# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1042007'
_audit_update_record             
;
2015-05-15 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H9 Gd O8'
_chemical_formula_weight         342.36

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           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.950(2)
_cell_length_b                   6.8081(14)
_cell_length_c                   11.381(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.76(3)
_cell_angle_gamma                90.00
_cell_volume                     844.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7741
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.6

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    7.871
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2538
_exptl_absorpt_correction_T_max  0.3020
_exptl_absorpt_process_details   CrystalClear


_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  SCX-MINI
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6792
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1462
_reflns_number_gt                1340
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0589P)²+3.7681P] where P=(Fo²+2Fc²)/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_number_reflns         1462
_refine_ls_number_parameters     118
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1296
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.173
_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
Gd1 Gd 0.84623(5) -0.02404(7) 0.90716(4) 0.0141(3) Uani 1 1 d . . .
O1W O 0.6515(8) -0.0518(12) 0.7843(7) 0.0253(19) Uani 1 1 d . . .
H1WA H 0.6586 -0.1618 0.7502 0.038 Uiso 1 1 d R . .
H1WB H 0.5774 -0.0326 0.7978 0.038 Uiso 1 1 d R . .
C1 C 0.8092(13) 0.4595(15) 0.8814(10) 0.021(3) Uani 1 1 d . . .
O4 O 0.7164(7) -0.1440(11) 1.0538(6) 0.0234(18) Uani 1 1 d U . .
O3 O 0.6984(8) 0.2176(10) 0.9803(6) 0.0224(19) Uani 1 1 d . . .
O2 O 0.8424(9) 0.6329(12) 0.8684(8) 0.039(2) Uani 1 1 d . . .
O5 O 0.5726(8) -0.1111(13) 1.1785(7) 0.030(2) Uani 1 1 d . . .
O2W O 0.8893(9) -0.0585(15) 0.6948(7) 0.037(2) Uani 1 1 d . . .
H2WA H 0.9654 -0.0840 0.6914 0.056 Uiso 1 1 d R . .
H2WB H 0.8491 -0.1539 0.6614 0.056 Uiso 1 1 d R . .
C4 C 0.6410(11) -0.0424(18) 1.1055(11) 0.023(3) Uani 1 1 d . . .
O6 O 1.0515(9) -0.0681(17) 0.9167(8) 0.050(3) Uani 1 1 d . . .
C3 C 0.6258(11) 0.1702(17) 1.0745(9) 0.021(3) Uani 1 1 d . . .
H3A H 0.5401 0.1980 1.0503 0.026 Uiso 1 1 calc R . .
H3B H 0.6515 0.2503 1.1430 0.026 Uiso 1 1 calc R . .
C2 C 0.7015(12) 0.4256(16) 0.9518(10) 0.023(3) Uani 1 1 d . . .
H2A H 0.7106 0.5031 1.0237 0.028 Uiso 1 1 calc R . .
H2B H 0.6258 0.4640 0.9060 0.028 Uiso 1 1 calc R . .
O1 O 0.8645(8) 0.3121(11) 0.8430(7) 0.029(2) Uani 1 1 d . . .
H6 H 1.0745 -0.1361 0.8612 0.044 Uiso 1 1 d 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
Gd1 0.0150(5) 0.0075(3) 0.0199(4) -0.00130(19) 0.0028(3) -0.00006(19)
O1W 0.021(6) 0.020(4) 0.035(5) -0.006(4) 0.001(4) 0.001(3)
C1 0.034(9) 0.006(6) 0.024(6) 0.002(4) -0.001(5) -0.003(5)
