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

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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data_gt44sq(1)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C97 H48 N9 Na3 O24 Pr2 Zn2, O'
_chemical_formula_sum            'C97 H48 N9 Na3 O25 Pr2 Zn2'
_chemical_formula_weight         2221.01

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   32.9263(6)
_cell_length_b                   35.2939(7)
_cell_length_c                   11.3229(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.9520(9)
_cell_angle_gamma                90.00
_cell_volume                     12368.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    7692
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      25.06

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4416
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7092
_exptl_absorpt_correction_T_max  0.8869
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruler-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42799
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         25.06
_reflns_number_total             11129
_reflns_number_gt                7692
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The crystal contains severely disordered crystallization solvent trapped
 within the channel voids, which could not be modeled by discrete atoms.
 The solvent consists of a mixture of water and dimethylacetamide.
 Its contribution to the diffraction pattern was subtracted by the Squeeze
 technique, using the PLATON software (Spek, 2009).
 The H-atoms of the water molecules metal-coordinated O19 and free O74 
 could not be located.

;

_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)+(0.0992P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11129
_refine_ls_number_parameters     637
_refine_ls_number_restraints     258
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1763
_refine_ls_wR_factor_gt          0.1611
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.001

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
Pr1 Pr 0.235161(13) 0.5000 0.24549(5) 0.03339(17) Uani 1 2 d SU . .
Pr2 Pr 0.290934(13) 0.5000 0.71506(5) 0.03760(18) Uani 1 2 d SU . .
Zn3 Zn 0.534942(18) 0.760655(16) 0.79747(5) 0.03126(17) Uani 1 1 d U . .
Na4 Na 0.67577(9) 1.0000 0.4817(3) 0.0366(7) Uani 1 2 d SU . .
Na5 Na 0.24761(6) 0.57666(5) 0.48043(18) 0.0347(4) Uani 1 1 d U . .
O6 O 0.71879(11) 0.95636(9) 0.6234(3) 0.0317(8) Uani 1 1 d U . .
O7 O 0.31360(10) 0.95798(9) 0.6627(3) 0.0315(8) Uani 1 1 d U . .
O8 O 0.26944(15) 0.5000 0.4816(5) 0.0332(12) Uani 1 2 d SU . .
O9 O 0.73023(11) 0.54292(9) 0.8674(3) 0.0352(8) Uani 1 1 d U . .
O10 O 0.73683(11) 0.56950(9) 0.6992(3) 0.0349(8) Uani 1 1 d U . .
O11 O 0.75508(12) 0.95733(10) 0.8275(3) 0.0406(9) Uani 1 1 d U . .
O12 O 0.35065(11) 0.54347(10) 0.8306(3) 0.0391(8) Uani 1 1 d U . .
O13 O 0.30561(11) 0.56974(10) 0.6601(3) 0.0421(9) Uani 1 1 d U . .
O14 O 0.32765(12) 0.95646(10) 0.8682(3) 0.0442(9) Uani 1 1 d U . .
O15 O 0.31505(16) 0.5000 0.3760(6) 0.0495(14) Uani 1 2 d SU . .
O16 O 0.24145(15) 0.63927(11) 0.4861(4) 0.0659(13) Uani 1 1 d U . .
O17 O 0.33953(16) 0.5000 0.5860(6) 0.0504(13) Uani 1 2 d SU . .
O18 O 0.5124(2) 0.75510(14) 0.6038(4) 0.0915(17) Uani 1 1 d U . .
O19 O 0.6060(2) 1.0000 0.4792(9) 0.124(3) Uani 1 2 d SU . .
N20 N 0.60078(13) 0.76151(11) 0.8305(3) 0.0289(9) Uani 1 1 d U . .
N21 N 0.47647(12) 0.76114(11) 0.8252(3) 0.0281(9) Uani 1 1 d U . .
N22 N 0.53830(12) 0.70305(11) 0.8305(4) 0.0296(9) Uani 1 1 d U . .
N23 N 0.53605(13) 0.81912(11) 0.8071(4) 0.0302(9) Uani 1 1 d U . .
N24 N 0.3096(2) 0.5000 0.4753(8) 0.0532(15) Uani 1 2 d SU . .
C25 C 0.50186(16) 0.84185(13) 0.7982(4) 0.0283(10) Uani 1 1 d U . .
C26 C 0.45291(14) 0.79260(14) 0.8327(4) 0.0270(10) Uani 1 1 d U . .
C27 C 0.46346(15) 0.83000(14) 0.8127(4) 0.0275(10) Uani 1 1 d U . .
C28 C 0.45259(16) 0.73031(14) 0.8331(4) 0.0308(11) Uani 1 1 d U . .
C29 C 0.43003(15) 0.85962(13) 0.8032(4) 0.0267(10) Uani 1 1 d U . .
C30 C 0.72466(17) 0.94461(13) 0.7335(4) 0.0293(11) Uani 1 1 d U . .
C31 C 0.69598(16) 0.91478(14) 0.7550(4) 0.0298(11) Uani 1 1 d U . .
C32 C 0.36989(15) 0.60381(13) 0.7737(4) 0.0288(10) Uani 1 1 d U . .
C33 C 0.56867(16) 0.84171(13) 0.7958(4) 0.0287(10) Uani 1 1 d U . .
C34 C 0.50350(16) 0.68086(14) 0.8143(4) 0.0322(11) Uani 1 1 d U . .
C35 C 0.33419(16) 0.94508(13) 0.7710(5) 0.0295(11) Uani 1 1 d U . .
C36 C 0.57123(16) 0.68052(13) 0.8255(4) 0.0320(11) Uani 1 1 d U . .
C37 C 0.41400(16) 0.74302(15) 0.8563(5) 0.0365(12) Uani 1 1 d U . .
H37 H 0.3925 0.7274 0.8697 0.044 Uiso 1 1 calc R . .
C38 C 0.42996(15) 0.66281(14) 0.8058(4) 0.0303(11) Uani 1 1 d U . .
C39 C 0.62574(16) 0.79221(14) 0.8327(4) 0.0308(11) Uani 1 1 d U . .
C40 C 0.46286(16) 0.69288(14) 0.8172(4) 0.0305(11) Uani 1 1 d U . .
C41 C 0.61285(16) 0.69237(14) 0.8366(4) 0.0311(11) Uani 1 1 d U . .
C42 C 0.36790(15) 0.91557(13) 0.7843(4) 0.0268(10) Uani 1 1 d U . .
C43 C 0.62668(16) 0.73029(14) 0.8443(4) 0.0324(11) Uani 1 1 d U . .
C44 C 0.61019(16) 0.82975(14) 0.8082(4) 0.0315(11) Uani 1 1 d U . .
C45 C 0.72308(15) 0.57024(14) 0.7919(5) 0.0305(11) Uani 1 1 d U . .
C46 C 0.41453(16) 0.78037(15) 0.8553(5) 0.0397(13) Uani 1 1 d U . .
H46 H 0.3932 0.7965 0.8673 0.048 Uiso 1 1 calc R . .
C47 C 0.69759(16) 0.60348(13) 0.8069(4) 0.0311(11) Uani 1 1 d U . .
C48 C 0.33984(16) 0.57090(15) 0.7534(5) 0.0352(11) Uani 1 1 d U . .
C49 C 0.64058(16) 0.85919(14) 0.7924(4) 0.0303(11) Uani 1 1 d U . .
C50 C 0.36036(17) 0.63430(14) 0.6899(5) 0.0392(12) Uani 1 1 d U . .
H50 H 0.3338 0.6350 0.6215 0.047 Uiso 1 1 calc R . .
C51 C 0.43709(17) 0.63341(16) 0.8891(5) 0.0402(13) Uani 1 1 d U . .
H51 H 0.4630 0.6331 0.9597 0.048 Uiso 1 1 calc R . .
C52 C 0.64425(16) 0.66233(14) 0.8304(5) 0.0328(11) Uani 1 1 d U . .
C53 C 0.68564(18) 0.63221(14) 0.7177(5) 0.0379(13) Uani 1 1 d U . .
H53 H 0.6956 0.6318 0.6482 0.046 Uiso 1 1 calc R . .
C54 C 0.55614(17) 0.64166(15) 0.8049(5) 0.0403(13) Uani 1 1 d U . .
H54 H 0.5727 0.6201 0.7998 0.048 Uiso 1 1 calc R . .
C55 C 0.40761(16) 0.60390(16) 0.8738(5) 0.0388(13) Uani 1 1 d U . .
H55 H 0.4138 0.5838 0.9331 0.047 Uiso 1 1 calc R . .
C56 C 0.55313(17) 0.88023(15) 0.7753(5) 0.0367(12) Uani 1 1 d U . .
H56 H 0.5687 0.9017 0.7630 0.044 Uiso 1 1 calc R . .
C57 C 0.51263(17) 0.88006(14) 0.7769(5) 0.0356(12) Uani 1 1 d U . .
H57 H 0.4942 0.9015 0.7658 0.043 Uiso 1 1 calc R . .
C58 C 0.65767(16) 0.63409(15) 0.9213(5) 0.0357(12) Uani 1 1 d U . .
H58 H 0.6482 0.6349 0.9917 0.043 Uiso 1 1 calc R . .
C59 C 0.51434(17) 0.64203(14) 0.7945(5) 0.0390(12) Uani 1 1 d U . .
H59 H 0.4954 0.6209 0.7775 0.047 Uiso 1 1 calc R . .
C60 C 0.66909(17) 0.78096(15) 0.8535(5) 0.0435(13) Uani 1 1 d U . .
H60 H 0.6929 0.7972 0.8606 0.052 Uiso 1 1 calc R . .
C61 C 0.38992(17) 0.66337(15) 0.7074(5) 0.0429(13) Uani 1 1 d U . .
H61 H 0.3830 0.6843 0.6514 0.051 Uiso 1 1 calc R . .
C62 C 0.66993(18) 0.74259(15) 0.8613(5) 0.0438(13) Uani 1 1 d U . .
H62 H 0.6945 0.7268 0.8754 0.053 Uiso 1 1 calc R . .
C63 C 0.65925(18) 0.66134(15) 0.7300(5) 0.0398(13) Uani 1 1 d U . .
H63 H 0.6513 0.6809 0.6689 0.048 Uiso 1 1 calc R . .
C64 C 0.68404(16) 0.60533(15) 0.9120(5) 0.0351(12) Uani 1 1 d U . .
H64 H 0.6932 0.5866 0.9760 0.042 Uiso 1 1 calc R . .
C65 C 0.5000 0.7620(3) 0.5000 0.057(2) Uani 1 2 d SU . .
C66 C 0.69963(19) 0.90304(17) 0.8732(5) 0.0477(15) Uani 1 1 d U . .
H66 H 0.7212 0.9138 0.9440 0.057 Uiso 1 1 calc R . .
C67 C 0.6720(2) 0.87554(18) 0.8908(5) 0.0507(16) Uani 1 1 d U . .
H67 H 0.6751 0.8679 0.9739 0.061 Uiso 1 1 calc R . .
C68 C 0.3916(2) 0.9010(2) 0.8955(5) 0.083(3) Uani 1 1 d U . .
H68 H 0.3875 0.9099 0.9698 0.099 Uiso 1 1 calc R . .
C69 C 0.4220(3) 0.8730(2) 0.9035(5) 0.082(3) Uani 1 1 d U . .
H69 H 0.4378 0.8628 0.9838 0.098 Uiso 1 1 calc R . .
C70 C 0.6379(3) 0.8706(3) 0.6753(6) 0.103(4) Uani 1 1 d U . .
H70 H 0.6172 0.8591 0.6044 0.124 Uiso 1 1 calc R . .
C71 C 0.6648(3) 0.8985(3) 0.6564(5) 0.096(3) Uani 1 1 d U . .
H71 H 0.6612 0.9064 0.5733 0.115 Uiso 1 1 calc R . .
C72 C 0.4064(3) 0.8744(3) 0.6929(5) 0.108(5) Uani 1 1 d U . .
H72 H 0.4110 0.8659 0.6190 0.130 Uiso 1 1 calc R . .
C73 C 0.3754(3) 0.9017(3) 0.6825(5) 0.106(4) Uani 1 1 d U . .
H73 H 0.3589 0.9110 0.6016 0.129 Uiso 1 1 calc R . .
O74 O 0.26442(15) 0.5000 -0.0154(4) 0.0368(12) Uiso 1 2 d S . .


_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
Pr1 O9 2.494(3) 5_666 ?
Pr1 O9 2.494(3) 2_656 ?
Pr1 O8 2.522(5) . ?
Pr1 O15 2.540(5) . ?
Pr1 O14 2.545(3) 4_546 ?
Pr1 O14 2.545(3) 7_566 ?
Pr1 O10 2.620(3) 2_656 ?
Pr1 O10 2.620(3) 5_666 ?
Pr1 O7 2.645(3) 4_546 ?
Pr1 O7 2.645(3) 7_566 ?
Pr1 N24 2.903(8) . ?
Pr1 C45 2.935(5) 2_656 ?
Pr2 O12 2.485(3) . ?
Pr2 O12 2.485(3) 6_565 ?
Pr2 O8 2.493(5) . ?
Pr2 O17 2.509(6) . ?
Pr2 O11 2.512(3) 8_465 ?
Pr2 O11 2.512(3) 3_445 ?
Pr2 O13 2.624(3) . ?
Pr2 O13 2.624(3) 6_565 ?
Pr2 O6 2.722(3) 3_445 ?
Pr2 O6 2.722(3) 8_465 ?
Pr2 C48 2.927(5) 6_565 ?
Pr2 C48 2.927(5) . ?
Zn3 N21 2.054(4) . ?
Zn3 N22 2.063(4) . ?
Zn3 N23 2.066(4) . ?
Zn3 N20 2.070(4) . ?
Zn3 O18 2.070(5) . ?
Na4 O19 2.289(8) . ?
Na4 O7 2.321(4) 2_656 ?
Na4 O7 2.321(4) 5_676 ?
Na4 O6 2.324(4) 6_575 ?
Na4 O6 2.324(4) . ?
Na4 Na5 3.597(3) 3 ?
Na4 Na5 3.597(3) 8_565 ?
Na4 Pr2 3.811(3) 3 ?
Na4 Pr1 3.814(3) 3 ?
Na5 O16 2.222(4) . ?
Na5 O10 2.275(4) 2_656 ?
Na5 O13 2.279(4) . ?
Na5 O6 2.435(4) 8_465 ?
Na5 O7 2.440(4) 7_566 ?
Na5 O8 2.798(2) . ?
Na5 Na4 3.597(3) 3_445 ?
O6 C30 1.264(5) . ?
O6 Na5 2.435(4) 8_565 ?
O6 Pr2 2.722(3) 3 ?
O7 C35 1.266(5) . ?
O7 Na4 2.321(4) 5_676 ?
O7 Na5 2.440(4) 7_566 ?
O7 Pr1 2.645(3) 7_566 ?
O8 N24 1.348(8) . ?
O8 Na5 2.798(2) 6_565 ?
O9 C45 1.256(6) . ?
O9 Pr1 2.494(3) 5_666 ?
O10 C45 1.277(6) . ?
O10 Na5 2.275(4) 2_656 ?
O10 Pr1 2.620(3) 5_666 ?
O11 C30 1.269(6) . ?
O11 Pr2 2.512(3) 3 ?
O12 C48 1.271(6) . ?
O13 C48 1.255(6) . ?
O14 C35 1.258(6) . ?
O14 Pr1 2.545(3) 7_566 ?
O15 N24 1.198(9) . ?
O17 N24 1.303(9) . ?
O18 C65 1.131(5) . ?
N20 C39 1.355(6) . ?
N20 C43 1.369(6) . ?
N21 C28 1.363(6) . ?
N21 C26 1.374(6) . ?
N22 C34 1.348(6) . ?
N22 C36 1.361(6) . ?
N23 C25 1.358(6) . ?
N23 C33 1.378(6) . ?
C25 C27 1.393(7) . ?
C25 C57 1.436(7) . ?
C26 C27 1.403(7) . ?
C26 C46 1.438(7) . ?
C27 C29 1.495(7) . ?
C28 C40 1.391(7) . ?
C28 C37 1.453(7) . ?
C29 C72 1.333(8) . ?
C29 C69 1.337(7) . ?
C30 C31 1.489(7) . ?
C30 Pr2 2.990(5) 3 ?
C31 C71 1.360(7) . ?
C31 C66 1.367(7) . ?
C32 C55 1.366(7) . ?
C32 C50 1.398(7) . ?
C32 C48 1.492(7) . ?
C33 C44 1.391(7) . ?
C33 C56 1.443(7) . ?
C34 C40 1.415(7) . ?
C34 C59 1.452(7) . ?
C35 C42 1.492(7) . ?
C35 Pr1 2.952(5) 7_566 ?
C36 C41 1.397(7) . ?
C36 C54 1.450(7) . ?
C37 C46 1.318(7) . ?
C38 C51 1.367(7) . ?
C38 C61 1.406(7) . ?
C38 C40 1.490(7) . ?
C39 C44 1.414(7) . ?
C39 C60 1.422(7) . ?
C41 C43 1.407(7) . ?
C41 C52 1.499(7) . ?
C42 C68 1.337(7) . ?
C42 C73 1.350(7) . ?
C43 C62 1.438(7) . ?
C44 C49 1.495(7) . ?
C45 C47 1.485(7) . ?
C45 Pr1 2.935(5) 5_666 ?
C47 C53 1.390(7) . ?
C47 C64 1.408(7) . ?
C49 C70 1.359(8) . ?
C49 C67 1.363(7) . ?
C50 C61 1.381(7) . ?
C51 C55 1.394(7) . ?
C52 C63 1.385(7) . ?
C52 C58 1.392(7) . ?
C53 C63 1.384(7) . ?
C54 C59 1.341(7) . ?
C56 C57 1.340(7) . ?
C58 C64 1.363(7) . ?
C60 C62 1.357(7) . ?
C65 O18 1.131(5) 2_656 ?
C66 C67 1.390(8) . ?
C68 C69 1.389(8) . ?
C70 C71 1.388(9) . ?
C72 C73 1.377(9) . ?

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
O9 Pr1 O9 74.79(15) 5_666 2_656 ?
O9 Pr1 O8 115.20(11) 5_666 . ?
O9 Pr1 O8 115.20(11) 2_656 . ?
O9 Pr1 O15 74.61(13) 5_666 . ?
O9 Pr1 O15 74.61(13) 2_656 . ?
O8 Pr1 O15 51.92(17) . . ?
O9 Pr1 O14 78.96(12) 5_666 4_546 ?
O9 Pr1 O14 122.81(11) 2_656 4_546 ?
O8 Pr1 O14 121.91(11) . 4_546 ?
O15 Pr1 O14 142.73(9) . 4_546 ?
O9 Pr1 O14 122.81(11) 5_666 7_566 ?
O9 Pr1 O14 78.96(12) 2_656 7_566 ?
O8 Pr1 O14 121.91(11) . 7_566 ?
O15 Pr1 O14 142.73(9) . 7_566 ?
O14 Pr1 O14 74.28(17) 4_546 7_566 ?
O9 Pr1 O10 120.39(11) 5_666 2_656 ?
O9 Pr1 O10 50.86(10) 2_656 2_656 ?
O8 Pr1 O10 75.71(8) . 2_656 ?
O15 Pr1 O10 69.56(7) . 2_656 ?
O14 Pr1 O10 147.67(12) 4_546 2_656 ?
O14 Pr1 O10 73.42(11) 7_566 2_656 ?
O9 Pr1 O10 50.86(10) 5_666 5_666 ?
O9 Pr1 O10 120.39(11) 2_656 5_666 ?
O8 Pr1 O10 75.71(8) . 5_666 ?
O15 Pr1 O10 69.56(7) . 5_666 ?
O14 Pr1 O10 73.42(11) 4_546 5_666 ?
O14 Pr1 O10 147.67(12) 7_566 5_666 ?
O10 Pr1 O10 138.84(15) 2_656 5_666 ?
O9 Pr1 O7 107.80(11) 5_666 4_546 ?
O9 Pr1 O7 170.61(11) 2_656 4_546 ?
O8 Pr1 O7 72.28(11) . 4_546 ?
O15 Pr1 O7 114.73(13) . 4_546 ?
O14 Pr1 O7 50.42(10) 4_546 4_546 ?
O14 Pr1 O7 92.28(11) 7_566 4_546 ?
O10 Pr1 O7 129.97(10) 2_656 4_546 ?
O10 Pr1 O7 65.96(10) 5_666 4_546 ?
O9 Pr1 O7 170.61(11) 5_666 7_566 ?
O9 Pr1 O7 107.80(11) 2_656 7_566 ?
O8 Pr1 O7 72.28(11) . 7_566 ?
O15 Pr1 O7 114.73(13) . 7_566 ?
O14 Pr1 O7 92.28(11) 4_546 7_566 ?
O14 Pr1 O7 50.42(10) 7_566 7_566 ?
O10 Pr1 O7 65.96(10) 2_656 7_566 ?
O10 Pr1 O7 129.97(10) 5_666 7_566 ?
O7 Pr1 O7 68.20(14) 4_546 7_566 ?
O9 Pr1 N24 93.78(15) 5_666 . ?
O9 Pr1 N24 93.78(15) 2_656 . ?
O8 Pr1 N24 27.65(18) . . ?
O15 Pr1 N24 24.27(17) . . ?
O14 Pr1 N24 138.17(10) 4_546 . ?
O14 Pr1 N24 138.17(10) 7_566 . ?
O10 Pr1 N24 70.44(8) 2_656 . ?
O10 Pr1 N24 70.44(8) 5_666 . ?
O7 Pr1 N24 95.03(15) 4_546 . ?
O7 Pr1 N24 95.03(15) 7_566 . ?
O9 Pr1 C45 96.93(13) 5_666 2_656 ?
O9 Pr1 C45 25.12(12) 2_656 2_656 ?
O8 Pr1 C45 95.20(11) . 2_656 ?
O15 Pr1 C45 68.95(11) . 2_656 ?
O14 Pr1 C45 140.97(12) 4_546 2_656 ?
O14 Pr1 C45 75.93(13) 7_566 2_656 ?
O10 Pr1 C45 25.79(12) 2_656 2_656 ?
O10 Pr1 C45 132.94(12) 5_666 2_656 ?
O7 Pr1 C45 155.15(12) 4_546 2_656 ?
O7 Pr1 C45 87.72(12) 7_566 2_656 ?
N24 Pr1 C45 80.53(13) . 2_656 ?
O12 Pr2 O12 76.24(16) . 6_565 ?
O12 Pr2 O8 116.47(11) . . ?
O12 Pr2 O8 116.47(11) 6_565 . ?
O12 Pr2 O17 76.09(13) . . ?
O12 Pr2 O17 76.09(13) 6_565 . ?
O8 Pr2 O17 52.32(17) . . ?
O12 Pr2 O11 77.71(12) . 8_465 ?
O12 Pr2 O11 121.83(11) 6_565 8_465 ?
O8 Pr2 O11 121.68(11) . 8_465 ?
O17 Pr2 O11 143.03(8) . 8_465 ?
O12 Pr2 O11 121.83(11) . 3_445 ?
O12 Pr2 O11 77.71(12) 6_565 3_445 ?
O8 Pr2 O11 121.68(11) . 3_445 ?
O17 Pr2 O11 143.03(8) . 3_445 ?
O11 Pr2 O11 73.68(16) 8_465 3_445 ?
O12 Pr2 O13 50.88(11) . . ?
O12 Pr2 O13 121.83(11) 6_565 . ?
O8 Pr2 O13 75.95(9) . . ?
O17 Pr2 O13 69.89(8) . . ?
O11 Pr2 O13 73.39(11) 8_465 . ?
O11 Pr2 O13 147.04(12) 3_445 . ?
O12 Pr2 O13 121.83(11) . 6_565 ?
O12 Pr2 O13 50.88(11) 6_565 6_565 ?
O8 Pr2 O13 75.95(9) . 6_565 ?
O17 Pr2 O13 69.89(8) . 6_565 ?
O11 Pr2 O13 147.04(12) 8_465 6_565 ?
O11 Pr2 O13 73.39(11) 3_445 6_565 ?
O13 Pr2 O13 139.49(17) . 6_565 ?
O12 Pr2 O6 168.73(11) . 3_445 ?
O12 Pr2 O6 106.39(11) 6_565 3_445 ?
O8 Pr2 O6 72.59(11) . 3_445 ?
O17 Pr2 O6 115.16(12) . 3_445 ?
O11 Pr2 O6 91.86(11) 8_465 3_445 ?
O11 Pr2 O6 49.76(10) 3_445 3_445 ?
O13 Pr2 O6 130.37(10) . 3_445 ?
O13 Pr2 O6 65.55(10) 6_565 3_445 ?
O12 Pr2 O6 106.39(11) . 8_465 ?
O12 Pr2 O6 168.73(11) 6_565 8_465 ?
O8 Pr2 O6 72.59(11) . 8_465 ?
O17 Pr2 O6 115.16(12) . 8_465 ?
O11 Pr2 O6 49.76(10) 8_465 8_465 ?
O11 Pr2 O6 91.86(11) 3_445 8_465 ?
O13 Pr2 O6 65.55(10) . 8_465 ?
O13 Pr2 O6 130.37(10) 6_565 8_465 ?
O6 Pr2 O6 68.91(14) 3_445 8_465 ?
O12 Pr2 C48 98.82(13) . 6_565 ?
O12 Pr2 C48 25.53(12) 6_565 6_565 ?
O8 Pr2 C48 95.75(12) . 6_565 ?
O17 Pr2 C48 70.03(11) . 6_565 ?
O11 Pr2 C48 140.11(13) 8_465 6_565 ?
O11 Pr2 C48 75.05(13) 3_445 6_565 ?
O13 Pr2 C48 134.49(13) . 6_565 ?
O13 Pr2 C48 25.39(12) 6_565 6_565 ?
O6 Pr2 C48 86.40(12) 3_445 6_565 ?
O6 Pr2 C48 154.78(13) 8_465 6_565 ?
O12 Pr2 C48 25.53(12) . . ?
O12 Pr2 C48 98.82(14) 6_565 . ?
O8 Pr2 C48 95.75(12) . . ?
O17 Pr2 C48 70.03(11) . . ?
O11 Pr2 C48 75.05(13) 8_465 . ?
O11 Pr2 C48 140.11(13) 3_445 . ?
O13 Pr2 C48 25.39(12) . . ?
O13 Pr2 C48 134.49(13) 6_565 . ?
O6 Pr2 C48 154.78(12) 3_445 . ?
O6 Pr2 C48 86.40(12) 8_465 . ?
C48 Pr2 C48 117.5(2) 6_565 . ?
N21 Zn3 N22 88.60(16) . . ?
N21 Zn3 N23 89.09(15) . . ?
N22 Zn3 N23 167.33(15) . . ?
N21 Zn3 N20 161.92(15) . . ?
N22 Zn3 N20 89.63(15) . . ?
N23 Zn3 N20 88.70(15) . . ?
N21 Zn3 O18 98.4(2) . . ?
N22 Zn3 O18 94.37(17) . . ?
N23 Zn3 O18 98.29(18) . . ?
N20 Zn3 O18 99.7(2) . . ?
O19 Na4 O7 112.6(2) . 2_656 ?
O19 Na4 O7 112.6(2) . 5_676 ?
O7 Na4 O7 79.44(18) 2_656 5_676 ?
O19 Na4 O6 112.4(2) . 6_575 ?
O7 Na4 O6 134.99(17) 2_656 6_575 ?
O7 Na4 O6 81.96(12) 5_676 6_575 ?
O19 Na4 O6 112.4(2) . . ?
O7 Na4 O6 81.96(12) 2_656 . ?
O7 Na4 O6 134.99(17) 5_676 . ?
O6 Na4 O6 83.00(18) 6_575 . ?
O19 Na4 Na5 131.22(5) . 3 ?
O7 Na4 Na5 102.73(12) 2_656 3 ?
O7 Na4 Na5 42.19(9) 5_676 3 ?
O6 Na4 Na5 42.07(9) 6_575 3 ?
O6 Na4 Na5 104.74(12) . 3 ?
O19 Na4 Na5 131.22(5) . 8_565 ?
O7 Na4 Na5 42.19(9) 2_656 8_565 ?
O7 Na4 Na5 102.73(12) 5_676 8_565 ?
O6 Na4 Na5 104.74(12) 6_575 8_565 ?
O6 Na4 Na5 42.07(9) . 8_565 ?
Na5 Na4 Na5 97.55(9) 3 8_565 ?
O19 Na4 Pr2 140.0(3) . 3 ?
O7 Na4 Pr2 97.75(11) 2_656 3 ?
O7 Na4 Pr2 97.75(11) 5_676 3 ?
O6 Na4 Pr2 45.05(9) 6_575 3 ?
O6 Na4 Pr2 45.05(9) . 3 ?
Na5 Na4 Pr2 60.17(5) 3 3 ?
Na5 Na4 Pr2 60.17(5) 8_565 3 ?
O19 Na4 Pr1 138.1(3) . 3 ?
O7 Na4 Pr1 43.05(9) 2_656 3 ?
O7 Na4 Pr1 43.05(9) 5_676 3 ?
O6 Na4 Pr1 98.43(11) 6_575 3 ?
O6 Na4 Pr1 98.43(11) . 3 ?
Na5 Na4 Pr1 60.13(5) 3 3 ?
Na5 Na4 Pr1 60.13(5) 8_565 3 ?
Pr2 Na4 Pr1 81.91(6) 3 3 ?
O16 Na5 O10 100.77(16) . 2_656 ?
O16 Na5 O13 97.92(17) . . ?
O10 Na5 O13 114.25(15) 2_656 . ?
O16 Na5 O6 113.37(17) . 8_465 ?
O10 Na5 O6 143.06(14) 2_656 8_465 ?
O13 Na5 O6 75.70(13) . 8_465 ?
O16 Na5 O7 117.03(16) . 7_566 ?
O10 Na5 O7 74.78(12) 2_656 7_566 ?
O13 Na5 O7 142.17(14) . 7_566 ?
O6 Na5 O7 77.34(12) 8_465 7_566 ?
O16 Na5 O8 170.84(18) . . ?
O10 Na5 O8 76.17(15) 2_656 . ?
O13 Na5 O8 75.91(14) . . ?
O6 Na5 O8 72.05(14) 8_465 . ?
O7 Na5 O8 70.81(13) 7_566 . ?
O16 Na5 Na4 132.94(15) . 3_445 ?
O10 Na5 Na4 105.61(11) 2_656 3_445 ?
O13 Na5 Na4 105.52(11) . 3_445 ?
O6 Na5 Na4 39.76(9) 8_465 3_445 ?
O7 Na5 Na4 39.69(9) 7_566 3_445 ?
O8 Na5 Na4 56.01(10) . 3_445 ?
O16 Na5 Pr1 139.07(14) . . ?
O10 Na5 Pr1 44.18(8) 2_656 . ?
O13 Na5 Pr1 114.53(11) . . ?
O6 Na5 Pr1 98.89(9) 8_465 . ?
O7 Na5 Pr1 45.23(8) 7_566 . ?
O8 Na5 Pr1 42.70(11) . . ?
Na4 Na5 Pr1 62.83(5) 3_445 . ?
O16 Na5 Pr2 136.02(14) . . ?
O10 Na5 Pr2 114.18(11) 2_656 . ?
O13 Na5 Pr2 44.27(9) . . ?
O6 Na5 Pr2 47.02(8) 8_465 . ?
O7 Na5 Pr2 97.96(9) 7_566 . ?
O8 Na5 Pr2 42.09(11) . . ?
Na4 Na5 Pr2 62.76(5) 3_445 . ?
Pr1 Na5 Pr2 84.46(4) . . ?
C30 O6 Na4 138.6(3) . . ?
C30 O6 Na5 122.4(3) . 8_565 ?
Na4 O6 Na5 98.17(14) . 8_565 ?
C30 O6 Pr2 89.4(3) . 3 ?
Na4 O6 Pr2 97.77(12) . 3 ?
Na5 O6 Pr2 92.11(11) 8_565 3 ?
C35 O7 Na4 138.8(3) . 5_676 ?
C35 O7 Na5 120.7(3) . 7_566 ?
Na4 O7 Na5 98.12(14) 5_676 7_566 ?
C35 O7 Pr1 91.0(3) . 7_566 ?
Na4 O7 Pr1 100.15(12) 5_676 7_566 ?
Na5 O7 Pr1 93.86(11) 7_566 7_566 ?
N24 O8 Pr2 97.3(5) . . ?
N24 O8 Pr1 92.1(5) . . ?
Pr2 O8 Pr1 170.6(2) . . ?
N24 O8 Na5 104.76(10) . . ?
Pr2 O8 Na5 89.11(12) . . ?
Pr1 O8 Na5 88.49(12) . . ?
N24 O8 Na5 104.76(10) . 6_565 ?
Pr2 O8 Na5 89.11(12) . 6_565 ?
Pr1 O8 Na5 88.49(12) . 6_565 ?
Na5 O8 Na5 150.4(2) . 6_565 ?
C45 O9 Pr1 97.4(3) . 5_666 ?
C45 O10 Na5 169.6(3) . 2_656 ?
C45 O10 Pr1 91.0(3) . 5_666 ?
Na5 O10 Pr1 98.58(13) 2_656 5_666 ?
C30 O11 Pr2 99.2(3) . 3 ?
C48 O12 Pr2 97.0(3) . . ?
C48 O13 Na5 170.4(4) . . ?
C48 O13 Pr2 90.9(3) . . ?
Na5 O13 Pr2 98.41(13) . . ?
C35 O14 Pr1 95.9(3) . 7_566 ?
N24 O15 Pr1 95.1(4) . . ?
N24 O17 Pr2 97.9(4) . . ?
C65 O18 Zn3 162.2(6) . . ?
C39 N20 C43 106.9(4) . . ?
C39 N20 Zn3 127.3(3) . . ?
C43 N20 Zn3 125.6(3) . . ?
C28 N21 C26 106.9(4) . . ?
C28 N21 Zn3 126.5(3) . . ?
C26 N21 Zn3 126.5(3) . . ?
C34 N22 C36 107.9(4) . . ?
C34 N22 Zn3 123.9(3) . . ?
C36 N22 Zn3 124.2(3) . . ?
C25 N23 C33 107.7(4) . . ?
C25 N23 Zn3 125.9(3) . . ?
C33 N23 Zn3 125.0(3) . . ?
O15 N24 O17 126.6(7) . . ?
O15 N24 O8 120.9(7) . . ?
O17 N24 O8 112.5(7) . . ?
O15 N24 Pr1 60.6(4) . . ?
O17 N24 Pr1 172.8(6) . . ?
O8 N24 Pr1 60.3(4) . . ?
O15 N24 Pr2 176.9(5) . . ?
O17 N24 Pr2 56.5(4) . . ?
O8 N24 Pr2 56.0(4) . . ?
Pr1 N24 Pr2 116.3(2) . . ?
N23 C25 C27 125.2(4) . . ?
N23 C25 C57 108.7(4) . . ?
C27 C25 C57 126.0(4) . . ?
N21 C26 C27 125.0(4) . . ?
N21 C26 C46 108.5(4) . . ?
C27 C26 C46 126.3(4) . . ?
C25 C27 C26 125.9(4) . . ?
C25 C27 C29 117.2(4) . . ?
C26 C27 C29 116.9(4) . . ?
N21 C28 C40 125.3(4) . . ?
N21 C28 C37 109.0(4) . . ?
C40 C28 C37 125.7(5) . . ?
C72 C29 C69 115.9(5) . . ?
C72 C29 C27 121.4(4) . . ?
C69 C29 C27 122.7(4) . . ?
O6 C30 O11 121.5(5) . . ?
O6 C30 C31 120.1(4) . . ?
O11 C30 C31 118.4(4) . . ?
O6 C30 Pr2 65.6(3) . 3 ?
O11 C30 Pr2 56.0(2) . 3 ?
C31 C30 Pr2 173.1(4) . 3 ?
C71 C31 C66 117.7(5) . . ?
C71 C31 C30 120.6(5) . . ?
C66 C31 C30 121.7(5) . . ?
C55 C32 C50 119.4(5) . . ?
C55 C32 C48 119.8(5) . . ?
C50 C32 C48 120.8(4) . . ?
N23 C33 C44 125.8(4) . . ?
N23 C33 C56 108.4(4) . . ?
C44 C33 C56 125.7(5) . . ?
N22 C34 C40 126.1(5) . . ?
N22 C34 C59 109.1(4) . . ?
C40 C34 C59 124.8(5) . . ?
O14 C35 O7 122.5(4) . . ?
O14 C35 C42 118.6(4) . . ?
O7 C35 C42 118.9(4) . . ?
O14 C35 Pr1 59.0(3) . 7_566 ?
O7 C35 Pr1 63.6(2) . 7_566 ?
C42 C35 Pr1 176.0(3) . 7_566 ?
N22 C36 C41 126.3(4) . . ?
N22 C36 C54 109.0(4) . . ?
C41 C36 C54 124.7(4) . . ?
C46 C37 C28 107.0(4) . . ?
C51 C38 C61 116.8(5) . . ?
C51 C38 C40 122.1(4) . . ?
C61 C38 C40 121.1(4) . . ?
N20 C39 C44 124.7(4) . . ?
N20 C39 C60 110.4(4) . . ?
C44 C39 C60 124.8(5) . . ?
C28 C40 C34 124.2(5) . . ?
C28 C40 C38 119.1(4) . . ?
C34 C40 C38 116.7(4) . . ?
C36 C41 C43 125.2(4) . . ?
C36 C41 C52 117.1(4) . . ?
C43 C41 C52 117.5(4) . . ?
C68 C42 C73 116.5(5) . . ?
C68 C42 C35 122.5(4) . . ?
C73 C42 C35 120.9(5) . . ?
N20 C43 C41 125.6(4) . . ?
N20 C43 C62 108.8(4) . . ?
C41 C43 C62 125.5(5) . . ?
C33 C44 C39 125.6(5) . . ?
C33 C44 C49 116.9(4) . . ?
C39 C44 C49 117.6(4) . . ?
O9 C45 O10 120.5(4) . . ?
O9 C45 C47 120.7(4) . . ?
O10 C45 C47 118.8(4) . . ?
O9 C45 Pr1 57.4(2) . 5_666 ?
O10 C45 Pr1 63.2(2) . 5_666 ?
C47 C45 Pr1 173.9(3) . 5_666 ?
C37 C46 C26 108.5(5) . . ?
C53 C47 C64 119.2(4) . . ?
C53 C47 C45 121.6(4) . . ?
C64 C47 C45 119.2(4) . . ?
O13 C48 O12 120.9(5) . . ?
O13 C48 C32 120.8(5) . . ?
O12 C48 C32 118.2(5) . . ?
O13 C48 Pr2 63.7(3) . . ?
O12 C48 Pr2 57.4(3) . . ?
C32 C48 Pr2 172.3(3) . . ?
C70 C49 C67 116.7(5) . . ?
C70 C49 C44 120.0(5) . . ?
C67 C49 C44 123.3(4) . . ?
C61 C50 C32 119.4(5) . . ?
C38 C51 C55 122.2(5) . . ?
C63 C52 C58 118.5(5) . . ?
C63 C52 C41 120.1(4) . . ?
C58 C52 C41 121.4(4) . . ?
C63 C53 C47 120.0(5) . . ?
C59 C54 C36 106.9(5) . . ?
C32 C55 C51 120.1(5) . . ?
C57 C56 C33 107.1(5) . . ?
C56 C57 C25 108.1(4) . . ?
C64 C58 C52 121.7(5) . . ?
C54 C59 C34 107.1(5) . . ?
C62 C60 C39 106.6(5) . . ?
C50 C61 C38 121.8(5) . . ?
C60 C62 C43 107.2(5) . . ?
C53 C63 C52 120.9(5) . . ?
C58 C64 C47 119.6(5) . . ?
O18 C65 O18 155.2(10) 2_656 . ?
C31 C66 C67 120.6(5) . . ?
C49 C67 C66 122.0(5) . . ?
C42 C68 C69 120.8(5) . . ?
C29 C69 C68 122.9(5) . . ?
C49 C70 C71 121.9(6) . . ?
C31 C71 C70 121.1(5) . . ?
C29 C72 C73 122.2(6) . . ?
C42 C73 C72 121.8(6) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 -0.003 -0.016 3925 823 ' '
2 0.000 0.500 0.507 597 120 ' '
3 0.500 0.000 0.317 597 120 ' '
_platon_squeeze_details          
;
 disordered DMF/DMA/water crystallization solvent.
;

