# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

data_added_by_encifer
# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C 

_journal_name_full               'Journal of Materials Chemistry C'

_journal_coden_Cambridge         ?
_publ_contact_author_name        'Prof Ning Ye'
_publ_contact_author_address     
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. CHINA
;
_publ_contact_author_email       nye@fjirsm.ac.cn
_publ_contact_author_phone       86-59183776076
_publ_contact_author_fax         86-59183750713

loop_
_publ_author_name
_publ_author_address
'Min Luo'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
'Chen-sheng Lin'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
'Guo-Hong Zou'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
'Wen-Dan Cheng'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;

_publ_section_title              
;
Sodium-Rare Earth Carbonates with Shorite Structure and Large Second Harmonic Generation Response
;

data_1

_audit_update_record             
;
2012-12-17 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 Gd Na3 O9'
_chemical_formula_sum            'C3 Gd Na3 O9'
_chemical_formula_weight         406.25

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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   Ama2
_space_group_name_Hall           'A 2 -2a '

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

_cell_length_a                   9.926(3)
_cell_length_b                   10.992(4)
_cell_length_c                   7.120(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     776.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    835
_cell_measurement_theta_min      3.2233
_cell_measurement_theta_max      27.5089

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.1500
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    8.741
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7944
_exptl_absorpt_process_details   ?

_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       
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2686
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         27.45
_reflns_number_total             873
_reflns_number_gt                854
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0218P)²+0.3427P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_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   0.06(2)
_refine_ls_number_reflns         873
_refine_ls_number_parameters     81
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0162
_refine_ls_wR_factor_ref         0.0437
_refine_ls_wR_factor_gt          0.0435
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.151
_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
Gd1 Gd 1.2500 0.77179(2) 0.01265(10) 0.00558(10) Uani 1 2 d S . .
O1 O 1.2500 0.8846(4) 0.3199(7) 0.0132(10) Uani 1 2 d S . .
O2 O 1.3869(3) 0.8345(3) -0.2545(5) 0.0092(7) Uani 1 1 d . . .
O3 O 1.3909(3) 0.6416(3) 0.2128(4) 0.0114(7) Uani 1 1 d . . .
O4 O 1.2500 1.0875(5) 0.3334(8) 0.0149(10) Uani 1 2 d S . .
O5 O 1.4894(3) 0.8045(4) 0.0959(6) 0.0147(8) Uani 1 1 d . . .
O6 O 1.2500 0.9907(4) 0.0565(6) 0.0097(12) Uani 1 2 d S . .
C1 C 1.2500 0.9877(6) 0.2412(10) 0.0074(13) Uani 1 2 d S . .
C2 C 1.5005(4) 0.7957(4) -0.3123(8) 0.0072(9) Uani 1 1 d . . .
Na1 Na 1.2500 0.9819(2) 0.6260(4) 0.0114(6) Uani 1 2 d S . .
Na2 Na 1.5000 1.0000 0.9448(4) 0.0130(6) Uani 1 2 d S . .
Na3 Na 1.2500 0.70621(16) 0.5105(10) 0.0026(4) Uiso 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
Gd1 0.00459(14) 0.00619(15) 0.00595(14) 0.0004(2) 0.000 0.000
O1 0.025(3) 0.009(3) 0.005(2) 0.0032(19) 0.000 0.000
O2 0.0057(15) 0.0125(17) 0.0093(17) 0.0014(13) 0.0025(12) 0.0017(13)
O3 0.0065(16) 0.0110(16) 0.0166(19) 0.0046(14) -0.0035(12) -0.0038(13)
O4 0.022(3) 0.011(3) 0.012(2) -0.0025(19) 0.000 0.000
O5 0.0115(18) 0.0138(18) 0.019(2) 0.0121(16) -0.0043(13) -0.0029(14)
O6 0.016(2) 0.007(2) 0.006(3) 0.0024(15) 0.000 0.000
C1 0.002(3) 0.010(3) 0.010(4) -0.001(2) 0.000 0.000
C2 0.010(2) 0.006(2) 0.005(3) 0.0042(19) -0.0010(15) -0.0011(16)
Na1 0.0106(13) 0.0100(14) 0.0135(16) 0.0029(11) 0.000 0.000
Na2 0.0122(14) 0.0116(14) 0.0151(14) 0.000 0.000 -0.0020(9)