O4 0.026(4) 0.016(3) 0.030(3) 0.006(3) 0.010(3) 0.009(3)
O3 0.028(5) 0.007(4) 0.035(4) 0.001(3) 0.017(4) 0.000(3)
O2 0.050(7) 0.013(5) 0.058(6) -0.001(4) 0.029(5) -0.005(4)
O5 0.024(6) 0.036(5) 0.032(4) 0.011(4) 0.012(4) 0.013(4)
O2W 0.035(7) 0.057(6) 0.020(4) 0.001(4) 0.009(4) 0.001(5)
C4 0.013(8) 0.021(7) 0.035(7) -0.001(5) 0.000(6) -0.004(5)
O6 0.036(7) 0.080(8) 0.032(5) -0.032(5) 0.001(4) 0.008(6)
C3 0.023(8) 0.017(6) 0.025(6) -0.003(5) 0.005(5) -0.004(5)
C2 0.036(8) 0.010(5) 0.026(6) 0.006(5) 0.009(5) 0.004(5)
O1 0.038(6) 0.011(4) 0.041(5) -0.007(4) 0.020(4) 0.001(4)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O6 2.260(10) . ?
Gd1 O6 2.284(9) 3_757 ?
Gd1 O2 2.377(9) 1_545 ?
Gd1 O1 2.416(8) . ?
Gd1 O1W 2.437(9) . ?
Gd1 O4 2.439(7) . ?
Gd1 O3 2.508(7) . ?
Gd1 O2W 2.520(8) . ?
Gd1 Gd1 3.8061(16) 3_757 ?
O1W H1WA 0.8509 . ?
O1W H1WB 0.8515 . ?
C1 O2 1.248(14) . ?
C1 O1 1.272(13) . ?
C1 C2 1.508(16) . ?
O4 C4 1.267(14) . ?
O3 C3 1.434(12) . ?
O3 C2 1.453(12) . ?
O2 Gd1 2.377(9) 1_565 ?
O5 C4 1.263(14) . ?
O2W H2WA 0.8560 . ?
O2W H2WB 0.8524 . ?
C4 C3 1.495(16) . ?
O6 Gd1 2.284(9) 3_757 ?
O6 H6 0.8414 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
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
O6 Gd1 O6 66.2(3) . 3_757 ?
O6 Gd1 O2 83.0(4) . 1_545 ?
O6 Gd1 O2 115.5(4) 3_757 1_545 ?
O6 Gd1 O1 91.6(4) . . ?
O6 Gd1 O1 87.5(4) 3_757 . ?
O2 Gd1 O1 151.1(3) 1_545 . ?
O6 Gd1 O1W 145.7(3) . . ?
O6 Gd1 O1W 148.1(3) 3_757 . ?
O2 Gd1 O1W 79.6(3) 1_545 . ?
O1 Gd1 O1W 89.7(3) . . ?
O6 Gd1 O4 124.6(3) . . ?
O6 Gd1 O4 76.1(3) 3_757 . ?
O2 Gd1 O4 78.3(3) 1_545 . ?
O1 Gd1 O4 126.6(2) . . ?
O1W Gd1 O4 80.2(3) . . ?
O6 Gd1 O3 138.0(3) . . ?
O6 Gd1 O3 78.7(3) 3_757 . ?
O2 Gd1 O3 134.9(3) 1_545 . ?
O1 Gd1 O3 63.6(2) . . ?
O1W Gd1 O3 71.6(3) . . ?
O4 Gd1 O3 63.4(2) . . ?
O6 Gd1 O2W 75.7(3) . . ?
O6 Gd1 O2W 138.2(3) 3_757 . ?
O2 Gd1 O2W 74.4(3) 1_545 . ?
O1 Gd1 O2W 76.7(3) . . ?
O1W Gd1 O2W 71.3(3) . . ?
O4 Gd1 O2W 143.4(3) . . ?
O3 Gd1 O2W 124.6(3) . . ?
O6 Gd1 Gd1 33.3(2) . 3_757 ?
O6 Gd1 Gd1 32.9(2) 3_757 3_757 ?
O2 Gd1 Gd1 100.7(3) 1_545 3_757 ?
O1 Gd1 Gd1 89.5(2) . 3_757 ?
O1W Gd1 Gd1 178.66(19) . 3_757 ?
O4 Gd1 Gd1 101.11(19) . 3_757 ?
O3 Gd1 Gd1 108.90(19) . 3_757 ?
O2W Gd1 Gd1 107.5(2) . 3_757 ?
Gd1 O1W H1WA 102.5 . . ?
Gd1 O1W H1WB 132.9 . . ?
H1WA O1W H1WB 110.4 . . ?
O2 C1 O1 123.4(12) . . ?
O2 C1 C2 117.4(10) . . ?
O1 C1 C2 119.1(9) . . ?
C4 O4 Gd1 125.9(7) . . ?
C3 O3 C2 114.4(8) . . ?
C3 O3 Gd1 121.7(6) . . ?
C2 O3 Gd1 122.3(6) . . ?
C1 O2 Gd1 155.1(8) . 1_565 ?
Gd1 O2W H2WA 109.8 . . ?
Gd1 O2W H2WB 111.2 . . ?
H2WA O2W H2WB 106.6 . . ?
O5 C4 O4 124.1(11) . . ?
O5 C4 C3 117.1(10) . . ?
O4 C4 C3 118.7(10) . . ?
Gd1 O6 Gd1 113.8(3) . 3_757 ?
Gd1 O6 H6 114.1 . . ?
Gd1 O6 H6 130.7 3_757 . ?
O3 C3 C4 109.8(9) . . ?
O3 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O3 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O3 C2 C1 107.7(9) . . ?
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 . . ?
C1 O1 Gd1 125.9(7) . . ?

