
O1 La1 O3 72.84(14) 32_545 83_455 ?
O1 La1 O3 64.13(14) 86_446 83_455 ?
O1 La1 O3 137.01(14) 42_535 83_455 ?
O1 La1 O3 137.01(14) . 83_455 ?
O1 La1 O3 64.13(14) 83_455 83_455 ?
O1 La1 O3 72.84(14) 22_455 83_455 ?
O3 La1 O3 120.0 32_545 83_455 ?
O3 La1 O3 120.0 . 83_455 ?
O2 Mn1 O2 91.7(2) 5_456 105_566 ?
O2 Mn1 O2 88.3(2) 5_456 . ?
O2 Mn1 O2 91.7(2) 105_566 . ?
O2 Mn1 O2 88.3(2) 5_456 9_546 ?
O2 Mn1 O2 180.000(1) 105_566 9_546 ?
O2 Mn1 O2 88.3(2) . 9_546 ?
O2 Mn1 O2 180.000(1) 5_456 101_656 ?
O2 Mn1 O2 88.3(2) 105_566 101_656 ?
O2 Mn1 O2 91.7(2) . 101_656 ?
O2 Mn1 O2 91.7(2) 9_546 101_656 ?
O2 Mn1 O2 91.7(2) 5_456 97_557 ?
O2 Mn1 O2 88.3(2) 105_566 97_557 ?
O2 Mn1 O2 180.000(1) . 97_557 ?
O2 Mn1 O2 91.7(2) 9_546 97_557 ?
O2 Mn1 O2 88.3(2) 101_656 97_557 ?
O4 Mn2 O4 90.000(1) 58 . ?
O4 Mn2 O4 90.000(2) 58 26_654 ?
O4 Mn2 O4 180.0 . 26_654 ?
O4 Mn2 O4 90.0 58 53_554 ?
O4 Mn2 O4 90.000(1) . 53_554 ?
O4 Mn2 O4 90.000(1) 26_654 53_554 ?
O4 Mn2 O4 90.0 58 6_565 ?
O4 Mn2 O4 90.000(1) . 6_565 ?
O4 Mn2 O4 90.000(1) 26_654 6_565 ?
O4 Mn2 O4 180.000(1) 53_554 6_565 ?
O4 Mn2 O4 180.000(1) 58 33_554 ?
O4 Mn2 O4 90.000(1) . 33_554 ?
O4 Mn2 O4 90.000(1) 26_654 33_554 ?
O4 Mn2 O4 90.000(1) 53_554 33_554 ?
O4 Mn2 O4 90.000(1) 6_565 33_554 ?
C1 O1 La1 125.1(6) . . ?
C1 O2 Mn1 140.4(6) . . ?
C2 O3 C2 112.6(9) . 22_455 ?
C2 O3 La1 123.7(4) . . ?
C2 O3 La1 123.7(4) 22_455 . ?
Mn2 O4 H4A 142.7 . . ?
O2 C1 O1 121.6(8) . . ?
O2 C1 C2 119.2(7) . . ?
O1 C1 C2 119.3(8) . . ?
O3 C2 C1 107.7(7) . . ?
O3 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O3 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 La1 O1 C1 156.1(7) 32_545 . . . ?
O1 La1 O1 C1 -137.9(7) 86_446 . . . ?
O1 La1 O1 C1 -73.7(6) 42_535 . . . ?
O1 La1 O1 C1 75.1(7) 83_455 . . . ?
O1 La1 O1 C1 -0.9(6) 22_455 . . . ?
O3 La1 O1 C1 -137.9(7) 32_545 . . . ?
O3 La1 O1 C1 -0.9(6) . . . . ?
O3 La1 O1 C1 106.3(6) 83_455 . . . ?
O2 Mn1 O2 C1 -144.1(8) 5_456 . . . ?
O2 Mn1 O2 C1 124.2(9) 105_566 . . . ?
O2 Mn1 O2 C1 -55.8(9) 9_546 . . . ?
O2 Mn1 O2 C1 35.9(8) 101_656 . . . ?
O2 Mn1 O2 C1 16(100) 97_557 . . . ?
O1 La1 O3 C2 -32.4(5) 32_545 . . . ?
O1 La1 O3 C2 147.6(5) 86_446 . . . ?
O1 La1 O3 C2 95.9(5) 42_535 . . . ?
O1 La1 O3 C2 2.0(5) . . . . ?
O1 La1 O3 C2 -84.1(5) 83_455 . . . ?
O1 La1 O3 C2 -178.0(5) 22_455 . . . ?
O3 La1 O3 C2 50.8(5) 32_545 . . . ?
O3 La1 O3 C2 -129.2(5) 83_455 . . . ?
O1 La1 O3 C2 147.6(5) 32_545 . . 22_455 ?
O1 La1 O3 C2 -32.4(5) 86_446 . . 22_455 ?
O1 La1 O3 C2 -84.1(5) 42_535 . . 22_455 ?
O1 La1 O3 C2 -178.0(5) . . . 22_455 ?
O1 La1 O3 C2 95.9(5) 83_455 . . 22_455 ?
O1 La1 O3 C2 2.0(5) 22_455 . . 22_455 ?
O3 La1 O3 C2 -129.2(5) 32_545 . . 22_455 ?
O3 La1 O3 C2 50.8(5) 83_455 . . 22_455 ?
Mn1 O2 C1 O1 160.6(6) . . . . ?
Mn1 O2 C1 C2 -19.7(13) . . . . ?
La1 O1 C1 O2 179.5(5) . . . . ?
La1 O1 C1 C2 -0.2(12) . . . . ?
C2 O3 C2 C1 177.4(9) 22_455 . . . ?
La1 O3 C2 C1 -2.6(9) . . . . ?
O2 C1 C2 O3 -178.0(7) . . . . ?
O1 C1 C2 O3 1.7(12) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.93
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.268
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.149