_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 O4 2.394(5) 5_544 ?
Gd1 O6 2.426(4) . ?
Gd1 O2 2.437(3) 3_755 ?
Gd1 O2 2.437(3) . ?
Gd1 O3 2.456(3) 3_755 ?
Gd1 O3 2.456(3) . ?
Gd1 O5 2.475(3) . ?
Gd1 O5 2.475(3) 3_755 ?
Gd1 O1 2.515(5) . ?
Gd1 C2 2.870(5) 6_865 ?
Gd1 C2 2.870(5) 8_465 ?
Gd1 C1 2.878(7) . ?
O1 C1 1.265(8) . ?
O2 C2 1.274(6) . ?
O3 C2 1.291(6) 6_865 ?
O4 C1 1.278(9) . ?
O4 Gd1 2.394(5) 5 ?
O5 C2 1.284(7) 6_865 ?
O6 C1 1.315(8) . ?
C2 O5 1.284(7) 6_864 ?
C2 O3 1.291(6) 6_864 ?
C2 Gd1 2.870(5) 6_864 ?

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 Gd1 O6 155.18(18) 5_544 . ?
O4 Gd1 O2 79.82(14) 5_544 3_755 ?
O6 Gd1 O2 79.63(11) . 3_755 ?
O4 Gd1 O2 79.82(14) 5_544 . ?
O6 Gd1 O2 79.62(11) . . ?
O2 Gd1 O2 67.77(15) 3_755 . ?
O4 Gd1 O3 79.44(13) 5_544 3_755 ?
O6 Gd1 O3 120.18(11) . 3_755 ?
O2 Gd1 O3 107.47(12) 3_755 3_755 ?
O2 Gd1 O3 159.24(11) . 3_755 ?
O4 Gd1 O3 79.44(13) 5_544 . ?
O6 Gd1 O3 120.18(11) . . ?
O2 Gd1 O3 159.24(11) 3_755 . ?
O2 Gd1 O3 107.47(12) . . ?
O3 Gd1 O3 69.41(16) 3_755 . ?
O4 Gd1 O5 104.50(11) 5_544 . ?
O6 Gd1 O5 79.94(10) . . ?
O2 Gd1 O5 132.93(12) 3_755 . ?
O2 Gd1 O5 67.09(12) . . ?
O3 Gd1 O5 119.47(12) 3_755 . ?
O3 Gd1 O5 53.05(11) . . ?
O4 Gd1 O5 104.50(11) 5_544 3_755 ?
O6 Gd1 O5 79.94(10) . 3_755 ?
O2 Gd1 O5 67.09(12) 3_755 3_755 ?
O2 Gd1 O5 132.93(12) . 3_755 ?
O3 Gd1 O5 53.05(11) 3_755 3_755 ?
O3 Gd1 O5 119.47(12) . 3_755 ?
O5 Gd1 O5 147.5(2) . 3_755 ?
O4 Gd1 O1 151.75(18) 5_544 . ?
O6 Gd1 O1 53.07(15) . . ?
O2 Gd1 O1 122.65(11) 3_755 . ?
O2 Gd1 O1 122.65(11) . . ?
O3 Gd1 O1 77.42(12) 3_755 . ?
O3 Gd1 O1 77.42(12) . . ?
O5 Gd1 O1 73.74(10) . . ?
O5 Gd1 O1 73.74(10) 3_755 . ?
O4 Gd1 C2 90.74(12) 5_544 6_865 ?
O6 Gd1 C2 101.56(11) . 6_865 ?
O2 Gd1 C2 153.28(14) 3_755 6_865 ?
O2 Gd1 C2 86.05(13) . 6_865 ?
O3 Gd1 C2 95.08(13) 3_755 6_865 ?
O3 Gd1 C2 26.64(13) . 6_865 ?
O5 Gd1 C2 26.51(14) . 6_865 ?
O5 Gd1 C2 139.61(14) 3_755 6_865 ?
O1 Gd1 C2 75.49(11) . 6_865 ?
O4 Gd1 C2 90.74(11) 5_544 8_465 ?
O6 Gd1 C2 101.56(11) . 8_465 ?
O2 Gd1 C2 86.05(13) 3_755 8_465 ?
O2 Gd1 C2 153.28(14) . 8_465 ?
O3 Gd1 C2 26.64(13) 3_755 8_465 ?
O3 Gd1 C2 95.08(13) . 8_465 ?
O5 Gd1 C2 139.61(14) . 8_465 ?
O5 Gd1 C2 26.51(14) 3_755 8_465 ?
O1 Gd1 C2 75.49(11) . 8_465 ?
C2 Gd1 C2 119.3(2) 6_865 8_465 ?
O4 Gd1 C1 177.78(18) 5_544 . ?
O6 Gd1 C1 27.04(17) . . ?
O2 Gd1 C1 102.00(14) 3_755 . ?
O2 Gd1 C1 102.00(14) . . ?
O3 Gd1 C1 98.75(14) 3_755 . ?
O3 Gd1 C1 98.75(14) . . ?
O5 Gd1 C1 75.22(11) . . ?
O5 Gd1 C1 75.22(11) 3_755 . ?
O1 Gd1 C1 26.03(17) . . ?
C2 Gd1 C1 88.14(12) 6_865 . ?
C2 Gd1 C1 88.14(12) 8_465 . ?
C1 O1 Gd1 93.2(4) . . ?
C2 O2 Gd1 130.6(3) . . ?
C2 O3 Gd1 94.8(3) 6_865 . ?
C1 O4 Gd1 178.7(5) . 5 ?
C2 O5 Gd1 94.1(3) 6_865 . ?
C1 O6 Gd1 96.0(4) . . ?
O1 C1 O4 122.8(7) . . ?
O1 C1 O6 117.7(6) . . ?
O4 C1 O6 119.4(6) . . ?
O1 C1 Gd1 60.7(4) . . ?
O4 C1 Gd1 176.4(5) . . ?
O6 C1 Gd1 57.0(3) . . ?
O2 C2 O5 121.3(4) . 6_864 ?
O2 C2 O3 121.0(5) . 6_864 ?
O5 C2 O3 117.6(4) 6_864 6_864 ?
O2 C2 Gd1 172.1(4) . 6_864 ?
O5 C2 Gd1 59.3(2) 6_864 6_864 ?
O3 C2 Gd1 58.5(2) 6_864 6_864 ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.143
_database_code_depnum_ccdc_archive 'CCDC 975760'
data_added_by_encifer
# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C 

