# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 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_p
_database_code_depnum_ccdc_archive 'CCDC 1043508'
_audit_update_record             
;
2015-01-14 deposited with the CCDC.
2015-03-23 downloaded from the CCDC.
;
_audit_creation_date             2013-12-17
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4465)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(Gd8 H32 O28)'
_chemical_formula_sum            'H8 Gd2 O7'
_chemical_formula_weight         434.56
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 '-x, y, -z+1/2'
4 'x, -y, -z'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z+1/2'
7 '-x+1/2, y+1/2, -z+1/2'
8 'x+1/2, -y+1/2, -z'
9 '-x, -y, -z'
10 'x, y, -z-1/2'
11 'x, -y, z-1/2'
12 '-x, y, z'
13 '-x+1/2, -y+1/2, -z'
14 'x+1/2, y+1/2, -z-1/2'
15 'x+1/2, -y+1/2, z-1/2'
16 '-x+1/2, y+1/2, z'

_cell_length_a                   16.583(3)
_cell_length_b                   12.975(3)
_cell_length_c                   7.3106(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1573.0(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    16.698
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5676
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         4.01
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                597
_reflns_number_total             730
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         6.179
_refine_diff_density_min         -2.606
_refine_diff_density_rms         0.615
_refine_ls_extinction_coef       0.00181(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0661
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.312
_refine_ls_shift/su_mean         0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1227P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1903
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H1 of O1, H2 of O2, H3 of O3, {H1WA,H1WB} of O1W, {H2WA,H2WB} of O2W
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) H2WA(0.5) H2WB(0.5)
3.a Riding coordinates:
 O1(H1), O2(H2), O3(H3), O1W(H1WA,H1WB), O2W(H2WA,H2WB)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.28768(4) 0.23117(6) 0.2500 0.0190(2) Uani 1 2 d S . .
Gd2 Gd 0.21796(4) 0.0000 0.0000 0.0201(2) Uani 1 2 d S . .
O1 O 0.1784(6) 0.1176(8) 0.2500 0.024(3) Uani 1 2 d S . .
H1 H 0.1309 0.1423 0.2500 0.029 Uiso 1 2 d SR . .
O2 O 0.3149(6) 0.0325(8) 0.2500 0.019(2) Uani 1 2 d S . .
H2 H 0.3622 0.0074 0.2500 0.022 Uiso 1 2 d SR . .
O3 O 0.2063(3) 0.3337(5) 0.0460(9) 0.0145(17) Uani 1 1 d . . .
H3 H 0.1584 0.3425 0.0841 0.017 Uiso 1 1 d R . .
O4 O 0.1630(6) 0.0973(8) -0.2500 0.027(3) Uani 1 2 d S . .
O1W O 0.4407(10) 0.2157(11) 0.2500 0.082(6) Uani 1 2 d S . .
H1WA H 0.4578 0.1598 0.2966 0.098 Uiso 0.50 1 d PR . .
H1WB H 0.4646 0.2674 0.2966 0.098 Uiso 0.50 1 d PR . .
O2W O 0.0620(9) 0.0000 0.0000 0.062(5) Uani 1 2 d S . .
H2WA H 0.0414 0.0523 -0.0523 0.075 Uiso 0.50 1 d PR . .
H2WB H 0.0414 -0.0091 0.1053 0.075 Uiso 0.50 1 d PR . .