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
O6 Gd1 O4 C4 127.9(9) . . . . ?
O6 Gd1 O4 C4 80.4(10) 3_757 . . . ?
O2 Gd1 O4 C4 -159.3(10) 1_545 . . . ?
O1 Gd1 O4 C4 4.2(11) . . . . ?
O1W Gd1 O4 C4 -78.0(9) . . . . ?
O3 Gd1 O4 C4 -3.8(9) . . . . ?
O2W Gd1 O4 C4 -116.9(10) . . . . ?
Gd1 Gd1 O4 C4 101.9(9) 3_757 . . . ?
O6 Gd1 O3 C3 -107.1(9) . . . . ?
O6 Gd1 O3 C3 -73.9(8) 3_757 . . . ?
O2 Gd1 O3 C3 41.1(10) 1_545 . . . ?
O1 Gd1 O3 C3 -166.7(9) . . . . ?
O1W Gd1 O3 C3 94.1(8) . . . . ?
O4 Gd1 O3 C3 6.1(8) . . . . ?
O2W Gd1 O3 C3 144.3(8) . . . . ?
Gd1 Gd1 O3 C3 -87.2(8) 3_757 . . . ?
O6 Gd1 O3 C2 57.6(10) . . . . ?
O6 Gd1 O3 C2 90.9(9) 3_757 . . . ?
O2 Gd1 O3 C2 -154.2(8) 1_545 . . . ?
O1 Gd1 O3 C2 -2.0(8) . . . . ?
O1W Gd1 O3 C2 -101.1(8) . . . . ?
O4 Gd1 O3 C2 170.8(9) . . . . ?
O2W Gd1 O3 C2 -51.0(9) . . . . ?
Gd1 Gd1 O3 C2 77.6(8) 3_757 . . . ?
O1 C1 O2 Gd1 -165.0(14) . . . 1_565 ?
C2 C1 O2 Gd1 12(3) . . . 1_565 ?
Gd1 O4 C4 O5 177.8(9) . . . . ?
Gd1 O4 C4 C3 1.2(15) . . . . ?
O6 Gd1 O6 Gd1 0.0 3_757 . . 3_757 ?
O2 Gd1 O6 Gd1 -121.9(5) 1_545 . . 3_757 ?
O1 Gd1 O6 Gd1 86.6(5) . . . 3_757 ?
O1W Gd1 O6 Gd1 178.4(3) . . . 3_757 ?
O4 Gd1 O6 Gd1 -51.4(7) . . . 3_757 ?
O3 Gd1 O6 Gd1 36.0(8) . . . 3_757 ?
O2W Gd1 O6 Gd1 162.4(6) . . . 3_757 ?
C2 O3 C3 C4 -173.4(10) . . . . ?
Gd1 O3 C3 C4 -7.6(13) . . . . ?
O5 C4 C3 O3 -172.7(10) . . . . ?
O4 C4 C3 O3 4.1(15) . . . . ?
C3 O3 C2 C1 162.5(10) . . . . ?
Gd1 O3 C2 C1 -3.3(13) . . . . ?
O2 C1 C2 O3 -166.2(11) . . . . ?
O1 C1 C2 O3 10.9(16) . . . . ?
O2 C1 O1 Gd1 161.9(9) . . . . ?
C2 C1 O1 Gd1 -15.0(17) . . . . ?
O6 Gd1 O1 C1 -135.5(11) . . . . ?
O6 Gd1 O1 C1 -69.4(11) 3_757 . . . ?
O2 Gd1 O1 C1 146.2(10) 1_545 . . . ?
O1W Gd1 O1 C1 78.8(11) . . . . ?
O4 Gd1 O1 C1 1.2(12) . . . . ?
O3 Gd1 O1 C1 9.2(10) . . . . ?
O2W Gd1 O1 C1 149.6(11) . . . . ?
Gd1 Gd1 O1 C1 -102.3(10) 3_757 . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         3.864
_refine_diff_density_min         -2.631
_refine_diff_density_rms         0.313
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1042008'
_audit_update_record             
;
2015-06-19 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H10 Gd O10'
_chemical_formula_weight         387.38

