# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_mm381a
_database_code_depnum_ccdc_archive 'CCDC 1474445'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H28 N2 Na O16 Y'
_chemical_formula_weight         544.24

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'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   19.2891(14)
_cell_length_b                   35.214(3)
_cell_length_c                   12.0446(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8181.3(11)
_cell_formula_units_Z            16
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9958
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      n/a
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_F_000             4480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.955
_shelx_estimated_absorpt_T_min   0.649
_shelx_estimated_absorpt_T_max   0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6057
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'

_exptl_special_details           
; 
 Data collection is performed with three batch runs at phi = 0.00 deg 
 (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg 
 (650 frames). 
 Frame width = 0.30 deg in omega. 
 Data is merged, corrected for decay (if any), and treated with multi-scan 
 absorption corrections (if required). All symmetry-equivalent reflections 
 are merged for centrosymmetric data. 
 Friedel pairs are not merged for noncentrosymmetric data. 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13330
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.076
_diffrn_reflns_theta_max         28.420
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             4461
_reflns_number_gt                4233
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_max     0.964
_reflns_Friedel_fraction_full    0.966

_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       'APEX II, Bruker (2009)'
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'

_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1222P)²+273.1190P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.187(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4461
_refine_ls_number_parameters     275
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2010
_refine_ls_wR_factor_gt          0.1985
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.009
_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
Y1 Y 0.16806(4) 0.09462(2) -0.00376(10) 0.0115(2) Uani 1 1 d . . . . .
Na1 Na 0.1123(3) 0.11654(16) -0.3158(4) 0.0309(11) Uani 1 1 d D . . . .
O1 O 0.2779(4) 0.0828(2) -0.0771(6) 0.0163(14) Uani 1 1 d . . . . .
O2 O 0.3528(6) 0.0434(3) -0.1549(10) 0.046(3) Uani 1 1 d . . . . .
O3 O 0.1539(4) 0.0681(2) -0.1855(6) 0.0176(15) Uani 1 1 d . . . . .
O4 O 0.1445(6) 0.0181(3) -0.2990(7) 0.034(2) Uani 1 1 d . . . . .
O5 O 0.2337(4) 0.0862(2) 0.1589(6) 0.0151(14) Uani 1 1 d . . . . .
O6 O 0.2419(5) 0.0796(3) 0.3429(8) 0.029(2) Uani 1 1 d . . . . .
O7 O 0.0478(4) 0.0811(2) -0.0347(6) 0.0185(15) Uani 1 1 d . U . . .
O8 O -0.0600(4) 0.0727(3) 0.0197(7) 0.029(2) Uani 1 1 d . U . . .
O9 O 0.1199(4) 0.1429(2) -0.1245(6) 0.0170(15) Uani 1 1 d . . . . .
H9C H 0.1431 0.1668 -0.1184 0.025 Uiso 1 1 d R U . . .
H9D H 0.0800 0.1417 -0.0711 0.025 Uiso 1 1 d R U . . .
O10 O 0.2465(4) 0.1514(2) 0.0106(6) 0.0179(14) Uani 1 1 d . . . . .
H10A H 0.2128 0.1697 -0.0120 0.027 Uiso 1 1 d R U . . .
H10B H 0.2705 0.1600 0.0802 0.027 Uiso 1 1 d R U . . .
O11 O 0.1158(4) 0.1386(2) 0.1196(7) 0.0200(16) Uani 1 1 d . . . . .
H11A H 0.0666 0.1391 0.1105 0.030 Uiso 1 1 d R U . . .
H11B H 0.1355 0.1648 0.1111 0.030 Uiso 1 1 d R U . . .
O12 O 0.0633(5) -0.0406(3) -0.3558(7) 0.0267(18) Uani 1 1 d . . . . .
H12A H 0.0556 -0.0156 -0.3278 0.040 Uiso 1 1 d R U . . .
H12B H 0.0210 -0.0568 -0.3440 0.040 Uiso 1 1 d R U . . .
O13 O 0.1324(13) 0.0712(5) -0.4629(14) 0.053(3) Uani 0.65 1 d D . P A 1
H13A H 0.1137 0.0941 -0.4927 0.079 Uiso 0.65 1 d R U P A 1
H13B H 0.1807 0.0756 -0.4344 0.079 Uiso 0.65 1 d R U P A 1
O14 O 0.2292(9) 0.1395(5) -0.3383(17) 0.053(3) Uani 0.65 1 d D . P A 1
H14A H 0.2373 0.1494 -0.2656 0.079 Uiso 0.65 1 d R U P A 1
H14B H 0.2113 0.1600 -0.3887 0.079 Uiso 0.65 1 d R U P A 1
O13' O 0.098(2) 0.0648(8) -0.446(3) 0.053(3) Uani 0.35 1 d D . P A 2
H13C H 0.0681 0.0512 -0.4945 0.079 Uiso 0.35 1 d R U P A 2
H13D H 0.1202 0.0867 -0.4862 0.079 Uiso 0.35 1 d R U P A 2
O14' O 0.2248(14) 0.1248(11) -0.395(3) 0.053(3) Uani 0.35 1 d D . P A 2
H14C H 0.1997 0.1347 -0.4565 0.079 Uiso 0.35 1 d R U P A 2
H14D H 0.2622 0.1430 -0.3715 0.079 Uiso 0.35 1 d R U P A 2
O15 O 0.3479(11) 0.0987(4) -0.3179(14) 0.077(5) Uani 1 1 d . . . . .
H15A H 0.3217 0.0809 -0.2754 0.115 Uiso 1 1 d R U . . .
H15B H 0.3638 0.1203 -0.2697 0.115 Uiso 1 1 d R U . . .
O16 O -0.0169(12) 0.0250(7) -0.5822(19) 0.052(4) Uani 0.6 1 d . . P B 2
H16A H -0.0128 0.0286 -0.5039 0.077 Uiso 0.6 1 d R U P B 2
H16B H -0.0630 0.0345 -0.6091 0.077 Uiso 0.6 1 d R U P B 2
O17 O 0.0079(18) 0.0534(10) -0.548(3) 0.052(4) Uani 0.4 1 d . . P C 1
H17A H 0.0428 0.0416 -0.5036 0.077 Uiso 0.4 1 d R U P C 1
H17B H -0.0384 0.0412 -0.5338 0.077 Uiso 0.4 1 d R U P C 1
N1 N 0.1962(4) 0.0225(2) -0.0087(8) 0.0156(15) Uani 1 1 d . . . . .
N2 N 0.1025(5) 0.0565(3) 0.1542(7) 0.0147(16) Uani 1 1 d . . . . .
C1 C 0.1747(6) 0.0024(3) 0.0937(10) 0.019(2) Uani 1 1 d . . . . .
H1A H 0.2089 0.0074 0.1533 0.023 Uiso 1 1 calc R U . . .
H1B H 0.1739 -0.0253 0.0798 0.023 Uiso 1 1 calc R U . . .
C2 C 0.1045(6) 0.0152(3) 0.1308(9) 0.019(2) Uani 1 1 d . . . . .
H2A H 0.0702 0.0091 0.0723 0.023 Uiso 1 1 calc R U . . .
H2B H 0.0913 0.0011 0.1986 0.023 Uiso 1 1 calc R U . . .
C3 C 0.2713(6) 0.0177(3) -0.0291(11) 0.026(3) Uani 1 1 d . . . . .
H3A H 0.2787 -0.0059 -0.0720 0.031 Uiso 1 1 calc R U . . .
H3B H 0.2953 0.0148 0.0431 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3029(6) 0.0505(4) -0.0914(11) 0.026(2) Uani 1 1 d . . . . .
C5 C 0.1586(7) 0.0056(4) -0.1065(12) 0.027(3) Uani 1 1 d . . . . .
H5A H 0.1831 -0.0177 -0.1303 0.032 Uiso 1 1 calc R U . . .
H5B H 0.1113 -0.0018 -0.0830 0.032 Uiso 1 1 calc R U . . .
C6 C 0.1533(6) 0.0321(3) -0.2032(10) 0.020(2) Uani 1 1 d . . . . .
C7 C 0.1347(6) 0.0648(3) 0.2624(9) 0.022(2) Uani 1 1 d . . . . .
H7A H 0.1324 0.0416 0.3089 0.027 Uiso 1 1 calc R U . . .
H7B H 0.1072 0.0847 0.3000 0.027 Uiso 1 1 calc R U . . .
C8 C 0.2096(5) 0.0778(3) 0.2563(10) 0.0166(18) Uani 1 1 d . . . . .
C9 C 0.0292(5) 0.0682(4) 0.1545(9) 0.020(2) Uani 1 1 d . U . . .
H9A H 0.0240 0.0920 0.1974 0.024 Uiso 1 1 calc R U . . .
H9B H 0.0009 0.0483 0.1910 0.024 Uiso 1 1 calc R U . . .
C10 C 0.0033(5) 0.0743(3) 0.0369(9) 0.0156(18) Uani 1 1 d . U . . .


_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 2.333(7) . ?
Y1 O5 2.351(7) . ?
Y1 O11 2.371(8) . ?
Y1 O3 2.395(7) . ?
Y1 O7 2.397(8) . ?
Y1 O9 2.423(8) . ?
Y1 O10 2.513(8) . ?
Y1 N1 2.599(8) . ?
Y1 N2 2.649(9) . ?
Y1 Na1 3.986(5) . ?
Y1 Na1 4.057(5) 3 ?
Na1 O14' 2.39(2) . ?
Na1 O14 2.411(18) . ?
Na1 O13 2.416(17) . ?
Na1 O13' 2.42(2) . ?
Na1 O1 2.418(9) 11_454 ?
Na1 O3 2.454(9) . ?
Na1 O9 2.488(9) . ?
Na1 O10 2.496(9) 11_454 ?
Na1 Y1 4.057(5) 11_454 ?
O1 C4 1.246(15) . ?
O1 Na1 2.418(9) 3 ?
O2 C4 1.254(16) . ?
O3 C6 1.284(13) . ?
O4 C6 1.267(13) . ?
O5 C8 1.297(13) . ?
O6 C8 1.216(14) . ?
O7 C10 1.240(13) . ?
O8 C10 1.241(12) . ?
O10 Na1 2.496(9) 3 ?
N1 C3 1.479(14) . ?
N1 C1 1.480(14) . ?
N1 C5 1.505(17) . ?
N2 C7 1.472(13) . ?
N2 C9 1.473(13) . ?
N2 C2 1.484(14) . ?
C1 C2 1.494(17) . ?
C3 C4 1.508(18) . ?
C5 C6 1.497(18) . ?
C7 C8 1.516(14) . ?
C9 C10 1.517(14) . ?