_journal_name_full               'Journal of Materials Chemistry C'

_journal_coden_Cambridge         ?
_publ_contact_author_name        'Prof Ning Ye'
_publ_contact_author_address     
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. CHINA
;
_publ_contact_author_email       nye@fjirsm.ac.cn
_publ_contact_author_phone       86-59183776076
_publ_contact_author_fax         86-59183750713

loop_
_publ_author_name
_publ_author_address
'Min Luo'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
'Chen-sheng Lin'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
'Guo-Hong Zou'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;
'Wen-Dan Cheng'
;
Key Laboratory of Optoelectronic Materials Chemistry and Physics
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou, Fujian 350002
P. R. China
;

_publ_section_title              
;
Sodium-Rare Earth Carbonates with Shorite Structure and Large Second Harmonic Generation Response
;

data_2

_audit_update_record             
;
2012-12-20 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 Na3 O9 Y'
_chemical_formula_sum            'C3 Na3 O9 Y'
_chemical_formula_weight         337.91

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'
Na Na 0.0362 0.0249 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Ama2
_space_group_name_Hall           'A 2 -2a '

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

_cell_length_a                   9.820(14)
_cell_length_b                   10.883(16)
_cell_length_c                   7.038(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     752.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1004
_cell_measurement_theta_min      3.4456
_cell_measurement_theta_max      27.5283

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.1000
_exptl_crystal_size_mid          0.0500
_exptl_crystal_size_min          0.0500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    7.964
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8166