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 0.0244(4) 0.0181(5) 0.0145(4) 0.000 0.000 -0.0001(3)
Gd2 0.0303(4) 0.0169(5) 0.0131(4) 0.0008(3) 0.000 0.000
O1 0.022(5) 0.022(6) 0.029(5) 0.000 0.000 0.006(5)
O2 0.019(5) 0.026(6) 0.011(4) 0.000 0.000 -0.009(4)
O3 0.018(3) 0.015(4) 0.011(3) -0.004(3) 0.000(3) -0.002(3)
O4 0.038(6) 0.017(6) 0.024(5) 0.000 0.000 -0.006(5)
O1W 0.139(15) 0.014(8) 0.092(13) 0.000 0.000 0.001(9)
O2W 0.096(12) 0.039(9) 0.052(9) 0.018(6) 0.000 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
Gd1 Gd1 3.8938(9) 13 ?
Gd1 Gd1 3.8938(9) 13_556 ?
Gd1 Gd2 3.6978(9) . ?
Gd1 Gd2 3.6978(9) 10_556 ?
Gd1 O1 2.336(10) . ?
Gd1 O2 2.617(10) . ?
Gd1 O3 2.324(7) 13 ?
Gd1 O3 2.324(7) 6 ?
Gd1 O3 2.411(7) . ?
Gd1 O3 2.411(7) 10_556 ?
Gd1 O4 2.371(10) 13 ?
Gd1 O1W 2.545(16) . ?
Gd2 Gd2 3.6553(8) 10 ?
Gd2 Gd2 3.6553(8) 10_556 ?
Gd2 O1 2.470(7) 11 ?
Gd2 O1 2.470(7) . ?
Gd2 O2 2.471(6) . ?
Gd2 O2 2.471(6) 11 ?
Gd2 O3 2.519(6) 16_545 ?
Gd2 O3 2.519(6) 13 ?
Gd2 O4 2.401(7) . ?
Gd2 O4 2.401(7) 11_556 ?
Gd2 O2W 2.587(15) . ?
O1 Gd2 2.470(7) 10_556 ?
O2 Gd2 2.471(6) 10_556 ?
O3 Gd1 2.324(7) 13 ?
O3 Gd2 2.519(6) 13 ?
O4 Gd1 2.371(10) 13 ?
O4 Gd2 2.401(7) 10 ?