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 O5 78.7(3) . . ?
O1 Y1 O11 137.7(3) . . ?
O5 Y1 O11 77.8(3) . . ?
O1 Y1 O3 71.8(3) . . ?
O5 Y1 O3 140.7(3) . . ?
O11 Y1 O3 141.1(3) . . ?
O1 Y1 O7 141.7(3) . . ?
O5 Y1 O7 128.7(3) . . ?
O11 Y1 O7 79.4(3) . . ?
O3 Y1 O7 70.7(3) . . ?
O1 Y1 O9 104.3(3) . . ?
O5 Y1 O9 142.7(3) . . ?
O11 Y1 O9 75.8(2) . . ?
O3 Y1 O9 71.4(3) . . ?
O7 Y1 O9 71.0(3) . . ?
O1 Y1 O10 67.7(3) . . ?
O5 Y1 O10 73.6(3) . . ?
O11 Y1 O10 72.2(3) . . ?
O3 Y1 O10 116.2(3) . . ?
O7 Y1 O10 138.7(3) . . ?
O9 Y1 O10 73.4(3) . . ?
O1 Y1 N1 68.1(3) . . ?
O5 Y1 N1 77.5(3) . . ?
O11 Y1 N1 137.8(3) . . ?
O3 Y1 N1 67.8(3) . . ?
O7 Y1 N1 90.2(3) . . ?
O9 Y1 N1 138.8(3) . . ?
O10 Y1 N1 130.8(3) . . ?
O1 Y1 N2 127.9(3) . . ?
O5 Y1 N2 66.1(3) . . ?
O11 Y1 N2 71.2(3) . . ?
O3 Y1 N2 113.9(3) . . ?
O7 Y1 N2 63.2(3) . . ?
O9 Y1 N2 127.1(3) . . ?
O10 Y1 N2 129.8(3) . . ?
N1 Y1 N2 67.7(3) . . ?
O1 Y1 Na1 85.6(2) . . ?
O5 Y1 Na1 162.9(2) . . ?
O11 Y1 Na1 110.5(2) . . ?
O3 Y1 Na1 35.2(2) . . ?
O7 Y1 Na1 68.3(2) . . ?
O9 Y1 Na1 36.3(2) . . ?
O10 Y1 Na1 94.2(2) . . ?
N1 Y1 Na1 103.0(2) . . ?
N2 Y1 Na1 130.3(2) . . ?
O1 Y1 Na1 32.0(2) . 3 ?
O5 Y1 Na1 72.5(2) . 3 ?
O11 Y1 Na1 106.7(2) . 3 ?
O3 Y1 Na1 93.9(2) . 3 ?
O7 Y1 Na1 158.7(2) . 3 ?
O9 Y1 Na1 90.4(2) . 3 ?
O10 Y1 Na1 35.77(19) . 3 ?
N1 Y1 Na1 97.6(2) . 3 ?
N2 Y1 Na1 138.0(2) . 3 ?
Na1 Y1 Na1 90.59(10) . 3 ?
O14 Na1 O13 89.4(8) . . ?
O14' Na1 O13' 86.3(15) . . ?
O14' Na1 O1 120.0(9) . 11_454 ?
O14 Na1 O1 112.1(5) . 11_454 ?
O13 Na1 O1 123.7(6) . 11_454 ?
O13' Na1 O1 116.4(10) . 11_454 ?
O14' Na1 O3 92.4(8) . . ?
O14 Na1 O3 89.9(5) . . ?
O13 Na1 O3 87.5(5) . . ?
O13' Na1 O3 85.8(9) . . ?
O1 Na1 O3 140.3(3) 11_454 . ?
O14' Na1 O9 105.6(11) . . ?
O14 Na1 O9 85.6(6) . . ?
O13 Na1 O9 156.3(6) . . ?
O13' Na1 O9 152.6(9) . . ?
O1 Na1 O9 79.4(3) 11_454 . ?
O3 Na1 O9 69.4(3) . . ?
O14' Na1 O10 172.2(10) . 11_454 ?
O14 Na1 O10 164.3(6) . 11_454 ?
O13 Na1 O10 104.3(7) . 11_454 ?
O13' Na1 O10 87.1(11) . 11_454 ?
O1 Na1 O10 66.8(3) 11_454 11_454 ?
O3 Na1 O10 83.2(3) . 11_454 ?
O9 Na1 O10 78.8(3) . 11_454 ?
O14' Na1 Y1 98.8(9) . . ?
O14 Na1 Y1 85.3(5) . . ?
O13 Na1 Y1 121.3(5) . . ?
O13' Na1 Y1 119.7(9) . . ?
O1 Na1 Y1 112.2(2) 11_454 . ?
O3 Na1 Y1 34.25(18) . . ?
O9 Na1 Y1 35.21(19) . . ?
O10 Na1 Y1 81.1(2) 11_454 . ?
O14' Na1 Y1 150.7(9) . 11_454 ?
O14 Na1 Y1 140.5(5) . 11_454 ?
O13 Na1 Y1 120.4(6) . 11_454 ?
O13' Na1 Y1 105.7(11) . 11_454 ?
O1 Na1 Y1 30.74(19) 11_454 11_454 ?
O3 Na1 Y1 114.7(3) . 11_454 ?
O9 Na1 Y1 76.0(2) . 11_454 ?
O10 Na1 Y1 36.05(19) 11_454 11_454 ?
Y1 Na1 Y1 98.10(11) . 11_454 ?
C4 O1 Y1 124.5(8) . . ?
C4 O1 Na1 114.9(7) . 3 ?
Y1 O1 Na1 117.3(3) . 3 ?
C6 O3 Y1 122.5(7) . . ?
C6 O3 Na1 125.2(7) . . ?
Y1 O3 Na1 110.5(3) . . ?
C8 O5 Y1 126.2(6) . . ?
C10 O7 Y1 126.9(7) . . ?
Y1 O9 Na1 108.5(3) . . ?
Na1 O10 Y1 108.2(3) 3 . ?
C3 N1 C1 111.0(9) . . ?
C3 N1 C5 107.3(9) . . ?
C1 N1 C5 109.2(8) . . ?
C3 N1 Y1 108.6(6) . . ?
C1 N1 Y1 112.9(7) . . ?
C5 N1 Y1 107.6(7) . . ?
C7 N2 C9 110.4(8) . . ?
C7 N2 C2 110.5(8) . . ?
C9 N2 C2 107.3(9) . . ?
C7 N2 Y1 109.6(6) . . ?
C9 N2 Y1 108.6(6) . . ?
C2 N2 Y1 110.4(6) . . ?
N1 C1 C2 111.0(9) . . ?
N2 C2 C1 112.1(9) . . ?
N1 C3 C4 113.0(9) . . ?
O1 C4 O2 124.3(13) . . ?
O1 C4 C3 118.3(11) . . ?
O2 C4 C3 117.4(12) . . ?
C6 C5 N1 113.3(10) . . ?
O4 C6 O3 122.5(11) . . ?
O4 C6 C5 118.3(10) . . ?
O3 C6 C5 119.0(10) . . ?
N2 C7 C8 114.7(9) . . ?
O6 C8 O5 125.5(9) . . ?
O6 C8 C7 117.5(10) . . ?
O5 C8 C7 117.0(9) . . ?
N2 C9 C10 110.7(8) . . ?
O7 C10 O8 125.1(10) . . ?
O7 C10 C9 116.7(9) . . ?
O8 C10 C9 118.2(9) . . ?

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
C3 N1 C1 C2 165.2(9) . . . . ?
C5 N1 C1 C2 -76.7(11) . . . . ?
Y1 N1 C1 C2 43.0(11) . . . . ?
C7 N2 C2 C1 -77.3(11) . . . . ?
C9 N2 C2 C1 162.2(9) . . . . ?
Y1 N2 C2 C1 44.0(10) . . . . ?
N1 C1 C2 N2 -59.7(12) . . . . ?
C1 N1 C3 C4 -151.3(10) . . . . ?
C5 N1 C3 C4 89.5(12) . . . . ?
Y1 N1 C3 C4 -26.6(11) . . . . ?
Y1 O1 C4 O2 161.1(11) . . . . ?
Na1 O1 C4 O2 -40.3(16) 3 . . . ?
Y1 O1 C4 C3 -18.7(15) . . . . ?
Na1 O1 C4 C3 139.9(9) 3 . . . ?
N1 C3 C4 O1 31.5(16) . . . . ?
N1 C3 C4 O2 -148.4(12) . . . . ?
C3 N1 C5 C6 -82.9(12) . . . . ?
C1 N1 C5 C6 156.8(10) . . . . ?
Y1 N1 C5 C6 33.9(12) . . . . ?
Y1 O3 C6 O4 178.6(10) . . . . ?
Na1 O3 C6 O4 15.2(17) . . . . ?
Y1 O3 C6 C5 2.7(15) . . . . ?
Na1 O3 C6 C5 -160.8(8) . . . . ?
N1 C5 C6 O4 156.9(11) . . . . ?
N1 C5 C6 O3 -27.0(16) . . . . ?
C9 N2 C7 C8 -143.6(10) . . . . ?
C2 N2 C7 C8 97.8(11) . . . . ?
Y1 N2 C7 C8 -24.0(11) . . . . ?
Y1 O5 C8 O6 -167.2(9) . . . . ?
Y1 O5 C8 C7 12.4(13) . . . . ?
N2 C7 C8 O6 -169.4(10) . . . . ?
N2 C7 C8 O5 11.0(14) . . . . ?
C7 N2 C9 C10 158.2(9) . . . . ?
C2 N2 C9 C10 -81.3(11) . . . . ?
Y1 N2 C9 C10 38.0(10) . . . . ?
Y1 O7 C10 O8 169.2(9) . . . . ?
Y1 O7 C10 C9 -9.6(14) . . . . ?
N2 C9 C10 O7 -22.7(15) . . . . ?
N2 C9 C10 O8 158.4(10) . . . . ?

_refine_diff_density_max         0.894
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.213

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1493009'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H28 Dy N2 Na O16'
_chemical_formula_weight         617.83

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'
Dy Dy -0.1892 4.4098 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

_cell_length_a                   35.4573(8)
_cell_length_b                   19.4184(4)
_cell_length_c                   12.0642(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8306.5(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9111
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_F_000             4912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    3.700
_shelx_estimated_absorpt_T_min   0.470
_shelx_estimated_absorpt_T_max   0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5128
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25322
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.069
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             5026
_reflns_number_gt                5014
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_max     0.948
_reflns_Friedel_fraction_full    0.974

