# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'ProfD La-Sheng Long'
_publ_contact_author_email       LSLONG@XMU.EDU.CN

_publ_section_title              
;
Lanthanide-based Metal-organic Framework with Dynamic
Porous property
;
loop_
_publ_author_name
'La-Sheng Long.'
'Rong-Bin Huang.'
'Jun Zhao.'
'Lan-Sun Zheng.'

# Attachment 'complex_1.cif'

data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 685597'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H22 La2 N4 O20'
_chemical_formula_weight         808.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   8.521(2)
_cell_length_b                   18.477(4)
_cell_length_c                   15.380(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2421.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    3337
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.21

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    3.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4339
_exptl_absorpt_correction_T_max  0.5202
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(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 Smart Apex 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            12529
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2460
_reflns_number_gt                2254
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 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^)+(0.0273P)^2^+32.4183P] 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    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2460
_refine_ls_number_parameters     173
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1204
_refine_ls_wR_factor_gt          0.1173
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.290
_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
La1 La 0.34396(5) 0.61676(2) 0.28446(3) 0.01251(16) Uani 1 1 d . . .
O1 O 1.1103(7) 0.5099(4) 0.6754(4) 0.0283(15) Uani 1 1 d U . .
O2 O 0.9110(7) 0.4542(3) 0.7341(4) 0.0179(13) Uani 1 1 d . . .
C1 C 0.9691(9) 0.4965(5) 0.6781(5) 0.0166(17) Uani 1 1 d . . .
C2 C 0.8591(9) 0.5281(4) 0.6150(5) 0.0159(17) Uani 1 1 d . . .
C3 C 0.8833(9) 0.5690(4) 0.5403(5) 0.0163(17) Uani 1 1 d . . .
H3A H 0.9796 0.5863 0.5190 0.020 Uiso 1 1 calc R . .
C4 C 0.7373(9) 0.5789(4) 0.5040(5) 0.0160(17) Uani 1 1 d . . .
C5 C 0.6859(9) 0.6122(5) 0.4214(5) 0.0172(17) Uani 1 1 d . . .
N1 N 0.6342(8) 0.5451(4) 0.5577(5) 0.0189(16) Uani 1 1 d . . .
H1A H 0.5333 0.5442 0.5490 0.023 Uiso 1 1 calc R . .
N2 N 0.7043(8) 0.5136(4) 0.6250(4) 0.0171(15) Uani 1 1 d . . .
O3 O 0.5428(7) 0.6091(3) 0.4059(4) 0.0240(14) Uani 1 1 d . . .
O4 O 0.7900(7) 0.6387(3) 0.3747(4) 0.0212(13) Uani 1 1 d . . .
C6 C 0.5303(13) 0.7500 0.2491(8) 0.014(2) Uani 1 2 d S . .
O5 O 0.5867(6) 0.6892(3) 0.2265(4) 0.0162(12) Uani 1 1 d . . .
O6 O 0.4036(9) 0.7500 0.2943(6) 0.0209(19) Uani 1 2 d S . .
O1W O 0.2200(8) 0.6445(4) 0.4312(4) 0.0341(17) Uani 1 1 d . . .
H1WA H 0.1886 0.6880 0.4347 0.051 Uiso 1 1 d R . .
H1WB H 0.2808 0.6348 0.4735 0.051 Uiso 1 1 d R . .
O2W O 0.0294(15) 0.2500 0.5357(7) 0.049(3) Uani 1 2 d S . .
H2WA H 0.1006 0.2500 0.5744 0.073 Uiso 1 2 d SR . .
H2WB H 0.0633 0.2500 0.4837 0.073 Uiso 1 2 d SR . .
O3W O 0.3212(8) 0.5927(4) 0.5885(5) 0.0418(19) Uani 1 1 d . . .
H3WA H 0.3245 0.6254 0.6272 0.063 Uiso 1 1 d R . .
H3WB H 0.2596 0.5594 0.6055 0.063 Uiso 1 1 d R . .
O4W O 0.535(3) 0.6571(15) 0.7218(15) 0.250(12) Uiso 1 1 d . . .
H4WA H 0.5819 0.6184 0.7368 0.376 Uiso 1 1 d R . .