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
Gd1 Gd1 Gd1 139.68(4) 13 13_556 ?
Gd2 Gd1 Gd1 62.447(19) . 13 ?
Gd2 Gd1 Gd1 117.74(3) 10_556 13 ?
Gd2 Gd1 Gd1 62.447(19) 10_556 13_556 ?
Gd2 Gd1 Gd1 117.74(3) . 13_556 ?
Gd2 Gd1 Gd2 59.242(18) 10_556 . ?
O1 Gd1 Gd1 80.22(8) . 13_556 ?
O1 Gd1 Gd1 80.22(8) . 13 ?
O1 Gd1 Gd2 41.04(17) . . ?
O1 Gd1 Gd2 41.04(17) . 10_556 ?
O1 Gd1 O2 60.8(3) . . ?
O1 Gd1 O3 85.1(3) . 10_556 ?
O1 Gd1 O3 85.1(3) . . ?
O1 Gd1 O4 149.3(4) . 13 ?
O1 Gd1 O1W 136.4(4) . . ?
O2 Gd1 Gd1 100.31(7) . 13_556 ?
O2 Gd1 Gd1 100.31(7) . 13 ?
O2 Gd1 Gd2 41.84(14) . 10_556 ?
O2 Gd1 Gd2 41.84(14) . . ?
O3 Gd1 Gd1 35.41(16) 13 13 ?
O3 Gd1 Gd1 33.96(16) 10_556 13_556 ?
O3 Gd1 Gd1 35.41(16) 6 13_556 ?
O3 Gd1 Gd1 109.38(16) . 13_556 ?
O3 Gd1 Gd1 158.95(15) 13 13_556 ?
O3 Gd1 Gd1 158.95(15) 6 13 ?
O3 Gd1 Gd1 33.96(16) . 13 ?
O3 Gd1 Gd1 109.38(16) 10_556 13 ?
O3 Gd1 Gd2 88.10(16) 10_556 10_556 ?
O3 Gd1 Gd2 42.22(16) 13 . ?
O3 Gd1 Gd2 125.33(15) 10_556 . ?
O3 Gd1 Gd2 88.10(16) . . ?
O3 Gd1 Gd2 100.37(17) 6 . ?
O3 Gd1 Gd2 125.33(15) . 10_556 ?
O3 Gd1 Gd2 100.37(17) 13 10_556 ?
O3 Gd1 Gd2 42.22(16) 6 10_556 ?
O3 Gd1 O1 78.74(17) 13 . ?
O3 Gd1 O1 78.74(17) 6 . ?
O3 Gd1 O2 68.66(17) 6 . ?
O3 Gd1 O2 129.8(2) . . ?
O3 Gd1 O2 68.66(17) 13 . ?
O3 Gd1 O2 129.8(2) 10_556 . ?
O3 Gd1 O3 76.4(3) . 10_556 ?
O3 Gd1 O3 69.4(3) 13 . ?
O3 Gd1 O3 143.09(17) 6 . ?
O3 Gd1 O3 137.2(3) 13 6 ?
O3 Gd1 O3 69.4(3) 6 10_556 ?
O3 Gd1 O3 143.09(17) 13 10_556 ?
O3 Gd1 O4 108.97(17) 6 13 ?
O3 Gd1 O4 108.97(17) 13 13 ?
O3 Gd1 O1W 85.93(18) 13 . ?
O3 Gd1 O1W 127.0(3) 10_556 . ?
O3 Gd1 O1W 127.0(3) . . ?
O3 Gd1 O1W 85.93(18) 6 . ?
O4 Gd1 Gd1 89.60(9) 13 13 ?
O4 Gd1 Gd1 89.60(9) 13 13_556 ?
O4 Gd1 Gd2 150.367(12) 13 . ?
O4 Gd1 Gd2 150.367(12) 13 10_556 ?
O4 Gd1 O2 149.9(3) 13 . ?
O4 Gd1 O3 71.0(3) 13 10_556 ?
O4 Gd1 O3 71.0(3) 13 . ?
O4 Gd1 O1W 74.3(4) 13 . ?
O1W Gd1 Gd1 109.26(4) . 13 ?
O1W Gd1 Gd1 109.26(4) . 13_556 ?
O1W Gd1 Gd2 104.4(3) . 10_556 ?
O1W Gd1 Gd2 104.4(3) . . ?
O1W Gd1 O2 75.5(4) . . ?
Gd2 Gd2 Gd1 119.621(9) 10 . ?
Gd2 Gd2 Gd1 60.379(9) 10_556 . ?
Gd2 Gd2 Gd2 180.0 10 10_556 ?
O1 Gd2 Gd1 161.81(18) 11 . ?