_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       'APEX II, Bruker (2009)'
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0001P)²+1193.4126P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2263 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5026
_refine_ls_number_parameters     280
_refine_ls_number_restraints     382
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1361
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.021
_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_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
C1 C 0.0151(4) 0.8962(8) 0.5757(13) 0.019(3) Uani 1 1 d . U . . .
H1A H 0.0010 0.9099 0.5083 0.022 Uiso 1 1 calc R U . . .
H1B H 0.0092 0.9299 0.6348 0.022 Uiso 1 1 calc R U . . .
C2 C 0.0024(5) 0.8254(9) 0.6119(15) 0.018(3) Uani 1 1 d . U . . .
H2A H -0.0252 0.8256 0.6243 0.022 Uiso 1 1 calc R U . . .
H2B H 0.0081 0.7916 0.5527 0.022 Uiso 1 1 calc R U . . .
C3 C 0.0649(4) 0.8656(7) 0.4443(12) 0.016(3) Uani 1 1 d . U . . .
H3A H 0.0850 0.8927 0.4076 0.019 Uiso 1 1 calc R U . . .
H3B H 0.0422 0.8680 0.3968 0.019 Uiso 1 1 calc R U . . .
C4 C 0.0775(4) 0.7915(7) 0.4516(14) 0.015(2) Uani 1 1 d . U . . .
C5 C 0.0685(4) 0.9721(7) 0.5519(12) 0.014(2) Uani 1 1 d . U . . .
H5A H 0.0925 0.9765 0.5108 0.017 Uiso 1 1 calc R U . . .
H5B H 0.0493 1.0004 0.5135 0.017 Uiso 1 1 calc R U . . .
C6 C 0.0736(4) 0.9981(7) 0.6673(12) 0.015(3) Uani 1 1 d . U . . .
C7 C 0.0175(5) 0.7292(8) 0.7319(14) 0.023(3) Uani 1 1 d . U . . .
H7A H 0.0159 0.7067 0.6585 0.028 Uiso 1 1 calc R U . . .
H7B H -0.0064 0.7202 0.7717 0.028 Uiso 1 1 calc R U . . .
C8 C 0.0497(5) 0.6976(9) 0.7964(15) 0.023(3) Uani 1 1 d . U . . .
C9 C 0.0055(5) 0.8409(11) 0.8140(16) 0.025(4) Uani 1 1 d . U . . .
H9A H -0.0022 0.8878 0.7912 0.030 Uiso 1 1 calc R U . . .
H9B H -0.0174 0.8160 0.8385 0.030 Uiso 1 1 calc R U . . .
C10 C 0.0320(4) 0.8462(8) 0.9083(13) 0.015(3) Uani 1 1 d . U . . .
Dy1 Dy 0.09434(2) 0.83227(3) 0.70916(10) 0.01041(15) Uani 1 1 d . U . . .
N1 N 0.0562(4) 0.8979(6) 0.5519(10) 0.015(2) Uani 1 1 d . U . . .
N2 N 0.0220(3) 0.8044(6) 0.7162(13) 0.016(2) Uani 1 1 d . U . . .
Na1 Na 0.1335(2) 0.6381(4) 0.7693(6) 0.0279(15) Uani 1 1 d . U . . .
O1 O 0.0861(3) 0.7667(6) 0.5464(9) 0.015(2) Uani 1 1 d . U . . .
O2 O 0.0801(4) 0.7585(7) 0.3621(10) 0.027(3) Uani 1 1 d . U . . .
O3 O 0.0807(3) 0.9530(5) 0.7414(8) 0.016(2) Uani 1 1 d . U . . .
O4 O 0.0718(4) 1.0609(6) 0.6859(9) 0.024(3) Uani 1 1 d . U . . .
O5 O 0.0825(3) 0.7222(5) 0.7798(9) 0.018(2) Uani 1 1 d . U . . .
O6 O 0.0424(4) 0.6484(8) 0.8588(13) 0.039(3) Uani 1 1 d . U . . .
O7 O 0.0674(3) 0.8457(6) 0.8889(9) 0.017(2) Uani 1 1 d . U . . .
O8 O 0.0178(4) 0.8553(8) 1.0020(10) 0.029(3) Uani 1 1 d . U . . .
O9 O 0.1388(3) 0.8850(6) 0.5876(9) 0.017(2) Uani 1 1 d . U . . .
H9C H 0.1486 0.9234 0.5954 0.025 Uiso 1 1 d R U . . .
H9D H 0.1516 0.8633 0.5430 0.025 Uiso 1 1 d R U . . .
O10 O 0.1430(3) 0.8802(6) 0.8308(10) 0.017(2) Uani 1 1 d . U . . .
H10A H 0.1492 0.9205 0.8206 0.025 Uiso 1 1 d R U . . .
H10B H 0.1629 0.8598 0.8418 0.025 Uiso 1 1 d R U . . .
O11 O 0.1513(3) 0.7539(5) 0.6946(9) 0.017(2) Uani 1 1 d . U . . .
H11C H 0.1568 0.7385 0.6334 0.025 Uiso 1 1 d R U . . .
H11D H 0.1704 0.7715 0.7205 0.025 Uiso 1 1 d R U . . .
O23 O 0.1771(10) 0.6129(18) 0.914(3) 0.037(5) Uani 0.5 1 d . U P A 1
H23A H 0.1750 0.5851 0.9657 0.055 Uiso 0.5 1 d R U P A 1
H23B H 0.1934 0.6094 0.8647 0.055 Uiso 0.5 1 d R U P A 1
O23' O 0.1837(11) 0.6412(18) 0.907(3) 0.037(5) Uani 0.5 1 d . U P A 2
H23C H 0.1944 0.6710 0.9426 0.055 Uiso 0.5 1 d R U P A 2
H23D H 0.2000 0.6281 0.8622 0.055 Uiso 0.5 1 d R U P A 2
O24 O 0.1085(11) 0.5202(18) 0.791(3) 0.051(6) Uani 0.5 1 d . U P A 1
H24A H 0.0854 0.5188 0.7883 0.077 Uiso 0.5 1 d R U P A 1
H24B H 0.1209 0.4848 0.7831 0.077 Uiso 0.5 1 d R U P A 1
O24' O 0.1213(11) 0.5335(18) 0.843(4) 0.051(6) Uani 0.5 1 d . U P A 2
H24C H 0.1253 0.4934 0.8225 0.077 Uiso 0.5 1 d R U P A 2
H24D H 0.1318 0.5275 0.9032 0.077 Uiso 0.5 1 d R U P A 2
O27 O 0.0255(9) 0.5165(16) 0.785(2) 0.037(5) Uani 0.5 1 d . . P B 1
H27A H 0.0027 0.5139 0.7746 0.056 Uiso 0.5 1 d R U P B 1
H27B H 0.0269 0.5562 0.8087 0.056 Uiso 0.5 1 d R U P B 1
O27' O 0.0500(9) 0.4917(16) 0.752(2) 0.037(5) Uani 0.5 1 d . . P C 2
H27C H 0.0577 0.4544 0.7263 0.056 Uiso 0.5 1 d R U P C 2
H27D H 0.0715 0.5035 0.7788 0.056 Uiso 0.5 1 d R U P C 2
O28 O 0.0988(5) 0.6517(12) 1.0196(18) 0.074(7) Uani 1 1 d . . . . .
H28A H 0.0822 0.6507 0.9723 0.112 Uiso 1 1 d R U . . .
H28B H 0.0911 0.6255 1.0678 0.112 Uiso 1 1 d R U . . .
O29 O 0.0410(3) 0.5628(6) 0.5597(10) 0.025(2) Uani 1 1 d . . . . .
H29A H 0.0233 0.5876 0.5422 0.037 Uiso 1 1 d R U . . .
H29B H 0.0366 0.5498 0.6229 0.037 Uiso 1 1 d R U . . .


_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
C1 N1 1.48(2) . ?
C1 C2 1.51(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.49(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.475(18) . ?
C3 C4 1.509(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O2 1.26(2) . ?
C4 O1 1.28(2) . ?
C5 C6 1.492(19) . ?
C5 N1 1.506(18) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.242(18) . ?
C6 O3 1.277(17) . ?
C7 N2 1.482(19) . ?
C7 C8 1.51(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O6 1.24(2) . ?
C8 O5 1.27(2) . ?
C9 C10 1.48(2) . ?
C9 N2 1.50(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O8 1.251(18) . ?
C10 O7 1.275(18) . ?
Dy1 O5 2.339(11) . ?
Dy1 O1 2.359(11) . ?
Dy1 O9 2.384(11) . ?
Dy1 O7 2.385(11) . ?
Dy1 O3 2.425(11) . ?
Dy1 O10 2.448(11) . ?
Dy1 O11 2.535(10) . ?
Dy1 N2 2.622(11) . ?
Dy1 N1 2.655(13) . ?
Dy1 Na1 3.974(7) 3 ?
Dy1 Na1 4.083(7) . ?
Na1 O24' 2.26(3) . ?
Na1 O23 2.38(3) . ?
Na1 O23' 2.43(4) . ?
Na1 O5 2.440(13) . ?
Na1 O10 2.466(14) 7_544 ?
Na1 O24 2.47(4) . ?
Na1 O7 2.487(13) 7_544 ?
Na1 O11 2.503(13) . ?
Na1 Dy1 3.974(7) 7_544 ?
Na1 H11C 2.6771 . ?
Na1 H23B 2.4771 . ?
Na1 H23D 2.6183 . ?
O7 Na1 2.487(13) 3 ?
O9 H9C 0.8285 . ?
O9 H9D 0.8199 . ?
O10 Na1 2.466(14) 3 ?
O10 H10A 0.8210 . ?
O10 H10B 0.8201 . ?
O11 H11C 0.8202 . ?
O11 H11D 0.8200 . ?
O23 H23A 0.8296 . ?
O23 H23B 0.8309 . ?
O23' H23C 0.8160 . ?
O23' H23D 0.8317 . ?
O24 H24A 0.8207 . ?
O24 H24B 0.8219 . ?
O24' H24C 0.8300 . ?
O24' H24D 0.8202 . ?
O27 H27A 0.8192 . ?
O27 H27B 0.8247 . ?
O27' H27C 0.8299 . ?
O27' H27D 0.8616 . ?
O28 H28A 0.8188 . ?
O28 H28B 0.8196 . ?
O29 H29A 0.8196 . ?
O29 H29B 0.8174 . ?