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.965
_refine_diff_density_min         -2.257
_refine_diff_density_rms         0.116
_database_code_depnum_ccdc_archive 'CCDC 1014715'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt46sq(2)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H53 N9 Na3 O23 Pr2'
_chemical_formula_sum            'C96 H53 N9 Na3 O23 Pr2'
_chemical_formula_weight         2051.26

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   33.0534(12)
_cell_length_b                   35.2658(13)
_cell_length_c                   11.3000(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.685(3)
_cell_angle_gamma                90.00
_cell_volume                     12402.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6502
_cell_measurement_theta_min      1.75
_cell_measurement_theta_max      25.42

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4108
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7737
_exptl_absorpt_correction_T_max  0.8837
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43564
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.42
_reflns_number_total             11614
_reflns_number_gt                6502
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The crystal contains severely disordered crystallization solvent trapped
 within the channel voids, which could not be modeled by discrete atoms.
 The solvent consists of a mixture of water and dimethylacetamide.
 Its contribution to the diffraction pattern was subtracted by the Squeeze
 technique, using the PLATON software (Spek, 2009).
 The H-atoms of the water molecules metal-coordinated and inter-layer one
 could not be located.
 Some of the aryl groups show partial rotational disorder as well.
;

_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)+(0.0894P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11614
_refine_ls_number_parameters     613
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1953
_refine_ls_wR_factor_gt          0.1801
_refine_ls_goodness_of_fit_ref   1.206
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.264076(12) 0.5000 0.79023(6) 0.0612(2) Uani 1 2 d S . .
Pr2 Pr 0.207775(12) 0.5000 1.15493(6) 0.0627(2) Uani 1 2 d S . .
Na3 Na -0.17867(9) 0.0000 0.1395(4) 0.0578(10) Uani 1 2 d S . .
Na4 Na 0.25145(7) 0.42474(6) 1.0017(3) 0.0621(8) Uani 1 1 d . . .
O5 O 0.23127(13) 0.5000 0.9645(5) 0.0516(16) Uani 1 2 d S . .
O6 O 0.22886(11) 0.45690(9) 0.6094(4) 0.0463(10) Uani 1 1 d . . .
O7 O 0.18573(17) 0.5000 0.7639(7) 0.068(2) Uani 1 2 d S . .
O8 O -0.19397(11) 0.43024(9) -0.0682(4) 0.0578(12) Uani 1 1 d . . .
O9 O 0.25596(12) 0.04374(10) 0.6630(4) 0.0568(12) Uani 1 1 d . . .
O10 O -0.17378(12) 0.04424(11) -0.2003(5) 0.0606(12) Uani 1 1 d . . .
O11 O -0.18699(10) 0.04238(9) -0.0231(4) 0.0493(11) Uani 1 1 d . . .
O12 O 0.23560(11) 0.42954(9) 0.7900(4) 0.0524(11) Uani 1 1 d . . .
O13 O -0.14743(10) 0.45520(10) -0.1484(4) 0.0549(12) Uani 1 1 d . . .
O14 O 0.16076(16) 0.5000 0.9266(7) 0.070(2) Uani 1 2 d S . .
H14 H 0.1799 0.5000 1.0106 0.084 Uiso 1 2 d SR . .
O15 O 0.25894(18) 0.36088(16) 1.0222(5) 0.110(2) Uani 1 1 d . . .
O16 O 0.22102(11) 0.04328(10) 0.7974(4) 0.0513(11) Uani 1 1 d . . .
O17 O -0.1104(3) 0.0000 0.2854(11) 0.157(4) Uani 1 2 d S . .
N18 N -0.02356(11) 0.23882(11) 0.1310(4) 0.0367(11) Uani 1 1 d . . .
N19 N 0.03693(12) 0.18110(11) 0.2617(4) 0.0402(12) Uani 1 1 d . . .
H19 H 0.0405 0.2063 0.2534 0.048 Uiso 1 1 d R . .
N20 N 0.09935(12) 0.24002(11) 0.3719(4) 0.0432(12) Uani 1 1 d . . .
N21 N 0.03725(11) 0.29871(11) 0.2532(4) 0.0427(12) Uani 1 1 d . . .
H21 H 0.0396 0.2743 0.2404 0.051 Uiso 1 1 calc R . .
N22 N 0.1907(2) 0.5000 0.8785(11) 0.067(3) Uani 1 2 d S . .
C23 C -0.13260(14) 0.08473(13) -0.0372(6) 0.0393(14) Uani 1 1 d . . .
C24 C -0.16632(15) 0.05510(13) -0.0879(7) 0.0447(17) Uani 1 1 d . . .
C25 C 0.19673(16) 0.08571(14) 0.6225(6) 0.0451(16) Uani 1 1 d . . .
C26 C 0.00184(15) 0.15842(13) 0.2032(6) 0.0430(15) Uani 1 1 d . . .
C27 C 0.00111(15) 0.32038(14) 0.1986(6) 0.0428(15) Uani 1 1 d . . .
C28 C -0.03664(15) 0.17017(13) 0.1152(5) 0.0385(14) Uani 1 1 d . . .
C29 C -0.15948(16) 0.42905(14) -0.0886(6) 0.0510(17) Uani 1 1 d . . .
C30 C 0.22589(17) 0.05607(15) 0.6987(7) 0.0489(17) Uani 1 1 d . . .
C31 C 0.22108(16) 0.42929(14) 0.6735(7) 0.0477(17) Uani 1 1 d . . .
C32 C -0.12932(15) 0.39592(13) -0.0454(6) 0.0461(16) Uani 1 1 d . . .
C33 C 0.06875(15) 0.32092(14) 0.3299(6) 0.0432(15) Uani 1 1 d . . .
C34 C -0.07073(14) 0.33761(14) 0.0540(6) 0.0431(15) Uani 1 1 d . . .
C35 C 0.19524(16) 0.39679(14) 0.6014(7) 0.0498(17) Uani 1 1 d . . .
C36 C -0.03753(15) 0.30763(13) 0.1112(6) 0.0435(15) Uani 1 1 d . . .
C37 C -0.04768(15) 0.27035(14) 0.0748(6) 0.0417(14) Uani 1 1 d . . .
C38 C -0.04715(15) 0.20759(13) 0.0784(5) 0.0395(14) Uani 1 1 d . . .
C39 C 0.11077(15) 0.17140(14) 0.4074(6) 0.0447(15) Uani 1 1 d . . .
C40 C -0.06984(15) 0.14021(13) 0.0628(6) 0.0411(15) Uani 1 1 d . . .
C41 C 0.12454(16) 0.27100(15) 0.4154(6) 0.0537(18) Uani 1 1 d . . .
C42 C 0.14149(16) 0.14155(14) 0.4815(6) 0.0461(16) Uani 1 1 d . . .
C43 C 0.12467(15) 0.20891(14) 0.4182(6) 0.0529(17) Uani 1 1 d . . .
C44 C 0.05487(17) 0.12070(14) 0.3270(6) 0.0521(17) Uani 1 1 d . . .
H44 H 0.0709 0.0994 0.3692 0.063 Uiso 1 1 calc R . .
C45 C 0.11034(15) 0.30823(14) 0.4019(6) 0.0507(17) Uani 1 1 d . . .
C46 C 0.14104(17) 0.33849(15) 0.4706(6) 0.0521(17) Uani 1 1 d . . .
C47 C 0.06984(15) 0.15910(14) 0.3382(6) 0.0476(16) Uani 1 1 d . . .
C48 C 0.01360(17) 0.12000(14) 0.2452(6) 0.0538(17) Uani 1 1 d . . .
H48 H -0.0041 0.0982 0.2204 0.065 Uiso 1 1 calc R . .
C49 C 0.16818(17) 0.22085(16) 0.4885(7) 0.073(2) Uani 1 1 d . . .
H49 H 0.1921 0.2049 0.5279 0.088 Uiso 1 1 calc R . .
C50 C -0.08707(15) 0.25751(14) -0.0226(6) 0.0527(18) Uani 1 1 d . . .
H50 H -0.1088 0.2732 -0.0769 0.063 Uiso 1 1 calc R . .
C51 C -0.08677(16) 0.21978(15) -0.0211(6) 0.0558(18) Uani 1 1 d . . .
H51 H -0.1082 0.2036 -0.0744 0.067 Uiso 1 1 calc R . .
C52 C 0.18183(18) 0.36894(15) 0.6689(7) 0.063(2) Uani 1 1 d . . .
H52 H 0.1904 0.3700 0.7579 0.075 Uiso 1 1 calc R . .
C53 C 0.05220(16) 0.35799(15) 0.3273(6) 0.0591(19) Uani 1 1 d . . .
H53 H 0.0671 0.3793 0.3730 0.071 Uiso 1 1 calc R . .
C54 C 0.16805(17) 0.25912(16) 0.4869(8) 0.086(3) Uani 1 1 d . . .
H54 H 0.1919 0.2753 0.5252 0.103 Uiso 1 1 calc R . .
C55 C 0.01040(17) 0.35753(16) 0.2461(7) 0.0593(19) Uani 1 1 d . . .
H55 H -0.0088 0.3785 0.2258 0.071 Uiso 1 1 calc R . .
C56 C 0.18231(17) 0.39552(16) 0.4743(7) 0.0566(18) Uani 1 1 d . . .
H56 H 0.1914 0.4148 0.4302 0.068 Uiso 1 1 calc R . .
C57 C 0.15595(17) 0.36645(16) 0.4067(7) 0.0604(19) Uani 1 1 d . . .
H57 H 0.1481 0.3655 0.3178 0.072 Uiso 1 1 calc R . .
C58 C -0.09210(16) 0.39434(17) -0.0715(6) 0.0576(18) Uani 1 1 d . . .
H58 H -0.0858 0.4133 -0.1225 0.069 Uiso 1 1 calc R . .
C59 C -0.13879(17) 0.36756(16) 0.0271(7) 0.064(2) Uani 1 1 d . . .
H59 H -0.1652 0.3682 0.0434 0.077 Uiso 1 1 calc R . .
C60 C -0.06336(17) 0.36502(16) -0.0233(6) 0.0557(18) Uani 1 1 d . . .
H60 H -0.0379 0.3638 -0.0442 0.067 Uiso 1 1 calc R . .
C61 C -0.10992(17) 0.33855(16) 0.0755(7) 0.063(2) Uani 1 1 d . . .
H61 H -0.1168 0.3191 0.1237 0.076 Uiso 1 1 calc R . .
C62 C 0.19992(19) 0.09789(18) 0.5123(7) 0.066(2) Uani 1 1 d . . .
H62 H 0.2208 0.0868 0.4821 0.080 Uiso 1 1 calc R . .
C63 C 0.15560(19) 0.33982(16) 0.6021(7) 0.070(2) Uani 1 1 d . . .
H63 H 0.1473 0.3203 0.6471 0.084 Uiso 1 1 calc R . .
C64 C 0.1734(2) 0.12610(19) 0.4430(8) 0.075(2) Uani 1 1 d . . .
H64 H 0.1771 0.1350 0.3680 0.090 Uiso 1 1 calc R . .
C65 C 0.1662(2) 0.1017(2) 0.6610(7) 0.084(2) Uani 1 1 d . . .
H65 H 0.1636 0.0937 0.7384 0.101 Uiso 1 1 calc R . .
C66 C -0.1092(3) 0.0985(3) -0.1035(9) 0.130(4) Uani 1 1 d . . .
H66 H -0.1129 0.0884 -0.1845 0.155 Uiso 1 1 calc R . .
C67 C -0.0790(3) 0.1278(3) -0.0549(8) 0.116(4) Uani 1 1 d . . .
H67 H -0.0649 0.1389 -0.1071 0.139 Uiso 1 1 calc R . .
C68 C 0.1391(2) 0.1288(2) 0.5933(8) 0.092(3) Uani 1 1 d . . .
H68 H 0.1180 0.1392 0.6241 0.111 Uiso 1 1 calc R . .
C69 C -0.1253(4) 0.0993(3) 0.0725(11) 0.212(7) Uani 1 1 d . . .
H69 H -0.1426 0.0914 0.1202 0.224 Uiso 1 1 calc R . .
C70 C -0.0930(3) 0.1263(3) 0.1248(11) 0.177(7) Uani 1 1 d . . .
H70 H -0.0879 0.1347 0.2085 0.212 Uiso 1 1 calc R . .
O72 O 0.23445(18) 0.5000 0.4740(7) 0.081(2) Uani 1 2 d S . .