O1 Gd2 Gd1 38.4(2) . . ?
O1 Gd2 Gd2 42.27(18) 11 10 ?
O1 Gd2 Gd2 137.73(18) . 10 ?
O1 Gd2 Gd2 42.27(18) . 10_556 ?
O1 Gd2 Gd2 137.73(18) 11 10_556 ?
O1 Gd2 O1 149.2(5) . 11 ?
O1 Gd2 O2 61.3(3) . . ?
O1 Gd2 O2 145.7(3) 11 . ?
O1 Gd2 O2 61.3(3) 11 11 ?
O1 Gd2 O2 145.7(3) . 11 ?
O1 Gd2 O3 124.3(2) 11 13 ?
O1 Gd2 O3 124.3(2) . 16_545 ?
O1 Gd2 O3 72.7(3) 11 16_545 ?
O1 Gd2 O3 72.7(3) . 13 ?
O1 Gd2 O2W 74.6(2) . . ?
O1 Gd2 O2W 74.6(2) 11 . ?
O2 Gd2 Gd1 45.0(2) . . ?
O2 Gd2 Gd1 107.5(2) 11 . ?
O2 Gd2 Gd2 42.29(16) . 10_556 ?
O2 Gd2 Gd2 137.71(16) 11 10_556 ?
O2 Gd2 Gd2 137.71(16) . 10 ?
O2 Gd2 Gd2 42.29(16) 11 10 ?
O2 Gd2 O2 98.8(3) 11 . ?
O2 Gd2 O3 68.2(2) . 13 ?
O2 Gd2 O3 73.9(3) 11 13 ?
O2 Gd2 O3 68.2(2) 11 16_545 ?
O2 Gd2 O3 73.9(3) . 16_545 ?
O2 Gd2 O2W 130.60(17) . . ?
O2 Gd2 O2W 130.60(17) 11 . ?
O3 Gd2 Gd1 38.31(15) 13 . ?
O3 Gd2 Gd1 118.23(15) 16_545 . ?
O3 Gd2 Gd2 97.68(15) 13 10_556 ?
O3 Gd2 Gd2 82.32(15) 16_545 10_556 ?
O3 Gd2 Gd2 97.68(15) 16_545 10 ?
O3 Gd2 Gd2 82.32(15) 13 10 ?
O3 Gd2 O3 120.2(3) 13 16_545 ?
O3 Gd2 O2W 119.89(14) 16_545 . ?
O3 Gd2 O2W 119.89(14) 13 . ?
O4 Gd2 Gd1 93.9(2) . . ?
O4 Gd2 Gd1 99.73(19) 11_556 . ?
O4 Gd2 Gd2 40.43(19) 11_556 10_556 ?
O4 Gd2 Gd2 139.57(19) . 10_556 ?
O4 Gd2 Gd2 139.57(19) 11_556 10 ?
O4 Gd2 Gd2 40.43(19) . 10 ?
O4 Gd2 O1 97.9(3) 11_556 11 ?
O4 Gd2 O1 97.9(3) . . ?
O4 Gd2 O1 70.2(3) 11_556 . ?
O4 Gd2 O1 70.2(3) . 11 ?
O4 Gd2 O2 76.9(3) . 11 ?
O4 Gd2 O2 76.9(3) 11_556 . ?
O4 Gd2 O2 136.1(3) . . ?
O4 Gd2 O2 136.1(3) 11_556 11 ?
O4 Gd2 O3 68.7(3) . 13 ?
O4 Gd2 O3 68.7(3) 11_556 16_545 ?
O4 Gd2 O3 137.8(2) . 16_545 ?
O4 Gd2 O3 137.8(2) 11_556 13 ?
O4 Gd2 O4 135.4(5) . 11_556 ?
O4 Gd2 O2W 67.7(2) 11_556 . ?
O4 Gd2 O2W 67.7(2) . . ?
O2W Gd2 Gd1 108.221(17) . . ?
O2W Gd2 Gd2 90.0 . 10 ?
O2W Gd2 Gd2 90.0 . 10_556 ?
Gd1 O1 Gd2 100.6(3) . 10_556 ?
Gd1 O1 Gd2 100.6(3) . . ?
Gd2 O1 Gd2 95.5(4) . 10_556 ?
Gd2 O2 Gd1 93.2(3) . . ?
Gd2 O2 Gd1 93.2(3) 10_556 . ?
Gd2 O2 Gd2 95.4(3) 10_556 . ?
Gd1 O3 Gd1 110.6(3) 13 . ?
Gd1 O3 Gd2 106.0(2) . 13 ?
Gd1 O3 Gd2 99.5(2) 13 13 ?
Gd1 O4 Gd2 111.3(3) 13 10 ?
Gd1 O4 Gd2 111.3(3) 13 . ?
Gd2 O4 Gd2 99.1(4) . 10 ?