_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       
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2804
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         27.39
_reflns_number_total             895
_reflns_number_gt                810
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0100P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_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   -0.011(13)
_refine_ls_number_reflns         895
_refine_ls_number_parameters     84
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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
Y1 Y -0.2500 0.72829(6) 0.50003(17) 0.01005(17) Uani 1 2 d S . .
O1 O -0.2500 0.9120(5) 0.6801(8) 0.0149(12) Uani 1 2 d S . .
O2 O -0.2500 0.6173(5) 0.1931(8) 0.0150(12) Uani 1 2 d S . .
O3 O -0.4881(3) 0.6923(4) 0.4161(5) 0.0170(9) Uani 1 1 d . . .
O4 O -0.2500 0.5111(4) 0.4587(7) 0.0133(14) Uani 1 2 d S . .
O5 O -0.3865(4) 0.6674(4) 0.7653(5) 0.0128(9) Uani 1 1 d . . .
O6 O -0.3899(4) 0.8574(3) 0.3034(5) 0.0144(9) Uani 1 1 d . . .
C1 C -0.2500 0.5119(7) 0.2733(11) 0.0095(16) Uani 1 2 d S . .
C2 C -0.4986(5) 0.7931(5) 0.3254(8) 0.0110(11) Uani 1 1 d . . .
Na1 Na -0.2500 0.0185(3) 0.3863(5) 0.0149(7) Uani 1 2 d S . .
Na2 Na -0.2500 -0.2051(2) 0.0008(9) 0.0082(5) Uani 1 2 d S . .
Na3 Na -0.5000 0.0000 0.0682(5) 0.0164(7) 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
Y1 0.0098(3) 0.0098(3) 0.0105(3) 0.0000(5) 0.000 0.000
O1 0.020(3) 0.007(3) 0.017(3) -0.003(2) 0.000 0.000
O2 0.025(3) 0.013(3) 0.007(3) -0.001(2) 0.000 0.000
O3 0.0149(19) 0.016(2) 0.020(2) 0.0113(17) -0.0029(16) -0.0029(16)
O4 0.015(2) 0.009(3) 0.016(4) 0.002(2) 0.000 0.000
O5 0.010(2) 0.017(2) 0.011(2) 0.0033(16) 0.0020(14) 0.0024(17)
O6 0.009(2) 0.013(2) 0.021(2) 0.0033(17) -0.0039(16) -0.0054(15)
C1 0.009(3) 0.007(4) 0.012(5) 0.000(3) 0.000 0.000
C2 0.009(3) 0.017(3) 0.006(3) -0.006(2) 0.002(2) 0.000(2)
Na1 0.0140(15) 0.0138(18) 0.0167(17) 0.0029(14) 0.000 0.000
Na2 0.0116(11) 0.0067(13) 0.0064(11) 0.002(3) 0.000 0.000
Na3 0.0159(15) 0.0153(17) 0.0179(16) 0.000 0.000 -0.0014(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
Y1 O1 2.367(6) . ?
Y1 O4 2.381(6) . ?
Y1 O5 2.392(4) 3_455 ?
Y1 O5 2.392(4) . ?
Y1 O6 2.404(4) . ?
Y1 O6 2.404(4) 3_455 ?
Y1 O3 2.443(5) . ?
Y1 O3 2.443(5) 3_455 ?
Y1 O2 2.475(6) . ?
Y1 C2 2.823(6) . ?
Y1 C2 2.823(6) 3_455 ?
Y1 C1 2.845(8) . ?
O1 C1 1.270(10) 5 ?
O2 C1 1.278(10) . ?
O3 C2 1.274(7) . ?
O4 C1 1.304(9) . ?
O5 C2 1.279(6) 6_465 ?
O6 C2 1.286(6) . ?
C1 O1 1.270(10) 5_544 ?