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
N1 C1 C2 111.5(13) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 110.7(13) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 C4 114.6(13) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
O2 C4 O1 124.0(12) . . ?
O2 C4 C3 117.2(14) . . ?
O1 C4 C3 118.8(13) . . ?
C6 C5 N1 111.1(12) . . ?
C6 C5 H5A 109.4 . . ?
N1 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
N1 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
O4 C6 O3 123.9(14) . . ?
O4 C6 C5 119.7(13) . . ?
O3 C6 C5 116.4(12) . . ?
N2 C7 C8 112.7(13) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
O6 C8 O5 124.9(17) . . ?
O6 C8 C7 117.9(15) . . ?
O5 C8 C7 117.2(14) . . ?
C10 C9 N2 113.0(15) . . ?
C10 C9 H9A 109.0 . . ?
N2 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
N2 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
O8 C10 O7 124.3(15) . . ?
O8 C10 C9 116.6(14) . . ?
O7 C10 C9 118.9(14) . . ?
O5 Dy1 O1 77.7(4) . . ?
O5 Dy1 O9 137.3(4) . . ?
O1 Dy1 O9 78.5(4) . . ?
O5 Dy1 O7 72.4(4) . . ?
O1 Dy1 O7 140.1(4) . . ?
O9 Dy1 O7 141.0(4) . . ?
O5 Dy1 O3 142.1(4) . . ?
O1 Dy1 O3 129.1(4) . . ?
O9 Dy1 O3 79.4(4) . . ?
O7 Dy1 O3 70.6(4) . . ?
O5 Dy1 O10 104.8(4) . . ?
O1 Dy1 O10 142.3(4) . . ?
O9 Dy1 O10 74.9(3) . . ?
O7 Dy1 O10 72.3(4) . . ?
O3 Dy1 O10 71.2(4) . . ?
O5 Dy1 O11 67.6(4) . . ?
O1 Dy1 O11 73.6(4) . . ?
O9 Dy1 O11 71.8(4) . . ?
O7 Dy1 O11 116.6(4) . . ?
O3 Dy1 O11 138.6(4) . . ?
O10 Dy1 O11 73.1(4) . . ?
O5 Dy1 N2 67.9(4) . . ?
O1 Dy1 N2 78.1(4) . . ?
O9 Dy1 N2 139.0(4) . . ?
O7 Dy1 N2 66.5(4) . . ?
O3 Dy1 N2 89.9(4) . . ?
O10 Dy1 N2 138.4(4) . . ?
O11 Dy1 N2 131.1(3) . . ?
O5 Dy1 N1 127.4(4) . . ?
O1 Dy1 N1 66.5(4) . . ?
O9 Dy1 N1 72.0(4) . . ?
O7 Dy1 N1 113.1(4) . . ?
O3 Dy1 N1 63.2(4) . . ?
O10 Dy1 N1 127.2(4) . . ?
O11 Dy1 N1 130.1(4) . . ?
N2 Dy1 N1 67.9(4) . . ?
O5 Dy1 Na1 86.7(3) . 3 ?
O1 Dy1 Na1 162.9(3) . 3 ?
O9 Dy1 Na1 109.4(3) . 3 ?
O7 Dy1 Na1 36.2(3) . 3 ?
O3 Dy1 Na1 68.0(3) . 3 ?
O10 Dy1 Na1 36.2(3) . 3 ?
O11 Dy1 Na1 94.1(3) . 3 ?
N2 Dy1 Na1 102.6(4) . 3 ?
N1 Dy1 Na1 130.0(3) . 3 ?
O5 Dy1 Na1 32.0(3) . . ?
O1 Dy1 Na1 72.0(3) . . ?
O9 Dy1 Na1 106.3(3) . . ?
O7 Dy1 Na1 94.4(3) . . ?
O3 Dy1 Na1 158.8(3) . . ?
O10 Dy1 Na1 90.3(3) . . ?
O11 Dy1 Na1 35.6(3) . . ?
N2 Dy1 Na1 97.9(3) . . ?
N1 Dy1 Na1 138.0(3) . . ?
Na1 Dy1 Na1 91.00(14) 3 . ?
C3 N1 C1 111.5(12) . . ?
C3 N1 C5 110.2(12) . . ?
C1 N1 C5 107.7(12) . . ?
C3 N1 Dy1 108.5(8) . . ?
C1 N1 Dy1 110.6(9) . . ?
C5 N1 Dy1 108.1(8) . . ?
C7 N2 C2 109.1(12) . . ?
C7 N2 C9 108.9(14) . . ?
C2 N2 C9 110.7(11) . . ?
C7 N2 Dy1 108.2(9) . . ?
C2 N2 Dy1 111.8(10) . . ?
C9 N2 Dy1 108.1(10) . . ?
O24' Na1 O23' 83.8(13) . . ?
O24' Na1 O5 116.0(11) . . ?
O23 Na1 O5 125.5(11) . . ?
O23' Na1 O5 119.3(10) . . ?
O24' Na1 O10 103.6(12) . 7_544 ?
O23 Na1 O10 155.6(11) . 7_544 ?
O23' Na1 O10 155.4(11) . 7_544 ?
O5 Na1 O10 78.9(4) . 7_544 ?
O23 Na1 O24 87.9(13) . . ?
O5 Na1 O24 110.3(10) . . ?
O10 Na1 O24 84.5(10) 7_544 . ?
O24' Na1 O7 95.0(11) . 7_544 ?
O23 Na1 O7 86.7(11) . 7_544 ?
O23' Na1 O7 85.9(10) . 7_544 ?
O5 Na1 O7 140.7(5) . 7_544 ?
O10 Na1 O7 70.3(4) 7_544 7_544 ?
O24 Na1 O7 90.8(10) . 7_544 ?
O24' Na1 O11 176.0(11) . . ?
O23 Na1 O11 106.6(9) . . ?
O23' Na1 O11 92.3(9) . . ?
O5 Na1 O11 66.7(4) . . ?
O10 Na1 O11 79.6(4) 7_544 . ?
O24 Na1 O11 164.2(10) . . ?
O7 Na1 O11 83.9(4) 7_544 . ?
O24' Na1 Dy1 99.5(11) . 7_544 ?
O23 Na1 Dy1 120.4(10) . 7_544 ?
O23' Na1 Dy1 120.3(10) . 7_544 ?
O5 Na1 Dy1 112.2(4) . 7_544 ?
O10 Na1 Dy1 35.9(3) 7_544 7_544 ?
O24 Na1 Dy1 85.4(10) . 7_544 ?
O7 Na1 Dy1 34.5(3) 7_544 7_544 ?
O11 Na1 Dy1 81.8(3) . 7_544 ?
O24' Na1 Dy1 146.6(10) . . ?
O23 Na1 Dy1 122.7(9) . . ?
O23' Na1 Dy1 110.3(9) . . ?
O5 Na1 Dy1 30.6(3) . . ?
O10 Na1 Dy1 76.3(3) 7_544 . ?
O24 Na1 Dy1 138.8(9) . . ?
O7 Na1 Dy1 115.6(4) 7_544 . ?
O11 Na1 Dy1 36.1(2) . . ?
Dy1 Na1 Dy1 98.74(16) 7_544 . ?
O24' Na1 H11C 162.8 . . ?
O23 Na1 H11C 113.5 . . ?
O23' Na1 H11C 100.1 . . ?
O5 Na1 H11C 76.9 . . ?
O10 Na1 H11C 66.3 7_544 . ?
O24 Na1 H11C 148.4 . . ?
O7 Na1 H11C 68.8 7_544 . ?
O11 Na1 H11C 17.8 . . ?
Dy1 Na1 H11C 64.0 7_544 . ?
Dy1 Na1 H11C 47.4 . . ?
O23 Na1 H23B 19.6 . . ?
O5 Na1 H23B 139.6 . . ?
O10 Na1 H23B 137.8 7_544 . ?
O24 Na1 H23B 92.8 . . ?
O7 Na1 H23B 67.7 7_544 . ?
O11 Na1 H23B 98.8 . . ?
Dy1 Na1 H23B 102.0 7_544 . ?
Dy1 Na1 H23B 125.6 . . ?
H11C Na1 H23B 100.7 . . ?
O24' Na1 H23D 86.4 . . ?
O23' Na1 H23D 18.5 . . ?
O5 Na1 H23D 134.0 . . ?
O10 Na1 H23D 137.2 7_544 . ?
O7 Na1 H23D 67.4 7_544 . ?
O11 Na1 H23D 89.6 . . ?
Dy1 Na1 H23D 101.8 7_544 . ?
Dy1 Na1 H23D 116.8 . . ?
H11C Na1 H23D 92.2 . . ?
C4 O1 Dy1 124.8(9) . . ?
C6 O3 Dy1 126.2(9) . . ?
C8 O5 Dy1 124.3(11) . . ?
C8 O5 Na1 115.8(10) . . ?
Dy1 O5 Na1 117.4(5) . . ?
C10 O7 Dy1 124.2(10) . . ?
C10 O7 Na1 124.8(10) . 3 ?
Dy1 O7 Na1 109.3(4) . 3 ?
Dy1 O9 H9C 126.4 . . ?
Dy1 O9 H9D 123.2 . . ?
H9C O9 H9D 107.9 . . ?
Dy1 O10 Na1 107.9(5) . 3 ?
Dy1 O10 H10A 117.4 . . ?
Na1 O10 H10A 100.4 3 . ?
Dy1 O10 H10B 121.3 . . ?
Na1 O10 H10B 102.0 3 . ?
H10A O10 H10B 104.7 . . ?
Na1 O11 Dy1 108.3(4) . . ?
Na1 O11 H11C 93.2 . . ?
Dy1 O11 H11C 117.9 . . ?
Na1 O11 H11D 116.5 . . ?
Dy1 O11 H11D 112.4 . . ?
H11C O11 H11D 107.5 . . ?
Na1 O23 H23A 128.8 . . ?
Na1 O23 H23B 86.8 . . ?
H23A O23 H23B 123.2 . . ?
Na1 O23' H23C 135.9 . . ?
Na1 O23' H23D 93.5 . . ?
H23C O23' H23D 103.5 . . ?
Na1 O24 H24A 112.6 . . ?
Na1 O24 H24B 124.7 . . ?
H24A O24 H24B 120.1 . . ?
Na1 O24' H24C 133.7 . . ?
Na1 O24' H24D 112.9 . . ?
H24C O24' H24D 93.3 . . ?
H27A O27 H27B 99.9 . . ?
H27C O27' H27D 94.8 . . ?
H28A O28 H28B 103.9 . . ?
H29A O29 H29B 106.0 . . ?

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
N1 C1 C2 N2 61.3(17) . . . . ?
N1 C3 C4 O2 170.1(14) . . . . ?
N1 C3 C4 O1 -12.3(19) . . . . ?
N1 C5 C6 O4 -157.0(15) . . . . ?
N1 C5 C6 O3 24.5(19) . . . . ?
N2 C7 C8 O6 146.1(17) . . . . ?
N2 C7 C8 O5 -36(2) . . . . ?
N2 C9 C10 O8 -158.0(16) . . . . ?
N2 C9 C10 O7 26(2) . . . . ?
C4 C3 N1 C1 -97.2(15) . . . . ?
C4 C3 N1 C5 143.1(12) . . . . ?
C4 C3 N1 Dy1 24.9(14) . . . . ?
C2 C1 N1 C3 76.4(15) . . . . ?
C2 C1 N1 C5 -162.6(13) . . . . ?
C2 C1 N1 Dy1 -44.6(14) . . . . ?
C6 C5 N1 C3 -158.6(12) . . . . ?
C6 C5 N1 C1 79.5(15) . . . . ?
C6 C5 N1 Dy1 -40.1(14) . . . . ?
C8 C7 N2 C2 151.9(14) . . . . ?
C8 C7 N2 C9 -87.2(16) . . . . ?
C8 C7 N2 Dy1 30.1(16) . . . . ?
C1 C2 N2 C7 -164.2(14) . . . . ?
C1 C2 N2 C9 76.0(16) . . . . ?
C1 C2 N2 Dy1 -44.6(15) . . . . ?
C10 C9 N2 C7 84.2(18) . . . . ?
C10 C9 N2 C2 -155.9(14) . . . . ?
C10 C9 N2 Dy1 -33.2(18) . . . . ?
O2 C4 O1 Dy1 166.0(12) . . . . ?
C3 C4 O1 Dy1 -11.5(18) . . . . ?
O4 C6 O3 Dy1 -169.9(12) . . . . ?
C5 C6 O3 Dy1 8(2) . . . . ?
O6 C8 O5 Dy1 -160.2(15) . . . . ?
C7 C8 O5 Dy1 22(2) . . . . ?
O6 C8 O5 Na1 39(2) . . . . ?
C7 C8 O5 Na1 -139.2(12) . . . . ?
O8 C10 O7 Dy1 -177.8(13) . . . . ?
C9 C10 O7 Dy1 -3(2) . . . . ?
O8 C10 O7 Na1 -15(2) . . . 3 ?
C9 C10 O7 Na1 160.7(12) . . . 3 ?

_refine_diff_density_max         2.381
_refine_diff_density_min         -2.810
_refine_diff_density_rms         0.224







# start Validation Reply Form
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Residual Density  0.58A From     Dy1      -2.66 eA-3  
RESPONSE: Residual density maximum 2.38 and minimum -2.81
are close in magnitude and located near Dy atom, at 0.71 A
and 0.65 A, respectively. However, the atom type for Dy 
is correct and these peaks do not have any chemical ground.
They are probably associated with a Fourier truncation.
;
# end Validation Reply Form
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1493010'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H28 Eu N2 Na O16'
_chemical_formula_weight         607.29

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'
Eu Eu -0.1578 3.6682 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

_cell_length_a                   35.4574(9)
_cell_length_b                   19.4184(4)
_cell_length_c                   12.0642(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8306.5(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      28.32

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_F_000             4864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.122
_shelx_estimated_absorpt_T_min   0.497
_shelx_estimated_absorpt_T_max   0.574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23062
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.069
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_point_group_measured_fraction_full 0.925
_reflns_number_total             4687
_reflns_number_gt                4670
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_max     0.801
_reflns_Friedel_fraction_full    0.843