####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 1043509'
_audit_update_record             
;
2015-01-14 deposited with the CCDC.
2015-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H3 Gd O3'
_chemical_formula_weight         208.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.2993(8)
_cell_length_b                   6.2993(8)
_cell_length_c                   3.6057(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     123.91(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.582
_exptl_crystal_F_000             182
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    26.470
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            219
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_av_R_equivalents  0.1226
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         3.735
_diffrn_reflns_theta_max         26.875
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measured_fraction_theta_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_point_group_measured_fraction_full 0.910
_reflns_number_total             93
_reflns_number_gt                87
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1320P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       1.9(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         93
_refine_ls_number_parameters     10
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1634
_refine_ls_wR_factor_gt          0.1613
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.6667 0.3333 0.2500 0.0105(19) Uani 1 6 d S T P . .
O1 O 0.6033(16) 0.687(2) 0.2500 0.015(3) Uani 1 2 d S T P . .
H1 H 0.7381 0.8216 0.2500 0.018 Uiso 1 2 d R U P . .

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 0.0043(19) 0.0043(19) 0.023(3) 0.000 0.000 0.0022(9)
O1 -0.004(6) 0.014(5) 0.023(6) 0.000 0.000 -0.007(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 O1 2.438(4) 8 ?
Gd1 O1 2.438(4) 8_556 ?
Gd1 O1 2.438(4) 9_656 ?
Gd1 O1 2.438(4) 9_655 ?
Gd1 O1 2.438(4) 7_665 ?
Gd1 O1 2.438(4) 7_666 ?
Gd1 O1 2.449(11) 3_665 ?
Gd1 O1 2.449(11) 2_655 ?
Gd1 O1 2.449(11) . ?
Gd1 Gd1 3.6057(6) 1_556 ?
Gd1 Gd1 3.6057(6) 1_554 ?
Gd1 Gd1 4.0592(4) 7_766 ?
O1 Gd1 2.438(4) 7_665 ?
O1 Gd1 2.438(4) 7_666 ?

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 Gd1 O1 95.4(2) 8 8_556 ?
O1 Gd1 O1 140.66(9) 8 9_656 ?
O1 Gd1 O1 71.33(18) 8_556 9_656 ?
O1 Gd1 O1 71.33(18) 8 9_655 ?
O1 Gd1 O1 140.66(9) 8_556 9_655 ?
O1 Gd1 O1 95.4(2) 9_656 9_655 ?
O1 Gd1 O1 71.33(18) 8 7_665 ?
O1 Gd1 O1 140.66(9) 8_556 7_665 ?
O1 Gd1 O1 140.66(9) 9_656 7_665 ?
O1 Gd1 O1 71.33(18) 9_655 7_665 ?
O1 Gd1 O1 140.66(9) 8 7_666 ?
O1 Gd1 O1 71.33(18) 8_556 7_666 ?
O1 Gd1 O1 71.33(18) 9_656 7_666 ?
O1 Gd1 O1 140.66(9) 9_655 7_666 ?
O1 Gd1 O1 95.4(2) 7_665 7_666 ?
O1 Gd1 O1 73.0(4) 8 3_665 ?
O1 Gd1 O1 73.0(4) 8_556 3_665 ?
O1 Gd1 O1 67.7(4) 9_656 3_665 ?
O1 Gd1 O1 67.7(4) 9_655 3_665 ?
O1 Gd1 O1 132.17(13) 7_665 3_665 ?
O1 Gd1 O1 132.17(13) 7_666 3_665 ?
O1 Gd1 O1 67.7(4) 8 2_655 ?
O1 Gd1 O1 67.7(4) 8_556 2_655 ?
O1 Gd1 O1 132.17(13) 9_656 2_655 ?
O1 Gd1 O1 132.17(13) 9_655 2_655 ?
O1 Gd1 O1 73.0(4) 7_665 2_655 ?
O1 Gd1 O1 73.0(4) 7_666 2_655 ?
O1 Gd1 O1 120.0 3_665 2_655 ?
O1 Gd1 O1 132.17(13) 8 . ?
O1 Gd1 O1 132.17(13) 8_556 . ?
O1 Gd1 O1 73.0(4) 9_656 . ?
O1 Gd1 O1 73.0(4) 9_655 . ?
O1 Gd1 O1 67.7(4) 7_665 . ?
O1 Gd1 O1 67.7(4) 7_666 . ?
O1 Gd1 O1 120.000(1) 3_665 . ?
O1 Gd1 O1 119.999(2) 2_655 . ?
O1 Gd1 Gd1 137.68(11) 8 1_556 ?
O1 Gd1 Gd1 42.32(11) 8_556 1_556 ?
O1 Gd1 Gd1 42.32(12) 9_656 1_556 ?
O1 Gd1 Gd1 137.68(11) 9_655 1_556 ?
O1 Gd1 Gd1 137.68(11) 7_665 1_556 ?
O1 Gd1 Gd1 42.32(11) 7_666 1_556 ?
O1 Gd1 Gd1 90.0 3_665 1_556 ?
O1 Gd1 Gd1 90.000(2) 2_655 1_556 ?
O1 Gd1 Gd1 90.000(1) . 1_556 ?
O1 Gd1 Gd1 42.32(11) 8 1_554 ?
O1 Gd1 Gd1 137.68(11) 8_556 1_554 ?
O1 Gd1 Gd1 137.68(12) 9_656 1_554 ?
O1 Gd1 Gd1 42.32(11) 9_655 1_554 ?
O1 Gd1 Gd1 42.32(11) 7_665 1_554 ?
O1 Gd1 Gd1 137.68(11) 7_666 1_554 ?
O1 Gd1 Gd1 90.000(1) 3_665 1_554 ?
O1 Gd1 Gd1 90.000(1) 2_655 1_554 ?
O1 Gd1 Gd1 90.000(1) . 1_554 ?
Gd1 Gd1 Gd1 180.0 1_556 1_554 ?
O1 Gd1 Gd1 106.8(3) 8 7_766 ?
O1 Gd1 Gd1 68.4(3) 8_556 7_766 ?
O1 Gd1 Gd1 33.9(3) 9_656 7_766 ?
O1 Gd1 Gd1 80.05(18) 9_655 7_766 ?
O1 Gd1 Gd1 150.4(3) 7_665 7_766 ?
O1 Gd1 Gd1 102.29(17) 7_666 7_766 ?
O1 Gd1 Gd1 33.76(13) 3_665 7_766 ?
O1 Gd1 Gd1 134.82(17) 2_655 7_766 ?
O1 Gd1 Gd1 97.3(2) . 7_766 ?
Gd1 Gd1 Gd1 63.632(5) 1_556 7_766 ?
Gd1 Gd1 Gd1 116.368(4) 1_554 7_766 ?
Gd1 O1 Gd1 95.4(2) 7_665 7_666 ?
Gd1 O1 Gd1 112.3(4) 7_665 . ?
Gd1 O1 Gd1 112.3(4) 7_666 . ?