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'
Gd Gd -0.1653 3.9035 '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           orthorhombic
_symmetry_space_group_name_H-M   Fddd

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

_cell_length_a                   9.6867(19)
_cell_length_b                   15.449(3)
_cell_length_c                   27.303(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4085.9(14)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.6

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_absorpt_coefficient_mu    6.535
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3030
_exptl_absorpt_correction_T_max  0.3548
_exptl_absorpt_process_details   CrystalClear

_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  SCX-MINI
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10269
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1176
_reflns_number_gt                1073
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0054P)²+55.4999P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.00092(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1176
_refine_ls_number_parameters     79
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0444
_refine_ls_wR_factor_gt          0.0432
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_restrained_S_all      1.167
_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
O1 O 0.3798(3) 0.72987(17) 0.51646(9) 0.0274(6) Uani 1 1 d . . .
Gd1 Gd 0.1250 0.6250 0.509444(9) 0.02009(12) Uani 1 2 d S . .
O1W O 0.2757(3) 0.6234(2) 0.43634(9) 0.0291(6) Uani 1 1 d . . .
H1WA H 0.2964 0.6763 0.4270 0.044 Uiso 1 1 d R . .
H1WB H 0.2344 0.5974 0.4117 0.044 Uiso 1 1 d R . .
O2 O 0.3625(3) 0.59402(17) 0.53806(11) 0.0292(6) Uani 1 1 d D . .
C0AA C 0.4347(4) 0.6598(2) 0.52924(14) 0.0195(7) Uani 1 1 d . . .
C1AA C 0.5878(5) 0.6597(3) 0.53208(17) 0.0331(10) Uani 1 1 d . . .
H1AA H 0.6327 0.7128 0.5340 0.040 Uiso 1 1 calc R . .
O2W O 0.4447(6) 0.4522(4) 0.5984(2) 0.1029(19) Uani 1 1 d G . .
H2WA H 0.5264 0.4401 0.5893 0.154 Uiso 1 1 d GD . .
H2WB H 0.4188 0.4988 0.5846 0.154 Uiso 1 1 d GD . .
O3 O 0.1144(3) 0.53856(16) 0.58426(9) 0.0219(6) Uani 1 1 d . . .
C2 C 0.1250 0.5745(3) 0.6250 0.0165(9) Uani 1 2 d S . .

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
O1 0.0359(15) 0.0220(14) 0.0243(14) 0.0034(11) -0.0001(14) 0.0062(13)
Gd1 0.03035(17) 0.01769(15) 0.01224(14) 0.000 0.000 0.00765(12)
O1W 0.0422(17) 0.0233(14) 0.0218(13) -0.0010(13) 0.0025(12) -0.0080(14)
O2 0.0302(16) 0.0228(14) 0.0345(16) 0.0037(12) 0.0001(14) -0.0040(13)
C0AA 0.0209(18) 0.0199(18) 0.0176(18) 0.0000(15) -0.0026(15) 0.0045(15)
C1AA 0.031(2) 0.028(2) 0.040(3) 0.0003(19) 0.000(2) -0.0008(17)
O2W 0.094(4) 0.111(5) 0.104(4) 0.068(4) -0.009(3) 0.018(3)
O3 0.0344(15) 0.0169(12) 0.0145(12) -0.0015(9) -0.0025(12) -0.0033(12)
C2 0.019(2) 0.014(2) 0.016(2) 0.000 -0.001(2) 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
O1 C0AA 1.256(4) . ?
O1 Gd1 2.351(3) 29_566 ?
Gd1 O1 2.351(3) 29_566 ?
Gd1 O1 2.351(3) 30_556 ?
Gd1 O3 2.443(2) . ?
Gd1 O3 2.443(2) 14_455 ?
Gd1 O1W 2.473(3) 14_455 ?
Gd1 O1W 2.473(3) . ?
Gd1 O2 2.476(3) . ?
Gd1 O2 2.476(3) 14_455 ?
O1W H1WA 0.8794 . ?
O1W H1WB 0.8795 . ?
O2 C0AA 1.256(5) . ?
C0AA C1AA 1.485(6) . ?
C1AA C1AA 1.292(9) 14 ?
C1AA H1AA 0.9300 . ?
O2W H2WA 0.8503 . ?
O2W H2WB 0.8496 . ?
O3 C2 1.247(3) . ?
C2 O3 1.247(3) 11_455 ?
C2 C2 1.561(9) 14_455 ?