_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       'APEX II, Bruker (2009)'
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0358P)²+17.6176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1940 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4687
_refine_ls_number_parameters     280
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0545
_refine_ls_wR_factor_gt          0.0545
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.004
_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
C1 C 0.01604(12) 0.8990(2) 0.5753(4) 0.0197(9) Uani 1 1 d . . . . .
H1A H 0.0020 0.9126 0.5099 0.024 Uiso 1 1 calc R U . . .
H1B H 0.0109 0.9325 0.6330 0.024 Uiso 1 1 calc R U . . .
C2 C 0.00240(14) 0.8293(2) 0.6130(4) 0.0183(10) Uani 1 1 d . . . . .
H2A H -0.0246 0.8312 0.6262 0.022 Uiso 1 1 calc R U . . .
H2B H 0.0070 0.7957 0.5551 0.022 Uiso 1 1 calc R U . . .
C3 C 0.06445(13) 0.8678(2) 0.4413(3) 0.0177(8) Uani 1 1 d . . . . .
H3A H 0.0838 0.8941 0.4033 0.021 Uiso 1 1 calc R U . . .
H3B H 0.0417 0.8700 0.3967 0.021 Uiso 1 1 calc R U . . .
C4 C 0.07718(10) 0.79331(19) 0.4480(4) 0.0134(7) Uani 1 1 d . . . . .
C5 C 0.06921(13) 0.9730(2) 0.5482(4) 0.0183(8) Uani 1 1 d . . . . .
H5A H 0.0504 1.0009 0.5107 0.022 Uiso 1 1 calc R U . . .
H5B H 0.0927 0.9770 0.5076 0.022 Uiso 1 1 calc R U . . .
C6 C 0.07471(12) 0.9996(2) 0.6652(4) 0.0173(8) Uani 1 1 d . . . . .
C7 C 0.01686(12) 0.7327(2) 0.7314(4) 0.0235(10) Uani 1 1 d . . . . .
H7A H 0.0160 0.7105 0.6595 0.028 Uiso 1 1 calc R U . . .
H7B H -0.0071 0.7244 0.7679 0.028 Uiso 1 1 calc R U . . .
C8 C 0.04815(13) 0.7007(2) 0.7998(4) 0.0197(8) Uani 1 1 d . . . . .
C9 C 0.00593(15) 0.8449(3) 0.8132(5) 0.0252(11) Uani 1 1 d . . . . .
H9A H -0.0171 0.8222 0.8363 0.030 Uiso 1 1 calc R U . . .
H9B H -0.0006 0.8914 0.7907 0.030 Uiso 1 1 calc R U . . .
C10 C 0.03250(11) 0.8487(2) 0.9108(4) 0.0158(8) Uani 1 1 d . . . . .
Eu1 Eu 0.09490(2) 0.83407(2) 0.70929(3) 0.00926(6) Uani 1 1 d . . . . .
N1 N 0.05689(11) 0.90035(18) 0.5491(3) 0.0145(7) Uani 1 1 d . . . . .
N2 N 0.02181(9) 0.80749(17) 0.7156(4) 0.0165(6) Uani 1 1 d . . . . .
Na1 Na 0.13278(6) 0.63919(11) 0.77214(18) 0.0273(4) Uani 1 1 d . . . . .
O1 O 0.08559(9) 0.76894(16) 0.5430(3) 0.0147(6) Uani 1 1 d . . . . .
O2 O 0.07873(11) 0.76126(18) 0.3591(3) 0.0240(7) Uani 1 1 d . . . . .
O3 O 0.08081(9) 0.95546(15) 0.7404(3) 0.0165(6) Uani 1 1 d . . . . .
O4 O 0.07357(12) 1.06293(17) 0.6805(3) 0.0289(8) Uani 1 1 d . . . . .
O5 O 0.08129(9) 0.72234(16) 0.7813(3) 0.0178(6) Uani 1 1 d . . . . .
O6 O 0.03996(12) 0.6532(2) 0.8642(4) 0.0383(10) Uani 1 1 d . . . . .
O7 O 0.06733(8) 0.84786(16) 0.8915(3) 0.0160(6) Uani 1 1 d . . . . .
O8 O 0.01794(9) 0.8547(2) 1.0043(3) 0.0280(8) Uani 1 1 d . . . . .
O9 O 0.13981(10) 0.88738(17) 0.5843(3) 0.0196(6) Uani 1 1 d . . . . .
H9C H 0.1496 0.9258 0.5920 0.029 Uiso 1 1 d R U . . .
H9D H 0.1526 0.8657 0.5397 0.029 Uiso 1 1 d R U . . .
O10 O 0.14373(8) 0.88372(16) 0.8315(3) 0.0146(6) Uani 1 1 d . . . . .
H10A H 0.1499 0.9240 0.8213 0.022 Uiso 1 1 d R U . . .
H10B H 0.1636 0.8633 0.8425 0.022 Uiso 1 1 d R U . . .
O11 O 0.15166(7) 0.75413(16) 0.6963(3) 0.0173(6) Uani 1 1 d . . . . .
H11C H 0.1571 0.7387 0.6351 0.026 Uiso 1 1 d R U . . .
H11D H 0.1707 0.7717 0.7222 0.026 Uiso 1 1 d R U . . .
O23 O 0.1787(15) 0.6085(17) 0.914(5) 0.054(5) Uani 0.5 1 d . U P A 1
H23A H 0.1765 0.5807 0.9657 0.081 Uiso 0.5 1 d R U P A 1
H23B H 0.1949 0.6050 0.8647 0.081 Uiso 0.5 1 d R U P A 1
O23' O 0.1799(16) 0.6282(17) 0.912(5) 0.054(5) Uani 0.5 1 d . U P A 2
H23C H 0.1906 0.6581 0.9480 0.081 Uiso 0.5 1 d R U P A 2
H23D H 0.1963 0.6152 0.8676 0.081 Uiso 0.5 1 d R U P A 2
O24 O 0.1099(6) 0.5158(10) 0.7750(19) 0.058(3) Uani 0.5 1 d . . P A 1
H24A H 0.0868 0.5144 0.7719 0.087 Uiso 0.5 1 d R U P A 1
H24B H 0.1223 0.4804 0.7666 0.087 Uiso 0.5 1 d R U P A 1
O24' O 0.1142(6) 0.5315(10) 0.8140(19) 0.058(3) Uani 0.5 1 d . . P A 2
H24C H 0.1182 0.4914 0.7931 0.087 Uiso 0.5 1 d R U P A 2
H24D H 0.1247 0.5255 0.8738 0.087 Uiso 0.5 1 d R U P A 2
O27 O 0.0305(4) 0.5225(5) 0.7857(9) 0.0551(19) Uani 0.5 1 d . . P B 1
H27A H 0.0077 0.5199 0.7755 0.083 Uiso 0.5 1 d R U P B 1
H27B H 0.0320 0.5622 0.8096 0.083 Uiso 0.5 1 d R U P B 1
O27' O 0.0441(4) 0.4896(5) 0.7483(9) 0.0551(19) Uani 0.5 1 d . . P C 2
H27C H 0.0517 0.4524 0.7230 0.083 Uiso 0.5 1 d R U P C 2
H27D H 0.0656 0.5014 0.7756 0.083 Uiso 0.5 1 d R U P C 2
O28 O 0.09957(15) 0.6484(4) 1.0084(7) 0.084(3) Uani 1 1 d . . . . .
H28A H 0.0830 0.6474 0.9611 0.126 Uiso 1 1 d R U . . .
H28B H 0.0919 0.6222 1.0565 0.126 Uiso 1 1 d R U . . .
O29 O 0.04122(9) 0.56392(19) 0.5631(3) 0.0253(7) Uani 1 1 d . . . . .
H29A H 0.0235 0.5887 0.5456 0.038 Uiso 1 1 d R U . . .
H29B H 0.0368 0.5509 0.6262 0.038 Uiso 1 1 d R U . . .


_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
C1 N1 1.483(6) . ?
C1 C2 1.508(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.478(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.471(5) . ?
C3 C4 1.517(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O2 1.241(5) . ?
C4 O1 1.275(5) . ?
C5 N1 1.478(5) . ?
C5 C6 1.515(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O4 1.244(5) . ?
C6 O3 1.267(5) . ?
C7 N2 1.475(5) . ?
C7 C8 1.516(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O6 1.240(6) . ?
C8 O5 1.268(5) . ?
C8 Eu1 3.264(4) . ?
C9 N2 1.494(7) . ?
C9 C10 1.510(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O8 1.246(5) . ?
C10 O7 1.257(5) . ?
Eu1 O5 2.387(3) . ?
Eu1 O1 2.394(3) . ?
Eu1 O7 2.421(3) . ?
Eu1 O9 2.425(3) . ?
Eu1 O3 2.439(3) . ?
Eu1 O10 2.470(3) . ?
Eu1 O11 2.546(3) . ?
Eu1 N2 2.644(3) . ?
Eu1 N1 2.685(4) . ?
Eu1 Na1 4.002(2) 3 ?
Eu1 Na1 4.086(2) . ?
Na1 O24' 2.25(2) . ?
Na1 O23' 2.39(5) . ?
Na1 O23 2.43(5) . ?
Na1 O5 2.440(4) . ?
Na1 O10 2.487(4) 7_544 ?
Na1 O7 2.501(4) 7_544 ?
Na1 O11 2.503(4) . ?
Na1 O24 2.530(18) . ?
Na1 Eu1 4.002(2) 7_544 ?
Na1 H23B 2.5582 . ?
Na1 H23D 2.5711 . ?
Na1 H24D 2.5422 . ?
O7 Na1 2.501(4) 3 ?
O9 H9C 0.8286 . ?
O9 H9D 0.8200 . ?
O10 Na1 2.487(4) 3 ?
O10 H10A 0.8210 . ?
O10 H10B 0.8201 . ?
O11 H11C 0.8202 . ?
O11 H11D 0.8200 . ?
O23 H23A 0.8296 . ?
O23 H23B 0.8309 . ?
O23' H23C 0.8160 . ?
O23' H23D 0.8317 . ?
O24 H24A 0.8207 . ?
O24 H24B 0.8219 . ?
O24' H24C 0.8300 . ?
O24' H24D 0.8202 . ?
O27 H27A 0.8192 . ?
O27 H27B 0.8247 . ?
O27' H27C 0.8299 . ?
O27' H27D 0.8616 . ?
O28 H28A 0.8188 . ?
O28 H28B 0.8196 . ?
O29 H29A 0.8195 . ?
O29 H29B 0.8173 . ?