_refine_diff_density_max         3.726
_refine_diff_density_min         -2.947
_refine_diff_density_rms         0.919

_shelxl_version_number           2013-2

_shelx_res_file                  
;
TITL p in P6(3)/m
CELL 0.71073 6.2993 6.2993 3.6057 90 90 120
ZERR 2 0.0008 0.0008 0.0006 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z

SFAC O H Gd
UNIT 6 6 2

L.S. 10
PLAN  5
BOND
fmap 2
acta
OMIT -3 54
OMIT 0 0 2
OMIT -3 7 2
OMIT 0 3 0
OMIT -2 6 1
OMIT 0 4 1
OMIT 0 2 3
REM <HKL>E:\[A][Inorganic%20Chemistry]\date\2014041703-2%20GdOH%203D\Re_%20GdO
REM H%203D   6 0 .%2072

WGHT    0.132000
EXTI    1.850607
FVAR       1.47386
GD1   3    0.666667    0.333333    0.250000    10.16667    0.00435    0.00435 =
         0.02293    0.00000    0.00000    0.00217
O1    1    0.603293    0.686587    0.250000    10.50000   -0.00398    0.01369 =
         0.02337    0.00000    0.00000   -0.00718
AFIX   3
H1    2    0.738143    0.821607    0.250000    10.50000   -1.20000
AFIX   0
HKLF 4

REM  p in P6(3)/m
REM R1 =  0.0681 for      87 Fo > 4sig(Fo)  and  0.0687 for all      93 data
REM     10 parameters refined using      0 restraints

END

WGHT      0.1320      0.0000

REM Highest difference peak  3.726,  deepest hole -2.947,  1-sigma level  0.919
Q1    1   0.6667  0.3333  0.0592  10.33333  0.05    3.73
Q2    1   0.5669  0.7820  0.0148  11.00000  0.05    2.45
Q3    1   0.7785  0.7905 -0.0057  11.00000  0.05    2.20
Q4    1   0.9032  1.0268  0.2500  10.50000  0.05    2.15
Q5    1   0.6539  0.5395  0.2500  10.50000  0.05    2.00
;
_shelx_res_checksum              54746