_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
Pr1 O6 2.498(4) . ?
Pr1 O6 2.498(4) 6_565 ?
Pr1 O7 2.505(6) . ?
Pr1 O5 2.548(6) . ?
Pr1 O10 2.553(4) 3_556 ?
Pr1 O10 2.553(4) 8_556 ?
Pr1 O11 2.646(4) 3_556 ?
Pr1 O11 2.646(4) 8_556 ?
Pr1 O12 2.657(3) . ?
Pr1 O12 2.657(3) 6_565 ?
Pr1 N22 2.918(8) . ?
Pr1 C31 2.952(5) 6_565 ?
Pr2 O14 2.524(6) . ?
Pr2 O13 2.526(3) 2_556 ?
Pr2 O13 2.526(3) 5_566 ?
Pr2 O9 2.527(4) 4_557 ?
Pr2 O9 2.527(4) 7_557 ?
Pr2 O5 2.522(6) . ?
Pr2 O8 2.631(3) 2_556 ?
Pr2 O8 2.631(3) 5_566 ?
Pr2 O16 2.703(3) 4_557 ?
Pr2 O16 2.703(3) 7_557 ?
Pr2 C29 2.926(5) 2_556 ?
Pr2 C29 2.926(5) 5_566 ?
Na3 O11 2.312(5) . ?
Na3 O11 2.312(5) 6 ?
Na3 O17 2.303(10) . ?
Na3 O16 2.339(5) 5_556 ?
Na3 O16 2.339(5) 2_556 ?
Na3 O5 2.967(5) 3_444 ?
Na3 Na4 3.519(3) 3_444 ?
Na3 Na4 3.519(3) 8_454 ?
Na3 Pr1 3.759(4) 3_444 ?
Na3 Pr2 3.816(3) 3_444 ?
Na4 O15 2.269(6) . ?
Na4 O12 2.276(5) . ?
Na4 O8 2.275(5) 2_556 ?
Na4 O16 2.421(5) 7_557 ?
Na4 O11 2.439(4) 8_556 ?
Na4 O5 2.735(2) . ?
Na4 Na3 3.519(3) 3_556 ?
O5 N22 1.366(9) . ?
O5 Na4 2.734(2) 6_565 ?
O5 Na3 2.968(5) 3_556 ?
O6 C31 1.290(7) . ?
O7 N22 1.249(10) . ?
O8 C29 1.238(7) . ?
O8 Na4 2.275(5) 2_556 ?
O8 Pr2 2.631(3) 5_566 ?
O9 C30 1.269(7) . ?
O9 Pr2 2.527(4) 7_557 ?
O10 C24 1.268(7) . ?
O10 Pr1 2.553(4) 3_444 ?
O11 C24 1.242(7) . ?
O11 Na4 2.439(4) 8_454 ?
O11 Pr1 2.646(4) 3_444 ?
O12 C31 1.240(7) . ?
O13 C29 1.283(7) . ?
O13 Pr2 2.526(3) 5_566 ?
O14 N22 1.279(10) . ?
O16 C30 1.263(7) . ?
O16 Na3 2.339(5) 5_556 ?
O16 Na4 2.421(5) 7_557 ?
O16 Pr2 2.703(3) 7_557 ?
N18 C38 1.365(6) . ?
N18 C37 1.391(6) . ?
N19 C47 1.378(6) . ?
N19 C26 1.380(6) . ?
N20 C41 1.361(6) . ?
N20 C43 1.372(6) . ?
N21 C33 1.356(6) . ?
N21 C27 1.377(6) . ?
C23 C69 1.287(10) . ?
C23 C66 1.336(9) . ?
C23 C24 1.494(6) . ?
C24 Pr1 2.972(5) 3_444 ?
C25 C62 1.354(9) . ?
C25 C65 1.349(8) . ?
C25 C30 1.485(8) . ?
C26 C28 1.388(7) . ?
C26 C48 1.445(7) . ?
C27 C36 1.400(7) . ?
C27 C55 1.410(7) . ?
C28 C38 1.392(7) . ?
C28 C40 1.495(6) . ?
C29 C32 1.506(6) . ?
C29 Pr2 2.927(5) 5_566 ?
C30 Pr2 3.001(6) 7_557 ?
C31 C35 1.496(7) . ?
C32 C58 1.359(8) . ?
C32 C59 1.394(8) . ?
C33 C53 1.414(7) . ?
C33 C45 1.414(7) . ?
C34 C60 1.378(8) . ?
C34 C61 1.396(7) . ?
C34 C36 1.504(6) . ?
C35 C56 1.355(9) . ?
C35 C52 1.403(8) . ?
C36 C37 1.385(7) . ?
C37 C50 1.465(7) . ?
C38 C51 1.473(7) . ?
C39 C47 1.384(7) . ?
C39 C43 1.392(7) . ?
C39 C42 1.506(7) . ?
C40 C70 1.296(10) . ?
C40 C67 1.334(9) . ?
C41 C45 1.385(7) . ?
C41 C54 1.454(7) . ?
C42 C68 1.368(10) . ?
C42 C64 1.381(8) . ?
C43 C49 1.452(7) . ?
C44 C48 1.366(8) . ?
C44 C47 1.432(7) . ?
C45 C46 1.497(7) . ?
C46 C57 1.406(8) . ?
C46 C63 1.401(9) . ?
C49 C54 1.350(8) . ?
C50 C51 1.331(7) . ?
C52 C63 1.391(7) . ?
C53 C55 1.377(8) . ?
C56 C57 1.394(7) . ?
C58 C60 1.385(7) . ?
C59 C61 1.380(7) . ?
C62 C64 1.382(8) . ?
C65 C68 1.358(9) . ?
C66 C67 1.414(8) . ?
C69 C70 1.405(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Pr1 O6 74.97(16) . 6_565 ?
O6 Pr1 O7 74.03(17) . . ?
O6 Pr1 O7 74.03(17) 6_565 . ?
O6 Pr1 O5 115.46(11) . . ?
O6 Pr1 O5 115.47(11) 6_565 . ?
O7 Pr1 O5 53.1(2) . . ?
O6 Pr1 O10 123.56(14) . 3_556 ?
O6 Pr1 O10 78.99(13) 6_565 3_556 ?
O7 Pr1 O10 142.18(9) . 3_556 ?
O5 Pr1 O10 120.90(13) . 3_556 ?
O6 Pr1 O10 78.99(13) . 8_556 ?
O6 Pr1 O10 123.56(14) 6_565 8_556 ?
O7 Pr1 O10 142.18(9) . 8_556 ?
O5 Pr1 O10 120.90(13) . 8_556 ?
O10 Pr1 O10 75.35(18) 3_556 8_556 ?
O6 Pr1 O11 170.84(12) . 3_556 ?
O6 Pr1 O11 107.44(12) 6_565 3_556 ?
O7 Pr1 O11 115.11(17) . 3_556 ?
O5 Pr1 O11 71.87(12) . 3_556 ?
O10 Pr1 O11 49.78(14) 3_556 3_556 ?
O10 Pr1 O11 92.56(12) 8_556 3_556 ?
O6 Pr1 O11 107.44(12) . 8_556 ?
O6 Pr1 O11 170.84(12) 6_565 8_556 ?
O7 Pr1 O11 115.11(17) . 8_556 ?
O5 Pr1 O11 71.87(12) . 8_556 ?
O10 Pr1 O11 92.56(12) 3_556 8_556 ?
O10 Pr1 O11 49.78(14) 8_556 8_556 ?
O11 Pr1 O11 68.79(16) 3_556 8_556 ?
O6 Pr1 O12 50.41(13) . . ?
O6 Pr1 O12 120.07(12) 6_565 . ?
O7 Pr1 O12 69.40(8) . . ?
O5 Pr1 O12 76.00(11) . . ?
O10 Pr1 O12 148.37(12) 3_556 . ?
O10 Pr1 O12 73.03(12) 8_556 . ?
O11 Pr1 O12 130.57(13) 3_556 . ?
O11 Pr1 O12 66.03(11) 8_556 . ?
O6 Pr1 O12 120.07(12) . 6_565 ?
O6 Pr1 O12 50.41(13) 6_565 6_565 ?
O7 Pr1 O12 69.40(8) . 6_565 ?
O5 Pr1 O12 75.99(11) . 6_565 ?
O10 Pr1 O12 73.04(12) 3_556 6_565 ?
O10 Pr1 O12 148.37(12) 8_556 6_565 ?
O11 Pr1 O12 66.03(11) 3_556 6_565 ?
O11 Pr1 O12 130.57(13) 8_556 6_565 ?
O12 Pr1 O12 138.55(16) . 6_565 ?
O6 Pr1 N22 93.89(19) . . ?
O6 Pr1 N22 93.89(18) 6_565 . ?
O7 Pr1 N22 25.2(2) . . ?
O5 Pr1 N22 27.9(2) . . ?
O10 Pr1 N22 137.37(13) 3_556 . ?
O10 Pr1 N22 137.37(14) 8_556 . ?
O11 Pr1 N22 94.75(19) 3_556 . ?
O11 Pr1 N22 94.75(19) 8_556 . ?
O12 Pr1 N22 70.44(10) . . ?
O12 Pr1 N22 70.44(10) 6_565 . ?
O6 Pr1 C31 97.30(15) . 6_565 ?
O6 Pr1 C31 25.69(16) 6_565 6_565 ?
O7 Pr1 C31 67.93(13) . 6_565 ?
O5 Pr1 C31 94.54(15) . 6_565 ?
O10 Pr1 C31 76.23(13) 3_556 6_565 ?
O10 Pr1 C31 142.60(16) 8_556 6_565 ?
O11 Pr1 C31 87.25(14) 3_556 6_565 ?
O11 Pr1 C31 155.00(16) 8_556 6_565 ?
O12 Pr1 C31 132.26(13) . 6_565 ?
O12 Pr1 C31 24.83(14) 6_565 6_565 ?
N22 Pr1 C31 79.76(16) . 6_565 ?
O14 Pr2 O13 76.22(15) . 2_556 ?
O14 Pr2 O13 76.22(15) . 5_566 ?
O13 Pr2 O13 77.44(16) 2_556 5_566 ?
O14 Pr2 O9 142.36(9) . 4_557 ?
O13 Pr2 O9 123.99(14) 2_556 4_557 ?
O13 Pr2 O9 78.19(12) 5_566 4_557 ?
O14 Pr2 O9 142.36(9) . 7_557 ?
O13 Pr2 O9 78.19(12) 2_556 7_557 ?
O13 Pr2 O9 123.99(14) 5_566 7_557 ?
O9 Pr2 O9 75.24(17) 4_557 7_557 ?
O14 Pr2 O5 52.29(18) . . ?
O13 Pr2 O5 116.24(12) 2_556 . ?
O13 Pr2 O5 116.24(12) 5_566 . ?
O9 Pr2 O5 119.77(12) 4_557 . ?
O9 Pr2 O5 119.77(12) 7_557 . ?
O14 Pr2 O8 69.47(10) . 2_556 ?
O13 Pr2 O8 50.80(12) 2_556 2_556 ?
O13 Pr2 O8 122.54(11) 5_566 2_556 ?
O9 Pr2 O8 148.14(13) 4_557 2_556 ?
O9 Pr2 O8 73.00(13) 7_557 2_556 ?
O5 Pr2 O8 75.32(10) . 2_556 ?
O14 Pr2 O8 69.47(9) . 5_566 ?
O13 Pr2 O8 122.54(11) 2_556 5_566 ?
O13 Pr2 O8 50.80(12) 5_566 5_566 ?
O9 Pr2 O8 73.00(13) 4_557 5_566 ?
O9 Pr2 O8 148.14(13) 7_557 5_566 ?
O5 Pr2 O8 75.32(10) . 5_566 ?
O8 Pr2 O8 138.5(2) 2_556 5_566 ?
O14 Pr2 O16 113.49(16) . 4_557 ?
O13 Pr2 O16 170.09(13) 2_556 4_557 ?
O13 Pr2 O16 106.17(11) 5_566 4_557 ?
O9 Pr2 O16 49.51(14) 4_557 4_557 ?
O9 Pr2 O16 92.31(12) 7_557 4_557 ?
O5 Pr2 O16 70.86(13) . 4_557 ?
O8 Pr2 O16 129.23(12) 2_556 4_557 ?
O8 Pr2 O16 64.92(11) 5_566 4_557 ?
O14 Pr2 O16 113.49(15) . 7_557 ?
O13 Pr2 O16 106.17(11) 2_556 7_557 ?
O13 Pr2 O16 170.09(13) 5_566 7_557 ?
O9 Pr2 O16 92.31(12) 4_557 7_557 ?
O9 Pr2 O16 49.51(14) 7_557 7_557 ?
O5 Pr2 O16 70.86(13) . 7_557 ?
O8 Pr2 O16 64.92(11) 2_556 7_557 ?
O8 Pr2 O16 129.23(12) 5_566 7_557 ?
O16 Pr2 O16 68.77(15) 4_557 7_557 ?
O14 Pr2 C29 69.10(14) . 2_556 ?
O13 Pr2 C29 25.91(15) 2_556 2_556 ?
O13 Pr2 C29 99.79(14) 5_566 2_556 ?
O9 Pr2 C29 143.00(17) 4_557 2_556 ?
O9 Pr2 C29 75.80(14) 7_557 2_556 ?
O5 Pr2 C29 94.57(15) . 2_556 ?
O8 Pr2 C29 25.01(14) 2_556 2_556 ?
O8 Pr2 C29 133.86(13) 5_566 2_556 ?
O16 Pr2 C29 153.78(14) 4_557 2_556 ?
O16 Pr2 C29 86.06(13) 7_557 2_556 ?
O14 Pr2 C29 69.10(14) . 5_566 ?
O13 Pr2 C29 99.79(14) 2_556 5_566 ?
O13 Pr2 C29 25.91(15) 5_566 5_566 ?
O9 Pr2 C29 75.80(14) 4_557 5_566 ?
O9 Pr2 C29 143.00(17) 7_557 5_566 ?
O5 Pr2 C29 94.57(15) . 5_566 ?
O8 Pr2 C29 133.86(13) 2_556 5_566 ?
O8 Pr2 C29 25.01(14) 5_566 5_566 ?
O16 Pr2 C29 86.06(13) 4_557 5_566 ?
O16 Pr2 C29 153.78(14) 7_557 5_566 ?
C29 Pr2 C29 117.5(2) 2_556 5_566 ?
O11 Na3 O11 80.5(2) . 6 ?
O11 Na3 O17 113.2(2) . . ?
O11 Na3 O17 113.2(2) 6 . ?
O11 Na3 O16 137.81(19) . 5_556 ?
O11 Na3 O16 84.09(15) 6 5_556 ?
O17 Na3 O16 108.9(3) . 5_556 ?
O11 Na3 O16 84.09(15) . 2_556 ?
O11 Na3 O16 137.81(19) 6 2_556 ?
O17 Na3 O16 108.9(3) . 2_556 ?
O16 Na3 O16 81.5(2) 5_556 2_556 ?
O11 Na3 O5 69.28(14) . 3_444 ?
O11 Na3 O5 69.28(14) 6 3_444 ?
O17 Na3 O5 176.5(4) . 3_444 ?
O16 Na3 O5 68.53(14) 5_556 3_444 ?
O16 Na3 O5 68.53(14) 2_556 3_444 ?
O11 Na3 Na4 104.55(15) . 3_444 ?
O11 Na3 Na4 43.61(11) 6 3_444 ?
O17 Na3 Na4 130.97(6) . 3_444 ?
O16 Na3 Na4 43.24(12) 5_556 3_444 ?
O16 Na3 Na4 104.84(13) 2_556 3_444 ?
O5 Na3 Na4 48.96(5) 3_444 3_444 ?
O11 Na3 Na4 43.61(11) . 8_454 ?
O11 Na3 Na4 104.55(15) 6 8_454 ?
O17 Na3 Na4 130.97(6) . 8_454 ?
O16 Na3 Na4 104.84(13) 5_556 8_454 ?
O16 Na3 Na4 43.24(12) 2_556 8_454 ?
O5 Na3 Na4 48.96(5) 3_444 8_454 ?
Na4 Na3 Na4 97.92(10) 3_444 8_454 ?
O11 Na3 Pr1 44.14(11) . 3_444 ?
O11 Na3 Pr1 44.14(11) 6 3_444 ?
O17 Na3 Pr1 141.0(3) . 3_444 ?
O16 Na3 Pr1 100.28(14) 5_556 3_444 ?
O16 Na3 Pr1 100.28(14) 2_556 3_444 ?
O5 Na3 Pr1 42.52(13) 3_444 3_444 ?
Na4 Na3 Pr1 60.79(7) 3_444 3_444 ?
Na4 Na3 Pr1 60.79(7) 8_454 3_444 ?
O11 Na3 Pr2 100.42(12) . 3_444 ?
O11 Na3 Pr2 100.42(12) 6 3_444 ?
O17 Na3 Pr2 135.1(3) . 3_444 ?
O16 Na3 Pr2 44.53(10) 5_556 3_444 ?
O16 Na3 Pr2 44.53(10) 2_556 3_444 ?
O5 Na3 Pr2 41.33(12) 3_444 3_444 ?
Na4 Na3 Pr2 60.73(6) 3_444 3_444 ?
Na4 Na3 Pr2 60.73(6) 8_454 3_444 ?
Pr1 Na3 Pr2 83.85(6) 3_444 3_444 ?
O15 Na4 O12 99.21(19) . . ?
O15 Na4 O8 97.19(19) . 2_556 ?
O12 Na4 O8 114.75(18) . 2_556 ?
O15 Na4 O16 111.9(2) . 7_557 ?
O12 Na4 O16 146.25(16) . 7_557 ?
O8 Na4 O16 75.08(16) 2_556 7_557 ?
O15 Na4 O11 114.66(18) . 8_556 ?
O12 Na4 O11 75.50(15) . 8_556 ?
O8 Na4 O11 145.03(16) 2_556 8_556 ?
O16 Na4 O11 79.72(15) 7_557 8_556 ?
O15 Na4 O5 172.6(2) . . ?
O12 Na4 O5 78.96(16) . . ?
O8 Na4 O5 77.32(15) 2_556 . ?
O16 Na4 O5 71.76(15) 7_557 . ?
O11 Na4 O5 71.97(14) 8_556 . ?
O15 Na4 Na3 132.11(17) . 3_556 ?
O12 Na4 Na3 107.07(13) . 3_556 ?
O8 Na4 Na3 106.63(13) 2_556 3_556 ?
O16 Na4 Na3 41.43(12) 7_557 3_556 ?
O11 Na4 Na3 40.84(12) 8_556 3_556 ?
O5 Na4 Na3 54.94(10) . 3_556 ?
O15 Na4 Pr1 138.46(17) . . ?
O12 Na4 Pr1 45.72(9) . . ?
O8 Na4 Pr1 116.24(12) 2_556 . ?
O16 Na4 Pr1 100.57(12) 7_557 . ?
O11 Na4 Pr1 45.77(9) 8_556 . ?
O5 Na4 Pr1 43.68(13) . . ?
Na3 Na4 Pr1 62.82(7) 3_556 . ?
O15 Na4 Pr2 135.01(17) . . ?
O12 Na4 Pr2 116.65(12) . . ?
O8 Na4 Pr2 44.47(9) 2_556 . ?
O16 Na4 Pr2 46.58(9) 7_557 . ?
O11 Na4 Pr2 100.60(11) 8_556 . ?
O5 Na4 Pr2 42.73(13) . . ?
Na3 Na4 Pr2 63.58(6) 3_556 . ?
Pr1 Na4 Pr2 86.24(5) . . ?
N22 O5 Pr2 95.5(5) . . ?
N22 O5 Pr1 91.3(5) . . ?
Pr2 O5 Pr1 173.23(18) . . ?
N22 O5 Na4 103.86(10) . 6_565 ?
Pr2 O5 Na4 89.89(14) . 6_565 ?
Pr1 O5 Na4 88.48(13) . 6_565 ?
N22 O5 Na4 103.86(10) . . ?
Pr2 O5 Na4 89.89(14) . . ?
Pr1 O5 Na4 88.48(13) . . ?
Na4 O5 Na4 152.17(19) 6_565 . ?
N22 O5 Na3 176.8(6) . 3_556 ?
Pr2 O5 Na3 87.67(17) . 3_556 ?
Pr1 O5 Na3 85.56(16) . 3_556 ?
Na4 O5 Na3 76.09(9) 6_565 3_556 ?
Na4 O5 Na3 76.09(9) . 3_556 ?
C31 O6 Pr1 97.2(4) . . ?
N22 O7 Pr1 96.2(4) . . ?
C29 O8 Na4 169.4(4) . 2_556 ?
C29 O8 Pr2 91.0(3) . 5_566 ?
Na4 O8 Pr2 98.25(13) 2_556 5_566 ?
C30 O9 Pr2 99.1(4) . 7_557 ?
C24 O10 Pr1 96.2(3) . 3_444 ?
C24 O11 Na3 139.5(3) . . ?
C24 O11 Na4 122.8(3) . 8_454 ?
Na3 O11 Na4 95.54(19) . 8_454 ?
C24 O11 Pr1 92.5(3) . 3_444 ?
Na3 O11 Pr1 98.37(13) . 3_444 ?
Na4 O11 Pr1 92.89(12) 8_454 3_444 ?
C31 O12 Na4 170.0(4) . . ?
C31 O12 Pr1 91.0(3) . . ?
Na4 O12 Pr1 96.45(15) . . ?
C29 O13 Pr2 94.8(3) . 5_566 ?
N22 O14 Pr2 97.8(5) . . ?
C30 O16 Na3 140.3(4) . 5_556 ?
C30 O16 Na4 122.9(3) . 7_557 ?
Na3 O16 Na4 95.3(2) 5_556 7_557 ?
C30 O16 Pr2 90.9(3) . 7_557 ?
Na3 O16 Pr2 98.12(14) 5_556 7_557 ?
Na4 O16 Pr2 92.83(13) 7_557 7_557 ?
C38 N18 C37 106.9(4) . . ?
C47 N19 C26 109.4(4) . . ?
C41 N20 C43 106.5(4) . . ?
C33 N21 C27 109.2(4) . . ?
O7 N22 O14 126.2(8) . . ?
O7 N22 O5 119.4(7) . . ?
O14 N22 O5 114.4(9) . . ?
O7 N22 Pr1 58.6(4) . . ?
O14 N22 Pr1 175.2(7) . . ?
O5 N22 Pr1 60.8(4) . . ?
O7 N22 Pr2 176.8(6) . . ?
O14 N22 Pr2 57.0(5) . . ?
O5 N22 Pr2 57.4(5) . . ?
Pr1 N22 Pr2 118.2(3) . . ?
C69 C23 C66 116.1(6) . . ?
C69 C23 C24 121.5(6) . . ?
C66 C23 C24 122.4(6) . . ?
O11 C24 O10 121.4(5) . . ?
O11 C24 C23 120.9(6) . . ?
O10 C24 C23 117.6(6) . . ?
O11 C24 Pr1 62.8(3) . 3_444 ?
O10 C24 Pr1 58.7(3) . 3_444 ?
C23 C24 Pr1 175.0(4) . 3_444 ?
C62 C25 C65 117.5(6) . . ?
C62 C25 C30 121.4(6) . . ?
C65 C25 C30 121.1(7) . . ?
N19 C26 C28 126.1(4) . . ?
N19 C26 C48 107.3(4) . . ?
C28 C26 C48 126.5(4) . . ?
N21 C27 C36 125.9(4) . . ?
N21 C27 C55 107.5(4) . . ?
C36 C27 C55 126.7(4) . . ?
C26 C28 C38 125.0(4) . . ?
C26 C28 C40 116.5(4) . . ?
C38 C28 C40 118.4(4) . . ?
O8 C29 O13 122.9(5) . . ?
O8 C29 C32 121.1(5) . . ?
O13 C29 C32 116.1(5) . . ?
O8 C29 Pr2 64.0(3) . 5_566 ?
O13 C29 Pr2 59.3(2) . 5_566 ?
C32 C29 Pr2 172.1(3) . 5_566 ?
O16 C30 O9 120.3(5) . . ?
O16 C30 C25 120.9(6) . . ?
O9 C30 C25 118.8(6) . . ?
O16 C30 Pr2 64.2(3) . 7_557 ?
O9 C30 Pr2 56.2(3) . 7_557 ?
C25 C30 Pr2 173.9(4) . 7_557 ?
O12 C31 O6 120.8(5) . . ?
O12 C31 C35 122.0(5) . . ?
O6 C31 C35 117.2(6) . . ?
O12 C31 Pr1 64.1(3) . . ?
O6 C31 Pr1 57.1(3) . . ?
C35 C31 Pr1 172.3(4) . . ?
C58 C32 C59 119.8(5) . . ?
C58 C32 C29 120.7(5) . . ?
C59 C32 C29 119.5(5) . . ?
N21 C33 C53 108.2(4) . . ?
N21 C33 C45 125.0(4) . . ?
C53 C33 C45 126.8(5) . . ?
C60 C34 C61 117.8(5) . . ?
C60 C34 C36 120.4(5) . . ?
C61 C34 C36 121.8(5) . . ?
C56 C35 C52 120.6(5) . . ?
C56 C35 C31 121.4(5) . . ?
C52 C35 C31 117.9(6) . . ?
C37 C36 C27 125.9(4) . . ?
C37 C36 C34 118.1(4) . . ?
C27 C36 C34 116.0(4) . . ?
C36 C37 N18 125.4(4) . . ?
C36 C37 C50 125.5(5) . . ?
N18 C37 C50 108.9(4) . . ?
N18 C38 C28 125.9(4) . . ?
N18 C38 C51 109.1(4) . . ?
C28 C38 C51 124.9(4) . . ?
C47 C39 C43 125.3(5) . . ?
C47 C39 C42 116.3(4) . . ?
C43 C39 C42 118.3(4) . . ?
C70 C40 C67 116.0(6) . . ?
C70 C40 C28 122.8(6) . . ?
C67 C40 C28 121.1(6) . . ?
N20 C41 C45 125.3(4) . . ?
N20 C41 C54 109.9(4) . . ?
C45 C41 C54 124.7(5) . . ?
C68 C42 C64 116.8(6) . . ?
C68 C42 C39 120.3(6) . . ?
C64 C42 C39 122.9(6) . . ?
N20 C43 C39 125.8(4) . . ?
N20 C43 C49 110.0(4) . . ?
C39 C43 C49 124.1(5) . . ?
C48 C44 C47 108.3(5) . . ?
C41 C45 C33 126.2(5) . . ?
C41 C45 C46 118.2(4) . . ?
C33 C45 C46 115.5(4) . . ?
C57 C46 C63 117.8(5) . . ?
C57 C46 C45 121.9(6) . . ?
C63 C46 C45 120.3(6) . . ?
N19 C47 C39 126.3(5) . . ?
N19 C47 C44 107.5(4) . . ?
C39 C47 C44 126.1(5) . . ?
C44 C48 C26 107.6(4) . . ?
C54 C49 C43 106.5(5) . . ?
C51 C50 C37 107.4(4) . . ?
C50 C51 C38 107.6(5) . . ?
C63 C52 C35 118.4(7) . . ?
C55 C53 C33 107.3(5) . . ?
C49 C54 C41 107.1(5) . . ?
C53 C55 C27 107.8(5) . . ?
C35 C56 C57 121.4(6) . . ?
C56 C57 C46 119.8(6) . . ?
C32 C58 C60 119.8(6) . . ?
C61 C59 C32 120.2(5) . . ?
C34 C60 C58 121.9(5) . . ?
C59 C61 C34 120.5(6) . . ?
C25 C62 C64 121.2(6) . . ?
C52 C63 C46 121.9(6) . . ?
C62 C64 C42 120.8(7) . . ?
C25 C65 C68 122.5(8) . . ?
C23 C66 C67 120.9(7) . . ?
C40 C67 C66 121.4(7) . . ?
C65 C68 C42 121.2(7) . . ?
C23 C69 C70 123.0(8) . . ?
C40 C70 C69 122.2(8) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.029 -0.007 0.001 5357 1637 ' '
_platon_squeeze_details          
;
 Severely disordered water and dimethyl acetamide solvent.
;

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.42
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.981
_refine_diff_density_min         -2.077
_refine_diff_density_rms         0.128
_database_code_depnum_ccdc_archive 'CCDC 1014716'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt41sq(3)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C97 H48 N9 Na3 Nd2 O24 Zn2, 3(O)'
_chemical_formula_sum            'C97 H48 N9 Na3 Nd2 O27 Zn2'
_chemical_formula_weight         2259.68

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'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   32.9517(15)
_cell_length_b                   35.3409(16)
_cell_length_c                   11.1750(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.1820(10)
_cell_angle_gamma                90.00
_cell_volume                     12291.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    8111
_cell_measurement_theta_min      1.31
_cell_measurement_theta_max      25.31

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4488
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5405
_exptl_absorpt_correction_T_max  0.7845
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43585
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         25.31
_reflns_number_total             11384
_reflns_number_gt                8111
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The crystal contains severely disordered crystallization solvent trapped
 within the channel voids, which could not be modeled by discrete atoms.
 Its contribution to the diffraction pattern was subtracted by the Squeeze
 technique, using the PLATON software (Spek, 2009).
 The -NMe2 fragment of the metal-coordinated DMF ligand is also disordered
 and could not be modeled.
 The H-atoms of the interstitial water molecules could not be located.

;

_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)+(0.0986P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11384
_refine_ls_number_parameters     661
_refine_ls_number_restraints     260
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1761
_refine_ls_wR_factor_gt          0.1621
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_restrained_S_all      1.202
_refine_ls_shift/su_max          0.019
_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
Nd1 Nd 0.207366(12) 0.0000 0.27624(5) 0.04347(16) Uani 1 2 d SU . .
Nd2 Nd -0.261070(12) 0.0000 0.24624(5) 0.04098(16) Uani 1 2 d SU . .
Zn3 Zn -0.033686(17) -0.262439(15) 0.20193(6) 0.02767(16) Uani 1 1 d U . .
Na4 Na -0.25011(6) -0.07638(5) 0.48584(19) 0.0332(5) Uani 1 1 d U . .
Na5 Na -0.17794(9) -0.5000 0.5128(3) 0.0419(7) Uani 1 2 d SU . .
O6 O -0.22165(10) -0.45717(9) 0.3709(3) 0.0302(8) Uani 1 1 d U . .
O7 O 0.18939(10) -0.45829(9) 0.3394(3) 0.0312(8) Uani 1 1 d U . .
O8 O -0.23402(10) -0.06938(9) 0.3056(4) 0.0343(8) Uani 1 1 d U . .
O9 O 0.19275(10) -0.06889(9) 0.3323(4) 0.0361(8) Uani 1 1 d U . .
O10 O -0.22802(14) 0.0000 0.4882(5) 0.0375(12) Uani 1 2 d SU . .
O11 O -0.15853(16) 0.0000 0.5901(5) 0.0418(13) Uani 1 2 d SU . .
O12 O -0.18249(16) 0.0000 0.3782(6) 0.0432(12) Uani 1 2 d SU . .
O13 O -0.22547(12) -0.04315(9) 0.1370(3) 0.0376(8) Uani 1 1 d U . .
O14 O -0.25631(12) -0.45702(10) 0.1657(3) 0.0400(9) Uani 1 1 d U . .
O15 O 0.17537(12) -0.45764(10) 0.1336(4) 0.0405(9) Uani 1 1 d U . .
O16 O 0.14658(11) -0.04267(9) 0.1649(4) 0.0376(9) Uani 1 1 d U . .
O17 O -0.25668(15) -0.13915(11) 0.4899(5) 0.0641(13) Uani 1 1 d U . .
O18 O -0.01338(18) -0.25289(15) 0.3953(4) 0.0769(15) Uani 1 1 d U . .
O19 O -0.1099(3) -0.5000 0.5014(15) 0.179(6) Uani 1 2 d SU . .
N20 N 0.02507(12) -0.26302(10) 0.1762(4) 0.0252(8) Uani 1 1 d U . .
N21 N -0.09930(12) -0.26304(11) 0.1691(4) 0.0266(9) Uani 1 1 d U . .
N22 N -0.03723(12) -0.20449(11) 0.1708(4) 0.0261(8) Uani 1 1 d U . .
N23 N -0.03498(12) -0.32059(11) 0.1923(4) 0.0280(9) Uani 1 1 d U . .
N24 N -0.1883(2) 0.0000 0.4835(8) 0.0486(16) Uani 1 2 d SU . .
C25 C -0.00022(15) -0.34336(13) 0.2024(4) 0.0273(10) Uani 1 1 d U . .
C26 C -0.06737(16) -0.34358(13) 0.2033(5) 0.0286(11) Uani 1 1 d U . .
C27 C -0.00199(15) -0.18238(13) 0.1867(4) 0.0257(10) Uani 1 1 d U . .
C28 C 0.12947(15) -0.10394(13) 0.2223(4) 0.0270(10) Uani 1 1 d U . .
C29 C 0.16836(15) -0.44599(13) 0.2305(5) 0.0256(10) Uani 1 1 d U . .
C30 C 0.07140(15) -0.36117(14) 0.1966(5) 0.0283(11) Uani 1 1 d U . .
C31 C -0.06952(15) -0.18208(13) 0.1793(5) 0.0284(10) Uani 1 1 d U . .
C32 C 0.13458(15) -0.41658(13) 0.2177(4) 0.0265(10) Uani 1 1 d U . .
C33 C 0.15823(16) -0.07043(14) 0.2419(5) 0.0316(11) Uani 1 1 d U . .
C34 C -0.12521(15) -0.23208(14) 0.1579(5) 0.0287(11) Uani 1 1 d U . .
C35 C 0.04931(15) -0.23149(13) 0.1673(4) 0.0263(10) Uani 1 1 d U . .
C36 C -0.22611(16) -0.44489(13) 0.2595(5) 0.0292(11) Uani 1 1 d U . .
C37 C 0.03854(15) -0.33157(13) 0.1879(4) 0.0262(10) Uani 1 1 d U . .
C38 C 0.04881(14) -0.29432(13) 0.1674(4) 0.0253(10) Uani 1 1 d U . .
C39 C -0.14258(15) -0.16416(13) 0.1737(5) 0.0294(11) Uani 1 1 d U . .
C40 C -0.11130(15) -0.19408(14) 0.1670(5) 0.0294(11) Uani 1 1 d U . .
C41 C -0.10862(16) -0.33148(14) 0.1919(5) 0.0312(11) Uani 1 1 d U . .
C42 C 0.13939(15) -0.13416(14) 0.3080(5) 0.0332(12) Uani 1 1 d U . .
H42 H 0.1655 -0.1341 0.3773 0.040 Uiso 1 1 calc R . .
C43 C 0.03844(15) -0.19413(13) 0.1819(4) 0.0250(10) Uani 1 1 d U . .
C44 C -0.12426(15) -0.29420(13) 0.1674(5) 0.0295(11) Uani 1 1 d U . .
C45 C -0.05170(16) -0.38200(14) 0.2254(5) 0.0338(12) Uani 1 1 d U . .
H45 H -0.0672 -0.4033 0.2389 0.041 Uiso 1 1 calc R . .
C46 C 0.07143(15) -0.16412(13) 0.1933(5) 0.0277(10) Uani 1 1 d U . .
C47 C 0.08787(16) -0.24404(15) 0.1442(5) 0.0356(12) Uani 1 1 d U . .
H47 H 0.1093 -0.2283 0.1306 0.043 Uiso 1 1 calc R . .
C48 C -0.18321(16) -0.13218(14) 0.2872(5) 0.0341(12) Uani 1 1 d U . .
H48 H -0.1931 -0.1311 0.3579 0.041 Uiso 1 1 calc R . .
C49 C -0.19642(16) -0.41577(13) 0.2400(5) 0.0298(11) Uani 1 1 d U . .
C50 C -0.19477(15) -0.10412(13) 0.1959(5) 0.0293(11) Uani 1 1 d U . .
C51 C 0.08773(16) -0.28221(14) 0.1454(5) 0.0349(12) Uani 1 1 d U . .
H51 H 0.1093 -0.2983 0.1340 0.042 Uiso 1 1 calc R . .
C52 C -0.05413(16) -0.14374(14) 0.2062(5) 0.0328(11) Uani 1 1 d U . .
H52 H -0.0701 -0.1225 0.2180 0.039 Uiso 1 1 calc R . .
C53 C -0.21932(15) -0.07058(14) 0.2133(5) 0.0311(10) Uani 1 1 d U . .
C54 C -0.01087(17) -0.38198(14) 0.2234(5) 0.0374(12) Uani 1 1 d U . .
H54 H 0.0074 -0.4034 0.2339 0.045 Uiso 1 1 calc R . .
C55 C -0.13936(16) -0.36102(14) 0.2065(5) 0.0309(11) Uani 1 1 d U . .
C56 C 0.11099(16) -0.16421(14) 0.2915(5) 0.0353(12) Uani 1 1 d U . .
H56 H 0.1185 -0.1852 0.3477 0.042 Uiso 1 1 calc R . .
C57 C -0.16833(17) -0.24425(15) 0.1406(6) 0.0419(14) Uani 1 1 d U . .
H57 H -0.1927 -0.2284 0.1260 0.050 Uiso 1 1 calc R . .
C58 C -0.01228(16) -0.14395(14) 0.2115(5) 0.0335(12) Uani 1 1 d U . .
H58 H 0.0066 -0.1229 0.2282 0.040 Uiso 1 1 calc R . .
C59 C -0.18147(16) -0.10684(14) 0.0909(5) 0.0339(12) Uani 1 1 d U . .
H59 H -0.1901 -0.0882 0.0261 0.041 Uiso 1 1 calc R . .
C60 C -0.15584(16) -0.13639(15) 0.0800(5) 0.0341(12) Uani 1 1 d U . .
H60 H -0.1470 -0.1380 0.0074 0.041 Uiso 1 1 calc R . .
C61 C 0.06273(16) -0.13406(15) 0.1085(5) 0.0364(12) Uani 1 1 d U . .
H61 H 0.0366 -0.1339 0.0393 0.044 Uiso 1 1 calc R . .
C62 C -0.15712(17) -0.16203(15) 0.2758(5) 0.0369(12) Uani 1 1 d U . .
H62 H -0.1493 -0.1811 0.3392 0.044 Uiso 1 1 calc R . .
C63 C -0.16791(17) -0.28280(15) 0.1489(5) 0.0426(13) Uani 1 1 d U . .
H63 H -0.1916 -0.2988 0.1436 0.051 Uiso 1 1 calc R . .
C64 C 0.09128(16) -0.10437(15) 0.1226(5) 0.0334(12) Uani 1 1 d U . .
H64 H 0.0846 -0.0842 0.0633 0.040 Uiso 1 1 calc R . .
C65 C -0.20009(18) -0.40242(17) 0.1235(5) 0.0464(15) Uani 1 1 d U . .
H65 H -0.2221 -0.4121 0.0518 0.056 Uiso 1 1 calc R . .
C66 C -0.17280(19) -0.37532(17) 0.1062(5) 0.0484(15) Uani 1 1 d U . .
H66 H -0.1770 -0.3661 0.0232 0.058 Uiso 1 1 calc R . .
C67 C 0.0000 -0.2646(2) 0.5000 0.057(2) Uani 1 2 d SU . .
C68 C -0.1645(2) -0.4011(2) 0.3401(6) 0.076(3) Uani 1 1 d U . .
H68 H -0.1617 -0.4093 0.4235 0.092 Uiso 1 1 calc R . .
C69 C -0.1362(3) -0.3745(2) 0.3227(6) 0.081(3) Uani 1 1 d U . .
H69 H -0.1139 -0.3654 0.3945 0.097 Uiso 1 1 calc R . .
C70 C 0.0772(3) -0.3776(3) 0.0953(6) 0.097(3) Uani 1 1 d U . .
H70 H 0.0592 -0.3703 0.0132 0.116 Uiso 1 1 calc R . .
C71 C 0.1083(3) -0.4047(3) 0.1053(6) 0.096(3) Uani 1 1 d U . .
H71 H 0.1112 -0.4152 0.0302 0.116 Uiso 1 1 calc R . .
C72 C 0.0985(3) -0.3722(3) 0.3071(6) 0.101(7) Uani 1 1 d U . .
H72 H 0.0962 -0.3612 0.3822 0.121 Uiso 1 1 calc R . .
C73 C 0.1301(3) -0.3993(3) 0.3178(7) 0.099(6) Uani 1 1 d U . .
H73 H 0.1491 -0.4056 0.3996 0.120 Uiso 1 1 calc R . .
O74 O 0.13963(17) -0.5000 -0.0438(5) 0.0434(13) Uani 1 2 d S . .
O75 O 0.10633(16) 0.0000 0.0016(5) 0.0410(13) Uani 1 2 d S . .
O76 O -0.2323(2) 0.0000 -0.0108(6) 0.069(2) Uani 1 2 d SU . .


_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
Nd1 O16 2.489(3) 6 ?
Nd1 O16 2.489(3) . ?
Nd1 O10 2.493(5) 5_556 ?
Nd1 O14 2.497(4) 8_545 ?
Nd1 O14 2.497(4) 3 ?
Nd1 O11 2.529(5) 5_556 ?
Nd1 O9 2.598(3) . ?
Nd1 O9 2.598(3) 6 ?
Nd1 O6 2.694(3) 3 ?
Nd1 O6 2.694(3) 8_545 ?
Nd1 C33 2.925(5) . ?
Nd1 C33 2.925(5) 6 ?
Nd2 O13 2.476(4) . ?
Nd2 O13 2.476(4) 6 ?
Nd2 O12 2.524(5) . ?
Nd2 O15 2.546(3) 8_445 ?
Nd2 O15 2.546(3) 3_455 ?
Nd2 O10 2.561(5) . ?
Nd2 O8 2.619(3) 6 ?
Nd2 O8 2.619(3) . ?
Nd2 O7 2.653(3) 8_445 ?
Nd2 O7 2.653(3) 3_455 ?
Nd2 C53 2.929(5) . ?
Zn3 N20 2.049(4) . ?
Zn3 N23 2.057(4) . ?
Zn3 O18 2.069(5) . ?
Zn3 N21 2.071(4) . ?
Zn3 N22 2.074(4) . ?
Na4 O17 2.231(4) . ?
Na4 O8 2.258(4) . ?
Na4 O9 2.291(4) 2_556 ?
Na4 O6 2.411(4) 7_446 ?
Na4 O7 2.452(4) 8_445 ?
Na4 O10 2.794(2) . ?
Na4 Na5 3.596(3) 7_446 ?
Na4 Nd1 3.725(2) 5_556 ?
Na5 O19 2.288(10) . ?
Na5 O6 2.319(4) . ?
Na5 O6 2.319(4) 6_545 ?
Na5 O7 2.336(4) 2_556 ?
Na5 O7 2.336(4) 5_546 ?
Na5 Na4 3.596(3) 4_446 ?
Na5 Na4 3.596(3) 7_446 ?
Na5 Nd1 3.835(3) 3_445 ?
Na5 Nd2 3.853(3) 7_446 ?
O6 C36 1.281(6) . ?
O6 Na4 2.411(4) 7_446 ?
O6 Nd1 2.694(3) 3_445 ?
O7 C29 1.263(6) . ?
O7 Na5 2.336(4) 5_546 ?
O7 Na4 2.452(4) 8_545 ?
O7 Nd2 2.653(3) 3_545 ?
O8 C53 1.276(6) . ?
O9 C33 1.250(6) . ?
O9 Na4 2.291(4) 2_556 ?
O10 N24 1.327(8) . ?
O10 Nd1 2.493(5) 5_556 ?
O10 Na4 2.794(2) 6 ?
O11 N24 1.271(9) . ?
O11 Nd1 2.529(5) 5_556 ?
O12 N24 1.252(9) . ?
O13 C53 1.263(6) . ?
O14 C36 1.259(6) . ?
O14 Nd1 2.497(4) 3_445 ?
O15 C29 1.249(6) . ?
O15 Nd2 2.546(3) 3_545 ?
O16 C33 1.278(6) . ?
O18 C67 1.181(5) . ?
N20 C38 1.377(6) . ?
N20 C35 1.394(6) . ?
N21 C34 1.368(6) . ?
N21 C44 1.371(6) . ?
N22 C31 1.355(6) . ?
N22 C27 1.362(6) . ?
N23 C25 1.374(6) . ?
N23 C26 1.378(6) . ?
N24 Nd1 2.952(9) 5_556 ?
C25 C37 1.403(7) . ?
C25 C54 1.448(7) . ?
C26 C41 1.390(7) . ?
C26 C45 1.445(6) . ?
C27 C43 1.413(7) . ?
C27 C58 1.448(7) . ?
C28 C64 1.380(7) . ?
C28 C42 1.399(7) . ?
C28 C33 1.487(7) . ?
C29 C32 1.495(6) . ?
C29 Nd2 2.969(5) 3_545 ?
C30 C72 1.322(8) . ?
C30 C70 1.342(8) . ?
C30 C37 1.486(7) . ?
C31 C40 1.403(7) . ?
C31 C52 1.444(7) . ?
C32 C73 1.325(8) . ?
C32 C71 1.337(8) . ?
C34 C40 1.412(7) . ?
C34 C57 1.436(7) . ?
C35 C43 1.392(6) . ?
C35 C47 1.447(7) . ?
C36 C49 1.485(7) . ?
C36 Nd1 2.984(5) 3_445 ?
C37 C38 1.397(7) . ?
C38 C51 1.447(7) . ?
C39 C62 1.377(7) . ?
C39 C60 1.397(7) . ?
C39 C40 1.496(7) . ?
C41 C44 1.408(7) . ?
C41 C55 1.500(7) . ?
C42 C56 1.387(7) . ?
C43 C46 1.494(6) . ?
C44 C63 1.442(7) . ?
C45 C54 1.353(7) . ?
C46 C61 1.389(7) . ?
C46 C56 1.401(7) . ?
C47 C51 1.349(7) . ?
C48 C50 1.383(7) . ?
C48 C62 1.393(7) . ?
C49 C65 1.352(7) . ?
C49 C68 1.361(8) . ?
C50 C59 1.385(7) . ?
C50 C53 1.484(7) . ?
C52 C58 1.361(7) . ?
C55 C69 1.356(8) . ?
C55 C66 1.383(7) . ?
C57 C63 1.365(7) . ?
C59 C60 1.373(7) . ?
C61 C64 1.383(7) . ?
C65 C66 1.370(7) . ?
C67 O18 1.181(5) 2_556 ?
C68 C69 1.382(8) . ?
C70 C71 1.379(8) . ?
C72 C73 1.389(9) . ?