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
N1 C1 C2 113.2(4) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.8 . . ?
N2 C2 C1 111.2(4) . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 114.6(3) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
O2 C4 O1 125.5(3) . . ?
O2 C4 C3 116.4(4) . . ?
O1 C4 C3 118.1(4) . . ?
N1 C5 C6 110.9(4) . . ?
N1 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 O3 124.6(4) . . ?
O4 C6 C5 118.0(4) . . ?
O3 C6 C5 117.3(4) . . ?
N2 C7 C8 112.8(3) . . ?
N2 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
O6 C8 O5 125.0(5) . . ?
O6 C8 C7 118.3(4) . . ?
O5 C8 C7 116.5(4) . . ?
O6 C8 Eu1 156.7(4) . . ?
O5 C8 Eu1 37.5(2) . . ?
C7 C8 Eu1 82.2(2) . . ?
N2 C9 C10 113.7(4) . . ?
N2 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N2 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
O8 C10 O7 125.1(4) . . ?
O8 C10 C9 116.9(4) . . ?
O7 C10 C9 117.9(4) . . ?
O5 Eu1 O1 78.29(11) . . ?
O5 Eu1 O7 71.83(11) . . ?
O1 Eu1 O7 139.79(11) . . ?
O5 Eu1 O9 138.35(11) . . ?
O1 Eu1 O9 78.16(11) . . ?
O7 Eu1 O9 141.51(11) . . ?
O5 Eu1 O3 141.38(11) . . ?
O1 Eu1 O3 127.68(10) . . ?
O7 Eu1 O3 70.77(10) . . ?
O9 Eu1 O3 79.50(11) . . ?
O5 Eu1 O10 106.22(11) . . ?
O1 Eu1 O10 143.40(11) . . ?
O7 Eu1 O10 72.42(10) . . ?
O9 Eu1 O10 75.18(10) . . ?
O3 Eu1 O10 71.00(10) . . ?
O5 Eu1 O11 68.16(10) . . ?
O1 Eu1 O11 74.66(11) . . ?
O7 Eu1 O11 116.25(11) . . ?
O9 Eu1 O11 72.73(11) . . ?
O3 Eu1 O11 139.52(10) . . ?
O10 Eu1 O11 73.77(10) . . ?
O5 Eu1 N2 67.27(11) . . ?
O1 Eu1 N2 77.64(12) . . ?
O7 Eu1 N2 66.39(12) . . ?
O9 Eu1 N2 138.16(13) . . ?
O3 Eu1 N2 89.05(10) . . ?
O10 Eu1 N2 138.27(12) . . ?
O11 Eu1 N2 131.11(10) . . ?
O5 Eu1 N1 126.61(11) . . ?
O1 Eu1 N1 65.22(11) . . ?
O7 Eu1 N1 113.46(11) . . ?
O9 Eu1 N1 71.18(12) . . ?
O3 Eu1 N1 62.91(10) . . ?
O10 Eu1 N1 126.47(11) . . ?
O11 Eu1 N1 130.15(11) . . ?
N2 Eu1 N1 67.81(12) . . ?
O5 Eu1 C8 18.88(11) . . ?
O1 Eu1 C8 77.93(11) . . ?
O7 Eu1 C8 65.10(11) . . ?
O9 Eu1 C8 151.68(11) . . ?
O3 Eu1 C8 127.72(11) . . ?
O10 Eu1 C8 117.80(11) . . ?
O11 Eu1 C8 86.45(11) . . ?
N2 Eu1 C8 48.50(11) . . ?
N1 Eu1 C8 111.49(12) . . ?
O5 Eu1 Na1 86.54(9) . 3 ?
O1 Eu1 Na1 163.47(8) . 3 ?
O7 Eu1 Na1 36.28(8) . 3 ?
O9 Eu1 Na1 110.03(9) . 3 ?
O3 Eu1 Na1 68.71(8) . 3 ?
O10 Eu1 Na1 36.31(8) . 3 ?
O11 Eu1 Na1 93.70(9) . 3 ?
N2 Eu1 Na1 102.64(10) . 3 ?
N1 Eu1 Na1 130.54(8) . 3 ?
C8 Eu1 Na1 89.85(9) . 3 ?
O5 Eu1 Na1 32.54(8) . . ?
O1 Eu1 Na1 73.24(8) . . ?
O7 Eu1 Na1 93.82(8) . . ?
O9 Eu1 Na1 107.15(9) . . ?
O3 Eu1 Na1 159.05(8) . . ?
O10 Eu1 Na1 91.17(8) . . ?
O11 Eu1 Na1 35.62(8) . . ?
N2 Eu1 Na1 97.81(8) . . ?
N1 Eu1 Na1 137.94(8) . . ?
C8 Eu1 Na1 50.93(9) . . ?
Na1 Eu1 Na1 90.44(4) 3 . ?
C3 N1 C5 110.5(4) . . ?
C3 N1 C1 111.0(3) . . ?
C5 N1 C1 107.9(3) . . ?
C3 N1 Eu1 109.8(2) . . ?
C5 N1 Eu1 108.3(3) . . ?
C1 N1 Eu1 109.2(3) . . ?
C7 N2 C2 109.6(4) . . ?
C7 N2 C9 109.4(4) . . ?
C2 N2 C9 110.1(3) . . ?
C7 N2 Eu1 108.2(2) . . ?
C2 N2 Eu1 112.1(3) . . ?
C9 N2 Eu1 107.3(3) . . ?
O24' Na1 O23' 87.9(11) . . ?
O24' Na1 O5 112.7(6) . . ?
O23' Na1 O5 123.4(11) . . ?
O23 Na1 O5 129.0(11) . . ?
O24' Na1 O10 93.3(5) . 7_544 ?
O23' Na1 O10 156.3(13) . 7_544 ?
O23 Na1 O10 153.1(12) . 7_544 ?
O5 Na1 O10 77.73(12) . 7_544 ?
O24' Na1 O7 92.9(6) . 7_544 ?
O23' Na1 O7 85.6(13) . 7_544 ?
O23 Na1 O7 83.8(13) . 7_544 ?
O5 Na1 O7 140.37(14) . 7_544 ?
O10 Na1 O7 70.79(11) 7_544 7_544 ?
O24' Na1 O11 171.5(5) . . ?
O23' Na1 O11 98.7(9) . . ?
O23 Na1 O11 107.2(10) . . ?
O5 Na1 O11 68.07(11) . . ?
O10 Na1 O11 78.54(12) 7_544 . ?
O7 Na1 O11 82.35(12) 7_544 . ?
O23 Na1 O24 88.5(10) . . ?
O5 Na1 O24 112.7(6) . . ?
O10 Na1 O24 81.4(5) 7_544 . ?
O7 Na1 O24 86.1(5) 7_544 . ?
O11 Na1 O24 159.3(5) . . ?
O24' Na1 Eu1 91.2(5) . 7_544 ?
O23' Na1 Eu1 120.4(13) . 7_544 ?
O23 Na1 Eu1 117.7(12) . 7_544 ?
O5 Na1 Eu1 111.58(10) . 7_544 ?
O10 Na1 Eu1 36.01(8) 7_544 7_544 ?
O7 Na1 Eu1 34.94(8) 7_544 7_544 ?
O11 Na1 Eu1 80.86(10) . 7_544 ?
O24 Na1 Eu1 79.8(5) . 7_544 ?
O24' Na1 Eu1 143.8(6) . . ?
O23' Na1 Eu1 116.4(8) . . ?
O23 Na1 Eu1 125.2(9) . . ?
O5 Na1 Eu1 31.75(8) . . ?
O10 Na1 Eu1 75.15(8) 7_544 . ?
O7 Na1 Eu1 114.37(10) 7_544 . ?
O11 Na1 Eu1 36.33(7) . . ?
O24 Na1 Eu1 140.7(6) . . ?
Eu1 Na1 Eu1 97.91(5) 7_544 . ?
O23 Na1 H23B 18.9 . . ?
O5 Na1 H23B 142.8 . . ?
O10 Na1 H23B 135.9 7_544 . ?
O7 Na1 H23B 65.3 7_544 . ?
O11 Na1 H23B 99.2 . . ?
O24 Na1 H23B 91.4 . . ?
Eu1 Na1 H23B 99.9 7_544 . ?
Eu1 Na1 H23B 127.2 . . ?
O24' Na1 H23D 89.3 . . ?
O23' Na1 H23D 18.8 . . ?
O5 Na1 H23D 139.0 . . ?
O10 Na1 H23D 137.5 7_544 . ?
O7 Na1 H23D 66.7 7_544 . ?
O11 Na1 H23D 95.2 . . ?
Eu1 Na1 H23D 101.6 7_544 . ?
Eu1 Na1 H23D 122.6 . . ?
O24' Na1 H24D 18.4 . . ?
O23' Na1 H24D 70.1 . . ?
O5 Na1 H24D 117.9 . . ?
O10 Na1 H24D 111.5 7_544 . ?
O7 Na1 H24D 96.0 7_544 . ?
O11 Na1 H24D 168.8 . . ?
Eu1 Na1 H24D 104.2 7_544 . ?
Eu1 Na1 H24D 149.0 . . ?
H23D Na1 H24D 74.0 . . ?
C4 O1 Eu1 126.1(2) . . ?
C6 O3 Eu1 125.4(3) . . ?
C8 O5 Eu1 123.6(3) . . ?
C8 O5 Na1 118.8(3) . . ?
Eu1 O5 Na1 115.71(13) . . ?
C10 O7 Eu1 124.5(3) . . ?
C10 O7 Na1 125.1(3) . 3 ?
Eu1 O7 Na1 108.78(12) . 3 ?
Eu1 O9 H9C 126.1 . . ?
Eu1 O9 H9D 123.4 . . ?
H9C O9 H9D 107.9 . . ?
Eu1 O10 Na1 107.68(12) . 3 ?
Eu1 O10 H10A 118.0 . . ?
Na1 O10 H10A 101.4 3 . ?
Eu1 O10 H10B 120.8 . . ?
Na1 O10 H10B 101.3 3 . ?
H10A O10 H10B 104.7 . . ?
Na1 O11 Eu1 108.05(11) . . ?
Na1 O11 H11C 93.9 . . ?
Eu1 O11 H11C 117.6 . . ?
Na1 O11 H11D 117.0 . . ?
Eu1 O11 H11D 112.0 . . ?
H11C O11 H11D 107.5 . . ?
Na1 O23 H23A 128.9 . . ?
Na1 O23 H23B 89.0 . . ?
H23A O23 H23B 123.2 . . ?
Na1 O23' H23C 129.6 . . ?
Na1 O23' H23D 93.2 . . ?
H23C O23' H23D 103.5 . . ?
Na1 O24 H24A 110.5 . . ?
Na1 O24 H24B 128.2 . . ?
H24A O24 H24B 120.1 . . ?
Na1 O24' H24C 139.0 . . ?
Na1 O24' H24D 101.4 . . ?
H24C O24' H24D 93.3 . . ?
H27A O27 H27B 99.9 . . ?
H27C O27' H27D 94.8 . . ?
H28A O28 H28B 103.9 . . ?
H29A O29 H29B 106.0 . . ?

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
N1 C1 C2 N2 61.2(5) . . . . ?
N1 C3 C4 O2 170.2(4) . . . . ?
N1 C3 C4 O1 -10.3(6) . . . . ?
N1 C5 C6 O4 -158.3(4) . . . . ?
N1 C5 C6 O3 22.9(5) . . . . ?
N2 C7 C8 O6 144.0(5) . . . . ?
N2 C7 C8 O5 -39.9(6) . . . . ?
N2 C7 C8 Eu1 -24.3(3) . . . . ?
N2 C9 C10 O8 -153.9(5) . . . . ?
N2 C9 C10 O7 28.5(7) . . . . ?
C4 C3 N1 C5 142.7(4) . . . . ?
C4 C3 N1 C1 -97.7(4) . . . . ?
C4 C3 N1 Eu1 23.2(4) . . . . ?
C6 C5 N1 C3 -159.9(3) . . . . ?
C6 C5 N1 C1 78.6(4) . . . . ?
C6 C5 N1 Eu1 -39.5(4) . . . . ?
C2 C1 N1 C3 76.4(5) . . . . ?
C2 C1 N1 C5 -162.3(4) . . . . ?
C2 C1 N1 Eu1 -44.8(4) . . . . ?
C8 C7 N2 C2 154.5(4) . . . . ?
C8 C7 N2 C9 -84.6(5) . . . . ?
C8 C7 N2 Eu1 32.0(5) . . . . ?
C1 C2 N2 C7 -162.9(4) . . . . ?
C1 C2 N2 C9 76.6(5) . . . . ?
C1 C2 N2 Eu1 -42.8(4) . . . . ?
C10 C9 N2 C7 82.4(5) . . . . ?
C10 C9 N2 C2 -157.0(4) . . . . ?
C10 C9 N2 Eu1 -34.8(5) . . . . ?
O2 C4 O1 Eu1 166.9(3) . . . . ?
C3 C4 O1 Eu1 -12.6(5) . . . . ?
O4 C6 O3 Eu1 -167.8(4) . . . . ?
C5 C6 O3 Eu1 10.9(5) . . . . ?
O6 C8 O5 Eu1 -158.2(4) . . . . ?
C7 C8 O5 Eu1 25.9(5) . . . . ?
O6 C8 O5 Na1 38.2(7) . . . . ?
C7 C8 O5 Na1 -137.6(3) . . . . ?
Eu1 C8 O5 Na1 -163.6(5) . . . . ?
O8 C10 O7 Eu1 178.9(4) . . . . ?
C9 C10 O7 Eu1 -3.8(6) . . . . ?
O8 C10 O7 Na1 -17.5(7) . . . 3 ?
C9 C10 O7 Na1 159.8(4) . . . 3 ?