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
C0AA O1 Gd1 156.1(3) . 29_566 ?
O1 Gd1 O1 145.00(13) 29_566 30_556 ?
O1 Gd1 O3 140.53(9) 29_566 . ?
O1 Gd1 O3 74.40(9) 30_556 . ?
O1 Gd1 O3 74.40(9) 29_566 14_455 ?
O1 Gd1 O3 140.53(9) 30_556 14_455 ?
O3 Gd1 O3 66.51(11) . 14_455 ?
O1 Gd1 O1W 74.70(10) 29_566 14_455 ?
O1 Gd1 O1W 77.20(10) 30_556 14_455 ?
O3 Gd1 O1W 130.97(9) . 14_455 ?
O3 Gd1 O1W 133.97(10) 14_455 14_455 ?
O1 Gd1 O1W 77.20(10) 29_566 . ?
O1 Gd1 O1W 74.70(10) 30_556 . ?
O3 Gd1 O1W 133.97(10) . . ?
O3 Gd1 O1W 130.97(9) 14_455 . ?
O1W Gd1 O1W 72.37(13) 14_455 . ?
O1 Gd1 O2 107.31(10) 29_566 . ?
O1 Gd1 O2 83.82(10) 30_556 . ?
O3 Gd1 O2 70.70(9) . . ?
O3 Gd1 O2 78.63(9) 14_455 . ?
O1W Gd1 O2 143.61(10) 14_455 . ?
O1W Gd1 O2 72.80(9) . . ?
O1 Gd1 O2 83.82(10) 29_566 14_455 ?
O1 Gd1 O2 107.31(10) 30_556 14_455 ?
O3 Gd1 O2 78.63(9) . 14_455 ?
O3 Gd1 O2 70.70(9) 14_455 14_455 ?
O1W Gd1 O2 72.80(9) 14_455 14_455 ?
O1W Gd1 O2 143.61(10) . 14_455 ?
O2 Gd1 O2 143.21(13) . 14_455 ?
Gd1 O1W H1WA 111.0 . . ?
Gd1 O1W H1WB 110.6 . . ?
H1WA O1W H1WB 108.0 . . ?
C0AA O2 Gd1 107.5(2) . . ?
O1 C0AA O2 121.0(4) . . ?
O1 C0AA C1AA 116.0(4) . . ?
O2 C0AA C1AA 123.0(4) . . ?
C1AA C1AA C0AA 124.0(5) 14 . ?
C1AA C1AA H1AA 118.0 14 . ?
C0AA C1AA H1AA 118.0 . . ?
H2WA O2W H2WB 109.4 . . ?
C2 O3 Gd1 119.9(2) . . ?
O3 C2 O3 127.2(4) . 11_455 ?
O3 C2 C2 116.4(2) . 14_455 ?
O3 C2 C2 116.4(2) 11_455 14_455 ?

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 Gd1 O2 C0AA -5.3(3) 29_566 . . . ?
O1 Gd1 O2 C0AA 140.8(3) 30_556 . . . ?
O3 Gd1 O2 C0AA -143.6(3) . . . . ?
O3 Gd1 O2 C0AA -74.8(2) 14_455 . . . ?
O1W Gd1 O2 C0AA 82.3(3) 14_455 . . . ?
O1W Gd1 O2 C0AA 64.9(2) . . . . ?
O2 Gd1 O2 C0AA -108.5(2) 14_455 . . . ?
Gd1 O1 C0AA O2 -176.5(4) 29_566 . . . ?
Gd1 O1 C0AA C1AA 2.3(8) 29_566 . . . ?
Gd1 O2 C0AA O1 11.2(4) . . . . ?
Gd1 O2 C0AA C1AA -167.5(3) . . . . ?
O1 C0AA C1AA C1AA -161.5(2) . . . 14 ?
O2 C0AA C1AA C1AA 17.3(5) . . . 14 ?
O1 Gd1 O3 C2 -11.5(3) 29_566 . . . ?
O1 Gd1 O3 C2 171.3(2) 30_556 . . . ?
O3 Gd1 O3 C2 -3.17(9) 14_455 . . . ?
O1W Gd1 O3 C2 -131.86(19) 14_455 . . . ?
O1W Gd1 O3 C2 121.86(19) . . . . ?
O2 Gd1 O3 C2 82.5(2) . . . . ?
O2 Gd1 O3 C2 -76.9(2) 14_455 . . . ?
Gd1 O3 C2 O3 -172.1(2) . . . 11_455 ?
Gd1 O3 C2 C2 7.9(2) . . . 14_455 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.106