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
O16 Nd1 O16 74.58(16) 6 . ?
O16 Nd1 O10 115.05(11) 6 5_556 ?
O16 Nd1 O10 115.05(11) . 5_556 ?
O16 Nd1 O14 123.99(12) 6 8_545 ?
O16 Nd1 O14 79.75(12) . 8_545 ?
O10 Nd1 O14 120.88(11) 5_556 8_545 ?
O16 Nd1 O14 79.75(12) 6 3 ?
O16 Nd1 O14 123.99(12) . 3 ?
O10 Nd1 O14 120.88(11) 5_556 3 ?
O14 Nd1 O14 74.92(17) 8_545 3 ?
O16 Nd1 O11 74.44(13) 6 5_556 ?
O16 Nd1 O11 74.44(13) . 5_556 ?
O10 Nd1 O11 51.86(16) 5_556 5_556 ?
O14 Nd1 O11 142.49(8) 8_545 5_556 ?
O14 Nd1 O11 142.49(8) 3 5_556 ?
O16 Nd1 O9 120.39(11) 6 . ?
O16 Nd1 O9 50.98(11) . . ?
O10 Nd1 O9 75.71(9) 5_556 . ?
O14 Nd1 O9 72.92(11) 8_545 . ?
O14 Nd1 O9 147.80(12) 3 . ?
O11 Nd1 O9 69.71(8) 5_556 . ?
O16 Nd1 O9 50.98(11) 6 6 ?
O16 Nd1 O9 120.39(11) . 6 ?
O10 Nd1 O9 75.71(9) 5_556 6 ?
O14 Nd1 O9 147.80(12) 8_545 6 ?
O14 Nd1 O9 72.92(11) 3 6 ?
O11 Nd1 O9 69.72(8) 5_556 6 ?
O9 Nd1 O9 139.13(16) . 6 ?
O16 Nd1 O6 107.94(11) 6 3 ?
O16 Nd1 O6 171.51(11) . 3 ?
O10 Nd1 O6 71.62(11) 5_556 3 ?
O14 Nd1 O6 92.33(11) 8_545 3 ?
O14 Nd1 O6 49.99(11) 3 3 ?
O11 Nd1 O6 114.00(12) 5_556 3 ?
O9 Nd1 O6 129.62(10) . 3 ?
O9 Nd1 O6 65.44(10) 6 3 ?
O16 Nd1 O6 171.51(11) 6 8_545 ?
O16 Nd1 O6 107.94(11) . 8_545 ?
O10 Nd1 O6 71.62(11) 5_556 8_545 ?
O14 Nd1 O6 49.99(11) 8_545 8_545 ?
O14 Nd1 O6 92.33(11) 3 8_545 ?
O11 Nd1 O6 114.00(12) 5_556 8_545 ?
O9 Nd1 O6 65.44(10) . 8_545 ?
O9 Nd1 O6 129.62(10) 6 8_545 ?
O6 Nd1 O6 68.39(14) 3 8_545 ?
O16 Nd1 C33 97.48(13) 6 . ?
O16 Nd1 C33 25.73(13) . . ?
O10 Nd1 C33 94.91(12) 5_556 . ?
O14 Nd1 C33 75.66(13) 8_545 . ?
O14 Nd1 C33 141.94(13) 3 . ?
O11 Nd1 C33 69.22(11) 5_556 . ?
O9 Nd1 C33 25.28(12) . . ?
O9 Nd1 C33 133.67(12) 6 . ?
O6 Nd1 C33 154.35(12) 3 . ?
O6 Nd1 C33 86.85(12) 8_545 . ?
O16 Nd1 C33 25.74(13) 6 6 ?
O16 Nd1 C33 97.49(13) . 6 ?
O10 Nd1 C33 94.91(12) 5_556 6 ?
O14 Nd1 C33 141.94(13) 8_545 6 ?
O14 Nd1 C33 75.66(13) 3 6 ?
O11 Nd1 C33 69.22(11) 5_556 6 ?
O9 Nd1 C33 133.67(12) . 6 ?
O9 Nd1 C33 25.27(12) 6 6 ?
O6 Nd1 C33 86.84(12) 3 6 ?
O6 Nd1 C33 154.35(12) 8_545 6 ?
C33 Nd1 C33 116.64(19) . 6 ?
O13 Nd2 O13 76.02(16) . 6 ?
O13 Nd2 O12 74.15(13) . . ?
O13 Nd2 O12 74.15(13) 6 . ?
O13 Nd2 O15 80.80(12) . 8_445 ?
O13 Nd2 O15 124.36(12) 6 8_445 ?
O12 Nd2 O15 143.94(9) . 8_445 ?
O13 Nd2 O15 124.36(12) . 3_455 ?
O13 Nd2 O15 80.80(12) 6 3_455 ?
O12 Nd2 O15 143.94(9) . 3_455 ?
O15 Nd2 O15 72.04(17) 8_445 3_455 ?
O13 Nd2 O10 114.47(11) . . ?
O13 Nd2 O10 114.47(11) 6 . ?
O12 Nd2 O10 52.00(17) . . ?
O15 Nd2 O10 121.16(11) 8_445 . ?
O15 Nd2 O10 121.16(11) 3_455 . ?
O13 Nd2 O8 121.64(11) . 6 ?
O13 Nd2 O8 51.06(11) 6 6 ?
O12 Nd2 O8 69.73(7) . 6 ?
O15 Nd2 O8 146.32(11) 8_445 6 ?
O15 Nd2 O8 74.39(11) 3_455 6 ?
O10 Nd2 O8 75.00(9) . 6 ?
O13 Nd2 O8 51.06(11) . . ?
O13 Nd2 O8 121.64(11) 6 . ?
O12 Nd2 O8 69.73(7) . . ?
O15 Nd2 O8 74.39(11) 8_445 . ?
O15 Nd2 O8 146.32(11) 3_455 . ?
O10 Nd2 O8 75.00(9) . . ?
O8 Nd2 O8 138.87(15) 6 . ?
O13 Nd2 O7 107.66(11) . 8_445 ?
O13 Nd2 O7 171.03(11) 6 8_445 ?
O12 Nd2 O7 114.59(13) . 8_445 ?
O15 Nd2 O7 49.82(11) 8_445 8_445 ?
O15 Nd2 O7 90.48(11) 3_455 8_445 ?
O10 Nd2 O7 71.88(11) . 8_445 ?
O8 Nd2 O7 128.53(11) 6 8_445 ?
O8 Nd2 O7 65.31(10) . 8_445 ?
O13 Nd2 O7 171.03(11) . 3_455 ?
O13 Nd2 O7 107.66(11) 6 3_455 ?
O12 Nd2 O7 114.59(13) . 3_455 ?
O15 Nd2 O7 90.48(11) 8_445 3_455 ?
O15 Nd2 O7 49.82(11) 3_455 3_455 ?
O10 Nd2 O7 71.88(11) . 3_455 ?
O8 Nd2 O7 65.31(10) 6 3_455 ?
O8 Nd2 O7 128.53(11) . 3_455 ?
O7 Nd2 O7 67.52(14) 8_445 3_455 ?
O13 Nd2 C53 25.28(13) . . ?
O13 Nd2 C53 98.30(13) 6 . ?
O12 Nd2 C53 68.86(11) . . ?
O15 Nd2 C53 77.37(13) 8_445 . ?
O15 Nd2 C53 141.51(13) 3_455 . ?
O10 Nd2 C53 94.48(11) . . ?
O8 Nd2 C53 133.97(12) 6 . ?
O8 Nd2 C53 25.82(12) . . ?
O7 Nd2 C53 87.19(12) 8_445 . ?
O7 Nd2 C53 153.81(13) 3_455 . ?
N20 Zn3 N23 89.25(15) . . ?
N20 Zn3 O18 98.73(19) . . ?
N23 Zn3 O18 102.20(18) . . ?
N20 Zn3 N21 162.72(16) . . ?
N23 Zn3 N21 88.74(15) . . ?
O18 Zn3 N21 98.46(19) . . ?
N20 Zn3 N22 89.43(15) . . ?
N23 Zn3 N22 168.06(16) . . ?
O18 Zn3 N22 89.73(18) . . ?
N21 Zn3 N22 88.99(15) . . ?
O17 Na4 O8 100.35(17) . . ?
O17 Na4 O9 98.87(16) . 2_556 ?
O8 Na4 O9 114.29(15) . 2_556 ?
O17 Na4 O6 114.48(17) . 7_446 ?
O8 Na4 O6 142.48(14) . 7_446 ?
O9 Na4 O6 74.95(13) 2_556 7_446 ?
O17 Na4 O7 116.57(16) . 8_445 ?
O8 Na4 O7 74.19(13) . 8_445 ?
O9 Na4 O7 141.96(14) 2_556 8_445 ?
O6 Na4 O7 77.93(13) 7_446 8_445 ?
O17 Na4 O10 170.89(17) . . ?
O8 Na4 O10 76.45(14) . . ?
O9 Na4 O10 75.14(14) 2_556 . ?
O6 Na4 O10 71.03(13) 7_446 . ?
O7 Na4 O10 71.08(13) 8_445 . ?
O17 Na4 Na5 132.68(15) . 7_446 ?
O8 Na4 Na5 105.66(11) . 7_446 ?
O9 Na4 Na5 105.22(11) 2_556 7_446 ?
O6 Na4 Na5 39.57(10) 7_446 7_446 ?
O7 Na4 Na5 40.10(9) 8_445 7_446 ?
O10 Na4 Na5 56.28(10) . 7_446 ?
O17 Na4 Nd1 136.27(15) . 5_556 ?
O8 Na4 Nd1 114.37(11) . 5_556 ?
O9 Na4 Nd1 43.53(9) 2_556 5_556 ?
O6 Na4 Nd1 46.19(8) 7_446 5_556 ?
O7 Na4 Nd1 98.53(9) 8_445 5_556 ?
O10 Na4 Nd1 42.01(11) . 5_556 ?
Na5 Na4 Nd1 63.14(5) 7_446 5_556 ?
O17 Na4 Nd2 138.24(15) . . ?
O8 Na4 Nd2 43.72(9) . . ?
O9 Na4 Nd2 114.19(11) 2_556 . ?
O6 Na4 Nd2 98.80(9) 7_446 . ?
O7 Na4 Nd2 45.12(8) 8_445 . ?
O10 Na4 Nd2 43.28(11) . . ?
Na5 Na4 Nd2 63.38(6) 7_446 . ?
Nd1 Na4 Nd2 85.00(4) 5_556 . ?
O19 Na5 O6 111.2(3) . . ?
O19 Na5 O6 111.2(3) . 6_545 ?
O6 Na5 O6 81.49(19) . 6_545 ?
O19 Na5 O7 115.4(3) . 2_556 ?
O6 Na5 O7 82.13(13) . 2_556 ?
O6 Na5 O7 133.40(17) 6_545 2_556 ?
O19 Na5 O7 115.4(3) . 5_546 ?
O6 Na5 O7 133.40(17) . 5_546 ?
O6 Na5 O7 82.13(13) 6_545 5_546 ?
O7 Na5 O7 78.28(19) 2_556 5_546 ?
O19 Na5 Na4 131.30(5) . 4_446 ?
O6 Na5 Na4 103.33(12) . 4_446 ?
O6 Na5 Na4 41.46(9) 6_545 4_446 ?
O7 Na5 Na4 102.17(13) 2_556 4_446 ?
O7 Na5 Na4 42.55(9) 5_546 4_446 ?
O19 Na5 Na4 131.30(5) . 7_446 ?
O6 Na5 Na4 41.47(9) . 7_446 ?
O6 Na5 Na4 103.32(12) 6_545 7_446 ?
O7 Na5 Na4 42.55(9) 2_556 7_446 ?
O7 Na5 Na4 102.17(13) 5_546 7_446 ?
Na4 Na5 Na4 97.28(9) 4_446 7_446 ?
O19 Na5 Nd1 136.4(4) . 3_445 ?
O6 Na5 Nd1 43.84(9) . 3_445 ?
O6 Na5 Nd1 43.84(9) 6_545 3_445 ?
O7 Na5 Nd1 97.82(11) 2_556 3_445 ?
O7 Na5 Nd1 97.82(11) 5_546 3_445 ?
Na4 Na5 Nd1 60.07(5) 4_446 3_445 ?
Na4 Na5 Nd1 60.07(5) 7_446 3_445 ?
O19 Na5 Nd2 141.7(4) . 7_446 ?
O6 Na5 Nd2 97.36(12) . 7_446 ?
O6 Na5 Nd2 97.36(12) 6_545 7_446 ?
O7 Na5 Nd2 42.53(10) 2_556 7_446 ?
O7 Na5 Nd2 42.53(10) 5_546 7_446 ?
Na4 Na5 Nd2 60.06(6) 4_446 7_446 ?
Na4 Na5 Nd2 60.06(6) 7_446 7_446 ?
Nd1 Na5 Nd2 81.92(6) 3_445 7_446 ?
C36 O6 Na5 137.1(3) . . ?
C36 O6 Na4 122.2(3) . 7_446 ?
Na5 O6 Na4 98.96(15) . 7_446 ?
C36 O6 Nd1 90.0(3) . 3_445 ?
Na5 O6 Nd1 99.55(12) . 3_445 ?
Na4 O6 Nd1 93.58(12) 7_446 3_445 ?
C29 O7 Na5 137.2(3) . 5_546 ?
C29 O7 Na4 122.7(3) . 8_545 ?
Na5 O7 Na4 97.35(14) 5_546 8_545 ?
C29 O7 Nd2 91.6(3) . 3_545 ?
Na5 O7 Nd2 100.95(12) 5_546 3_545 ?
Na4 O7 Nd2 93.97(11) 8_545 3_545 ?
C53 O8 Na4 168.5(3) . . ?
C53 O8 Nd2 90.8(3) . . ?
Na4 O8 Nd2 99.70(13) . . ?
C33 O9 Na4 168.1(3) . 2_556 ?
C33 O9 Nd1 92.1(3) . . ?
Na4 O9 Nd1 99.09(12) 2_556 . ?
N24 O10 Nd1 96.4(5) . 5_556 ?
N24 O10 Nd2 92.3(5) . . ?
Nd1 O10 Nd2 171.3(2) 5_556 . ?
N24 O10 Na4 104.89(10) . 6 ?
Nd1 O10 Na4 89.41(12) 5_556 6 ?
Nd2 O10 Na4 88.34(11) . 6 ?
N24 O10 Na4 104.89(10) . . ?
Nd1 O10 Na4 89.41(12) 5_556 . ?
Nd2 O10 Na4 88.34(11) . . ?
Na4 O10 Na4 150.14(19) 6 . ?
N24 O11 Nd1 96.3(4) . 5_556 ?
N24 O12 Nd2 96.0(4) . . ?
C53 O13 Nd2 97.8(3) . . ?
C36 O14 Nd1 99.9(3) . 3_445 ?
C29 O15 Nd2 97.0(3) . 3_545 ?
C33 O16 Nd1 96.5(3) . . ?
C67 O18 Zn3 149.9(6) . . ?
C38 N20 C35 106.5(4) . . ?
C38 N20 Zn3 127.1(3) . . ?
C35 N20 Zn3 126.3(3) . . ?
C34 N21 C44 106.7(4) . . ?
C34 N21 Zn3 126.3(3) . . ?
C44 N21 Zn3 126.7(3) . . ?
C31 N22 C27 108.1(4) . . ?
C31 N22 Zn3 124.6(3) . . ?
C27 N22 Zn3 123.1(3) . . ?
C25 N23 C26 107.2(4) . . ?
C25 N23 Zn3 125.3(3) . . ?
C26 N23 Zn3 126.0(3) . . ?
O12 N24 O11 124.9(7) . . ?
O12 N24 O10 119.6(7) . . ?
O11 N24 O10 115.5(7) . . ?
O12 N24 Nd2 58.9(4) . . ?
O11 N24 Nd2 176.2(6) . . ?
O10 N24 Nd2 60.8(4) . . ?
O12 N24 Nd1 176.7(5) . 5_556 ?
O11 N24 Nd1 58.4(4) . 5_556 ?
O10 N24 Nd1 57.1(4) . 5_556 ?
Nd2 N24 Nd1 117.8(2) . 5_556 ?
N23 C25 C37 125.6(4) . . ?
N23 C25 C54 109.0(4) . . ?
C37 C25 C54 125.3(4) . . ?
N23 C26 C41 124.9(4) . . ?
N23 C26 C45 109.0(4) . . ?
C41 C26 C45 126.0(4) . . ?
N22 C27 C43 126.9(4) . . ?
N22 C27 C58 108.7(4) . . ?
C43 C27 C58 124.4(4) . . ?
C64 C28 C42 119.3(4) . . ?
C64 C28 C33 119.7(5) . . ?
C42 C28 C33 120.8(4) . . ?
O15 C29 O7 121.5(4) . . ?
O15 C29 C32 119.3(4) . . ?
O7 C29 C32 119.2(4) . . ?
O15 C29 Nd2 58.3(2) . 3_545 ?
O7 C29 Nd2 63.3(2) . 3_545 ?
C32 C29 Nd2 175.4(3) . 3_545 ?
C72 C30 C70 114.9(5) . . ?
C72 C30 C37 121.5(5) . . ?
C70 C30 C37 123.6(5) . . ?
N22 C31 C40 125.8(4) . . ?
N22 C31 C52 109.5(4) . . ?
C40 C31 C52 124.8(4) . . ?
C73 C32 C71 115.5(5) . . ?
C73 C32 C29 121.8(5) . . ?
C71 C32 C29 122.7(5) . . ?
O9 C33 O16 120.2(4) . . ?
O9 C33 C28 121.4(5) . . ?
O16 C33 C28 118.4(4) . . ?
O9 C33 Nd1 62.6(2) . . ?
O16 C33 Nd1 57.7(2) . . ?
C28 C33 Nd1 174.4(3) . . ?
N21 C34 C40 125.2(4) . . ?
N21 C34 C57 109.5(4) . . ?
C40 C34 C57 125.3(4) . . ?
C43 C35 N20 125.1(4) . . ?
C43 C35 C47 125.9(4) . . ?
N20 C35 C47 109.0(4) . . ?
O14 C36 O6 120.0(4) . . ?
O14 C36 C49 119.5(5) . . ?
O6 C36 C49 120.5(5) . . ?
O14 C36 Nd1 55.5(3) . 3_445 ?
O6 C36 Nd1 64.5(3) . 3_445 ?
C49 C36 Nd1 174.2(4) . 3_445 ?
C38 C37 C25 125.3(4) . . ?
C38 C37 C30 117.6(4) . . ?
C25 C37 C30 117.1(4) . . ?
N20 C38 C37 124.8(4) . . ?
N20 C38 C51 109.3(4) . . ?
C37 C38 C51 125.6(4) . . ?
C62 C39 C60 118.4(5) . . ?
C62 C39 C40 120.9(4) . . ?
C60 C39 C40 120.7(4) . . ?
C31 C40 C34 125.4(4) . . ?
C31 C40 C39 116.8(4) . . ?
C34 C40 C39 117.6(4) . . ?
C26 C41 C44 126.1(5) . . ?
C26 C41 C55 116.8(4) . . ?
C44 C41 C55 117.1(4) . . ?
C56 C42 C28 119.9(4) . . ?
C35 C43 C27 124.4(4) . . ?
C35 C43 C46 118.4(4) . . ?
C27 C43 C46 117.2(4) . . ?
N21 C44 C41 124.7(4) . . ?
N21 C44 C63 110.1(4) . . ?
C41 C44 C63 125.0(5) . . ?
C54 C45 C26 107.3(4) . . ?
C61 C46 C56 117.8(4) . . ?
C61 C46 C43 120.2(4) . . ?
C56 C46 C43 121.9(4) . . ?
C51 C47 C35 107.4(4) . . ?
C50 C48 C62 120.3(5) . . ?
C65 C49 C68 117.4(5) . . ?
C65 C49 C36 121.9(5) . . ?
C68 C49 C36 120.7(5) . . ?
C48 C50 C59 119.2(5) . . ?
C48 C50 C53 120.4(5) . . ?
C59 C50 C53 120.3(4) . . ?
C47 C51 C38 107.7(4) . . ?
C58 C52 C31 106.6(4) . . ?
O13 C53 O8 120.1(5) . . ?
O13 C53 C50 119.9(5) . . ?
O8 C53 C50 120.0(4) . . ?
O13 C53 Nd2 56.9(3) . . ?
O8 C53 Nd2 63.4(2) . . ?
C50 C53 Nd2 174.6(3) . . ?
C45 C54 C25 107.4(4) . . ?
C69 C55 C66 115.9(5) . . ?
C69 C55 C41 120.5(5) . . ?
C66 C55 C41 123.6(5) . . ?
C42 C56 C46 121.1(5) . . ?
C63 C57 C34 107.6(4) . . ?
C52 C58 C27 107.1(4) . . ?
C60 C59 C50 120.2(5) . . ?
C59 C60 C39 121.2(5) . . ?
C64 C61 C46 121.5(5) . . ?
C39 C62 C48 120.7(5) . . ?
C57 C63 C44 106.0(5) . . ?
C28 C64 C61 120.4(5) . . ?
C49 C65 C66 121.6(5) . . ?
C65 C66 C55 121.8(5) . . ?
O18 C67 O18 139.1(10) 2_556 . ?
C49 C68 C69 121.1(6) . . ?
C55 C69 C68 122.2(6) . . ?
C30 C70 C71 122.7(6) . . ?
C32 C71 C70 121.9(6) . . ?
C30 C72 C73 122.7(6) . . ?
C32 C73 C72 122.3(6) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 -0.003 -0.017 3722 964 ' '
2 0.000 0.500 0.509 499 115 ' '
3 0.500 0.000 0.376 499 115 ' '
_platon_squeeze_details          
;
 disordered crystallization solvent (DMA + water)
;
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.31
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.823
_refine_diff_density_min         -2.734
_refine_diff_density_rms         0.127
_database_code_depnum_ccdc_archive 'CCDC 1014717'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt43sq(4)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C97 H54 N9 Na4 O26 Sm2 Zn2'
_chemical_formula_sum            'C97 H54 N9 Na4 O26 Sm2 Zn2'
_chemical_formula_weight         2284.96

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   32.8029(17)
_cell_length_b                   35.0128(18)
_cell_length_c                   11.4791(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.1980(9)
_cell_angle_gamma                90.00
_cell_volume                     12373.2(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9470
_cell_measurement_theta_min      1.76
_cell_measurement_theta_max      25.38

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4540
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7217
_exptl_absorpt_correction_T_max  0.8730
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43885
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.38
_reflns_number_total             11388
_reflns_number_gt                9470
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The crystal contains severely disordered crystallization solvent trapped
 within the channel voids, which could not be modeled by discrete atoms.
 Its contribution to the diffraction pattern was subtracted by the Squeeze
 technique, using the PLATON software (Spek, 2009).
 Some of the water protons couldn't be located.
;

_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)+(0.0645P)²+9.7661P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11388
_refine_ls_number_parameters     649
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1088
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.002
_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
Sm1 Sm 0.205378(8) 0.0000 0.78887(2) 0.01072(8) Uani 1 2 d SU . .
Sm2 Sm 0.262709(8) 0.0000 1.23385(2) 0.01112(8) Uani 1 2 d SU . .
Zn3 Zn -0.036691(13) -0.262435(12) 0.70667(3) 0.01235(11) Uani 1 1 d U . .
Na4 Na -0.25077(5) -0.07734(4) 0.98946(11) 0.0163(3) Uani 1 1 d U . .
Na5 Na -0.17572(7) -0.5000 1.00371(17) 0.0217(5) Uani 1 2 d SU . .
Na6 Na -0.23190(8) 0.0000 0.49452(16) 0.0228(5) Uani 1 2 d SU . .
O7 O -0.22499(8) -0.45778(7) 0.8663(2) 0.0141(5) Uani 1 1 d U . .
O8 O -0.26200(8) -0.45845(7) 0.6657(2) 0.0139(5) Uani 1 1 d U . .
O9 O -0.23592(8) -0.06826(7) 0.8132(2) 0.0170(6) Uani 1 1 d U . .
O10 O 0.18264(12) 0.0000 1.1204(3) 0.0187(8) Uani 1 2 d SU . .
O11 O -0.23257(8) -0.04177(7) 0.6424(2) 0.0152(6) Uani 1 1 d U . .
O12 O 0.18803(8) -0.45916(7) 0.8477(2) 0.0153(6) Uani 1 1 d U . .
O13 O 0.17544(9) -0.45790(8) 0.6465(2) 0.0208(6) Uani 1 1 d U . .
O14 O 0.15603(11) 0.0000 0.9108(3) 0.0218(8) Uani 1 2 d SU . .
O15 O 0.22663(11) 0.0000 1.0108(3) 0.0180(8) Uani 1 2 d SU . .
O16 O 0.14574(8) -0.04216(7) 0.6677(2) 0.0181(6) Uani 1 1 d U . .
O17 O 0.19120(8) -0.06840(7) 0.8365(2) 0.0174(6) Uani 1 1 d U . .
O18 O -0.31197(15) 0.0000 0.4454(3) 0.0340(10) Uani 1 2 d SU . .
H18 H -0.3238 -0.0214 0.4631 0.041 Uiso 1 1 d R . .
O19 O -0.01460(14) -0.25576(11) 0.8975(3) 0.0631(12) Uani 1 1 d U . .
O20 O -0.25817(13) -0.14026(10) 0.9964(3) 0.0593(10) Uani 1 1 d U . .
O21 O -0.15589(18) 0.0000 0.5484(6) 0.072(2) Uani 1 2 d SU . .
H21 H -0.1555 -0.0214 0.5923 0.086 Uiso 1 1 d R . .
O22 O -0.1098(3) -0.5000 1.0111(9) 0.054(4) Uiso 1 2 d SU . .
H22A H -0.0936 -0.5000 1.0922 0.081 Uiso 1 2 d SR . .
H22B H -0.0937 -0.5000 0.9614 0.081 Uiso 1 2 d SR . .
N23 N -0.03915(10) -0.32105(9) 0.6923(3) 0.0139(6) Uani 1 1 d U . .
N24 N -0.03991(10) -0.20423(9) 0.6730(2) 0.0134(6) Uani 1 1 d U . .
N25 N 0.02179(10) -0.26346(8) 0.6761(2) 0.0122(6) Uani 1 1 d U . .
N26 N -0.10296(10) -0.26224(8) 0.6718(2) 0.0131(6) Uani 1 1 d U . .
N27 N 0.18625(17) 0.0000 1.0140(4) 0.0289(11) Uani 1 2 d SU . .
C29 C -0.23118(12) -0.44593(10) 0.7563(3) 0.0135(8) Uani 1 1 d U . .
C30 C -0.22374(12) -0.06936(11) 0.7181(3) 0.0148(8) Uani 1 1 d U . .
C31 C -0.20164(12) -0.41626(10) 0.7358(3) 0.0128(8) Uani 1 1 d U . .
C32 C -0.19875(12) -0.10250(11) 0.6995(3) 0.0168(8) Uani 1 1 d U . .
C33 C -0.12853(12) -0.29346(11) 0.6674(3) 0.0165(8) Uani 1 1 d U . .
C34 C 0.16662(12) -0.44660(11) 0.7391(3) 0.0159(8) Uani 1 1 d U . .
C35 C 0.12785(12) -0.10380(11) 0.7240(3) 0.0166(8) Uani 1 1 d U . .
C36 C -0.00486(12) -0.34469(10) 0.7002(3) 0.0134(7) Uani 1 1 d U . .
C37 C 0.15709(12) -0.06982(11) 0.7439(3) 0.0164(8) Uani 1 1 d U . .
C38 C 0.13174(12) -0.41807(11) 0.7230(3) 0.0146(8) Uani 1 1 d U . .
C39 C -0.07233(12) -0.34393(10) 0.7015(3) 0.0143(8) Uani 1 1 d U . .
C40 C -0.14507(12) -0.36071(11) 0.7025(3) 0.0213(8) Uani 1 1 d U . .
C41 C 0.04602(12) -0.23240(11) 0.6699(3) 0.0169(8) Uani 1 1 d U . .
C42 C -0.00430(12) -0.18146(11) 0.6884(3) 0.0161(8) Uani 1 1 d U . .
C43 C 0.06748(12) -0.36291(11) 0.6979(3) 0.0143(8) Uani 1 1 d U . .
C44 C -0.18722(14) -0.13206(11) 0.7864(3) 0.0232(9) Uani 1 1 d U . .
H44 H -0.1974 -0.1319 0.8544 0.028 Uiso 1 1 calc R . .
C45 C -0.07228(13) -0.18085(11) 0.6794(3) 0.0169(8) Uani 1 1 d U . .
C46 C 0.06937(12) -0.16435(11) 0.6956(3) 0.0186(8) Uani 1 1 d U . .
C47 C -0.14560(13) -0.16245(11) 0.6741(3) 0.0192(8) Uani 1 1 d U . .
C48 C -0.11389(12) -0.33147(11) 0.6883(3) 0.0142(8) Uani 1 1 d U . .
C49 C -0.05734(13) -0.38308(11) 0.7186(3) 0.0208(8) Uani 1 1 d U . .
H49 H -0.0735 -0.4045 0.7290 0.025 Uiso 1 1 calc R . .
C50 C 0.04530(12) -0.29515(11) 0.6686(3) 0.0148(8) Uani 1 1 d U . .
C51 C 0.03418(12) -0.33282(11) 0.6872(3) 0.0149(8) Uani 1 1 d U . .
C52 C -0.05648(13) -0.14216(11) 0.7024(3) 0.0217(9) Uani 1 1 d U . .
H52 H -0.0726 -0.1204 0.7107 0.026 Uiso 1 1 calc R . .
C53 C -0.12895(12) -0.23080(11) 0.6586(3) 0.0167(8) Uani 1 1 d U . .
C54 C 0.08441(13) -0.28305(12) 0.6484(4) 0.0238(9) Uani 1 1 d U . .
H54 H 0.1058 -0.2993 0.6364 0.029 Uiso 1 1 calc R . .
C55 C -0.01470(13) -0.14265(11) 0.7098(3) 0.0216(9) Uani 1 1 d U . .
H55 H 0.0044 -0.1214 0.7260 0.026 Uiso 1 1 calc R . .
C56 C -0.11453(13) -0.19248(11) 0.6686(3) 0.0179(8) Uani 1 1 d U . .
C57 C 0.08507(13) -0.24515(12) 0.6498(4) 0.0239(9) Uani 1 1 d U . .
H57 H 0.1071 -0.2293 0.6396 0.029 Uiso 1 1 calc R . .
C58 C -0.20376(14) -0.40554(13) 0.6189(3) 0.0265(10) Uani 1 1 d U . .
H58 H -0.2248 -0.4169 0.5485 0.032 Uiso 1 1 calc R . .
C59 C -0.16094(14) -0.16167(12) 0.7740(4) 0.0260(10) Uani 1 1 d U . .
H59 H -0.1532 -0.1816 0.8338 0.031 Uiso 1 1 calc R . .
C60 C -0.01667(13) -0.38374(11) 0.7172(3) 0.0200(8) Uani 1 1 d U . .
H60 H 0.0011 -0.4057 0.7257 0.024 Uiso 1 1 calc R . .
C61 C 0.09147(13) -0.10674(12) 0.6195(3) 0.0246(9) Uani 1 1 d U . .
H61 H 0.0862 -0.0880 0.5560 0.030 Uiso 1 1 calc R . .
C62 C 0.03571(12) -0.19421(11) 0.6840(3) 0.0160(8) Uani 1 1 d U . .
C63 C -0.17300(14) -0.24296(12) 0.6389(4) 0.0297(10) Uani 1 1 d U . .
H63 H -0.1976 -0.2269 0.6246 0.036 Uiso 1 1 calc R . .
C64 C 0.06252(14) -0.13627(12) 0.6051(3) 0.0271(10) Uani 1 1 d U . .
H64 H 0.0375 -0.1375 0.5322 0.033 Uiso 1 1 calc R . .
C65 C -0.18494(14) -0.10352(11) 0.5978(3) 0.0217(9) Uani 1 1 d U . .
H65 H -0.1933 -0.0839 0.5370 0.026 Uiso 1 1 calc R . .
C66 C -0.17125(17) -0.39819(16) 0.8366(4) 0.0443(17) Uani 1 1 d U . .
H66 H -0.1693 -0.4049 0.9186 0.053 Uiso 1 1 calc R . .
C67 C -0.17247(13) -0.28126(12) 0.6448(4) 0.0264(9) Uani 1 1 d U . .
H67 H -0.1967 -0.2974 0.6358 0.032 Uiso 1 1 calc R . .
C68 C 0.10766(15) -0.16268(13) 0.7974(4) 0.0363(12) Uani 1 1 d U . .
H68 H 0.1141 -0.1823 0.8582 0.044 Uiso 1 1 calc R . .
C69 C -0.14421(17) -0.37087(16) 0.8186(4) 0.0433(16) Uani 1 1 d U . .
H69 H -0.1242 -0.3585 0.8889 0.052 Uiso 1 1 calc R . .
C70 C -0.17575(14) -0.37847(12) 0.6025(3) 0.0273(10) Uani 1 1 d U . .
H70 H -0.1775 -0.3718 0.5207 0.033 Uiso 1 1 calc R . .
C71 C 0.13641(14) -0.13276(13) 0.8111(4) 0.0336(11) Uani 1 1 d U . .
H71 H 0.1624 -0.1321 0.8813 0.040 Uiso 1 1 calc R . .
C72 C -0.15874(13) -0.13348(12) 0.5857(3) 0.0224(9) Uani 1 1 d U . .
H72 H -0.1496 -0.1342 0.5156 0.027 Uiso 1 1 calc R . .
C73 C 0.11124(15) -0.40097(14) 0.6116(4) 0.0356(12) Uani 1 1 d U . .
H73 H 0.1187 -0.4079 0.5415 0.043 Uiso 1 1 calc R . .
C74 C 0.07953(16) -0.37350(14) 0.5994(4) 0.0392(13) Uani 1 1 d U . .
H74 H 0.0658 -0.3618 0.5210 0.047 Uiso 1 1 calc R . .
C75 C 0.08730(17) -0.38165(16) 0.8103(4) 0.0497(16) Uani 1 1 d U . .
H75 H 0.0788 -0.3757 0.8793 0.060 Uiso 1 1 calc R . .
C76 C 0.0000 -0.2644(2) 1.0000 0.047(2) Uani 1 2 d SU . .
C77 C 0.11923(17) -0.40875(16) 0.8230(4) 0.0463(15) Uani 1 1 d U . .
H77 H 0.1326 -0.4210 0.9007 0.056 Uiso 1 1 calc R . .