_refine_diff_density_max         0.513
_refine_diff_density_min         -3.019
_refine_diff_density_rms         0.148




# start Validation Reply Form

_vrf_PLAT974_shelx               
;
PROBLEM: Check Calcd Negative Residual Density on     Eu1      -3.01 eA-3  
RESPONSE: Residual density maximum -3.02 is located at
Eu1 atom site (at 0.03A). This has no chemical
ground, the atom type for Eu is correct. The problem 
may rely in an unaccounted twinning, although twinrotmat
routine hasn't detected the latter.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1493011'
_audit_update_record             
;
2016-07-13 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H28 N2 Na O16 Tb'
_chemical_formula_weight         614.25

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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

_cell_length_a                   35.306(3)
_cell_length_b                   19.2934(15)
_cell_length_c                   12.0542(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8211.0(12)
_cell_formula_units_Z            16
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9908
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_F_000             4896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    3.548
_shelx_estimated_absorpt_T_min   0.552
_shelx_estimated_absorpt_T_max   0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22910
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.074
_diffrn_reflns_theta_max         28.375
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5106
_reflns_number_gt                5071
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

_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       'APEX II, Bruker (2009)'
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+202.5643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5106
_refine_ls_number_parameters     281
_refine_ls_number_restraints     142
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0846
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_restrained_S_all      1.281
_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_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
Tb1 Tb 0.09459(2) 0.83249(2) 0.70912(6) 0.00820(9) Uani 1 1 d . . . . .
Na1 Na 0.13345(12) 0.6381(2) 0.7705(3) 0.0264(9) Uani 1 1 d . . . . .
C1 C 0.0157(3) 0.8960(5) 0.5755(7) 0.0171(16) Uani 1 1 d . U . . .
H1A H 0.0013 0.9092 0.5083 0.021 Uiso 1 1 calc R U . . .
H1B H 0.0099 0.9304 0.6341 0.021 Uiso 1 1 calc R U . . .
C2 C 0.0025(3) 0.8253(5) 0.6137(8) 0.0150(18) Uani 1 1 d . U . . .
H2A H -0.0251 0.8264 0.6270 0.018 Uiso 1 1 calc R U . . .
H2B H 0.0076 0.7908 0.5547 0.018 Uiso 1 1 calc R U . . .
C3 C 0.0645(3) 0.8662(4) 0.4426(7) 0.0154(16) Uani 1 1 d . U . . .
H3A H 0.0842 0.8935 0.4040 0.019 Uiso 1 1 calc R U . . .
H3B H 0.0413 0.8680 0.3968 0.019 Uiso 1 1 calc R U . . .
C4 C 0.0775(2) 0.7922(4) 0.4500(8) 0.0130(14) Uani 1 1 d . U . . .
C5 C 0.0683(3) 0.9718(4) 0.5500(7) 0.0152(16) Uani 1 1 d . U . . .
H5A H 0.0488 1.0000 0.5123 0.018 Uiso 1 1 calc R U . . .
H5B H 0.0923 0.9767 0.5081 0.018 Uiso 1 1 calc R U . . .
C6 C 0.0738(3) 0.9981(4) 0.6664(7) 0.0139(15) Uani 1 1 d . U . . .
C7 C 0.0176(3) 0.7288(5) 0.7318(8) 0.0202(19) Uani 1 1 d . U . . .
H7A H 0.0166 0.7058 0.6584 0.024 Uiso 1 1 calc R U . . .
H7B H -0.0067 0.7197 0.7701 0.024 Uiso 1 1 calc R U . . .
C8 C 0.0495(3) 0.6981(5) 0.7987(7) 0.0178(17) Uani 1 1 d . U . . .
C9 C 0.0057(3) 0.8417(7) 0.8149(9) 0.025(2) Uani 1 1 d . U . . .
H9A H -0.0018 0.8891 0.7925 0.030 Uiso 1 1 calc R U . . .
H9B H -0.0173 0.8170 0.8397 0.030 Uiso 1 1 calc R U . . .
C10 C 0.0326(2) 0.8466(5) 0.9095(7) 0.0140(15) Uani 1 1 d . U . . .
N1 N 0.0566(2) 0.8987(4) 0.5503(6) 0.0110(13) Uani 1 1 d . U . . .
N2 N 0.02196(17) 0.8046(4) 0.7154(7) 0.0137(12) Uani 1 1 d . U . . .
O1 O 0.08614(18) 0.7674(3) 0.5448(5) 0.0133(12) Uani 1 1 d . U . . .
O2 O 0.0794(2) 0.7590(4) 0.3608(6) 0.0233(16) Uani 1 1 d . U . . .
O3 O 0.08083(19) 0.9532(3) 0.7413(5) 0.0150(12) Uani 1 1 d . U . . .
O4 O 0.0721(2) 1.0617(3) 0.6844(5) 0.0246(16) Uani 1 1 d . U . . .
O5 O 0.08233(18) 0.7217(3) 0.7818(5) 0.0155(12) Uani 1 1 d . U . . .
O6 O 0.0423(2) 0.6486(5) 0.8616(7) 0.037(2) Uani 1 1 d . U . . .
O7 O 0.06750(17) 0.8466(3) 0.8905(5) 0.0138(12) Uani 1 1 d . U . . .
O8 O 0.0182(2) 0.8546(5) 1.0038(6) 0.0266(17) Uani 1 1 d . U . . .
O9 O 0.1386(2) 0.8858(4) 0.5854(5) 0.0178(14) Uani 1 1 d . . . . .
H9C H 0.1484 0.9242 0.5932 0.027 Uiso 1 1 d R U . . .
H9D H 0.1514 0.8641 0.5408 0.027 Uiso 1 1 d R U . . .
O10 O 0.14304(18) 0.8808(3) 0.8306(5) 0.0121(12) Uani 1 1 d . . . . .
H10A H 0.1492 0.9211 0.8204 0.018 Uiso 1 1 d R U . . .
H10B H 0.1629 0.8605 0.8416 0.018 Uiso 1 1 d R U . . .
O11 O 0.15139(16) 0.7540(3) 0.6950(5) 0.0157(12) Uani 1 1 d . . . . .
H11C H 0.1568 0.7386 0.6337 0.024 Uiso 1 1 d R U . . .
H11D H 0.1705 0.7716 0.7208 0.024 Uiso 1 1 d R U . . .
O23 O 0.178(2) 0.613(3) 0.918(5) 0.047(9) Uani 0.5 1 d . U P A 1
H23A H 0.1755 0.5847 0.9697 0.071 Uiso 0.5 1 d R U P A 1
H23B H 0.1939 0.6091 0.8687 0.071 Uiso 0.5 1 d R U P A 1
O23' O 0.182(2) 0.636(3) 0.908(5) 0.047(9) Uani 0.5 1 d . U P A 2
H23C H 0.1923 0.6660 0.9438 0.071 Uiso 0.5 1 d R U P A 2
H23D H 0.1980 0.6232 0.8633 0.071 Uiso 0.5 1 d R U P A 2
O24 O 0.1098(8) 0.5200(13) 0.788(2) 0.052(5) Uani 0.5 1 d . . P A 1
H24A H 0.0867 0.5186 0.7845 0.078 Uiso 0.5 1 d R U P A 1
H24B H 0.1222 0.4846 0.7793 0.078 Uiso 0.5 1 d R U P A 1
O24' O 0.1197(8) 0.5336(14) 0.839(2) 0.052(5) Uani 0.5 1 d . . P A 2
H24C H 0.1236 0.4935 0.8179 0.078 Uiso 0.5 1 d R U P A 2
H24D H 0.1302 0.5275 0.8987 0.078 Uiso 0.5 1 d R U P A 2
O27 O 0.0262(6) 0.5188(10) 0.7846(16) 0.041(3) Uani 0.5 1 d . . P B 1
H27A H 0.0034 0.5162 0.7744 0.062 Uiso 0.5 1 d R U P B 1
H27B H 0.0277 0.5585 0.8085 0.062 Uiso 0.5 1 d R U P B 1
O27' O 0.0497(6) 0.4918(10) 0.7526(15) 0.041(3) Uani 0.5 1 d . . P C 2
H27C H 0.0574 0.4546 0.7274 0.062 Uiso 0.5 1 d R U P C 2
H27D H 0.0712 0.5036 0.7799 0.062 Uiso 0.5 1 d R U P C 2
O28 O 0.0994(3) 0.6500(7) 1.0185(10) 0.067(4) Uani 1 1 d . . . . .
H28A H 0.0828 0.6490 0.9712 0.101 Uiso 1 1 d R U . . .
H28B H 0.0917 0.6237 1.0666 0.101 Uiso 1 1 d R U . . .
O29 O 0.0410(2) 0.5634(4) 0.5629(6) 0.0239(15) Uani 1 1 d . . . . .
H29A H 0.0232 0.5882 0.5453 0.036 Uiso 1 1 d R U . . .
H29B H 0.0366 0.5504 0.6260 0.036 Uiso 1 1 d R U . . .


_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
Tb1 O5 2.351(6) . ?
Tb1 O1 2.365(6) . ?
Tb1 O9 2.386(7) . ?
Tb1 O7 2.402(6) . ?
Tb1 O3 2.411(6) . ?
Tb1 O10 2.437(6) . ?
Tb1 O11 2.519(6) . ?
Tb1 N2 2.621(6) . ?
Tb1 N1 2.664(7) . ?
Tb1 Na1 3.980(4) 3 ?
Tb1 Na1 4.062(4) . ?
Na1 O24' 2.23(3) . ?
Na1 O23' 2.37(7) . ?
Na1 O23 2.41(7) . ?
Na1 O5 2.424(7) . ?
Na1 O24 2.44(3) . ?
Na1 O7 2.469(7) 7_544 ?
Na1 O10 2.477(8) 7_544 ?
Na1 O11 2.496(8) . ?
Na1 Tb1 3.980(4) 7_544 ?
Na1 H11C 2.6758 . ?
Na1 H23B 2.5029 . ?
Na1 H23D 2.5543 . ?
Na1 H24D 2.6361 . ?
C1 N1 1.479(12) . ?
C1 C2 1.511(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.461(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.469(10) . ?
C3 C4 1.502(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O2 1.253(11) . ?
C4 O1 1.275(11) . ?
C5 N1 1.468(11) . ?
C5 C6 1.504(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.248(11) . ?
C6 O3 1.275(11) . ?
C7 N2 1.484(11) . ?
C7 C8 1.508(13) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O6 1.246(12) . ?
C8 O5 1.262(11) . ?
C9 C10 1.486(14) . ?
C9 N2 1.510(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O8 1.254(10) . ?
C10 O7 1.255(10) . ?
O7 Na1 2.469(7) 3 ?
O9 H9C 0.8236 . ?
O9 H9D 0.8172 . ?
O10 Na1 2.477(8) 3 ?
O10 H10A 0.8159 . ?
O10 H10B 0.8163 . ?
O11 H11C 0.8188 . ?
O11 H11D 0.8165 . ?
O23 H23A 0.8270 . ?
O23 H23B 0.8288 . ?
O23' H23C 0.8124 . ?
O23' H23D 0.8292 . ?
O24 H24A 0.8172 . ?
O24 H24B 0.8172 . ?
O24' H24C 0.8251 . ?
O24' H24D 0.8188 . ?
O27 H27A 0.8157 . ?
O27 H27B 0.8200 . ?
O27' H27C 0.8254 . ?
O27' H27D 0.8582 . ?
O28 H28A 0.8167 . ?
O28 H28B 0.8168 . ?
O29 H29A 0.8156 . ?
O29 H29B 0.8161 . ?