H4WB H 0.5983 0.6848 0.6950 0.376 Uiso 1 1 d R . .
O5W O 0.494(3) 0.7500 0.5128(18) 0.179(11) Uiso 1 2 d S . .
H5WA H 0.5085 0.7873 0.4815 0.269 Uiso 0.50 1 d PR . .
H5WB H 0.5085 0.7127 0.4815 0.269 Uiso 0.50 1 d PR . .
O6W O 0.222(7) 0.2500 0.368(3) 0.135(15) Uani 0.50 2 d SPU . .
O6W' O 0.026(7) 0.2500 0.356(2) 0.140(16) Uani 0.50 2 d SPU . .

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 0.0077(2) 0.0140(2) 0.0159(3) 0.00173(19) 0.00012(18) -0.00019(17)
O1 0.013(3) 0.041(3) 0.031(3) 0.010(3) -0.003(2) -0.004(2)
O2 0.016(3) 0.017(3) 0.021(3) 0.009(2) -0.003(2) 0.002(2)
C1 0.014(4) 0.022(4) 0.013(4) -0.005(4) 0.000(3) 0.002(4)
C2 0.011(4) 0.019(4) 0.017(4) 0.002(3) -0.001(3) 0.001(3)
C3 0.006(4) 0.022(4) 0.021(4) 0.001(3) -0.001(3) -0.005(3)
C4 0.015(4) 0.017(4) 0.016(4) 0.001(3) -0.002(3) 0.000(3)
C5 0.011(4) 0.026(4) 0.015(4) -0.004(4) -0.001(3) -0.002(3)
N1 0.007(3) 0.026(4) 0.024(4) 0.007(3) -0.001(3) -0.002(3)
N2 0.016(4) 0.022(4) 0.013(4) 0.005(3) -0.002(3) -0.004(3)
O3 0.015(3) 0.034(4) 0.023(3) 0.005(3) -0.003(3) -0.001(3)
O4 0.016(3) 0.024(3) 0.024(3) 0.002(3) 0.005(2) 0.002(2)
C6 0.005(5) 0.012(5) 0.026(6) 0.000 -0.005(5) 0.000
O5 0.015(3) 0.015(3) 0.019(3) -0.005(2) 0.001(2) 0.001(2)
O6 0.011(4) 0.015(4) 0.037(5) 0.000 0.011(4) 0.000
O1W 0.028(4) 0.046(4) 0.028(4) 0.005(3) 0.004(3) 0.019(3)
O2W 0.074(9) 0.039(6) 0.033(6) 0.000 0.011(6) 0.000
O3W 0.025(4) 0.056(5) 0.045(5) 0.012(4) 0.008(3) -0.006(3)
O6W 0.22(4) 0.08(2) 0.10(3) 0.000 0.03(3) 0.000
O6W' 0.25(4) 0.11(3) 0.055(19) 0.000 -0.02(3) 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 O6 2.5184(19) . ?
La1 O4 2.524(6) 6_556 ?
La1 O3 2.526(6) . ?
La1 O1W 2.544(6) . ?
La1 O2 2.554(6) 5_666 ?
La1 O5 2.575(5) 6_556 ?
La1 O2 2.585(5) 2_664 ?
La1 O5 2.620(6) . ?
La1 N2 2.812(7) 5_666 ?
La1 O1 2.906(7) 2_664 ?
La1 C6 2.980(7) . ?
La1 C1 3.097(8) 2_664 ?
O1 C1 1.229(10) . ?
O1 La1 2.906(7) 2_665 ?
O2 C1 1.264(10) . ?
O2 La1 2.554(6) 5_666 ?
O2 La1 2.585(5) 2_665 ?
C1 C2 1.470(11) . ?
C1 La1 3.097(8) 2_665 ?
C2 N2 1.355(10) . ?
C2 C3 1.391(11) . ?
C3 C4 1.376(11) . ?
C3 H3A 0.9400 . ?
C4 N1 1.357(10) . ?
C4 C5 1.478(11) . ?
C5 O4 1.242(10) . ?
C5 O3 1.244(10) . ?
N1 N2 1.330(9) . ?
N1 H1A 0.8700 . ?
N2 La1 2.812(7) 5_666 ?
O4 La1 2.524(6) 6_656 ?
C6 O5 1.270(8) . ?