_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
Sm1 O15 2.398(3) . ?
Sm1 O16 2.462(2) 6 ?
Sm1 O16 2.462(2) . ?
Sm1 O14 2.479(3) . ?
Sm1 O8 2.511(2) 8_545 ?
Sm1 O8 2.511(2) 3 ?
Sm1 O17 2.535(3) . ?
Sm1 O17 2.535(3) 6 ?
Sm1 O7 2.606(2) 3 ?
Sm1 O7 2.606(2) 8_545 ?
Sm1 C37 2.861(4) . ?
Sm1 C37 2.861(4) 6 ?
Sm2 O15 2.421(3) . ?
Sm2 O11 2.471(2) 5_557 ?
Sm2 O11 2.471(2) 2_557 ?
Sm2 O10 2.496(4) . ?
Sm2 O13 2.500(2) 4_557 ?
Sm2 O13 2.500(2) 7_547 ?
Sm2 O9 2.539(3) 2_557 ?
Sm2 O9 2.539(3) 5_557 ?
Sm2 O12 2.565(2) 4_557 ?
Sm2 O12 2.565(2) 7_547 ?
Sm2 N27 2.879(5) . ?
Sm2 C30 2.885(4) 2_557 ?
Zn3 N23 2.058(3) . ?
Zn3 N25 2.066(3) . ?
Zn3 O19 2.069(3) . ?
Zn3 N26 2.070(3) . ?
Zn3 N24 2.070(3) . ?
Na4 O20 2.221(4) . ?
Na4 O9 2.261(3) . ?
Na4 O17 2.283(3) 2_557 ?
Na4 O7 2.408(3) 7_447 ?
Na4 O12 2.461(3) 8_445 ?
Na4 O15 2.8216(17) 5_557 ?
Na4 Na5 3.645(2) 7_447 ?
Na4 Sm2 3.6556(14) 5_557 ?
Na4 Sm1 3.6617(14) 5_557 ?
Na5 O22 2.136(11) . ?
Na5 O7 2.351(3) . ?
Na5 O7 2.351(3) 6_545 ?
Na5 O12 2.365(3) 2_557 ?
Na5 O12 2.365(3) 5_547 ?
Na5 Na4 3.645(2) 4_447 ?
Na5 Na4 3.645(2) 7_447 ?
Na5 Sm1 3.828(2) 3_445 ?
Na5 Sm2 3.840(2) 3_445 ?
Na6 O11 2.247(3) 6 ?
Na6 O11 2.247(3) . ?
Na6 O8 2.299(3) 7_446 ?
Na6 O8 2.299(3) 4_456 ?
Na6 O21 2.353(6) . ?
Na6 O18 2.489(5) . ?
Na6 Sm2 3.5944(19) 5_557 ?
Na6 Sm1 3.6461(18) 5_556 ?
O7 C29 1.276(4) . ?
O7 Na4 2.408(3) 7_447 ?
O7 Sm1 2.606(2) 3_445 ?
O8 C29 1.253(4) . ?
O8 Na6 2.299(3) 7_446 ?
O8 Sm1 2.511(2) 3_445 ?
O9 C30 1.286(4) . ?
O9 Sm2 2.539(2) 5_557 ?
O10 N27 1.267(5) . ?
O11 C30 1.264(4) . ?
O11 Sm2 2.471(2) 5_557 ?
O12 C34 1.280(4) . ?
O12 Na5 2.365(3) 5_547 ?
O12 Na4 2.461(3) 8_545 ?
O12 Sm2 2.565(2) 7_547 ?
O13 C34 1.258(4) . ?
O13 Sm2 2.500(2) 7_547 ?
O14 N27 1.255(6) . ?
O15 N27 1.338(6) . ?
O15 Na4 2.8216(17) 5_557 ?
O15 Na4 2.8216(17) 2_557 ?
O16 C37 1.272(4) . ?
O17 C37 1.250(4) . ?
O17 Na4 2.283(3) 2_557 ?
O19 C76 1.147(3) . ?
N23 C36 1.374(5) . ?
N23 C39 1.385(5) . ?
N24 C45 1.363(5) . ?
N24 C42 1.374(5) . ?
N25 C41 1.364(5) . ?
N25 C50 1.371(5) . ?
N26 C33 1.368(5) . ?
N26 C53 1.369(5) . ?
C29 C31 1.494(5) . ?
C29 Sm1 2.931(4) 3_445 ?
C30 C32 1.479(5) . ?
C30 Sm2 2.885(4) 5_557 ?
C31 C58 1.372(5) . ?
C31 C66 1.392(5) . ?
C32 C65 1.390(5) . ?
C32 C44 1.396(5) . ?
C33 C48 1.407(5) . ?
C33 C67 1.438(5) . ?
C34 C38 1.481(5) . ?
C34 Sm2 2.910(4) 7_547 ?
C35 C61 1.373(5) . ?
C35 C71 1.383(5) . ?
C35 C37 1.496(5) . ?
C36 C51 1.402(5) . ?
C36 C60 1.452(5) . ?
C38 C73 1.361(5) . ?
C38 C77 1.385(6) . ?
C39 C48 1.389(5) . ?
C39 C49 1.447(5) . ?
C40 C69 1.371(5) . ?
C40 C70 1.385(5) . ?
C40 C48 1.495(5) . ?
C41 C62 1.402(5) . ?
C41 C57 1.448(5) . ?
C42 C62 1.404(5) . ?
C42 C55 1.443(5) . ?
C43 C74 1.371(5) . ?
C43 C75 1.392(6) . ?
C43 C51 1.492(5) . ?
C44 C59 1.387(5) . ?
C45 C56 1.408(5) . ?
C45 C52 1.442(5) . ?
C46 C68 1.390(5) . ?
C46 C64 1.391(5) . ?
C46 C62 1.493(5) . ?
C47 C72 1.394(5) . ?
C47 C59 1.403(5) . ?
C47 C56 1.481(5) . ?
C49 C60 1.340(6) . ?
C50 C51 1.404(5) . ?
C50 C54 1.444(5) . ?
C52 C55 1.344(6) . ?
C53 C56 1.414(5) . ?
C53 C63 1.447(6) . ?
C54 C57 1.327(6) . ?
C58 C70 1.377(5) . ?
C61 C64 1.375(5) . ?
C63 C67 1.343(6) . ?
C65 C72 1.393(5) . ?
C66 C69 1.368(6) . ?
C68 C71 1.382(6) . ?
C73 C74 1.388(6) . ?
C75 C77 1.383(6) . ?
C76 O19 1.147(3) 2_557 ?

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
O15 Sm1 O16 118.89(8) . 6 ?
O15 Sm1 O16 118.89(8) . . ?
O16 Sm1 O16 73.68(12) 6 . ?
O15 Sm1 O14 53.63(11) . . ?
O16 Sm1 O14 76.86(8) 6 . ?
O16 Sm1 O14 76.86(8) . . ?
O15 Sm1 O8 125.04(8) . 8_545 ?
O16 Sm1 O8 116.05(7) 6 8_545 ?
O16 Sm1 O8 75.19(8) . 8_545 ?
O14 Sm1 O8 143.74(6) . 8_545 ?
O15 Sm1 O8 125.04(8) . 3 ?
O16 Sm1 O8 75.19(8) 6 3 ?
O16 Sm1 O8 116.05(7) . 3 ?
O14 Sm1 O8 143.74(6) . 3 ?
O8 Sm1 O8 70.80(11) 8_545 3 ?
O15 Sm1 O17 77.19(5) . . ?
O16 Sm1 O17 121.28(8) 6 . ?
O16 Sm1 O17 52.15(8) . . ?
O14 Sm1 O17 70.96(6) . . ?
O8 Sm1 O17 73.74(8) 8_545 . ?
O8 Sm1 O17 144.53(8) 3 . ?
O15 Sm1 O17 77.19(5) . 6 ?
O16 Sm1 O17 52.15(8) 6 6 ?
O16 Sm1 O17 121.28(8) . 6 ?
O14 Sm1 O17 70.97(6) . 6 ?
O8 Sm1 O17 144.53(8) 8_545 6 ?
O8 Sm1 O17 73.73(8) 3 6 ?
O17 Sm1 O17 141.70(11) . 6 ?
O15 Sm1 O7 74.86(8) . 3 ?
O16 Sm1 O7 106.52(8) 6 3 ?
O16 Sm1 O7 164.72(8) . 3 ?
O14 Sm1 O7 118.29(8) . 3 ?
O8 Sm1 O7 91.54(8) 8_545 3 ?
O8 Sm1 O7 50.92(7) 3 3 ?
O17 Sm1 O7 131.82(8) . 3 ?
O17 Sm1 O7 66.11(8) 6 3 ?
O15 Sm1 O7 74.86(8) . 8_545 ?
O16 Sm1 O7 164.72(8) 6 8_545 ?
O16 Sm1 O7 106.52(8) . 8_545 ?
O14 Sm1 O7 118.29(8) . 8_545 ?
O8 Sm1 O7 50.92(7) 8_545 8_545 ?
O8 Sm1 O7 91.54(8) 3 8_545 ?
O17 Sm1 O7 66.11(8) . 8_545 ?
O17 Sm1 O7 131.82(8) 6 8_545 ?
O7 Sm1 O7 69.12(11) 3 8_545 ?
O15 Sm1 C37 97.55(8) . . ?
O16 Sm1 C37 97.35(10) 6 . ?
O16 Sm1 C37 26.29(9) . . ?
O14 Sm1 C37 70.91(8) . . ?
O8 Sm1 C37 73.77(9) 8_545 . ?
O8 Sm1 C37 135.27(9) 3 . ?
O17 Sm1 C37 25.90(9) . . ?
O17 Sm1 C37 135.61(10) 6 . ?
O7 Sm1 C37 155.74(9) 3 . ?
O7 Sm1 C37 86.70(9) 8_545 . ?
O15 Sm1 C37 97.55(8) . 6 ?
O16 Sm1 C37 26.29(9) 6 6 ?
O16 Sm1 C37 97.35(10) . 6 ?
O14 Sm1 C37 70.91(8) . 6 ?
O8 Sm1 C37 135.27(9) 8_545 6 ?
O8 Sm1 C37 73.78(9) 3 6 ?
O17 Sm1 C37 135.61(10) . 6 ?
O17 Sm1 C37 25.90(9) 6 6 ?
O7 Sm1 C37 86.70(9) 3 6 ?
O7 Sm1 C37 155.74(9) 8_545 6 ?
C37 Sm1 C37 117.37(15) . 6 ?
O15 Sm2 O11 117.47(8) . 5_557 ?
O15 Sm2 O11 117.47(8) . 2_557 ?
O11 Sm2 O11 72.59(11) 5_557 2_557 ?
O15 Sm2 O10 53.59(11) . . ?
O11 Sm2 O10 75.05(8) 5_557 . ?
O11 Sm2 O10 75.04(8) 2_557 . ?
O15 Sm2 O13 126.05(8) . 4_557 ?
O11 Sm2 O13 75.24(9) 5_557 4_557 ?
O11 Sm2 O13 116.30(8) 2_557 4_557 ?
O10 Sm2 O13 142.62(7) . 4_557 ?
O15 Sm2 O13 126.05(8) . 7_547 ?
O11 Sm2 O13 116.30(8) 5_557 7_547 ?
O11 Sm2 O13 75.24(9) 2_557 7_547 ?
O10 Sm2 O13 142.62(7) . 7_547 ?
O13 Sm2 O13 72.25(13) 4_557 7_547 ?
O15 Sm2 O9 76.60(6) . 2_557 ?
O11 Sm2 O9 120.10(8) 5_557 2_557 ?
O11 Sm2 O9 52.22(7) 2_557 2_557 ?
O10 Sm2 O9 70.40(6) . 2_557 ?
O13 Sm2 O9 145.82(9) 4_557 2_557 ?
O13 Sm2 O9 73.60(9) 7_547 2_557 ?
O15 Sm2 O9 76.60(6) . 5_557 ?
O11 Sm2 O9 52.22(7) 5_557 5_557 ?
O11 Sm2 O9 120.10(8) 2_557 5_557 ?
O10 Sm2 O9 70.40(6) . 5_557 ?
O13 Sm2 O9 73.60(9) 4_557 5_557 ?
O13 Sm2 O9 145.82(9) 7_547 5_557 ?
O9 Sm2 O9 140.50(12) 2_557 5_557 ?
O15 Sm2 O12 75.73(8) . 4_557 ?
O11 Sm2 O12 107.91(8) 5_557 4_557 ?
O11 Sm2 O12 165.38(8) 2_557 4_557 ?
O10 Sm2 O12 119.45(8) . 4_557 ?
O13 Sm2 O12 51.52(7) 4_557 4_557 ?
O13 Sm2 O12 92.01(8) 7_547 4_557 ?
O9 Sm2 O12 131.50(8) 2_557 4_557 ?
O9 Sm2 O12 67.23(8) 5_557 4_557 ?
O15 Sm2 O12 75.73(8) . 7_547 ?
O11 Sm2 O12 165.38(8) 5_557 7_547 ?
O11 Sm2 O12 107.91(8) 2_557 7_547 ?
O10 Sm2 O12 119.45(8) . 7_547 ?
O13 Sm2 O12 92.01(8) 4_557 7_547 ?
O13 Sm2 O12 51.52(7) 7_547 7_547 ?
O9 Sm2 O12 67.23(8) 2_557 7_547 ?
O9 Sm2 O12 131.50(8) 5_557 7_547 ?
O12 Sm2 O12 67.78(11) 4_557 7_547 ?
O15 Sm2 N27 27.54(12) . . ?
O11 Sm2 N27 95.94(10) 5_557 . ?
O11 Sm2 N27 95.94(10) 2_557 . ?
O10 Sm2 N27 26.05(12) . . ?
O13 Sm2 N27 141.05(7) 4_557 . ?
O13 Sm2 N27 141.05(7) 7_547 . ?
O9 Sm2 N27 71.39(6) 2_557 . ?
O9 Sm2 N27 71.39(6) 5_557 . ?
O12 Sm2 N27 98.51(10) 4_557 . ?
O12 Sm2 N27 98.51(10) 7_547 . ?
O15 Sm2 C30 96.61(8) . 2_557 ?
O11 Sm2 C30 95.55(9) 5_557 2_557 ?
O11 Sm2 C30 25.85(9) 2_557 2_557 ?
O10 Sm2 C30 69.13(8) . 2_557 ?
O13 Sm2 C30 136.08(9) 4_557 2_557 ?
O13 Sm2 C30 74.21(10) 7_547 2_557 ?
O9 Sm2 C30 26.45(9) 2_557 2_557 ?
O9 Sm2 C30 133.57(9) 5_557 2_557 ?
O12 Sm2 C30 156.32(9) 4_557 2_557 ?
O12 Sm2 C30 88.69(9) 7_547 2_557 ?
N27 Sm2 C30 81.84(9) . 2_557 ?
N23 Zn3 N25 88.97(12) . . ?
N23 Zn3 O19 100.80(13) . . ?
N25 Zn3 O19 100.09(15) . . ?
N23 Zn3 N26 88.76(12) . . ?
N25 Zn3 N26 160.36(11) . . ?
O19 Zn3 N26 99.50(15) . . ?
N23 Zn3 N24 165.59(11) . . ?
N25 Zn3 N24 88.63(12) . . ?
O19 Zn3 N24 93.61(13) . . ?
N26 Zn3 N24 88.75(12) . . ?
O20 Na4 O9 103.39(13) . . ?
O20 Na4 O17 100.13(12) . 2_557 ?
O9 Na4 O17 112.33(11) . 2_557 ?
O20 Na4 O7 114.57(13) . 7_447 ?
O9 Na4 O7 140.18(11) . 7_447 ?
O17 Na4 O7 73.40(9) 2_557 7_447 ?
O20 Na4 O12 117.68(13) . 8_445 ?
O9 Na4 O12 73.38(9) . 8_445 ?
O17 Na4 O12 139.80(11) 2_557 8_445 ?
O7 Na4 O12 78.57(9) 7_447 8_445 ?
O20 Na4 O15 170.49(14) . 5_557 ?
O9 Na4 O15 73.55(10) . 5_557 ?
O17 Na4 O15 73.36(10) 2_557 5_557 ?
O7 Na4 O15 70.74(9) 7_447 5_557 ?
O12 Na4 O15 70.49(9) 8_445 5_557 ?
O20 Na4 Na5 130.91(12) . 7_447 ?
O9 Na4 Na5 105.27(8) . 7_447 ?
O17 Na4 Na5 104.60(8) 2_557 7_447 ?
O7 Na4 Na5 39.44(7) 7_447 7_447 ?
O12 Na4 Na5 39.97(6) 8_445 7_447 ?
O15 Na4 Na5 58.33(8) 5_557 7_447 ?
O20 Na4 Sm2 140.66(10) . 5_557 ?
O9 Na4 Sm2 43.32(7) . 5_557 ?
O17 Na4 Sm2 111.35(8) 2_557 5_557 ?
O7 Na4 Sm2 97.08(7) 7_447 5_557 ?
O12 Na4 Sm2 44.46(6) 8_445 5_557 ?
O15 Na4 Sm2 41.45(6) 5_557 5_557 ?
Na5 Na4 Sm2 63.46(4) 7_447 5_557 ?
O20 Na4 Sm1 137.05(10) . 5_557 ?
O9 Na4 Sm1 110.88(8) . 5_557 ?
O17 Na4 Sm1 43.17(7) 2_557 5_557 ?
O7 Na4 Sm1 45.25(6) 7_447 5_557 ?
O12 Na4 Sm1 96.81(7) 8_445 5_557 ?
O15 Na4 Sm1 40.90(6) 5_557 5_557 ?
Na5 Na4 Sm1 63.19(4) 7_447 5_557 ?
Sm2 Na4 Sm1 81.89(3) 5_557 5_557 ?
O22 Na5 O7 118.6(2) . . ?
O22 Na5 O7 118.6(2) . 6_545 ?
O7 Na5 O7 77.93(13) . 6_545 ?
O22 Na5 O12 113.2(2) . 2_557 ?
O7 Na5 O12 81.65(9) . 2_557 ?
O7 Na5 O12 127.98(13) 6_545 2_557 ?
O22 Na5 O12 113.2(2) . 5_547 ?
O7 Na5 O12 127.98(13) . 5_547 ?
O7 Na5 O12 81.65(9) 6_545 5_547 ?
O12 Na5 O12 74.41(13) 2_557 5_547 ?
O22 Na5 Na4 131.90(4) . 4_447 ?
O7 Na5 Na4 100.08(9) . 4_447 ?
O7 Na5 Na4 40.59(6) 6_545 4_447 ?
O12 Na5 Na4 98.90(9) 2_557 4_447 ?
O12 Na5 Na4 41.95(7) 5_547 4_447 ?
O22 Na5 Na4 131.90(4) . 7_447 ?
O7 Na5 Na4 40.59(6) . 7_447 ?
O7 Na5 Na4 100.08(9) 6_545 7_447 ?
O12 Na5 Na4 41.95(7) 2_557 7_447 ?
O12 Na5 Na4 98.90(9) 5_547 7_447 ?
Na4 Na5 Na4 95.97(7) 4_447 7_447 ?
O22 Na5 Sm1 144.9(3) . 3_445 ?
O7 Na5 Sm1 41.94(7) . 3_445 ?
O7 Na5 Sm1 41.94(7) 6_545 3_445 ?
O12 Na5 Sm1 94.30(9) 2_557 3_445 ?
O12 Na5 Sm1 94.30(9) 5_547 3_445 ?
Na4 Na5 Sm1 58.62(4) 4_447 3_445 ?
Na4 Na5 Sm1 58.62(4) 7_447 3_445 ?
O22 Na5 Sm2 137.7(3) . 3_445 ?
O7 Na5 Sm2 93.37(9) . 3_445 ?
O7 Na5 Sm2 93.37(9) 6_545 3_445 ?
O12 Na5 Sm2 40.75(7) 2_557 3_445 ?
O12 Na5 Sm2 40.75(7) 5_547 3_445 ?
Na4 Na5 Sm2 58.41(4) 4_447 3_445 ?
Na4 Na5 Sm2 58.41(4) 7_447 3_445 ?
Sm1 Na5 Sm2 77.42(4) 3_445 3_445 ?
O11 Na6 O11 81.24(13) 6 . ?
O11 Na6 O8 174.66(14) 6 7_446 ?
O11 Na6 O8 99.88(9) . 7_446 ?
O11 Na6 O8 99.88(9) 6 4_456 ?
O11 Na6 O8 174.65(14) . 4_456 ?
O8 Na6 O8 78.52(13) 7_446 4_456 ?
O11 Na6 O21 95.00(15) 6 . ?
O11 Na6 O21 95.00(15) . . ?
O8 Na6 O21 90.11(14) 7_446 . ?
O8 Na6 O21 90.11(15) 4_456 . ?
O11 Na6 O18 83.48(11) 6 . ?
O11 Na6 O18 83.48(11) . . ?
O8 Na6 O18 91.44(11) 7_446 . ?
O8 Na6 O18 91.44(11) 4_456 . ?
O21 Na6 O18 177.99(17) . . ?
O11 Na6 Sm2 42.73(7) 6 5_557 ?
O11 Na6 Sm2 42.74(7) . 5_557 ?
O8 Na6 Sm2 136.14(8) 7_446 5_557 ?
O8 Na6 Sm2 136.14(8) 4_456 5_557 ?
O21 Na6 Sm2 111.21(16) . 5_557 ?
O18 Na6 Sm2 66.78(9) . 5_557 ?
O11 Na6 Sm1 137.88(7) 6 5_556 ?
O11 Na6 Sm1 137.88(7) . 5_556 ?
O8 Na6 Sm1 42.94(7) 7_446 5_556 ?
O8 Na6 Sm1 42.94(7) 4_456 5_556 ?
O21 Na6 Sm1 71.15(15) . 5_556 ?
O18 Na6 Sm1 110.86(10) . 5_556 ?
Sm2 Na6 Sm1 177.64(7) 5_557 5_556 ?
C29 O7 Na5 134.9(2) . . ?
C29 O7 Na4 122.4(2) . 7_447 ?
Na5 O7 Na4 99.98(10) . 7_447 ?
C29 O7 Sm1 91.5(2) . 3_445 ?
Na5 O7 Sm1 100.99(9) . 3_445 ?
Na4 O7 Sm1 93.75(9) 7_447 3_445 ?
C29 O8 Na6 135.1(2) . 7_446 ?
C29 O8 Sm1 96.5(2) . 3_445 ?
Na6 O8 Sm1 98.49(10) 7_446 3_445 ?
C30 O9 Na4 168.9(2) . . ?
C30 O9 Sm2 91.9(2) . 5_557 ?
Na4 O9 Sm2 99.03(10) . 5_557 ?
N27 O10 Sm2 94.1(3) . . ?
C30 O11 Na6 163.2(3) . . ?
C30 O11 Sm2 95.7(2) . 5_557 ?
Na6 O11 Sm2 99.16(10) . 5_557 ?
C34 O12 Na5 137.6(2) . 5_547 ?
C34 O12 Na4 120.9(2) . 8_545 ?
Na5 O12 Na4 98.08(9) 5_547 8_545 ?
C34 O12 Sm2 92.2(2) . 7_547 ?
Na5 O12 Sm2 102.25(10) 5_547 7_547 ?
Na4 O12 Sm2 93.32(9) 8_545 7_547 ?
C34 O13 Sm2 95.8(2) . 7_547 ?
N27 O14 Sm1 94.4(3) . . ?
N27 O15 Sm1 95.8(2) . . ?
N27 O15 Sm2 95.6(2) . . ?
Sm1 O15 Sm2 168.53(16) . . ?
N27 O15 Na4 106.32(7) . 5_557 ?
Sm1 O15 Na4 88.71(7) . 5_557 ?
Sm2 O15 Na4 88.07(7) . 5_557 ?
N27 O15 Na4 106.32(7) . 2_557 ?
Sm1 O15 Na4 88.71(7) . 2_557 ?
Sm2 O15 Na4 88.07(7) . 2_557 ?
Na4 O15 Na4 147.35(15) 5_557 2_557 ?
C37 O16 Sm1 94.7(2) . . ?
C37 O17 Na4 169.4(3) . 2_557 ?
C37 O17 Sm1 91.8(2) . . ?
Na4 O17 Sm1 98.80(10) 2_557 . ?
C76 O19 Zn3 157.8(4) . . ?
C36 N23 C39 107.1(3) . . ?
C36 N23 Zn3 125.9(2) . . ?
C39 N23 Zn3 125.5(2) . . ?
C45 N24 C42 106.8(3) . . ?
C45 N24 Zn3 124.9(2) . . ?
C42 N24 Zn3 124.1(2) . . ?
C41 N25 C50 107.0(3) . . ?
C41 N25 Zn3 126.0(2) . . ?
C50 N25 Zn3 126.9(2) . . ?
C33 N26 C53 106.7(3) . . ?
C33 N26 Zn3 126.5(2) . . ?
C53 N26 Zn3 126.6(2) . . ?
O14 N27 O10 127.1(5) . . ?
O14 N27 O15 116.2(4) . . ?
O10 N27 O15 116.7(4) . . ?
O14 N27 Sm1 59.7(2) . . ?
O10 N27 Sm1 173.2(4) . . ?
O15 N27 Sm1 56.5(2) . . ?
O14 N27 Sm2 173.0(4) . . ?
O10 N27 Sm2 59.9(3) . . ?
O15 N27 Sm2 56.8(2) . . ?
Sm1 N27 Sm2 113.28(18) . . ?
O8 C29 O7 121.0(3) . . ?
O8 C29 C31 119.6(3) . . ?
O7 C29 C31 119.4(3) . . ?
O8 C29 Sm1 58.35(18) . 3_445 ?
O7 C29 Sm1 62.73(19) . 3_445 ?
C31 C29 Sm1 175.6(3) . 3_445 ?
O11 C30 O9 119.8(3) . . ?
O11 C30 C32 120.4(3) . . ?
O9 C30 C32 119.8(3) . . ?
O11 C30 Sm2 58.46(18) . 5_557 ?
O9 C30 Sm2 61.61(19) . 5_557 ?
C32 C30 Sm2 173.2(3) . 5_557 ?
C58 C31 C66 118.0(4) . . ?
C58 C31 C29 121.9(3) . . ?
C66 C31 C29 120.2(3) . . ?
C65 C32 C44 119.6(4) . . ?
C65 C32 C30 120.0(3) . . ?
C44 C32 C30 120.3(3) . . ?
N26 C33 C48 125.5(3) . . ?
N26 C33 C67 109.5(3) . . ?
C48 C33 C67 125.0(4) . . ?
O13 C34 O12 120.4(3) . . ?
O13 C34 C38 120.0(3) . . ?
O12 C34 C38 119.6(3) . . ?
O13 C34 Sm2 58.73(19) . 7_547 ?
O12 C34 Sm2 61.71(19) . 7_547 ?
C38 C34 Sm2 177.3(3) . 7_547 ?
C61 C35 C71 118.4(4) . . ?
C61 C35 C37 120.7(3) . . ?
C71 C35 C37 120.9(3) . . ?
N23 C36 C51 124.8(3) . . ?
N23 C36 C60 109.0(3) . . ?
C51 C36 C60 126.1(3) . . ?
O17 C37 O16 121.2(3) . . ?
O17 C37 C35 120.0(3) . . ?
O16 C37 C35 118.7(3) . . ?
O17 C37 Sm1 62.32(19) . . ?
O16 C37 Sm1 59.06(18) . . ?
C35 C37 Sm1 173.3(3) . . ?
C73 C38 C77 118.9(4) . . ?
C73 C38 C34 121.6(3) . . ?
C77 C38 C34 119.5(3) . . ?
N23 C39 C48 125.3(3) . . ?
N23 C39 C49 108.6(3) . . ?
C48 C39 C49 125.9(3) . . ?
C69 C40 C70 117.0(4) . . ?
C69 C40 C48 119.9(3) . . ?
C70 C40 C48 123.1(3) . . ?
N25 C41 C62 125.9(3) . . ?
N25 C41 C57 109.0(3) . . ?
C62 C41 C57 125.1(4) . . ?
N24 C42 C62 125.1(3) . . ?
N24 C42 C55 109.1(3) . . ?
C62 C42 C55 125.8(4) . . ?
C74 C43 C75 117.5(4) . . ?
C74 C43 C51 122.3(3) . . ?
C75 C43 C51 120.2(3) . . ?
C59 C44 C32 120.3(3) . . ?
N24 C45 C56 125.7(3) . . ?
N24 C45 C52 109.7(3) . . ?
C56 C45 C52 124.6(4) . . ?
C68 C46 C64 117.7(4) . . ?
C68 C46 C62 122.0(3) . . ?
C64 C46 C62 120.3(3) . . ?
C72 C47 C59 118.2(4) . . ?
C72 C47 C56 122.0(3) . . ?
C59 C47 C56 119.7(3) . . ?
C39 C48 C33 125.4(3) . . ?
C39 C48 C40 117.1(3) . . ?
C33 C48 C40 117.4(3) . . ?
C60 C49 C39 107.9(3) . . ?
N25 C50 C51 124.7(3) . . ?
N25 C50 C54 108.8(3) . . ?
C51 C50 C54 126.3(3) . . ?
C36 C51 C50 126.1(3) . . ?
C36 C51 C43 116.8(3) . . ?
C50 C51 C43 117.0(3) . . ?
C55 C52 C45 107.1(4) . . ?
N26 C53 C56 125.2(3) . . ?
N26 C53 C63 109.3(3) . . ?
C56 C53 C63 125.4(4) . . ?
C57 C54 C50 107.6(4) . . ?
C52 C55 C42 107.3(4) . . ?
C45 C56 C53 125.0(4) . . ?
C45 C56 C47 117.5(3) . . ?
C53 C56 C47 117.5(3) . . ?
C54 C57 C41 107.4(4) . . ?
C31 C58 C70 120.7(3) . . ?
C44 C59 C47 120.6(4) . . ?
C49 C60 C36 107.4(3) . . ?
C35 C61 C64 121.2(4) . . ?
C41 C62 C42 125.0(3) . . ?
C41 C62 C46 118.5(3) . . ?
C42 C62 C46 116.5(3) . . ?
C67 C63 C53 106.9(4) . . ?
C61 C64 C46 121.0(4) . . ?
C32 C65 C72 119.6(3) . . ?
C69 C66 C31 120.5(4) . . ?
C63 C67 C33 107.5(4) . . ?
C71 C68 C46 120.7(4) . . ?
C66 C69 C40 122.1(4) . . ?
C58 C70 C40 121.6(3) . . ?
C68 C71 C35 120.9(4) . . ?
C65 C72 C47 121.4(3) . . ?
C38 C73 C74 120.6(4) . . ?
C43 C74 C73 121.6(4) . . ?
C77 C75 C43 121.0(4) . . ?
O19 C76 O19 149.5(8) . 2_557 ?
C75 C77 C38 120.3(4) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 -0.003 -0.001 3820 1026 ' '
2 0.000 0.500 0.009 530 109 ' '
3 0.500 0.000 0.860 530 109 ' '
_platon_squeeze_details          
;
 disordered DMA + water solvent.
;