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
O5 Tb1 O1 78.8(2) . . ?
O5 Tb1 O9 138.1(2) . . ?
O1 Tb1 O9 77.7(2) . . ?
O5 Tb1 O7 72.0(2) . . ?
O1 Tb1 O7 140.6(2) . . ?
O9 Tb1 O7 141.2(2) . . ?
O5 Tb1 O3 141.4(2) . . ?
O1 Tb1 O3 128.5(2) . . ?
O9 Tb1 O3 79.4(2) . . ?
O7 Tb1 O3 70.3(2) . . ?
O5 Tb1 O10 104.7(2) . . ?
O1 Tb1 O10 142.7(2) . . ?
O9 Tb1 O10 75.74(19) . . ?
O7 Tb1 O10 71.9(2) . . ?
O3 Tb1 O10 71.0(2) . . ?
O5 Tb1 O11 68.0(2) . . ?
O1 Tb1 O11 74.0(2) . . ?
O9 Tb1 O11 72.5(2) . . ?
O7 Tb1 O11 116.5(2) . . ?
O3 Tb1 O11 138.8(2) . . ?
O10 Tb1 O11 73.3(2) . . ?
O5 Tb1 N2 67.8(2) . . ?
O1 Tb1 N2 78.0(2) . . ?
O9 Tb1 N2 138.0(3) . . ?
O7 Tb1 N2 66.9(2) . . ?
O3 Tb1 N2 89.8(2) . . ?
O10 Tb1 N2 138.4(2) . . ?
O11 Tb1 N2 131.1(2) . . ?
O5 Tb1 N1 127.7(2) . . ?
O1 Tb1 N1 65.8(2) . . ?
O9 Tb1 N1 70.8(2) . . ?
O7 Tb1 N1 113.5(2) . . ?
O3 Tb1 N1 63.3(2) . . ?
O10 Tb1 N1 127.0(2) . . ?
O11 Tb1 N1 129.8(2) . . ?
N2 Tb1 N1 68.1(2) . . ?
O5 Tb1 Na1 85.95(17) . 3 ?
O1 Tb1 Na1 163.30(17) . 3 ?
O9 Tb1 Na1 110.27(18) . 3 ?
O7 Tb1 Na1 35.76(16) . 3 ?
O3 Tb1 Na1 68.09(16) . 3 ?
O10 Tb1 Na1 36.25(16) . 3 ?
O11 Tb1 Na1 94.05(16) . 3 ?
N2 Tb1 Na1 102.6(2) . 3 ?
N1 Tb1 Na1 130.28(16) . 3 ?
O5 Tb1 Na1 32.27(16) . . ?
O1 Tb1 Na1 72.82(16) . . ?
O9 Tb1 Na1 106.96(18) . . ?
O7 Tb1 Na1 94.21(17) . . ?
O3 Tb1 Na1 158.57(16) . . ?
O10 Tb1 Na1 90.39(16) . . ?
O11 Tb1 Na1 35.72(16) . . ?
N2 Tb1 Na1 97.81(17) . . ?
N1 Tb1 Na1 138.08(16) . . ?
Na1 Tb1 Na1 90.64(8) 3 . ?
O24' Na1 O23' 83.4(13) . . ?
O24' Na1 O5 114.7(8) . . ?
O23' Na1 O5 120.3(16) . . ?
O23 Na1 O5 125.1(16) . . ?
O23 Na1 O24 88.2(13) . . ?
O5 Na1 O24 111.3(7) . . ?
O24' Na1 O7 95.4(8) . 7_544 ?
O23' Na1 O7 86.3(17) . 7_544 ?
O23 Na1 O7 87.0(16) . 7_544 ?
O5 Na1 O7 140.7(3) . 7_544 ?
O24 Na1 O7 89.5(7) . 7_544 ?
O24' Na1 O10 102.0(7) . 7_544 ?
O23' Na1 O10 156.1(16) . 7_544 ?
O23 Na1 O10 155.9(16) . 7_544 ?
O5 Na1 O10 79.0(2) . 7_544 ?
O24 Na1 O10 84.0(7) . 7_544 ?
O7 Na1 O10 70.1(2) 7_544 7_544 ?
O24' Na1 O11 177.9(8) . . ?
O23' Na1 O11 95.0(10) . . ?
O23 Na1 O11 106.7(11) . . ?
O5 Na1 O11 67.3(2) . . ?
O24 Na1 O11 162.9(7) . . ?
O7 Na1 O11 83.2(2) 7_544 . ?
O10 Na1 O11 79.0(2) 7_544 . ?
O24' Na1 Tb1 98.4(7) . 7_544 ?
O23' Na1 Tb1 121.0(16) . 7_544 ?
O23 Na1 Tb1 120.9(16) . 7_544 ?
O5 Na1 Tb1 112.2(2) . 7_544 ?
O24 Na1 Tb1 83.9(6) . 7_544 ?
O7 Na1 Tb1 34.65(15) 7_544 7_544 ?
O10 Na1 Tb1 35.57(15) 7_544 7_544 ?
O11 Na1 Tb1 81.26(18) . 7_544 ?
O24' Na1 Tb1 145.9(8) . . ?
O23' Na1 Tb1 112.5(13) . . ?
O23 Na1 Tb1 122.7(13) . . ?
O5 Na1 Tb1 31.18(16) . . ?
O24 Na1 Tb1 139.8(7) . . ?
O7 Na1 Tb1 114.9(2) 7_544 . ?
O10 Na1 Tb1 75.89(17) 7_544 . ?
O11 Na1 Tb1 36.10(14) . . ?
Tb1 Na1 Tb1 98.21(9) 7_544 . ?
O24' Na1 H11C 161.7 . . ?
O23' Na1 H11C 102.7 . . ?
O23 Na1 H11C 113.7 . . ?
O5 Na1 H11C 77.4 . . ?
O24 Na1 H11C 146.7 . . ?
O7 Na1 H11C 68.1 7_544 . ?
O10 Na1 H11C 65.7 7_544 . ?
O11 Na1 H11C 17.8 . . ?
Tb1 Na1 H11C 63.5 7_544 . ?
Tb1 Na1 H11C 47.4 . . ?
O23 Na1 H23B 19.3 . . ?
O5 Na1 H23B 139.2 . . ?
O24 Na1 H23B 92.5 . . ?
O7 Na1 H23B 68.3 7_544 . ?
O10 Na1 H23B 138.3 7_544 . ?
O11 Na1 H23B 99.0 . . ?
Tb1 Na1 H23B 102.7 7_544 . ?
Tb1 Na1 H23B 125.5 . . ?
H11C Na1 H23B 101.0 . . ?
O24' Na1 H23D 86.0 . . ?
O23' Na1 H23D 18.9 . . ?
O5 Na1 H23D 135.6 . . ?
O7 Na1 H23D 67.4 7_544 . ?
O10 Na1 H23D 137.3 7_544 . ?
O11 Na1 H23D 92.0 . . ?
Tb1 Na1 H23D 102.1 7_544 . ?
Tb1 Na1 H23D 119.0 . . ?
H11C Na1 H23D 94.4 . . ?
O24' Na1 H24D 16.9 . . ?
O23' Na1 H24D 67.1 . . ?
O5 Na1 H24D 118.2 . . ?
O7 Na1 H24D 98.1 7_544 . ?
O10 Na1 H24D 118.6 7_544 . ?
O11 Na1 H24D 161.8 . . ?
Tb1 Na1 H24D 110.1 7_544 . ?
Tb1 Na1 H24D 147.0 . . ?
H11C Na1 H24D 163.9 . . ?
H23D Na1 H24D 72.0 . . ?
N1 C1 C2 113.3(8) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N2 C2 C1 111.0(7) . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 114.3(7) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
O2 C4 O1 124.3(7) . . ?
O2 C4 C3 116.8(8) . . ?
O1 C4 C3 118.9(8) . . ?
N1 C5 C6 111.0(7) . . ?
N1 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
O4 C6 O3 123.6(8) . . ?
O4 C6 C5 119.2(8) . . ?
O3 C6 C5 117.2(7) . . ?
N2 C7 C8 112.4(7) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
O6 C8 O5 124.3(9) . . ?
O6 C8 C7 118.3(9) . . ?
O5 C8 C7 117.2(8) . . ?
C10 C9 N2 113.4(8) . . ?
C10 C9 H9A 108.9 . . ?
N2 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
N2 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O8 C10 O7 124.2(8) . . ?
O8 C10 C9 116.5(8) . . ?
O7 C10 C9 119.1(8) . . ?
C5 N1 C3 110.8(7) . . ?
C5 N1 C1 108.0(7) . . ?
C3 N1 C1 110.6(7) . . ?
C5 N1 Tb1 108.7(5) . . ?
C3 N1 Tb1 109.6(5) . . ?
C1 N1 Tb1 109.1(5) . . ?
C2 N2 C7 109.4(7) . . ?
C2 N2 C9 111.0(7) . . ?
C7 N2 C9 108.8(8) . . ?
C2 N2 Tb1 112.3(6) . . ?
C7 N2 Tb1 107.9(5) . . ?
C9 N2 Tb1 107.3(6) . . ?
C4 O1 Tb1 125.5(5) . . ?
C6 O3 Tb1 125.5(5) . . ?
C8 O5 Tb1 123.9(6) . . ?
C8 O5 Na1 116.9(6) . . ?
Tb1 O5 Na1 116.6(3) . . ?
C10 O7 Tb1 123.9(6) . . ?
C10 O7 Na1 125.0(6) . 3 ?
Tb1 O7 Na1 109.6(2) . 3 ?
Tb1 O9 H9C 126.1 . . ?
Tb1 O9 H9D 123.3 . . ?
H9C O9 H9D 107.8 . . ?
Tb1 O10 Na1 108.2(3) . 3 ?
Tb1 O10 H10A 117.5 . . ?
Na1 O10 H10A 100.7 3 . ?
Tb1 O10 H10B 121.2 . . ?
Na1 O10 H10B 101.7 3 . ?
H10A O10 H10B 104.6 . . ?
Na1 O11 Tb1 108.2(2) . . ?
Na1 O11 H11C 93.6 . . ?
Tb1 O11 H11C 117.8 . . ?
Na1 O11 H11D 116.3 . . ?
Tb1 O11 H11D 112.4 . . ?
H11C O11 H11D 107.5 . . ?
Na1 O23 H23A 129.0 . . ?
Na1 O23 H23B 86.4 . . ?
H23A O23 H23B 123.4 . . ?
Na1 O23' H23C 133.9 . . ?
Na1 O23' H23D 92.9 . . ?
H23C O23' H23D 105.0 . . ?
Na1 O24 H24A 111.6 . . ?
Na1 O24 H24B 126.0 . . ?
H24A O24 H24B 120.1 . . ?
Na1 O24' H24C 134.2 . . ?
Na1 O24' H24D 110.8 . . ?
H24C O24' H24D 93.4 . . ?
H27A O27 H27B 99.9 . . ?
H27C O27' H27D 94.8 . . ?
H28A O28 H28B 104.1 . . ?
H29A O29 H29B 106.0 . . ?

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
N1 C1 C2 N2 60.8(10) . . . . ?
N1 C3 C4 O2 170.2(8) . . . . ?
N1 C3 C4 O1 -10.6(11) . . . . ?
N1 C5 C6 O4 -157.9(9) . . . . ?
N1 C5 C6 O3 23.4(12) . . . . ?
N2 C7 C8 O6 146.3(9) . . . . ?
N2 C7 C8 O5 -38.0(12) . . . . ?
N2 C9 C10 O8 -156.8(10) . . . . ?
N2 C9 C10 O7 27.4(14) . . . . ?
C6 C5 N1 C3 -159.3(7) . . . . ?
C6 C5 N1 C1 79.4(9) . . . . ?
C6 C5 N1 Tb1 -38.9(8) . . . . ?
C4 C3 N1 C5 143.0(7) . . . . ?
C4 C3 N1 C1 -97.2(8) . . . . ?
C4 C3 N1 Tb1 23.1(8) . . . . ?
C2 C1 N1 C5 -161.9(7) . . . . ?
C2 C1 N1 C3 76.7(9) . . . . ?
C2 C1 N1 Tb1 -43.8(8) . . . . ?
C1 C2 N2 C7 -163.0(8) . . . . ?
C1 C2 N2 C9 76.9(10) . . . . ?
C1 C2 N2 Tb1 -43.2(9) . . . . ?
C8 C7 N2 C2 153.7(8) . . . . ?
C8 C7 N2 C9 -84.9(9) . . . . ?
C8 C7 N2 Tb1 31.2(9) . . . . ?
C10 C9 N2 C2 -156.3(9) . . . . ?
C10 C9 N2 C7 83.2(11) . . . . ?
C10 C9 N2 Tb1 -33.2(11) . . . . ?
O2 C4 O1 Tb1 167.2(7) . . . . ?
C3 C4 O1 Tb1 -11.9(11) . . . . ?
O4 C6 O3 Tb1 -169.5(7) . . . . ?
C5 C6 O3 Tb1 9.1(11) . . . . ?
O6 C8 O5 Tb1 -160.8(8) . . . . ?
C7 C8 O5 Tb1 23.8(11) . . . . ?
O6 C8 O5 Na1 38.3(12) . . . . ?
C7 C8 O5 Na1 -137.1(7) . . . . ?
O8 C10 O7 Tb1 -179.2(8) . . . . ?
C9 C10 O7 Tb1 -3.8(12) . . . . ?
O8 C10 O7 Na1 -14.6(14) . . . 3 ?
C9 C10 O7 Na1 160.8(7) . . . 3 ?

_refine_diff_density_max         1.100
_refine_diff_density_min         -2.789
_refine_diff_density_rms         0.161



# start Validation Reply Form
_vrf_PLAT972_shelx               
;
PROBLEM: Check Calcd Residual Density  1.80A From      O6      -2.51 eA-3  
RESPONSE: Electron density minimum of -2.51eA-3 is located at
1.80A from O6.
;
# end Validation Reply Form