C2 O5 1.279(6) 6_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
O1 Y1 O4 154.66(19) . . ?
O1 Y1 O5 79.42(17) . 3_455 ?
O4 Y1 O5 79.65(14) . 3_455 ?
O1 Y1 O5 79.42(17) . . ?
O4 Y1 O5 79.65(15) . . ?
O5 Y1 O5 68.2(2) 3_455 . ?
O1 Y1 O6 79.29(16) . . ?
O4 Y1 O6 120.66(14) . . ?
O5 Y1 O6 158.70(14) 3_455 . ?
O5 Y1 O6 106.91(15) . . ?
O1 Y1 O6 79.29(16) . 3_455 ?
O4 Y1 O6 120.66(14) . 3_455 ?
O5 Y1 O6 106.91(15) 3_455 3_455 ?
O5 Y1 O6 158.70(14) . 3_455 ?
O6 Y1 O6 69.7(2) . 3_455 ?
O1 Y1 O3 105.35(10) . . ?
O4 Y1 O3 79.13(10) . . ?
O5 Y1 O3 132.90(13) 3_455 . ?
O5 Y1 O3 66.91(15) . . ?
O6 Y1 O3 53.67(13) . . ?
O6 Y1 O3 120.10(15) 3_455 . ?
O1 Y1 O3 105.35(10) . 3_455 ?
O4 Y1 O3 79.13(10) . 3_455 ?
O5 Y1 O3 66.91(15) 3_455 3_455 ?
O5 Y1 O3 132.90(13) . 3_455 ?
O6 Y1 O3 120.10(15) . 3_455 ?
O6 Y1 O3 53.67(13) 3_455 3_455 ?
O3 Y1 O3 146.3(2) . 3_455 ?
O1 Y1 O2 151.58(19) . . ?
O4 Y1 O2 53.76(18) . . ?
O5 Y1 O2 123.08(15) 3_455 . ?
O5 Y1 O2 123.08(15) . . ?
O6 Y1 O2 77.47(16) . . ?
O6 Y1 O2 77.47(16) 3_455 . ?
O3 Y1 O2 73.19(10) . . ?
O3 Y1 O2 73.19(10) 3_455 . ?
O1 Y1 C2 91.25(14) . . ?
O4 Y1 C2 101.24(13) . . ?
O5 Y1 C2 153.36(14) 3_455 . ?
O5 Y1 C2 85.66(17) . . ?
O6 Y1 C2 26.98(14) . . ?
O6 Y1 C2 95.59(17) 3_455 . ?
O3 Y1 C2 26.77(14) . . ?
O3 Y1 C2 139.68(16) 3_455 . ?
O2 Y1 C2 75.05(13) . . ?
O1 Y1 C2 91.25(14) . 3_455 ?
O4 Y1 C2 101.24(13) . 3_455 ?
O5 Y1 C2 85.66(17) 3_455 3_455 ?
O5 Y1 C2 153.36(14) . 3_455 ?
O6 Y1 C2 95.59(17) . 3_455 ?
O6 Y1 C2 26.98(14) 3_455 3_455 ?
O3 Y1 C2 139.68(16) . 3_455 ?
O3 Y1 C2 26.77(14) 3_455 3_455 ?
O2 Y1 C2 75.05(13) . 3_455 ?
C2 Y1 C2 119.7(2) . 3_455 ?
O1 Y1 C1 178.2(2) . . ?
O4 Y1 C1 27.10(19) . . ?
O5 Y1 C1 102.02(18) 3_455 . ?
O5 Y1 C1 102.02(18) . . ?
O6 Y1 C1 99.28(18) . . ?
O6 Y1 C1 99.28(18) 3_455 . ?
O3 Y1 C1 74.44(10) . . ?
O3 Y1 C1 74.44(10) 3_455 . ?
O2 Y1 C1 26.7(2) . . ?
C2 Y1 C1 87.87(15) . . ?
C2 Y1 C1 87.87(15) 3_455 . ?
C1 O1 Y1 178.8(5) 5 . ?
C1 O2 Y1 93.0(5) . . ?
C2 O3 Y1 93.5(3) . . ?
C1 O4 Y1 96.6(4) . . ?
C2 O5 Y1 131.3(4) 6_465 . ?
C2 O6 Y1 95.0(3) . . ?
O1 C1 O2 122.7(7) 5_544 . ?
O1 C1 O4 120.7(7) 5_544 . ?
O2 C1 O4 116.6(7) . . ?
O1 C1 Y1 177.0(6) 5_544 . ?
O2 C1 Y1 60.3(4) . . ?
O4 C1 Y1 56.3(4) . . ?
O3 C2 O5 121.8(5) . 6_464 ?
O3 C2 O6 117.5(5) . . ?
O5 C2 O6 120.6(5) 6_464 . ?
O3 C2 Y1 59.8(3) . . ?
O5 C2 Y1 172.2(4) 6_464 . ?
O6 C2 Y1 58.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.39
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.141

_database_code_depnum_ccdc_archive 'CCDC 975761'