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.38
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.876
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 1014718'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt42sq(5)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C97 H54 Gd2 N9 Na4 O26 Zn2'
_chemical_formula_sum            'C97 H54 Gd2 N9 Na4 O26 Zn2'
_chemical_formula_weight         2298.74

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'
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'
Zn Zn 0.2839 1.4301 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   32.9116(9)
_cell_length_b                   34.7726(9)
_cell_length_c                   11.5106(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.958(2)
_cell_angle_gamma                90.00
_cell_volume                     12381.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    11928
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      26.37

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4556
_exptl_absorpt_coefficient_mu    1.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_T_max  0.8043
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            102054
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         26.37
_reflns_number_total             12882
_reflns_number_gt                11928
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The crystal contains severely disordered crystallization solvent trapped
 within the channel voids, which could not be modeled by discrete atoms.
 Its contribution to the diffraction pattern was subtracted by the Squeeze
 technique, using the PLATON software.
 Some protons of the water species couldn't be located.
;

_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)+(0.0471P)²+4.9565P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12882
_refine_ls_number_parameters     659
_refine_ls_number_restraints     273
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0871
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.207680(5) 0.0000 0.793156(16) 0.00887(5) Uani 1 2 d SU . .
Gd2 Gd 0.263052(5) 0.0000 1.232439(16) 0.00862(5) Uani 1 2 d SU . .
Zn3 Zn -0.036038(9) -0.261577(8) 0.70641(3) 0.01341(7) Uani 1 1 d U . .
Na4 Na -0.25183(3) -0.07780(3) 0.98761(9) 0.0147(2) Uani 1 1 d U . .
Na5 Na -0.23424(5) 0.0000 0.49117(14) 0.0179(3) Uani 1 2 d SU . .
Na6 Na -0.17558(5) -0.5000 1.00719(15) 0.0198(3) Uani 1 2 d SU . .
O7 O -0.26048(6) -0.45865(5) 0.66902(17) 0.0137(4) Uani 1 1 d U . .
O8 O -0.22326(6) -0.45777(5) 0.86859(17) 0.0146(4) Uani 1 1 d U . .
O9 O 0.22880(8) 0.0000 1.0122(2) 0.0128(5) Uani 1 2 d SU . .
O10 O 0.17596(6) -0.45816(6) 0.64657(18) 0.0192(4) Uani 1 1 d U . .
O11 O 0.18470(8) 0.0000 1.1204(2) 0.0168(5) Uani 1 2 d SU . .
O12 O -0.23442(6) -0.04144(5) 0.64115(17) 0.0142(4) Uani 1 1 d U . .
O13 O 0.15816(8) 0.0000 0.9119(2) 0.0169(5) Uani 1 2 d SU . .
O14 O 0.19310(6) -0.06861(5) 0.83912(17) 0.0157(4) Uani 1 1 d U . .
O15 O -0.23639(6) -0.06834(5) 0.81197(17) 0.0156(4) Uani 1 1 d U . .
O16 O 0.18782(6) -0.45887(5) 0.84682(17) 0.0147(4) Uani 1 1 d U . .
O17 O 0.14907(6) -0.04165(5) 0.67022(18) 0.0164(4) Uani 1 1 d U . .
O18 O -0.31514(11) 0.0000 0.4422(3) 0.0279(7) Uani 1 2 d SU . .
H18 H -0.3232 -0.0213 0.4813 0.033 Uiso 1 1 d R . .
N19 N -0.03960(7) -0.20302(6) 0.6716(2) 0.0142(4) Uani 1 1 d U . .
N20 N -0.10204(7) -0.26166(6) 0.6708(2) 0.0135(4) Uani 1 1 d U . .
N21 N 0.02178(7) -0.26247(6) 0.6739(2) 0.0123(4) Uani 1 1 d U . .
N22 N -0.03854(7) -0.32067(6) 0.6911(2) 0.0130(4) Uani 1 1 d U . .
C23 C -0.22966(8) -0.44588(7) 0.7595(2) 0.0118(5) Uani 1 1 d U . .
O24 O -0.15757(12) 0.0000 0.5319(4) 0.0463(10) Uani 1 2 d SU . .
H24 H -0.1536 -0.0183 0.5825 0.056 Uiso 1 1 d R . .
C25 C -0.19998(8) -0.41630(7) 0.7378(2) 0.0128(5) Uani 1 1 d U . .
C26 C 0.16718(8) -0.44664(7) 0.7386(2) 0.0131(5) Uani 1 1 d U . .
O27 O -0.26000(10) -0.14124(7) 0.9933(3) 0.0486(7) Uani 1 1 d DU . .
C28 C -0.22488(8) -0.06885(7) 0.7181(2) 0.0135(5) Uani 1 1 d U . .
C29 C 0.15939(8) -0.06945(7) 0.7456(3) 0.0149(5) Uani 1 1 d U . .
N30 N 0.18855(11) 0.0000 1.0155(3) 0.0217(7) Uani 1 2 d SU . .
C31 C 0.13205(8) -0.41768(7) 0.7223(2) 0.0144(5) Uani 1 1 d U . .
C32 C -0.19884(9) -0.10183(8) 0.6989(3) 0.0162(5) Uani 1 1 d U . .
C33 C -0.00441(9) -0.17993(7) 0.6854(3) 0.0160(5) Uani 1 1 d U . .
C34 C 0.12941(8) -0.10319(8) 0.7243(3) 0.0165(5) Uani 1 1 d U . .
C35 C -0.11296(8) -0.33127(7) 0.6872(2) 0.0136(5) Uani 1 1 d U . .
C36 C -0.07222(9) -0.17942(7) 0.6765(3) 0.0155(5) Uani 1 1 d U . .
C37 C 0.03443(8) -0.33233(8) 0.6849(3) 0.0149(5) Uani 1 1 d U . .
C38 C -0.12750(8) -0.29313(8) 0.6662(3) 0.0160(5) Uani 1 1 d U . .
C39 C 0.04495(8) -0.29436(8) 0.6656(3) 0.0153(5) Uani 1 1 d U . .
C40 C -0.11399(9) -0.19148(8) 0.6661(3) 0.0174(5) Uani 1 1 d U . .
C41 C 0.06821(8) -0.36239(7) 0.6965(3) 0.0161(5) Uani 1 1 d U . .
C42 C -0.14389(8) -0.36080(7) 0.7022(3) 0.0147(5) Uani 1 1 d U . .
C43 C -0.20301(10) -0.40545(9) 0.6207(3) 0.0243(6) Uani 1 1 d U . .
H43 H -0.2243 -0.4167 0.5512 0.029 Uiso 1 1 calc R . .
C44 C -0.07111(8) -0.34376(7) 0.7008(3) 0.0145(5) Uani 1 1 d U . .
C45 C -0.00436(8) -0.34431(7) 0.6988(2) 0.0146(5) Uani 1 1 d U . .
C46 C 0.09204(9) -0.10369(8) 0.6232(3) 0.0203(6) Uani 1 1 d U . .
H46 H 0.0865 -0.0837 0.5637 0.024 Uiso 1 1 calc R . .
C47 C 0.03549(8) -0.19263(8) 0.6804(3) 0.0164(5) Uani 1 1 d U . .
C48 C 0.06937(9) -0.16288(8) 0.6929(3) 0.0190(6) Uani 1 1 d U . .
C49 C -0.18719(11) -0.13139(9) 0.7844(3) 0.0274(7) Uani 1 1 d U . .
H49 H -0.1972 -0.1314 0.8525 0.033 Uiso 1 1 calc R . .
C50 C -0.12798(9) -0.23004(8) 0.6571(3) 0.0176(5) Uani 1 1 d U . .
C51 C -0.05667(9) -0.38321(8) 0.7167(3) 0.0200(6) Uani 1 1 d U . .
H51 H -0.0730 -0.4048 0.7258 0.024 Uiso 1 1 calc R . .
C52 C -0.18484(9) -0.10249(8) 0.5976(3) 0.0194(6) Uani 1 1 d U . .
H52 H -0.1935 -0.0827 0.5371 0.023 Uiso 1 1 calc R . .
C53 C -0.17489(10) -0.37791(10) 0.6038(3) 0.0278(7) Uani 1 1 d U . .
H53 H -0.1772 -0.3707 0.5221 0.033 Uiso 1 1 calc R . .
C54 C 0.04590(8) -0.23121(8) 0.6662(3) 0.0161(5) Uani 1 1 d U . .
C55 C 0.08406(9) -0.28248(9) 0.6433(3) 0.0239(6) Uani 1 1 d U . .
H55 H 0.1052 -0.2989 0.6304 0.029 Uiso 1 1 calc R . .
C56 C -0.14527(9) -0.16125(8) 0.6725(3) 0.0191(6) Uani 1 1 d U . .
C57 C -0.16082(11) -0.16103(9) 0.7709(3) 0.0293(7) Uani 1 1 d U . .
H57 H -0.1533 -0.1814 0.8295 0.035 Uiso 1 1 calc R . .
C58 C -0.05669(10) -0.14004(8) 0.6964(3) 0.0211(6) Uani 1 1 d U . .
H58 H -0.0728 -0.1181 0.7034 0.025 Uiso 1 1 calc R . .
C59 C -0.01558(9) -0.38366(8) 0.7163(3) 0.0219(6) Uani 1 1 d U . .
H59 H 0.0025 -0.4056 0.7257 0.026 Uiso 1 1 calc R . .
C60 C 0.08445(9) -0.24376(9) 0.6444(3) 0.0254(7) Uani 1 1 d U . .
H60 H 0.1061 -0.2277 0.6330 0.030 Uiso 1 1 calc R . .
C61 C 0.13800(10) -0.13357(9) 0.8077(3) 0.0327(8) Uani 1 1 d U . .
H61 H 0.1643 -0.1340 0.8761 0.039 Uiso 1 1 calc R . .
C62 C -0.01514(9) -0.14062(8) 0.7030(3) 0.0206(6) Uani 1 1 d U . .
H62 H 0.0037 -0.1191 0.7167 0.025 Uiso 1 1 calc R . .
C63 C -0.17187(10) -0.24221(9) 0.6381(3) 0.0287(7) Uani 1 1 d U . .
H63 H -0.1963 -0.2260 0.6240 0.034 Uiso 1 1 calc R . .
C64 C -0.15826(9) -0.13200(8) 0.5849(3) 0.0197(6) Uani 1 1 d U . .
H64 H -0.1488 -0.1322 0.5156 0.024 Uiso 1 1 calc R . .
C65 C 0.06237(9) -0.13327(9) 0.6077(3) 0.0218(6) Uani 1 1 d U . .
H65 H 0.0367 -0.1332 0.5373 0.026 Uiso 1 1 calc R . .
C66 C 0.11113(13) -0.40124(12) 0.6106(3) 0.0411(10) Uani 1 1 d U . .
H66 H 0.1180 -0.4089 0.5403 0.050 Uiso 1 1 calc R . .
C67 C -0.17001(14) -0.39847(14) 0.8367(3) 0.0427(13) Uani 1 1 d U . .
H67 H -0.1683 -0.4050 0.9183 0.051 Uiso 1 1 calc R . .
C68 C 0.10841(10) -0.16328(9) 0.7915(3) 0.0343(8) Uani 1 1 d U . .
H68 H 0.1148 -0.1841 0.8483 0.041 Uiso 1 1 calc R . .
C69 C -0.14222(13) -0.37102(14) 0.8188(3) 0.0441(12) Uani 1 1 d U . .
H69 H -0.1217 -0.3591 0.8885 0.055 Uiso 1 1 calc R . .
C70 C -0.17150(9) -0.28097(9) 0.6444(3) 0.0264(7) Uani 1 1 d U . .
H70 H -0.1956 -0.2972 0.6361 0.032 Uiso 1 1 calc R . .
O71 O -0.00373(19) -0.2579(2) 0.8970(6) 0.0317(14) Uani 0.50 1 d PU . .
O71' O -0.02260(18) -0.2583(2) 0.8978(6) 0.0288(13) Uani 0.50 1 d PU . .
O72 O -0.10897(10) -0.5000 1.0089(3) 0.058(3) Uani 1 2 d SU . .
H72A H -0.0953 -0.5000 1.0961 0.080 Uiso 1 2 d SR . .
H72B H -0.0872 -0.5000 0.9718 0.080 Uiso 1 2 d SR . .
C73 C 0.07959(10) -0.3733(3) 0.5984(3) 0.0420(10) Uani 1 1 d U . .
H73 H 0.0658 -0.3616 0.5202 0.050 Uiso 1 1 calc R . .
C74 C 0.11984(14) -0.40808(14) 0.8218(3) 0.0459(12) Uani 1 1 d U . .
H74 H 0.1328 -0.4205 0.8992 0.056 Uiso 1 1 calc R . .
C75 C 0.08840(15) -0.38003(15) 0.8082(4) 0.0550(15) Uani 1 1 d U . .
H75 H 0.0807 -0.3729 0.8777 0.066 Uiso 1 1 calc R . .
C76 C 0.0000 -0.26286(15) 1.0000 0.0369(17) Uani 1 2 d SU . .


_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 O9 2.376(3) . ?
Gd1 O17 2.4408(18) 6 ?
Gd1 O17 2.4408(18) . ?
Gd1 O13 2.459(3) . ?
Gd1 O7 2.4959(17) 8_545 ?
Gd1 O7 2.4959(18) 3 ?
Gd1 O14 2.5249(18) 6 ?
Gd1 O14 2.5249(18) . ?
Gd1 O8 2.5938(18) 3 ?
Gd1 O8 2.5938(18) 8_545 ?
Gd1 N30 2.837(4) . ?
Gd1 C29 2.840(3) . ?
Gd2 O9 2.397(3) . ?
Gd2 O12 2.4532(18) 5_557 ?
Gd2 O12 2.4532(18) 2_557 ?
Gd2 O11 2.458(3) . ?
Gd2 O10 2.4852(19) 4_557 ?
Gd2 O10 2.4852(19) 7_547 ?
Gd2 O15 2.5240(18) 2_557 ?
Gd2 O15 2.5240(18) 5_557 ?
Gd2 O16 2.5493(18) 4_557 ?
Gd2 O16 2.5493(18) 7_547 ?
Gd2 N30 2.840(4) . ?
Gd2 C28 2.850(3) 2_557 ?
Zn3 N21 2.061(2) . ?
Zn3 N22 2.061(2) . ?
Zn3 N20 2.068(2) . ?
Zn3 N19 2.071(2) . ?
Zn3 O71 2.090(6) . ?
Zn3 O71' 2.097(6) . ?
Na4 O27 2.226(3) . ?
Na4 O15 2.271(2) . ?
Na4 O14 2.277(2) 2_557 ?
Na4 O8 2.422(2) 7_447 ?
Na4 O16 2.449(2) 8_445 ?
Na4 O9 2.8092(12) 5_557 ?
Na4 Na6 3.6232(15) 7_447 ?
Na4 Gd2 3.6376(10) 5_557 ?
Na4 Gd1 3.6462(10) 5_557 ?
Na5 O12 2.250(2) . ?
Na5 O12 2.250(2) 6 ?
Na5 O7 2.298(2) 7_446 ?
Na5 O7 2.298(2) 4_456 ?
Na5 O24 2.404(4) . ?
Na5 O18 2.526(4) . ?
Na5 Gd2 3.6166(14) 5_557 ?
Na5 Gd1 3.6644(14) 5_556 ?
Na6 O72 2.185(3) . ?
Na6 O8 2.336(2) 6_545 ?
Na6 O8 2.336(2) . ?
Na6 O16 2.344(2) 2_557 ?
Na6 O16 2.344(2) 5_547 ?
Na6 Na4 3.6230(15) 4_447 ?
Na6 Na4 3.6230(15) 7_447 ?
Na6 Gd1 3.7909(16) 3_445 ?
Na6 Gd2 3.7918(17) 3_445 ?
O7 C23 1.261(3) . ?
O7 Na5 2.298(2) 7_446 ?
O7 Gd1 2.4960(17) 3_445 ?
O8 C23 1.270(3) . ?
O8 Na4 2.422(2) 7_447 ?
O8 Gd1 2.5940(18) 3_445 ?
O9 N30 1.338(4) . ?
O9 Na4 2.8092(12) 5_557 ?
O9 Na4 2.8092(12) 2_557 ?
O10 C26 1.255(3) . ?
O10 Gd2 2.4854(19) 7_547 ?
O11 N30 1.256(4) . ?
O12 C28 1.266(3) . ?
O12 Gd2 2.4531(18) 5_557 ?
O13 N30 1.268(4) . ?
O14 C29 1.255(3) . ?
O14 Na4 2.277(2) 2_557 ?
O15 C28 1.261(3) . ?
O15 Gd2 2.5241(17) 5_557 ?
O16 C26 1.271(3) . ?
O16 Na6 2.344(2) 5_547 ?
O16 Na4 2.449(2) 8_545 ?
O16 Gd2 2.5494(18) 7_547 ?
O17 C29 1.266(3) . ?
N19 C36 1.368(3) . ?
N19 C33 1.373(3) . ?
N20 C38 1.368(3) . ?
N20 C50 1.368(3) . ?
N21 C54 1.367(3) . ?
N21 C39 1.368(3) . ?
N22 C45 1.371(3) . ?
N22 C44 1.374(3) . ?
C23 C25 1.497(3) . ?
C23 Gd1 2.914(2) 3_445 ?
C25 C43 1.370(4) . ?
C25 C67 1.373(4) . ?
C26 C31 1.496(3) . ?
C26 Gd2 2.882(2) 7_547 ?
C28 C32 1.492(3) . ?
C28 Gd2 2.850(3) 5_557 ?
C29 C34 1.498(3) . ?
C31 C66 1.359(4) . ?
C31 C74 1.379(5) . ?
C32 C49 1.383(4) . ?
C32 C52 1.393(4) . ?
C33 C47 1.405(4) . ?
C33 C62 1.443(4) . ?
C34 C46 1.375(4) . ?
C34 C61 1.390(4) . ?
C35 C44 1.401(4) . ?
C35 C38 1.403(4) . ?
C35 C42 1.496(3) . ?
C36 C40 1.403(4) . ?
C36 C58 1.452(4) . ?
C37 C39 1.402(4) . ?
C37 C45 1.403(4) . ?
C37 C41 1.498(3) . ?
C38 C70 1.446(4) . ?
C39 C55 1.456(4) . ?
C40 C50 1.410(4) . ?
C40 C56 1.491(4) . ?
C41 C73 1.359(4) . ?
C41 C75 1.374(5) . ?
C42 C69 1.372(4) . ?
C42 C53 1.375(4) . ?
C43 C53 1.391(4) . ?
C44 C51 1.443(4) . ?
C45 C59 1.449(4) . ?
C46 C65 1.387(4) . ?
C47 C54 1.408(4) . ?
C47 C48 1.491(4) . ?
C48 C65 1.386(4) . ?
C48 C68 1.394(4) . ?
C49 C57 1.390(4) . ?
C50 C63 1.448(4) . ?
C51 C59 1.354(4) . ?
C52 C64 1.388(4) . ?
C54 C60 1.442(4) . ?
C55 C60 1.346(4) . ?
C56 C57 1.393(4) . ?
C56 C64 1.392(4) . ?
C58 C62 1.344(4) . ?
C61 C68 1.388(4) . ?
C63 C70 1.349(4) . ?
C66 C73 1.394(4) . ?
C67 C69 1.385(5) . ?
O71 O71' 0.624(5) . ?
O71 C76 1.162(6) . ?
O71' C76 1.168(6) . ?
C74 C75 1.391(5) . ?
C76 O71 1.162(6) 2_557 ?
C76 O71' 1.168(6) 2_557 ?