C6 O5 1.270(8) 7_575 ?
C6 O6 1.284(14) . ?
C6 La1 2.980(6) 7_575 ?
O5 La1 2.575(5) 6_656 ?
O6 La1 2.5184(19) 7_575 ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8501 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8499 . ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8500 . ?
O5W H5WA 0.8499 . ?
O5W H5WB 0.8499 . ?
O6W O6W' 1.68(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 La1 O4 86.4(2) . 6_556 ?
O6 La1 O3 82.8(2) . . ?
O4 La1 O3 148.07(19) 6_556 . ?
O6 La1 O1W 80.4(3) . . ?
O4 La1 O1W 138.8(2) 6_556 . ?
O3 La1 O1W 68.5(2) . . ?
O6 La1 O2 132.9(2) . 5_666 ?
O4 La1 O2 79.58(18) 6_556 5_666 ?
O3 La1 O2 128.63(18) . 5_666 ?
O1W La1 O2 81.3(2) . 5_666 ?
O6 La1 O5 70.6(2) . 6_556 ?
O4 La1 O5 72.40(18) 6_556 6_556 ?
O3 La1 O5 130.46(19) . 6_556 ?
O1W La1 O5 66.42(19) . 6_556 ?
O2 La1 O5 62.32(17) 5_666 6_556 ?
O6 La1 O2 110.5(2) . 2_664 ?
O4 La1 O2 86.45(18) 6_556 2_664 ?
O3 La1 O2 69.59(19) . 2_664 ?
O1W La1 O2 134.7(2) . 2_664 ?
O2 La1 O2 113.14(19) 5_666 2_664 ?
O5 La1 O2 158.79(18) 6_556 2_664 ?
O6 La1 O5 50.3(2) . . ?
O4 La1 O5 74.44(18) 6_556 . ?
O3 La1 O5 75.57(18) . . ?
O1W La1 O5 121.8(2) . . ?
O2 La1 O5 153.65(18) 5_666 . ?
O5 La1 O5 112.58(18) 6_556 . ?
O2 La1 O5 61.30(17) 2_664 . ?
O6 La1 N2 146.8(2) . 5_666 ?
O4 La1 N2 126.2(2) 6_556 5_666 ?
O3 La1 N2 71.6(2) . 5_666 ?
O1W La1 N2 70.9(2) . 5_666 ?
O2 La1 N2 59.40(18) 5_666 5_666 ?
O5 La1 N2 110.70(19) 6_556 5_666 ?
O2 La1 N2 80.31(19) 2_664 5_666 ?
O5 La1 N2 136.18(18) . 5_666 ?
O6 La1 O1 142.6(2) . 2_664 ?
O4 La1 O1 66.04(19) 6_556 2_664 ?
O3 La1 O1 106.96(19) . 2_664 ?
O1W La1 O1 136.9(2) . 2_664 ?
O2 La1 O1 68.64(17) 5_666 2_664 ?
O5 La1 O1 119.69(18) 6_556 2_664 ?
O2 La1 O1 46.36(17) 2_664 2_664 ?
O5 La1 O1 96.29(17) . 2_664 ?
N2 La1 O1 67.4(2) 5_666 2_664 ?
O6 La1 C6 25.3(3) . . ?
O4 La1 C6 77.7(3) 6_556 . ?
O3 La1 C6 79.9(3) . . ?
O1W La1 C6 102.5(3) . . ?
O2 La1 C6 149.0(2) 5_666 . ?
O5 La1 C6 90.7(2) 6_556 . ?
O2 La1 C6 86.2(2) 2_664 . ?
O5 La1 C6 25.2(2) . . ?
N2 La1 C6 151.2(3) 5_666 . ?
O1 La1 C6 119.3(3) 2_664 . ?
O6 La1 C1 126.0(2) . 2_664 ?
O4 La1 C1 71.9(2) 6_556 2_664 ?
O3 La1 C1 90.4(2) . 2_664 ?
O1W La1 C1 144.9(2) . 2_664 ?
O2 La1 C1 91.8(2) 5_666 2_664 ?
O5 La1 C1 139.00(19) 6_556 2_664 ?
O2 La1 C1 23.55(19) 2_664 2_664 ?
O5 La1 C1 76.10(19) . 2_664 ?