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
O9 Gd1 O17 120.16(6) . 6 ?
O9 Gd1 O17 120.16(6) . . ?
O17 Gd1 O17 72.80(9) 6 . ?
O9 Gd1 O13 54.50(8) . . ?
O17 Gd1 O13 77.27(7) 6 . ?
O17 Gd1 O13 77.27(7) . . ?
O9 Gd1 O7 125.43(6) . 8_545 ?
O17 Gd1 O7 114.40(6) 6 8_545 ?
O17 Gd1 O7 74.29(6) . 8_545 ?
O13 Gd1 O7 143.68(4) . 8_545 ?
O9 Gd1 O7 125.43(6) . 3 ?
O17 Gd1 O7 74.29(6) 6 3 ?
O17 Gd1 O7 114.40(6) . 3 ?
O13 Gd1 O7 143.68(4) . 3 ?
O7 Gd1 O7 70.36(8) 8_545 3 ?
O9 Gd1 O14 77.60(5) . 6 ?
O17 Gd1 O14 52.53(6) 6 6 ?
O17 Gd1 O14 120.87(6) . 6 ?
O13 Gd1 O14 70.98(4) . 6 ?
O7 Gd1 O14 144.23(6) 8_545 6 ?
O7 Gd1 O14 73.89(6) 3 6 ?
O9 Gd1 O14 77.60(5) . . ?
O17 Gd1 O14 120.87(6) 6 . ?
O17 Gd1 O14 52.53(6) . . ?
O13 Gd1 O14 70.98(4) . . ?
O7 Gd1 O14 73.89(6) 8_545 . ?
O7 Gd1 O14 144.23(6) 3 . ?
O14 Gd1 O14 141.77(9) 6 . ?
O9 Gd1 O8 74.88(6) . 3 ?
O17 Gd1 O8 106.67(6) 6 3 ?
O17 Gd1 O8 163.48(6) . 3 ?
O13 Gd1 O8 119.03(6) . 3 ?
O7 Gd1 O8 91.53(6) 8_545 3 ?
O7 Gd1 O8 51.28(6) 3 3 ?
O14 Gd1 O8 66.58(6) 6 3 ?
O14 Gd1 O8 132.24(6) . 3 ?
O9 Gd1 O8 74.88(6) . 8_545 ?
O17 Gd1 O8 163.48(6) 6 8_545 ?
O17 Gd1 O8 106.68(6) . 8_545 ?
O13 Gd1 O8 119.03(6) . 8_545 ?
O7 Gd1 O8 51.28(6) 8_545 8_545 ?
O7 Gd1 O8 91.53(6) 3 8_545 ?
O14 Gd1 O8 132.24(6) 6 8_545 ?
O14 Gd1 O8 66.58(6) . 8_545 ?
O8 Gd1 O8 68.95(8) 3 8_545 ?
O9 Gd1 N30 28.01(9) . . ?
O17 Gd1 N30 98.53(7) 6 . ?
O17 Gd1 N30 98.52(7) . . ?
O13 Gd1 N30 26.50(9) . . ?
O7 Gd1 N30 141.48(5) 8_545 . ?
O7 Gd1 N30 141.48(5) 3 . ?
O14 Gd1 N30 72.20(4) 6 . ?
O14 Gd1 N30 72.20(4) . . ?
O8 Gd1 N30 97.87(7) 3 . ?
O8 Gd1 N30 97.87(7) 8_545 . ?
O9 Gd1 C29 98.41(6) . . ?
O17 Gd1 C29 96.51(7) 6 . ?
O17 Gd1 C29 26.37(7) . . ?
O13 Gd1 C29 70.95(6) . . ?
O7 Gd1 C29 73.52(7) 8_545 . ?
O7 Gd1 C29 134.14(7) 3 . ?
O14 Gd1 C29 135.24(7) 6 . ?
O14 Gd1 C29 26.22(7) . . ?
O8 Gd1 C29 156.16(7) 3 . ?
O8 Gd1 C29 87.24(7) 8_545 . ?
N30 Gd1 C29 83.79(7) . . ?
O9 Gd2 O12 119.35(6) . 5_557 ?
O9 Gd2 O12 119.35(6) . 2_557 ?
O12 Gd2 O12 71.94(8) 5_557 2_557 ?
O9 Gd2 O11 54.18(8) . . ?
O12 Gd2 O11 76.38(7) 5_557 . ?
O12 Gd2 O11 76.38(7) 2_557 . ?
O9 Gd2 O10 126.22(6) . 4_557 ?
O12 Gd2 O10 73.99(6) 5_557 4_557 ?
O12 Gd2 O10 114.31(6) 2_557 4_557 ?
O11 Gd2 O10 142.75(5) . 4_557 ?
O9 Gd2 O10 126.22(6) . 7_547 ?
O12 Gd2 O10 114.31(6) 5_557 7_547 ?
O12 Gd2 O10 73.99(6) 2_557 7_547 ?
O11 Gd2 O10 142.75(5) . 7_547 ?
O10 Gd2 O10 71.65(10) 4_557 7_547 ?
O9 Gd2 O15 77.31(5) . 2_557 ?
O12 Gd2 O15 119.72(6) 5_557 2_557 ?
O12 Gd2 O15 52.40(6) 2_557 2_557 ?
O11 Gd2 O15 70.36(4) . 2_557 ?
O10 Gd2 O15 145.38(6) 4_557 2_557 ?
O10 Gd2 O15 73.79(7) 7_547 2_557 ?
O9 Gd2 O15 77.31(5) . 5_557 ?
O12 Gd2 O15 52.40(6) 5_557 5_557 ?
O12 Gd2 O15 119.72(6) 2_557 5_557 ?
O11 Gd2 O15 70.36(4) . 5_557 ?
O10 Gd2 O15 73.79(6) 4_557 5_557 ?
O10 Gd2 O15 145.38(7) 7_547 5_557 ?
O15 Gd2 O15 140.58(9) 2_557 5_557 ?
O9 Gd2 O16 75.42(6) . 4_557 ?
O12 Gd2 O16 107.56(6) 5_557 4_557 ?
O12 Gd2 O16 163.90(6) 2_557 4_557 ?
O11 Gd2 O16 119.48(6) . 4_557 ?
O10 Gd2 O16 51.87(6) 4_557 4_557 ?
O10 Gd2 O16 92.25(6) 7_547 4_557 ?
O15 Gd2 O16 132.43(6) 2_557 4_557 ?
O15 Gd2 O16 67.57(6) 5_557 4_557 ?
O9 Gd2 O16 75.42(6) . 7_547 ?
O12 Gd2 O16 163.90(6) 5_557 7_547 ?
O12 Gd2 O16 107.56(6) 2_557 7_547 ?
O11 Gd2 O16 119.48(6) . 7_547 ?
O10 Gd2 O16 92.25(6) 4_557 7_547 ?
O10 Gd2 O16 51.87(6) 7_547 7_547 ?
O15 Gd2 O16 67.57(6) 2_557 7_547 ?
O15 Gd2 O16 132.43(6) 5_557 7_547 ?
O16 Gd2 O16 68.25(8) 4_557 7_547 ?
O9 Gd2 N30 28.01(9) . . ?
O12 Gd2 N30 97.49(7) 5_557 . ?
O12 Gd2 N30 97.49(7) 2_557 . ?
O11 Gd2 N30 26.18(9) . . ?
O10 Gd2 N30 141.48(5) 4_557 . ?
O10 Gd2 N30 141.48(5) 7_547 . ?
O15 Gd2 N30 71.69(5) 2_557 . ?
O15 Gd2 N30 71.69(5) 5_557 . ?
O16 Gd2 N30 98.51(7) 4_557 . ?
O16 Gd2 N30 98.51(7) 7_547 . ?
O9 Gd2 C28 97.53(6) . 2_557 ?
O12 Gd2 C28 95.17(7) 5_557 2_557 ?
O12 Gd2 C28 26.27(7) 2_557 2_557 ?
O11 Gd2 C28 69.50(6) . 2_557 ?
O10 Gd2 C28 134.96(7) 4_557 2_557 ?
O10 Gd2 C28 73.93(7) 7_547 2_557 ?
O15 Gd2 C28 26.26(7) 2_557 2_557 ?
O15 Gd2 C28 133.22(7) 5_557 2_557 ?
O16 Gd2 C28 156.84(7) 4_557 2_557 ?
O16 Gd2 C28 88.67(7) 7_547 2_557 ?
N30 Gd2 C28 82.44(7) . 2_557 ?
N21 Zn3 N22 88.96(8) . . ?
N21 Zn3 N20 159.43(9) . . ?
N22 Zn3 N20 88.46(8) . . ?
N21 Zn3 N19 88.54(8) . . ?
N22 Zn3 N19 164.91(9) . . ?
N20 Zn3 N19 88.67(8) . . ?
N21 Zn3 O71 91.20(17) . . ?
N22 Zn3 O71 98.2(2) . . ?
N20 Zn3 O71 109.37(17) . . ?
N19 Zn3 O71 96.7(2) . . ?
N21 Zn3 O71' 108.34(17) . . ?
N22 Zn3 O71' 97.6(2) . . ?
N20 Zn3 O71' 92.23(17) . . ?
N19 Zn3 O71' 97.3(2) . . ?
O71 Zn3 O71' 17.15(15) . . ?
O27 Na4 O15 103.65(10) . . ?
O27 Na4 O14 100.85(10) . 2_557 ?
O15 Na4 O14 112.24(8) . 2_557 ?
O27 Na4 O8 114.42(10) . 7_447 ?
O15 Na4 O8 139.92(8) . 7_447 ?
O14 Na4 O8 73.38(7) 2_557 7_447 ?
O27 Na4 O16 117.17(10) . 8_445 ?
O15 Na4 O16 73.31(7) . 8_445 ?
O14 Na4 O16 139.53(8) 2_557 8_445 ?
O8 Na4 O16 78.41(7) 7_447 8_445 ?
O27 Na4 O9 171.73(10) . 5_557 ?
O15 Na4 O9 73.67(7) . 5_557 ?
O14 Na4 O9 73.50(7) 2_557 5_557 ?
O8 Na4 O9 70.24(7) 7_447 5_557 ?
O16 Na4 O9 69.93(7) 8_445 5_557 ?
O27 Na4 Na6 130.73(9) . 7_447 ?
O15 Na4 Na6 104.82(6) . 7_447 ?
O14 Na4 Na6 104.37(6) 2_557 7_447 ?
O8 Na4 Na6 39.52(5) 7_447 7_447 ?
O16 Na4 Na6 39.82(5) 8_445 7_447 ?
O9 Na4 Na6 57.33(5) 5_557 7_447 ?
O27 Na4 Gd2 140.63(9) . 5_557 ?
O15 Na4 Gd2 43.33(5) . 5_557 ?
O14 Na4 Gd2 111.07(6) 2_557 5_557 ?
O8 Na4 Gd2 96.80(5) 7_447 5_557 ?
O16 Na4 Gd2 44.40(4) 8_445 5_557 ?
O9 Na4 Gd2 41.20(5) 5_557 5_557 ?
Na6 Na4 Gd2 62.96(3) 7_447 5_557 ?
O27 Na4 Gd1 137.60(9) . 5_557 ?
O15 Na4 Gd1 110.57(6) . 5_557 ?
O14 Na4 Gd1 43.20(5) 2_557 5_557 ?
O8 Na4 Gd1 45.26(5) 7_447 5_557 ?
O16 Na4 Gd1 96.50(5) 8_445 5_557 ?
O9 Na4 Gd1 40.65(5) 5_557 5_557 ?
Na6 Na4 Gd1 62.86(3) 7_447 5_557 ?
Gd2 Na4 Gd1 81.48(2) 5_557 5_557 ?
O12 Na5 O12 79.64(10) . 6 ?
O12 Na5 O7 101.28(7) . 7_446 ?
O12 Na5 O7 175.68(10) 6 7_446 ?
O12 Na5 O7 175.68(10) . 4_456 ?
O12 Na5 O7 101.28(7) 6 4_456 ?
O7 Na5 O7 77.49(10) 7_446 4_456 ?
O12 Na5 O24 97.34(10) . . ?
O12 Na5 O24 97.34(10) 6 . ?
O7 Na5 O24 86.76(10) 7_446 . ?
O7 Na5 O24 86.76(10) 4_456 . ?
O12 Na5 O18 83.84(8) . . ?
O12 Na5 O18 83.85(8) 6 . ?
O7 Na5 O18 92.04(8) 7_446 . ?
O7 Na5 O18 92.04(8) 4_456 . ?
O24 Na5 O18 178.45(13) . . ?
O12 Na5 Gd2 41.84(5) . 5_557 ?
O12 Na5 Gd2 41.84(5) 6 5_557 ?
O7 Na5 Gd2 137.32(5) 7_446 5_557 ?
O7 Na5 Gd2 137.32(5) 4_456 5_557 ?
O24 Na5 Gd2 113.66(11) . 5_557 ?
O18 Na5 Gd2 67.89(8) . 5_557 ?
O12 Na5 Gd1 138.51(5) . 5_556 ?
O12 Na5 Gd1 138.51(5) 6 5_556 ?
O7 Na5 Gd1 42.19(5) 7_446 5_556 ?
O7 Na5 Gd1 42.19(5) 4_456 5_556 ?
O24 Na5 Gd1 67.65(10) . 5_556 ?
O18 Na5 Gd1 110.80(8) . 5_556 ?
Gd2 Na5 Gd1 178.69(5) 5_557 5_556 ?
O72 Na6 O8 116.38(9) . 6_545 ?
O72 Na6 O8 116.38(9) . . ?
O8 Na6 O8 77.90(10) 6_545 . ?
O72 Na6 O16 114.26(9) . 2_557 ?
O8 Na6 O16 129.30(10) 6_545 2_557 ?
O8 Na6 O16 82.31(7) . 2_557 ?
O72 Na6 O16 114.26(9) . 5_547 ?
O8 Na6 O16 82.31(7) 6_545 5_547 ?
O8 Na6 O16 129.30(10) . 5_547 ?
O16 Na6 O16 75.20(10) 2_557 5_547 ?
O72 Na6 Na4 131.67(3) . 4_447 ?
O8 Na6 Na4 41.30(5) 6_545 4_447 ?
O8 Na6 Na4 100.81(7) . 4_447 ?
O16 Na6 Na4 99.67(7) 2_557 4_447 ?
O16 Na6 Na4 42.00(5) 5_547 4_447 ?
O72 Na6 Na4 131.67(3) . 7_447 ?
O8 Na6 Na4 100.81(7) 6_545 7_447 ?
O8 Na6 Na4 41.30(5) . 7_447 ?
O16 Na6 Na4 42.00(5) 2_557 7_447 ?
O16 Na6 Na4 99.67(7) 5_547 7_447 ?
Na4 Na6 Na4 96.60(5) 4_447 7_447 ?
O72 Na6 Gd1 142.84(11) . 3_445 ?
O8 Na6 Gd1 42.30(5) 6_545 3_445 ?
O8 Na6 Gd1 42.30(5) . 3_445 ?
O16 Na6 Gd1 94.69(6) 2_557 3_445 ?
O16 Na6 Gd1 94.69(6) 5_547 3_445 ?
Na4 Na6 Gd1 58.87(3) 4_447 3_445 ?
Na4 Na6 Gd1 58.87(3) 7_447 3_445 ?
O72 Na6 Gd2 139.51(10) . 3_445 ?
O8 Na6 Gd2 94.38(6) 6_545 3_445 ?
O8 Na6 Gd2 94.39(6) . 3_445 ?
O16 Na6 Gd2 41.21(5) 2_557 3_445 ?
O16 Na6 Gd2 41.21(5) 5_547 3_445 ?
Na4 Na6 Gd2 58.70(3) 4_447 3_445 ?
Na4 Na6 Gd2 58.70(3) 7_447 3_445 ?
Gd1 Na6 Gd2 77.65(3) 3_445 3_445 ?
C23 O7 Na5 134.61(17) . 7_446 ?
C23 O7 Gd1 96.12(15) . 3_445 ?
Na5 O7 Gd1 99.63(7) 7_446 3_445 ?
C23 O8 Na6 136.57(17) . . ?
C23 O8 Na4 121.95(16) . 7_447 ?
Na6 O8 Na4 99.18(8) . 7_447 ?
C23 O8 Gd1 91.30(15) . 3_445 ?
Na6 O8 Gd1 100.40(7) . 3_445 ?
Na4 O8 Gd1 93.19(6) 7_447 3_445 ?
N30 O9 Gd1 95.5(2) . . ?
N30 O9 Gd2 94.7(2) . . ?
Gd1 O9 Gd2 169.73(12) . . ?
N30 O9 Na4 105.63(5) . 5_557 ?
Gd1 O9 Na4 88.97(6) . 5_557 ?
Gd2 O9 Na4 88.27(6) . 5_557 ?
N30 O9 Na4 105.63(5) . 2_557 ?
Gd1 O9 Na4 88.97(6) . 2_557 ?
Gd2 O9 Na4 88.27(6) . 2_557 ?
Na4 O9 Na4 148.72(10) 5_557 2_557 ?
C26 O10 Gd2 95.07(15) . 7_547 ?
N30 O11 Gd2 94.1(2) . . ?
C28 O12 Na5 162.59(17) . . ?
C28 O12 Gd2 94.64(15) . 5_557 ?
Na5 O12 Gd2 100.43(7) . 5_557 ?
N30 O13 Gd1 93.6(2) . . ?
C29 O14 Na4 170.27(18) . 2_557 ?
C29 O14 Gd1 91.03(15) . . ?
Na4 O14 Gd1 98.68(7) 2_557 . ?
C28 O15 Na4 169.96(17) . . ?
C28 O15 Gd2 91.45(15) . 5_557 ?
Na4 O15 Gd2 98.56(7) . 5_557 ?
C26 O16 Na6 137.86(17) . 5_547 ?
C26 O16 Na4 121.03(16) . 8_545 ?
Na6 O16 Na4 98.18(8) 5_547 8_545 ?
C26 O16 Gd2 91.67(15) . 7_547 ?
Na6 O16 Gd2 101.51(7) 5_547 7_547 ?
Na4 O16 Gd2 93.36(6) 8_545 7_547 ?
C29 O17 Gd1 94.68(15) . . ?
C36 N19 C33 106.7(2) . . ?
C36 N19 Zn3 125.12(18) . . ?
C33 N19 Zn3 124.23(17) . . ?
C38 N20 C50 106.8(2) . . ?
C38 N20 Zn3 126.63(17) . . ?
C50 N20 Zn3 126.42(18) . . ?
C54 N21 C39 106.9(2) . . ?
C54 N21 Zn3 126.34(17) . . ?
C39 N21 Zn3 126.62(17) . . ?
C45 N22 C44 106.8(2) . . ?
C45 N22 Zn3 125.73(17) . . ?
C44 N22 Zn3 125.82(17) . . ?
O7 C23 O8 121.2(2) . . ?
O7 C23 C25 119.4(2) . . ?
O8 C23 C25 119.4(2) . . ?
O7 C23 Gd1 58.40(12) . 3_445 ?
O8 C23 Gd1 62.87(13) . 3_445 ?
C25 C23 Gd1 176.11(18) . 3_445 ?
C43 C25 C67 118.8(3) . . ?
C43 C25 C23 121.4(2) . . ?
C67 C25 C23 119.8(3) . . ?
O10 C26 O16 121.3(2) . . ?
O10 C26 C31 119.9(2) . . ?
O16 C26 C31 118.7(2) . . ?
O10 C26 Gd2 59.21(13) . 7_547 ?
O16 C26 Gd2 62.16(13) . 7_547 ?
C31 C26 Gd2 177.63(18) . 7_547 ?
O15 C28 O12 120.9(2) . . ?
O15 C28 C32 119.6(2) . . ?
O12 C28 C32 119.5(2) . . ?
O15 C28 Gd2 62.30(13) . 5_557 ?
O12 C28 Gd2 59.08(13) . 5_557 ?
C32 C28 Gd2 171.71(19) . 5_557 ?
O14 C29 O17 121.5(2) . . ?
O14 C29 C34 119.9(2) . . ?
O17 C29 C34 118.6(2) . . ?
O14 C29 Gd1 62.75(13) . . ?
O17 C29 Gd1 58.95(13) . . ?
C34 C29 Gd1 172.49(18) . . ?
O11 N30 O13 126.7(3) . . ?
O11 N30 O9 116.9(3) . . ?
O13 N30 O9 116.3(3) . . ?
O11 N30 Gd1 173.4(3) . . ?
O13 N30 Gd1 59.88(18) . . ?
O9 N30 Gd1 56.46(17) . . ?
O11 N30 Gd2 59.67(18) . . ?
O13 N30 Gd2 173.6(3) . . ?
O9 N30 Gd2 57.26(17) . . ?
Gd1 N30 Gd2 113.72(12) . . ?
C66 C31 C74 119.1(3) . . ?
C66 C31 C26 121.5(3) . . ?
C74 C31 C26 119.4(3) . . ?
C49 C32 C52 119.5(2) . . ?
C49 C32 C28 120.0(2) . . ?
C52 C32 C28 120.5(2) . . ?
N19 C33 C47 125.1(2) . . ?
N19 C33 C62 109.4(2) . . ?
C47 C33 C62 125.5(2) . . ?
C46 C34 C61 119.2(3) . . ?
C46 C34 C29 119.8(2) . . ?
C61 C34 C29 121.0(3) . . ?
C44 C35 C38 125.2(2) . . ?
C44 C35 C42 117.1(2) . . ?
C38 C35 C42 117.6(2) . . ?
N19 C36 C40 125.3(2) . . ?
N19 C36 C58 109.5(2) . . ?
C40 C36 C58 125.3(2) . . ?
C39 C37 C45 125.5(2) . . ?
C39 C37 C41 117.1(2) . . ?
C45 C37 C41 117.3(2) . . ?
N20 C38 C35 125.5(2) . . ?
N20 C38 C70 109.7(2) . . ?
C35 C38 C70 124.7(2) . . ?
N21 C39 C37 125.4(2) . . ?
N21 C39 C55 109.3(2) . . ?
C37 C39 C55 125.2(2) . . ?
C36 C40 C50 125.2(2) . . ?
C36 C40 C56 117.3(2) . . ?
C50 C40 C56 117.4(2) . . ?
C73 C41 C75 118.1(3) . . ?
C73 C41 C37 121.8(2) . . ?
C75 C41 C37 120.1(3) . . ?
C69 C42 C53 117.7(3) . . ?
C69 C42 C35 119.2(3) . . ?
C53 C42 C35 123.0(3) . . ?
C25 C43 C53 120.0(3) . . ?
N22 C44 C35 125.0(2) . . ?
N22 C44 C51 109.5(2) . . ?
C35 C44 C51 125.3(2) . . ?
N22 C45 C37 124.9(2) . . ?
N22 C45 C59 109.4(2) . . ?
C37 C45 C59 125.5(2) . . ?
C34 C46 C65 120.4(3) . . ?
C33 C47 C54 124.9(2) . . ?
C33 C47 C48 117.2(2) . . ?
C54 C47 C48 117.9(2) . . ?
C65 C48 C68 117.9(3) . . ?
C65 C48 C47 120.6(2) . . ?
C68 C48 C47 121.5(3) . . ?
C32 C49 C57 120.3(3) . . ?
N20 C50 C40 125.5(2) . . ?
N20 C50 C63 109.5(2) . . ?
C40 C50 C63 124.9(2) . . ?
C59 C51 C44 107.2(2) . . ?
C64 C52 C32 120.1(3) . . ?
C42 C53 C43 121.6(3) . . ?
N21 C54 C47 125.5(2) . . ?
N21 C54 C60 109.6(2) . . ?
C47 C54 C60 124.9(2) . . ?
C60 C55 C39 106.7(2) . . ?
C57 C56 C64 118.5(2) . . ?
C57 C56 C40 119.7(3) . . ?
C64 C56 C40 121.7(3) . . ?
C49 C57 C56 120.8(3) . . ?
C62 C58 C36 106.9(2) . . ?
C51 C59 C45 107.0(2) . . ?
C55 C60 C54 107.4(2) . . ?
C34 C61 C68 120.3(3) . . ?
C58 C62 C33 107.4(2) . . ?
C70 C63 C50 107.1(2) . . ?
C52 C64 C56 120.8(3) . . ?
C48 C65 C46 121.3(3) . . ?
C31 C66 C73 120.5(3) . . ?
C25 C67 C69 120.8(3) . . ?
C61 C68 C48 120.8(3) . . ?
C42 C69 C67 121.1(3) . . ?
C63 C70 C38 107.0(3) . . ?
O71' O71 C76 75.0(10) . . ?
O71' O71 Zn3 82.1(10) . . ?
C76 O71 Zn3 154.2(5) . . ?
O71 O71' C76 73.9(10) . . ?
O71 O71' Zn3 80.8(10) . . ?
C76 O71' Zn3 152.1(4) . . ?
C41 C73 C66 121.2(3) . . ?
C31 C74 C75 119.5(3) . . ?
C41 C75 C74 121.4(3) . . ?
O71 C76 O71 162.8(9) 2_557 . ?
O71 C76 O71' 31.1(3) 2_557 2_557 ?
O71 C76 O71' 144.6(4) . 2_557 ?
O71 C76 O71' 144.6(4) 2_557 . ?
O71 C76 O71' 31.1(3) . . ?
O71' C76 O71' 164.3(9) 2_557 . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.009 -0.003 -0.001 3851 903 ' '
2 0.000 0.500 0.010 541 114 ' '
3 0.500 0.000 0.851 541 114 ' '
_platon_squeeze_details          
;
 Disordered DMF/DMA/water solvent.
;

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 1014719'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt40sq(6)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C97 H50 Dy2 N9 Na4 O25 Zn2'
_chemical_formula_sum            'C97 H50 Dy2 N9 Na4 O25 Zn2'
_chemical_formula_weight         2289.21

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'
Zn Zn 0.2839 1.4301 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'

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

_cell_length_a                   32.7734(13)
_cell_length_b                   34.8731(14)
_cell_length_c                   11.4924(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7290(18)
_cell_angle_gamma                90.00
_cell_volume                     12363.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    10097
_cell_measurement_theta_min      1.76
_cell_measurement_theta_max      25.38

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4524
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_T_max  0.7893
_exptl_absorpt_process_details   'Blessing, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1.0 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45837
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.38
_reflns_number_total             11524
_reflns_number_gt                10097
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The crystal contains severely disordered crystallization solvent trapped
 within the channel voids, which could not be modeled by discrete atoms.
 Its contribution to the diffraction pattern was subtracted by the Squeeze
 technique, using the PLATON software.
 H-atoms of the metal coordinated water O20 could not be located.

;

_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)+(0.0590P)²+4.0066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11524
_refine_ls_number_parameters     646
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.003

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
Dy1 Dy 0.292314(7) 0.0000 0.20509(2) 0.00973(8) Uani 1 2 d S . .
Dy2 Dy 0.237173(7) 0.0000 -0.23206(2) 0.00892(8) Uani 1 2 d S . .
Zn3 Zn 0.536237(13) 0.261399(12) 0.29527(4) 0.01640(11) Uani 1 1 d . . .
Na4 Na 0.32388(6) 0.5000 0.00731(19) 0.0162(4) Uani 1 2 d S . .
Na5 Na 0.75203(4) 0.07731(4) 0.01261(12) 0.0139(3) Uani 1 1 d . . .
Na6 Na 0.76674(7) 0.5000 0.49117(19) 0.0214(5) Uani 1 2 d S . .
O7 O 0.73418(8) 0.04067(7) 0.3585(2) 0.0120(5) Uani 1 1 d . . .
O8 O 0.76126(8) 0.45897(7) 0.3310(2) 0.0132(5) Uani 1 1 d . . .
O9 O 0.27068(10) 0.0000 -0.0130(3) 0.0102(7) Uani 1 2 d S . .
O10 O 0.72347(8) 0.45817(7) 0.1319(2) 0.0146(5) Uani 1 1 d . . .
O11 O 0.32347(8) 0.45856(7) 0.3534(2) 0.0165(6) Uani 1 1 d . . .
O12 O 0.35080(8) 0.04085(7) 0.3275(2) 0.0165(6) Uani 1 1 d . . .
O13 O 0.31201(7) 0.45938(7) 0.1537(2) 0.0141(5) Uani 1 1 d . . .
O14 O 0.31505(11) 0.0000 -0.1216(3) 0.0161(8) Uani 1 2 d S . .
O15 O 0.73652(8) 0.06778(7) 0.1878(2) 0.0143(5) Uani 1 1 d . . .
O16 O 0.34145(11) 0.0000 0.0881(3) 0.0163(8) Uani 1 2 d S . .
O17 O 0.30661(8) 0.06781(7) 0.1598(2) 0.0147(5) Uani 1 1 d . . .
O18 O 0.68634(14) 0.5000 0.4414(4) 0.0312(10) Uani 1 2 d S . .
H18 H 0.6761 0.5221 0.4850 0.037 Uiso 1 1 d R . .
O19 O 0.75959(13) 0.14060(9) 0.0065(3) 0.0472(10) Uani 1 1 d . . .
O20 O 0.84389(17) 0.5000 0.5412(5) 0.0501(19) Uani 1 2 d S . .
O21 O 0.51342(18) 0.25597(11) 0.1033(3) 0.0477(15) Uani 1 1 d . . .
N22 N 0.53963(9) 0.20287(8) 0.3301(3) 0.0128(6) Uani 1 1 d . . .
N23 N 0.47776(9) 0.26240(8) 0.3271(3) 0.0123(6) Uani 1 1 d . . .
N24 N 0.60268(9) 0.26146(8) 0.3307(3) 0.0143(6) Uani 1 1 d . . .
N25 N 0.53851(9) 0.32029(8) 0.3085(3) 0.0133(6) Uani 1 1 d . . .
N26 N 0.31085(16) 0.0000 -0.0171(5) 0.0249(11) Uani 1 2 d S . .
C27 C 0.70080(11) 0.41636(10) 0.2629(3) 0.0110(7) Uani 1 1 d . . .
C28 C 0.33257(11) 0.44698(10) 0.2617(3) 0.0129(7) Uani 1 1 d . . .
C29 C 0.57257(11) 0.17937(10) 0.3253(3) 0.0135(7) Uani 1 1 d . . .
C30 C 0.50413(11) 0.34392(10) 0.3005(3) 0.0124(7) Uani 1 1 d . . .
C31 C 0.73001(11) 0.44626(10) 0.2412(3) 0.0119(7) Uani 1 1 d . . .
C32 C 0.34054(11) 0.06893(10) 0.2534(3) 0.0145(8) Uani 1 1 d . . .
C33 C 0.37035(11) 0.10271(10) 0.2746(4) 0.0154(8) Uani 1 1 d . . .
C34 C 0.62821(11) 0.29291(11) 0.3352(4) 0.0159(8) Uani 1 1 d . . .
C35 C 0.46404(11) 0.19272(11) 0.3196(3) 0.0156(8) Uani 1 1 d . . .
C36 C 0.50419(12) 0.17988(10) 0.3153(3) 0.0155(8) Uani 1 1 d . . .
C37 C 0.43142(11) 0.36235(10) 0.3029(3) 0.0147(8) Uani 1 1 d . . .
C38 C 0.51530(12) 0.38324(10) 0.2821(4) 0.0183(8) Uani 1 1 d . . .
H38 H 0.4972 0.4051 0.2722 0.022 Uiso 1 1 calc R . .
C39 C 0.61342(11) 0.33097(10) 0.3130(3) 0.0131(7) Uani 1 1 d . . .
C40 C 0.45344(11) 0.23127(10) 0.3336(3) 0.0141(8) Uani 1 1 d . . .
C41 C 0.72498(11) 0.06833(10) 0.2815(3) 0.0124(7) Uani 1 1 d . . .
C42 C 0.61437(12) 0.19146(11) 0.3348(4) 0.0165(8) Uani 1 1 d . . .
C43 C 0.69896(11) 0.10127(10) 0.3014(3) 0.0146(8) Uani 1 1 d . . .
C44 C 0.64444(11) 0.36057(10) 0.2979(4) 0.0141(7) Uani 1 1 d . . .
C45 C 0.45457(11) 0.29431(11) 0.3348(3) 0.0154(8) Uani 1 1 d . . .
C46 C 0.46508(11) 0.33213(10) 0.3150(3) 0.0135(7) Uani 1 1 d . . .
C47 C 0.57132(11) 0.34349(10) 0.2981(3) 0.0144(7) Uani 1 1 d . . .
C48 C 0.36753(11) 0.41807(10) 0.2784(3) 0.0133(7) Uani 1 1 d . . .
C49 C 0.62857(11) 0.22980(11) 0.3440(4) 0.0164(8) Uani 1 1 d . . .
C50 C 0.55679(12) 0.38274(11) 0.2816(4) 0.0176(8) Uani 1 1 d . . .
H50 H 0.5731 0.4043 0.2721 0.021 Uiso 1 1 calc R . .
C51 C 0.43023(12) 0.16282(11) 0.3069(4) 0.0180(8) Uani 1 1 d . . .
C52 C 0.51519(13) 0.14084(11) 0.2977(4) 0.0196(8) Uani 1 1 d . . .
H52 H 0.4963 0.1194 0.2841 0.024 Uiso 1 1 calc R . .
C53 C 0.64581(12) 0.16111(10) 0.3289(4) 0.0175(8) Uani 1 1 d . . .
C54 C 0.40737(12) 0.10337(11) 0.3760(4) 0.0193(8) Uani 1 1 d . . .
H54 H 0.4128 0.0834 0.4355 0.023 Uiso 1 1 calc R . .
C55 C 0.70336(13) 0.40551(12) 0.3792(4) 0.0238(9) Uani 1 1 d . . .
H55 H 0.7244 0.4169 0.4489 0.029 Uiso 1 1 calc R . .
C56 C 0.68754(14) 0.13115(11) 0.2167(4) 0.0226(9) Uani 1 1 d . . .
H56 H 0.6979 0.1313 0.1488 0.027 Uiso 1 1 calc R . .
C57 C 0.55673(13) 0.14020(11) 0.3040(4) 0.0197(8) Uani 1 1 d . . .
H57 H 0.5728 0.1183 0.2961 0.024 Uiso 1 1 calc R . .
C58 C 0.41546(12) 0.28244(11) 0.3568(4) 0.0220(9) Uani 1 1 d . . .
H58 H 0.3942 0.2988 0.3695 0.026 Uiso 1 1 calc R . .
C59 C 0.43707(12) 0.13327(12) 0.3923(4) 0.0219(9) Uani 1 1 d . . .
H59 H 0.4625 0.1334 0.4633 0.026 Uiso 1 1 calc R . .
C60 C 0.41495(12) 0.24389(12) 0.3557(4) 0.0228(9) Uani 1 1 d . . .
H60 H 0.3932 0.2279 0.3675 0.027 Uiso 1 1 calc R . .
C61 C 0.36171(13) 0.13308(12) 0.1914(4) 0.0296(10) Uani 1 1 d . . .
H61 H 0.3356 0.1333 0.1226 0.035 Uiso 1 1 calc R . .
C62 C 0.68529(12) 0.10230(11) 0.4036(4) 0.0188(8) Uani 1 1 d . . .
H62 H 0.6942 0.0828 0.4648 0.023 Uiso 1 1 calc R . .
C63 C 0.67540(14) 0.37787(13) 0.3967(4) 0.0269(10) Uani 1 1 d . . .
H63 H 0.6777 0.3707 0.4784 0.032 Uiso 1 1 calc R . .
C64 C 0.66138(14) 0.16064(12) 0.2295(4) 0.0243(9) Uani 1 1 d . . .
H64 H 0.6539 0.1808 0.1705 0.029 Uiso 1 1 calc R . .
C65 C 0.67254(13) 0.24218(12) 0.3641(4) 0.0272(10) Uani 1 1 d . . .
H65 H 0.6972 0.2261 0.3795 0.033 Uiso 1 1 calc R . .
C66 C 0.65864(12) 0.13182(11) 0.4161(4) 0.0189(8) Uani 1 1 d . . .
H66 H 0.6490 0.1320 0.4853 0.023 Uiso 1 1 calc R . .
C67 C 0.38843(16) 0.40150(14) 0.3901(4) 0.0359(12) Uani 1 1 d . . .
H67 H 0.3813 0.4091 0.4603 0.043 Uiso 1 1 calc R . .
C68 C 0.39113(13) 0.16309(12) 0.2083(4) 0.0281(10) Uani 1 1 d . . .
H68 H 0.3845 0.1840 0.1520 0.034 Uiso 1 1 calc R . .
C69 C 0.67223(12) 0.28064(12) 0.3572(4) 0.0249(9) Uani 1 1 d . . .
H69 H 0.6964 0.2967 0.3653 0.030 Uiso 1 1 calc R . .
C70 C 0.42022(15) 0.37344(14) 0.4031(4) 0.0365(12) Uani 1 1 d . . .
H70 H 0.4341 0.3620 0.4815 0.044 Uiso 1 1 calc R . .
C71 C 0.67047(18) 0.39879(19) 0.1636(4) 0.0561(18) Uani 1 1 d . . .
H71 H 0.6684 0.4058 0.0819 0.067 Uiso 1 1 calc R . .
C72 C 0.5000 0.2648(2) 0.0000 0.053(2) Uani 1 2 d S . .
C73 C 0.38010(17) 0.40826(17) 0.1787(4) 0.0454(15) Uani 1 1 d . . .
H73 H 0.3675 0.4208 0.1016 0.054 Uiso 1 1 calc R . .
C74 C 0.64304(18) 0.37098(18) 0.1818(4) 0.0532(17) Uani 1 1 d . . .
H74 H 0.6228 0.3589 0.1121 0.064 Uiso 1 1 calc R . .
C75 C 0.41108(18) 0.38009(18) 0.1917(5) 0.0528(17) Uani 1 1 d . . .
H75 H 0.4185 0.3728 0.1217 0.063 Uiso 1 1 calc R . .