N2 La1 C1 76.0(2) 5_666 2_664 ?
O1 La1 C1 23.35(19) 2_664 2_664 ?
C6 La1 C1 100.8(3) . 2_664 ?
C1 O1 La1 87.1(5) . 2_665 ?
C1 O2 La1 125.1(5) . 5_666 ?
C1 O2 La1 101.6(5) . 2_665 ?
La1 O2 La1 117.4(2) 5_666 2_665 ?
O1 C1 O2 122.1(8) . . ?
O1 C1 C2 121.5(8) . . ?
O2 C1 C2 116.4(7) . . ?
O1 C1 La1 69.6(5) . 2_665 ?
O2 C1 La1 54.8(4) . 2_665 ?
C2 C1 La1 160.8(6) . 2_665 ?
N2 C2 C3 110.2(7) . . ?
N2 C2 C1 117.9(7) . . ?
C3 C2 C1 131.8(7) . . ?
C4 C3 C2 105.9(7) . . ?
C4 C3 H3A 127.1 . . ?
C2 C3 H3A 127.1 . . ?
N1 C4 C3 106.1(7) . . ?
N1 C4 C5 121.5(7) . . ?
C3 C4 C5 132.2(8) . . ?
O4 C5 O3 127.4(8) . . ?
O4 C5 C4 116.7(7) . . ?
O3 C5 C4 115.9(7) . . ?
N2 N1 C4 112.6(7) . . ?
N2 N1 H1A 123.7 . . ?
C4 N1 H1A 123.7 . . ?
N1 N2 C2 105.2(7) . . ?
N1 N2 La1 134.0(5) . 5_666 ?
C2 N2 La1 111.6(5) . 5_666 ?
C5 O3 La1 142.8(6) . . ?
C5 O4 La1 128.9(5) . 6_656 ?
O5 C6 O5 124.4(11) . 7_575 ?
O5 C6 O6 117.8(5) . . ?
O5 C6 O6 117.8(5) 7_575 . ?
O5 C6 La1 61.4(4) . . ?
O5 C6 La1 169.2(7) 7_575 . ?
O6 C6 La1 56.8(2) . . ?
O5 C6 La1 169.2(7) . 7_575 ?
O5 C6 La1 61.4(4) 7_575 7_575 ?
O6 C6 La1 56.8(2) . 7_575 ?
La1 C6 La1 111.4(4) . 7_575 ?
C6 O5 La1 143.1(6) . 6_656 ?
C6 O5 La1 93.5(5) . . ?
La1 O5 La1 115.4(2) 6_656 . ?
C6 O6 La1 97.9(2) . . ?
C6 O6 La1 97.9(2) . 7_575 ?
La1 O6 La1 155.7(4) . 7_575 ?
La1 O1W H1WA 112.1 . . ?
La1 O1W H1WB 112.5 . . ?
H1WA O1W H1WB 110.0 . . ?
H2WA O2W H2WB 114.7 . . ?
H3WA O3W H3WB 108.7 . . ?
H4WA O4W H4WB 109.9 . . ?
H5WA O5W H5WB 108.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O3W 0.87 2.11 2.847(10) 142.6 .
O1W H1WA O2W 0.85 2.23 2.929(11) 139.6 5_566
O1W H1WB O3W 0.85 1.96 2.740(10) 151.5 .
O2W H2WA O4 0.85 2.39 2.915(11) 120.5 5_666
O2W H2WA O4 0.85 2.39 2.915(11) 120.5 3_646
O2W H2WB O6W' 0.85 2.00 2.77(4) 151.1 .
O2W H2WB O6W 0.85 2.24 3.06(5) 162.7 .
O3W H3WA O4W 0.85 2.38 2.99(3) 128.9 .
O3W H3WB O1 0.85 1.90 2.712(9) 159.3 1_455
O4W H4WA O1 0.85 2.43 3.21(3) 153.1 6_557
O4W H4WB O6W 0.85 2.18 3.02(5) 174.6 5_666
O5W H5WA O3 0.85 2.26 3.107(16) 176.3 7_575
O5W H5WB O3 0.85 2.26 3.107(16) 176.3 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.356
_refine_diff_density_min         -2.208
_refine_diff_density_rms         0.200