_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
Dy1 O9 2.363(3) . ?
Dy1 O12 2.421(2) . ?
Dy1 O12 2.421(2) 6 ?
Dy1 O16 2.421(4) . ?
Dy1 O8 2.485(2) 8_455 ?
Dy1 O8 2.485(2) 3_445 ?
Dy1 O17 2.500(2) . ?
Dy1 O17 2.500(2) 6 ?
Dy1 O10 2.578(2) 3_445 ?
Dy1 O10 2.578(2) 8_455 ?
Dy1 N26 2.818(5) . ?
Dy1 C32 2.827(4) . ?
Dy2 O9 2.383(3) . ?
Dy2 O7 2.434(2) 5_655 ?
Dy2 O7 2.434(2) 2_655 ?
Dy2 O14 2.437(3) . ?
Dy2 O11 2.473(2) 4_545 ?
Dy2 O11 2.473(2) 7 ?
Dy2 O15 2.509(2) 2_655 ?
Dy2 O15 2.509(2) 5_655 ?
Dy2 O13 2.528(2) 4_545 ?
Dy2 O13 2.528(2) 7 ?
Dy2 N26 2.811(5) . ?
Dy2 C41 2.831(4) 2_655 ?
Zn3 N25 2.059(3) . ?
Zn3 N23 2.069(3) . ?
Zn3 N24 2.076(3) . ?
Zn3 N22 2.076(3) . ?
Zn3 O21 2.085(4) . ?
Na4 O10 2.328(3) 2_655 ?
Na4 O10 2.328(3) 5_665 ?
Na4 O13 2.331(3) 6_565 ?
Na4 O13 2.331(3) . ?
Na4 Na5 3.594(2) 8_455 ?
Na4 Na5 3.594(2) 3_455 ?
Na4 Dy2 3.764(2) 7 ?
Na4 Dy1 3.766(2) 7 ?
Na5 O19 2.225(3) . ?
Na5 O15 2.261(3) . ?
Na5 O17 2.271(3) 2_655 ?
Na5 O10 2.415(3) 7_655 ?
Na5 O13 2.445(3) 8 ?
Na5 O9 2.7973(16) 5_655 ?
Na5 Na4 3.594(2) 3_545 ?
Na5 Dy2 3.6265(14) 5_655 ?
Na5 Dy1 3.6311(14) 5_655 ?
Na6 O7 2.243(3) 4_656 ?
Na6 O7 2.243(3) 7_656 ?
Na6 O8 2.290(3) . ?
Na6 O8 2.290(3) 6_565 ?
Na6 O20 2.396(6) . ?
Na6 O18 2.500(5) . ?
Na6 Dy2 3.625(2) 3_556 ?
Na6 Dy1 3.657(2) 3 ?
O7 C41 1.274(4) . ?
O7 Na6 2.243(3) 7_656 ?
O7 Dy2 2.434(2) 5_655 ?
O8 C31 1.264(4) . ?
O8 Dy1 2.485(2) 3 ?
O9 N26 1.333(6) . ?
O9 Na5 2.7971(16) 5_655 ?
O9 Na5 2.7971(16) 2_655 ?
O10 C31 1.271(4) . ?
O10 Na4 2.328(3) 5_665 ?
O10 Na5 2.415(3) 7_655 ?
O10 Dy1 2.578(2) 3 ?
O11 C28 1.255(4) . ?
O11 Dy2 2.472(2) 7 ?
O12 C32 1.267(4) . ?
O13 C28 1.271(4) . ?
O13 Na5 2.445(3) 8_455 ?
O13 Dy2 2.529(2) 7 ?
O14 N26 1.254(6) . ?
O15 C41 1.257(4) . ?
O15 Dy2 2.509(2) 5_655 ?
O16 N26 1.285(6) . ?
O17 C32 1.260(4) . ?
O17 Na5 2.271(3) 2_655 ?
O21 C72 1.160(4) . ?
N22 C29 1.371(5) . ?
N22 C36 1.374(5) . ?
N23 C40 1.364(5) . ?
N23 C45 1.367(5) . ?
N24 C49 1.369(5) . ?
N24 C34 1.370(5) . ?
N25 C30 1.374(4) . ?
N25 C47 1.383(5) . ?
C27 C55 1.364(5) . ?
C27 C71 1.379(6) . ?
C27 C31 1.492(5) . ?
C28 C48 1.490(5) . ?
C28 Dy2 2.869(3) 7 ?
C29 C42 1.402(5) . ?
C29 C57 1.453(5) . ?
C30 C46 1.406(5) . ?
C30 C38 1.453(5) . ?
C31 Dy1 2.903(3) 3 ?
C32 C33 1.497(5) . ?
C33 C54 1.369(5) . ?
C33 C61 1.391(6) . ?
C34 C39 1.406(5) . ?
C34 C69 1.443(5) . ?
C35 C36 1.407(5) . ?
C35 C40 1.411(5) . ?
C35 C51 1.492(5) . ?
C36 C52 1.440(5) . ?
C37 C75 1.373(6) . ?
C37 C70 1.376(6) . ?
C37 C46 1.498(5) . ?
C38 C50 1.362(5) . ?
C39 C47 1.401(5) . ?
C39 C44 1.500(5) . ?
C40 C60 1.438(5) . ?
C41 C43 1.494(5) . ?
C41 Dy2 2.831(4) 5_655 ?
C42 C49 1.408(5) . ?
C42 C53 1.495(5) . ?
C43 C56 1.389(5) . ?
C43 C62 1.392(5) . ?
C44 C74 1.368(6) . ?
C44 C63 1.380(5) . ?
C45 C46 1.401(5) . ?
C45 C58 1.448(5) . ?
C47 C50 1.440(5) . ?
C48 C67 1.363(6) . ?
C48 C73 1.384(6) . ?
C49 C65 1.446(5) . ?
C51 C59 1.388(6) . ?
C51 C68 1.395(5) . ?
C52 C57 1.339(6) . ?
C53 C66 1.393(5) . ?
C53 C64 1.400(6) . ?
C54 C59 1.395(5) . ?
C55 C63 1.390(5) . ?
C56 C64 1.379(6) . ?
C58 C60 1.345(6) . ?
C61 C68 1.392(6) . ?
C62 C66 1.389(5) . ?
C65 C69 1.343(6) . ?
C67 C70 1.400(6) . ?
C71 C74 1.385(6) . ?
C72 O21 1.160(4) 2_655 ?
C73 C75 1.384(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Dy1 O12 120.77(8) . . ?
O9 Dy1 O12 120.77(8) . 6 ?
O12 Dy1 O12 72.09(12) . 6 ?
O9 Dy1 O16 55.17(11) . . ?
O12 Dy1 O16 77.18(9) . . ?
O12 Dy1 O16 77.18(9) 6 . ?
O9 Dy1 O8 125.63(8) . 8_455 ?
O12 Dy1 O8 73.87(8) . 8_455 ?
O12 Dy1 O8 113.58(8) 6 8_455 ?
O16 Dy1 O8 143.46(6) . 8_455 ?
O9 Dy1 O8 125.63(8) . 3_445 ?
O12 Dy1 O8 113.57(8) . 3_445 ?
O12 Dy1 O8 73.87(8) 6 3_445 ?
O16 Dy1 O8 143.46(6) . 3_445 ?
O8 Dy1 O8 70.34(11) 8_455 3_445 ?
O9 Dy1 O17 77.83(6) . . ?
O12 Dy1 O17 52.92(8) . . ?
O12 Dy1 O17 120.70(8) 6 . ?
O16 Dy1 O17 71.20(6) . . ?
O8 Dy1 O17 73.67(8) 8_455 . ?
O8 Dy1 O17 143.97(8) 3_445 . ?
O9 Dy1 O17 77.83(6) . 6 ?
O12 Dy1 O17 120.70(8) . 6 ?
O12 Dy1 O17 52.92(8) 6 6 ?
O16 Dy1 O17 71.20(6) . 6 ?
O8 Dy1 O17 143.97(8) 8_455 6 ?
O8 Dy1 O17 73.67(8) 3_445 6 ?
O17 Dy1 O17 142.21(12) . 6 ?
O9 Dy1 O10 74.79(8) . 3_445 ?
O12 Dy1 O10 163.06(9) . 3_445 ?
O12 Dy1 O10 106.90(8) 6 3_445 ?
O16 Dy1 O10 119.46(8) . 3_445 ?
O8 Dy1 O10 91.75(8) 8_455 3_445 ?
O8 Dy1 O10 51.59(8) 3_445 3_445 ?
O17 Dy1 O10 132.24(8) . 3_445 ?
O17 Dy1 O10 66.52(8) 6 3_445 ?
O9 Dy1 O10 74.79(8) . 8_455 ?
O12 Dy1 O10 106.90(8) . 8_455 ?
O12 Dy1 O10 163.06(9) 6 8_455 ?
O16 Dy1 O10 119.46(8) . 8_455 ?
O8 Dy1 O10 51.59(8) 8_455 8_455 ?
O8 Dy1 O10 91.75(8) 3_445 8_455 ?
O17 Dy1 O10 66.52(8) . 8_455 ?
O17 Dy1 O10 132.24(8) 6 8_455 ?
O10 Dy1 O10 68.92(11) 3_445 8_455 ?
O9 Dy1 N26 28.11(12) . . ?
O12 Dy1 N26 98.98(10) . . ?
O12 Dy1 N26 98.98(10) 6 . ?
O16 Dy1 N26 27.06(13) . . ?
O8 Dy1 N26 141.64(7) 8_455 . ?
O8 Dy1 N26 141.64(7) 3_445 . ?
O17 Dy1 N26 72.44(6) . . ?
O17 Dy1 N26 72.44(6) 6 . ?
O10 Dy1 N26 97.87(10) 3_445 . ?
O10 Dy1 N26 97.87(10) 8_455 . ?
O9 Dy1 C32 98.96(8) . . ?
O12 Dy1 C32 26.52(9) . . ?
O12 Dy1 C32 96.07(9) 6 . ?
O16 Dy1 C32 71.11(8) . . ?
O8 Dy1 C32 73.01(9) 8_455 . ?
O8 Dy1 C32 133.41(9) 3_445 . ?
O17 Dy1 C32 26.46(9) . . ?
O17 Dy1 C32 135.53(9) 6 . ?
O10 Dy1 C32 156.20(9) 3_445 . ?
O10 Dy1 C32 87.29(9) 8_455 . ?
N26 Dy1 C32 84.29(9) . . ?
O9 Dy2 O7 119.84(8) . 5_655 ?
O9 Dy2 O7 119.84(8) . 2_655 ?
O7 Dy2 O7 71.27(11) 5_655 2_655 ?
O9 Dy2 O14 54.66(11) . . ?
O7 Dy2 O14 76.33(9) 5_655 . ?
O7 Dy2 O14 76.33(9) 2_655 . ?
O9 Dy2 O11 126.30(8) . 4_545 ?
O7 Dy2 O11 73.82(9) 5_655 4_545 ?
O7 Dy2 O11 113.73(8) 2_655 4_545 ?
O14 Dy2 O11 142.66(7) . 4_545 ?
O9 Dy2 O11 126.30(8) . 7 ?
O7 Dy2 O11 113.73(8) 5_655 7 ?
O7 Dy2 O11 73.82(8) 2_655 7 ?
O14 Dy2 O11 142.66(7) . 7 ?
O11 Dy2 O11 71.54(12) 4_545 7 ?
O9 Dy2 O15 77.37(6) . 2_655 ?
O7 Dy2 O15 119.65(8) 5_655 2_655 ?
O7 Dy2 O15 52.90(8) 2_655 2_655 ?
O14 Dy2 O15 70.52(6) . 2_655 ?
O11 Dy2 O15 145.18(8) 4_545 2_655 ?
O11 Dy2 O15 73.71(8) 7 2_655 ?
O9 Dy2 O15 77.37(6) . 5_655 ?
O7 Dy2 O15 52.90(8) 5_655 5_655 ?
O7 Dy2 O15 119.65(8) 2_655 5_655 ?
O14 Dy2 O15 70.52(6) . 5_655 ?
O11 Dy2 O15 73.71(8) 4_545 5_655 ?
O11 Dy2 O15 145.18(8) 7 5_655 ?
O15 Dy2 O15 140.86(12) 2_655 5_655 ?
O9 Dy2 O13 75.27(8) . 4_545 ?
O7 Dy2 O13 107.87(8) 5_655 4_545 ?
O7 Dy2 O13 163.64(8) 2_655 4_545 ?
O14 Dy2 O13 119.73(8) . 4_545 ?
O11 Dy2 O13 52.10(8) 4_545 4_545 ?
O11 Dy2 O13 92.33(8) 7 4_545 ?
O15 Dy2 O13 132.24(8) 2_655 4_545 ?
O15 Dy2 O13 67.46(8) 5_655 4_545 ?
O9 Dy2 O13 75.27(8) . 7 ?
O7 Dy2 O13 163.64(8) 5_655 7 ?
O7 Dy2 O13 107.87(8) 2_655 7 ?
O14 Dy2 O13 119.73(8) . 7 ?
O11 Dy2 O13 92.33(8) 4_545 7 ?
O11 Dy2 O13 52.10(8) 7 7 ?
O15 Dy2 O13 67.46(8) 2_655 7 ?
O15 Dy2 O13 132.24(8) 5_655 7 ?
O13 Dy2 O13 68.14(11) 4_545 7 ?
O9 Dy2 N26 28.23(13) . . ?
O7 Dy2 N26 97.72(10) 5_655 . ?
O7 Dy2 N26 97.72(10) 2_655 . ?
O14 Dy2 N26 26.42(13) . . ?
O11 Dy2 N26 141.63(7) 4_545 . ?
O11 Dy2 N26 141.63(7) 7 . ?
O15 Dy2 N26 71.78(6) 2_655 . ?
O15 Dy2 N26 71.78(6) 5_655 . ?
O13 Dy2 N26 98.56(10) 4_545 . ?
O13 Dy2 N26 98.56(10) 7 . ?
O9 Dy2 C41 97.77(8) . 2_655 ?
O7 Dy2 C41 95.00(9) 5_655 2_655 ?
O7 Dy2 C41 26.67(9) 2_655 2_655 ?
O14 Dy2 C41 69.62(8) . 2_655 ?
O11 Dy2 C41 134.59(9) 4_545 2_655 ?
O11 Dy2 C41 73.63(9) 7 2_655 ?
O15 Dy2 C41 26.34(9) 2_655 2_655 ?
O15 Dy2 C41 133.63(9) 5_655 2_655 ?
O13 Dy2 C41 156.64(9) 4_545 2_655 ?
O13 Dy2 C41 88.57(9) 7 2_655 ?
N26 Dy2 C41 82.63(9) . 2_655 ?
N25 Zn3 N23 89.00(11) . . ?
N25 Zn3 N24 88.57(11) . . ?
N23 Zn3 N24 159.77(13) . . ?
N25 Zn3 N22 165.55(12) . . ?
N23 Zn3 N22 88.57(11) . . ?
N24 Zn3 N22 88.79(11) . . ?
N25 Zn3 O21 99.20(14) . . ?
N23 Zn3 O21 99.54(18) . . ?
N24 Zn3 O21 100.68(18) . . ?
N22 Zn3 O21 95.25(14) . . ?
O10 Na4 O10 77.60(14) 2_655 5_665 ?
O10 Na4 O13 129.93(12) 2_655 6_565 ?
O10 Na4 O13 83.12(10) 5_665 6_565 ?
O10 Na4 O13 83.12(10) 2_655 . ?
O10 Na4 O13 129.93(12) 5_665 . ?
O13 Na4 O13 74.85(14) 6_565 . ?
O10 Na4 Na5 41.66(7) 2_655 8_455 ?
O10 Na4 Na5 101.13(9) 5_665 8_455 ?
O13 Na4 Na5 100.00(9) 6_565 8_455 ?
O13 Na4 Na5 42.42(7) . 8_455 ?
O10 Na4 Na5 101.13(9) 2_655 3_455 ?
O10 Na4 Na5 41.66(7) 5_665 3_455 ?
O13 Na4 Na5 42.42(7) 6_565 3_455 ?
O13 Na4 Na5 100.00(9) . 3_455 ?
Na5 Na4 Na5 97.22(7) 8_455 3_455 ?
O10 Na4 Dy2 94.93(8) 2_655 7 ?
O10 Na4 Dy2 94.93(8) 5_665 7 ?
O13 Na4 Dy2 41.18(7) 6_565 7 ?
O13 Na4 Dy2 41.19(7) . 7 ?
Na5 Na4 Dy2 59.01(4) 8_455 7 ?
Na5 Na4 Dy2 59.01(4) 3_455 7 ?
O10 Na4 Dy1 42.35(7) 2_655 7 ?
O10 Na4 Dy1 42.35(7) 5_665 7 ?
O13 Na4 Dy1 95.12(8) 6_565 7 ?
O13 Na4 Dy1 95.12(8) . 7 ?
Na5 Na4 Dy1 59.07(4) 8_455 7 ?
Na5 Na4 Dy1 59.07(4) 3_455 7 ?
Dy2 Na4 Dy1 77.84(4) 7 7 ?
O19 Na5 O15 103.60(13) . . ?
O19 Na5 O17 100.81(13) . 2_655 ?
O15 Na5 O17 112.15(11) . 2_655 ?
O19 Na5 O10 114.83(13) . 7_655 ?
O15 Na5 O10 139.79(11) . 7_655 ?
O17 Na5 O10 72.86(9) 2_655 7_655 ?
O19 Na5 O13 117.84(13) . 8 ?
O15 Na5 O13 72.81(9) . 8 ?
O17 Na5 O13 139.15(10) 2_655 8 ?
O10 Na5 O13 78.96(9) 7_655 8 ?
O19 Na5 O9 171.40(14) . 5_655 ?
O15 Na5 O9 73.57(10) . 5_655 ?
O17 Na5 O9 73.35(10) 2_655 5_655 ?
O10 Na5 O9 69.98(9) 7_655 5_655 ?
O13 Na5 O9 69.47(9) 8 5_655 ?
O19 Na5 Na4 131.53(12) . 3_545 ?
O15 Na5 Na4 104.50(8) . 3_545 ?
O17 Na5 Na4 104.02(8) 2_655 3_545 ?
O10 Na5 Na4 39.84(7) 7_655 3_545 ?
O13 Na5 Na4 40.01(7) 8 3_545 ?
O9 Na5 Na4 56.85(7) 5_655 3_545 ?
O19 Na5 Dy2 140.70(11) . 5_655 ?
O15 Na5 Dy2 43.12(6) . 5_655 ?
O17 Na5 Dy2 110.70(8) 2_655 5_655 ?
O10 Na5 Dy2 96.90(7) 7_655 5_655 ?
O13 Na5 Dy2 44.10(6) 8 5_655 ?
O9 Na5 Dy2 41.06(7) 5_655 5_655 ?
Na4 Na5 Dy2 62.83(4) 3_545 5_655 ?
O19 Na5 Dy1 137.53(11) . 5_655 ?
O15 Na5 Dy1 110.27(8) . 5_655 ?
O17 Na5 Dy1 42.83(7) 2_655 5_655 ?
O10 Na5 Dy1 45.13(6) 7_655 5_655 ?
O13 Na5 Dy1 96.52(7) 8 5_655 ?
O9 Na5 Dy1 40.59(7) 5_655 5_655 ?
Na4 Na5 Dy1 62.83(4) 3_545 5_655 ?
Dy2 Na5 Dy1 81.35(3) 5_655 5_655 ?
O7 Na6 O7 78.43(14) 4_656 7_656 ?
O7 Na6 O8 175.03(14) 4_656 . ?
O7 Na6 O8 101.89(9) 7_656 . ?
O7 Na6 O8 101.89(9) 4_656 6_565 ?
O7 Na6 O8 175.03(14) 7_656 6_565 ?
O8 Na6 O8 77.35(14) . 6_565 ?
O7 Na6 O20 95.87(15) 4_656 . ?
O7 Na6 O20 95.87(14) 7_656 . ?
O8 Na6 O20 89.03(14) . . ?
O8 Na6 O20 89.03(14) 6_565 . ?
O7 Na6 O18 83.64(12) 4_656 . ?
O7 Na6 O18 83.64(12) 7_656 . ?
O8 Na6 O18 91.46(12) . . ?
O8 Na6 O18 91.46(12) 6_565 . ?
O20 Na6 O18 179.37(18) . . ?
O7 Na6 Dy2 41.16(7) 4_656 3_556 ?
O7 Na6 Dy2 41.16(7) 7_656 3_556 ?
O8 Na6 Dy2 137.19(8) . 3_556 ?
O8 Na6 Dy2 137.19(8) 6_565 3_556 ?
O20 Na6 Dy2 111.24(16) . 3_556 ?
O18 Na6 Dy2 68.13(11) . 3_556 ?
O7 Na6 Dy1 139.39(7) 4_656 3 ?
O7 Na6 Dy1 139.39(7) 7_656 3 ?
O8 Na6 Dy1 42.02(7) . 3 ?
O8 Na6 Dy1 42.01(7) 6_565 3 ?
O20 Na6 Dy1 70.88(15) . 3 ?
O18 Na6 Dy1 109.76(12) . 3 ?
Dy2 Na6 Dy1 177.89(7) 3_556 3 ?
C41 O7 Na6 162.1(2) . 7_656 ?
C41 O7 Dy2 94.3(2) . 5_655 ?
Na6 O7 Dy2 101.51(10) 7_656 5_655 ?
C31 O8 Na6 134.2(2) . . ?
C31 O8 Dy1 96.0(2) . 3 ?
Na6 O8 Dy1 99.90(9) . 3 ?
N26 O9 Dy1 95.3(3) . . ?
N26 O9 Dy2 94.0(3) . . ?
Dy1 O9 Dy2 170.70(15) . . ?
N26 O9 Na5 105.45(7) . 5_655 ?
Dy1 O9 Na5 89.03(7) . 5_655 ?
Dy2 O9 Na5 88.49(7) . 5_655 ?
N26 O9 Na5 105.45(7) . 2_655 ?
Dy1 O9 Na5 89.03(7) . 2_655 ?
Dy2 O9 Na5 88.49(7) . 2_655 ?
Na5 O9 Na5 149.08(14) 5_655 2_655 ?
C31 O10 Na4 137.3(2) . 5_665 ?
C31 O10 Na5 121.9(2) . 7_655 ?
Na4 O10 Na5 98.50(11) 5_665 7_655 ?
C31 O10 Dy1 91.5(2) . 3 ?
Na4 O10 Dy1 100.18(9) 5_665 3 ?
Na5 O10 Dy1 93.25(9) 7_655 3 ?
C28 O11 Dy2 95.0(2) . 7 ?
C32 O12 Dy1 94.9(2) . . ?
C28 O13 Na4 138.5(2) . . ?
C28 O13 Na5 120.8(2) . 8_455 ?
Na4 O13 Na5 97.57(10) . 8_455 ?
C28 O13 Dy2 92.0(2) . 7 ?
Na4 O13 Dy2 101.44(10) . 7 ?
Na5 O13 Dy2 93.61(8) 8_455 7 ?
N26 O14 Dy2 93.7(3) . . ?
C41 O15 Na5 169.8(2) . . ?
C41 O15 Dy2 91.3(2) . 5_655 ?
Na5 O15 Dy2 98.87(9) . 5_655 ?
N26 O16 Dy1 94.0(3) . . ?
C32 O17 Na5 169.5(2) . 2_655 ?
C32 O17 Dy1 91.4(2) . . ?
Na5 O17 Dy1 99.02(9) 2_655 . ?
C72 O21 Zn3 159.4(5) . . ?
C29 N22 C36 106.9(3) . . ?
C29 N22 Zn3 124.9(2) . . ?
C36 N22 Zn3 124.2(2) . . ?
C40 N23 C45 107.2(3) . . ?
C40 N23 Zn3 126.1(2) . . ?
C45 N23 Zn3 126.4(2) . . ?
C49 N24 C34 107.1(3) . . ?
C49 N24 Zn3 126.2(2) . . ?
C34 N24 Zn3 126.5(2) . . ?
C30 N25 C47 106.7(3) . . ?
C30 N25 Zn3 125.8(2) . . ?
C47 N25 Zn3 125.9(2) . . ?
O14 N26 O16 126.8(5) . . ?
O14 N26 O9 117.6(4) . . ?
O16 N26 O9 115.6(4) . . ?
O14 N26 Dy1 174.2(4) . . ?
O16 N26 Dy1 59.0(3) . . ?
O9 N26 Dy1 56.6(2) . . ?
O14 N26 Dy2 59.9(2) . . ?
O16 N26 Dy2 173.3(4) . . ?
O9 N26 Dy2 57.7(2) . . ?
Dy1 N26 Dy2 114.35(17) . . ?
C55 C27 C71 118.4(4) . . ?
C55 C27 C31 121.8(3) . . ?
C71 C27 C31 119.7(3) . . ?
O11 C28 O13 120.8(3) . . ?
O11 C28 C48 120.0(3) . . ?
O13 C28 C48 119.1(3) . . ?
O11 C28 Dy2 59.13(17) . 7 ?
O13 C28 Dy2 61.73(18) . 7 ?
C48 C28 Dy2 177.4(2) . 7 ?
N22 C29 C42 125.4(3) . . ?
N22 C29 C57 109.1(3) . . ?
C42 C29 C57 125.5(3) . . ?
N25 C30 C46 125.1(3) . . ?
N25 C30 C38 109.5(3) . . ?
C46 C30 C38 125.3(3) . . ?
O8 C31 O10 120.8(3) . . ?
O8 C31 C27 119.8(3) . . ?
O10 C31 C27 119.4(3) . . ?
O8 C31 Dy1 58.35(17) . 3 ?
O10 C31 Dy1 62.59(17) . 3 ?
C27 C31 Dy1 175.5(2) . 3 ?
O17 C32 O12 120.5(3) . . ?
O17 C32 C33 120.2(3) . . ?
O12 C32 C33 119.2(3) . . ?
O17 C32 Dy1 62.11(18) . . ?
O12 C32 Dy1 58.57(18) . . ?
C33 C32 Dy1 172.8(3) . . ?
C54 C33 C61 119.2(3) . . ?
C54 C33 C32 119.6(3) . . ?
C61 C33 C32 121.1(3) . . ?
N24 C34 C39 125.4(3) . . ?
N24 C34 C69 109.3(3) . . ?
C39 C34 C69 125.1(3) . . ?
C36 C35 C40 125.2(3) . . ?
C36 C35 C51 116.5(3) . . ?
C40 C35 C51 118.3(3) . . ?
N22 C36 C35 124.9(3) . . ?
N22 C36 C52 109.1(3) . . ?
C35 C36 C52 126.0(3) . . ?
C75 C37 C70 118.0(4) . . ?
C75 C37 C46 120.9(4) . . ?
C70 C37 C46 121.1(3) . . ?
C50 C38 C30 106.8(3) . . ?
C47 C39 C34 125.5(3) . . ?
C47 C39 C44 116.7(3) . . ?
C34 C39 C44 117.7(3) . . ?
N23 C40 C35 125.5(3) . . ?
N23 C40 C60 109.3(3) . . ?
C35 C40 C60 125.2(3) . . ?
O15 C41 O7 121.0(3) . . ?
O15 C41 C43 119.7(3) . . ?
O7 C41 C43 119.3(3) . . ?
O15 C41 Dy2 62.36(18) . 5_655 ?
O7 C41 Dy2 59.03(17) . 5_655 ?
C43 C41 Dy2 171.7(2) . 5_655 ?
C29 C42 C49 125.5(3) . . ?
C29 C42 C53 117.0(3) . . ?
C49 C42 C53 117.4(3) . . ?
C56 C43 C62 119.0(3) . . ?
C56 C43 C41 120.1(3) . . ?
C62 C43 C41 120.8(3) . . ?
C74 C44 C63 117.4(4) . . ?
C74 C44 C39 119.6(3) . . ?
C63 C44 C39 123.0(3) . . ?
N23 C45 C46 125.7(3) . . ?
N23 C45 C58 108.9(3) . . ?
C46 C45 C58 125.3(3) . . ?
C45 C46 C30 125.3(3) . . ?
C45 C46 C37 117.6(3) . . ?
C30 C46 C37 117.0(3) . . ?
N25 C47 C39 124.7(3) . . ?
N25 C47 C50 109.6(3) . . ?
C39 C47 C50 125.5(3) . . ?
C67 C48 C73 118.6(4) . . ?
C67 C48 C28 121.9(3) . . ?
C73 C48 C28 119.5(3) . . ?
N24 C49 C42 125.5(3) . . ?
N24 C49 C65 108.9(3) . . ?
C42 C49 C65 125.6(3) . . ?
C38 C50 C47 107.3(3) . . ?
C59 C51 C68 117.6(3) . . ?
C59 C51 C35 120.8(3) . . ?
C68 C51 C35 121.5(4) . . ?
C57 C52 C36 107.8(3) . . ?
C66 C53 C64 118.3(3) . . ?
C66 C53 C42 122.2(3) . . ?
C64 C53 C42 119.5(3) . . ?
C33 C54 C59 120.3(4) . . ?
C27 C55 C63 120.5(4) . . ?
C64 C56 C43 121.0(4) . . ?
C52 C57 C29 107.0(3) . . ?
C60 C58 C45 107.1(3) . . ?
C51 C59 C54 121.4(4) . . ?
C58 C60 C40 107.4(3) . . ?
C68 C61 C33 120.4(4) . . ?
C66 C62 C43 119.9(3) . . ?
C44 C63 C55 121.4(4) . . ?
C56 C64 C53 120.5(4) . . ?
C69 C65 C49 107.5(3) . . ?
C62 C66 C53 121.1(4) . . ?
C48 C67 C70 121.0(4) . . ?
C61 C68 C51 120.8(4) . . ?
C65 C69 C34 107.1(3) . . ?
C37 C70 C67 120.4(4) . . ?
C27 C71 C74 120.6(4) . . ?
O21 C72 O21 149.4(9) . 2_655 ?
C48 C73 C75 119.9(4) . . ?
C44 C74 C71 121.5(4) . . ?
C37 C75 C73 121.9(4) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.001 584 170 ' '
2 -0.015 0.404 -0.001 3834 981 ' '
3 0.500 0.500 0.900 578 169 ' '
_platon_squeeze_details          
;
 disordered solvent (water + DMA) in the channel voids.
;

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.38
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.244
_refine_diff_density_min         -2.023
_refine_diff_density_rms         0.121

#==============================END===========================
_database_code_depnum_ccdc_archive 'CCDC 1014720'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt47sq

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H60 Dy2 N8 Na O20'
_chemical_formula_sum            'C96 H60 Dy2 N8 Na O20'
_chemical_formula_weight         1993.51

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0069(4)
_cell_length_b                   13.8090(4)
_cell_length_c                   17.8205(6)
_cell_angle_alpha                77.1170(15)
_cell_angle_beta                 75.4350(12)
_cell_angle_gamma                76.6300(12)
_cell_volume                     2739.29(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    12603
_cell_measurement_theta_min      1.78
_cell_measurement_theta_max      28.43

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             995
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4011
_exptl_absorpt_correction_T_max  0.6793
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. φ and ω scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49469
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         28.43
_reflns_number_total             13665
_reflns_number_gt                12603
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_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)+(0.0370P)²+0.2239P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13665
_refine_ls_number_parameters     575
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0584
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_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
Dy1 Dy 0.196440(5) 0.033058(5) 0.067582(4) 0.01027(3) Uani 1 1 d . . .
Na2 Na -0.5000 1.0000 0.0000 0.01383(17) Uani 1 2 d S . .
O3 O -0.34448(9) 0.86043(8) -0.03153(7) 0.0154(2) Uani 1 1 d . . .
H3A H -0.3222 0.8118 0.0010 0.023 Uiso 1 1 d R . .
H3B H -0.3342 0.8359 -0.0724 0.049(8) Uiso 1 1 d R . .
O4 O 0.13857(11) 0.11813(9) -0.83013(7) 0.0213(3) Uani 1 1 d . . .
O5 O 0.12131(10) 0.16419(9) -0.01633(7) 0.0208(3) Uani 1 1 d . . .
O6 O -0.82466(10) 0.93012(9) -0.02347(7) 0.0166(2) Uani 1 1 d . . .
O7 O -0.65724(10) 0.98037(10) -0.04345(7) 0.0223(3) Uani 1 1 d . . .
O8 O 0.00156(10) 0.01484(9) 0.10754(7) 0.0197(2) Uani 1 1 d . . .
H8A H -0.0335 -0.0049 0.1560 0.030 Uiso 1 1 d R . .
H8B H -0.0466 0.0290 0.0755 0.030 Uiso 1 1 d R . .
O9 O -0.62872(10) 0.94679(10) -0.88135(7) 0.0251(3) Uani 1 1 d . . .
O10 O 0.27171(11) 0.20867(11) -0.83413(8) 0.0297(3) Uani 1 1 d . . .
O11 O 0.24643(12) 0.26790(11) -0.07735(8) 0.0333(3) Uani 1 1 d . . .
O12 O -0.79198(11) 0.89200(10) -0.82341(8) 0.0273(3) Uani 1 1 d . . .
N13 N -0.32446(12) 0.54271(10) -0.31427(8) 0.0147(3) Uani 1 1 d . . .
H13 H -0.3199 0.5387 -0.3636 0.018 Uiso 0.50 1 calc PR . .
N14 N -0.16019(12) 0.42780(11) -0.42769(8) 0.0164(3) Uani 1 1 d . . .
H14 H -0.2224 0.4759 -0.4296 0.020 Uiso 0.50 1 calc PR . .
N15 N -0.46014(13) 0.64767(11) -0.43175(8) 0.0169(3) Uani 1 1 d . . .
H15 H -0.4058 0.5929 -0.4274 0.020 Uiso 0.50 1 calc PR . .
N16 N -0.30747(12) 0.51841(11) -0.54016(8) 0.0171(3) Uani 1 1 d . . .
H16 H -0.3083 0.5254 -0.4921 0.021 Uiso 0.50 1 calc PR . .
C17 C -0.72044(14) 0.93202(12) -0.06237(9) 0.0140(3) Uani 1 1 d . . .
C18 C -0.66943(14) 0.87564(12) -0.12842(9) 0.0147(3) Uani 1 1 d . . .
C19 C -0.68683(15) 0.89390(12) -0.82477(9) 0.0171(3) Uani 1 1 d . . .
C20 C -0.56078(14) 0.75337(12) -0.24247(9) 0.0153(3) Uani 1 1 d . . .
C21 C -0.29098(15) 0.51240(12) -0.18898(9) 0.0169(3) Uani 1 1 d . . .
H21 H -0.2566 0.4834 -0.1446 0.020 Uiso 1 1 calc R . .
C22 C -0.51270(15) 0.83141(14) -0.76232(10) 0.0230(4) Uani 1 1 d . . .
H22 H -0.4681 0.8684 -0.8065 0.028 Uiso 1 1 calc R . .
C23 C -0.25011(14) 0.48660(12) -0.26679(9) 0.0149(3) Uani 1 1 d . . .
C24 C -0.49924(15) 0.81442(14) -0.22190(10) 0.0195(3) Uani 1 1 d . . .
H24 H -0.4193 0.8141 -0.2468 0.023 Uiso 1 1 calc R . .
C25 C -0.10510(15) 0.30084(13) -0.16733(10) 0.0190(3) Uani 1 1 d . . .
H25 H -0.1786 0.2812 -0.1594 0.023 Uiso 1 1 calc R . .
C26 C -0.03301(15) 0.25700(12) -0.11440(10) 0.0191(3) Uani 1 1 d . . .
H26 H -0.0569 0.2070 -0.0708 0.023 Uiso 1 1 calc R . .
C27 C -0.73359(15) 0.81764(13) -0.15051(10) 0.0192(3) Uani 1 1 d . . .
H27 H -0.8140 0.8192 -0.1264 0.023 Uiso 1 1 calc R . .
C28 C 0.07426(15) 0.28583(12) -0.12472(10) 0.0176(3) Uani 1 1 d . . .
C29 C -0.38732(15) 0.58554(13) -0.19114(9) 0.0177(3) Uani 1 1 d . . .
H29 H -0.4335 0.6174 -0.1485 0.021 Uiso 1 1 calc R . .
C30 C -0.55219(14) 0.87514(13) -0.16614(10) 0.0184(3) Uani 1 1 d . . .
H30 H -0.5090 0.9166 -0.1534 0.022 Uiso 1 1 calc R . .
C31 C -0.38164(15) 0.57524(13) -0.58714(9) 0.0182(3) Uani 1 1 d . . .
C32 C -0.07117(15) 0.37326(12) -0.23195(10) 0.0173(3) Uani 1 1 d . . .
C33 C -0.63069(15) 0.83461(13) -0.75876(9) 0.0185(3) Uani 1 1 d . . .
C34 C -0.49454(14) 0.68273(12) -0.29745(9) 0.0157(3) Uani 1 1 d . . .
C35 C 0.17615(14) 0.18086(13) -0.80509(10) 0.0176(3) Uani 1 1 d . . .
C36 C 0.09708(15) 0.22570(13) -0.73687(10) 0.0173(3) Uani 1 1 d . . .
C37 C -0.01381(15) 0.20237(13) -0.70411(10) 0.0204(3) Uani 1 1 d . . .
H37 H -0.0387 0.1533 -0.7227 0.024 Uiso 1 1 calc R . .
C38 C -0.14660(14) 0.41919(12) -0.29047(9) 0.0160(3) Uani 1 1 d . . .
C39 C -0.40714(14) 0.60623(12) -0.27039(9) 0.0159(3) Uani 1 1 d . . .
C40 C -0.51631(15) 0.70246(13) -0.37353(10) 0.0172(3) Uani 1 1 d . . .
C41 C 0.13450(15) 0.29463(13) -0.70678(10) 0.0190(3) Uani 1 1 d . . .
H41 H 0.2109 0.3094 -0.7274 0.023 Uiso 1 1 calc R . .
C42 C -0.08812(16) 0.25028(14) -0.64455(11) 0.0237(4) Uani 1 1 d . . .
H42 H -0.1636 0.2338 -0.6226 0.028 Uiso 1 1 calc R . .
C43 C 0.06036(15) 0.34159(13) -0.64681(10) 0.0189(3) Uani 1 1 d . . .
H43 H 0.0871 0.3875 -0.6260 0.023 Uiso 1 1 calc R . .
C44 C 0.10831(16) 0.35884(14) -0.18923(11) 0.0262(4) Uani 1 1 d . . .
H44 H 0.1812 0.3793 -0.1968 0.031 Uiso 1 1 calc R . .
C45 C -0.05270(15) 0.32253(13) -0.61665(9) 0.0176(3) Uani 1 1 d . . .
C46 C -0.46777(15) 0.65962(13) -0.57039(9) 0.0182(3) Uani 1 1 d . . .
C47 C -0.67957(15) 0.75793(13) -0.20765(10) 0.0193(3) Uani 1 1 d . . .
H47 H -0.7238 0.7199 -0.2232 0.023 Uiso 1 1 calc R . .
C48 C -0.46013(15) 0.77424(15) -0.70146(10) 0.0237(4) Uani 1 1 d . . .
H48 H -0.3794 0.7716 -0.7045 0.028 Uiso 1 1 calc R . .
C49 C -0.10068(15) 0.37503(13) -0.48677(10) 0.0189(3) Uani 1 1 d . . .
C50 C -0.50293(15) 0.69272(13) -0.49793(9) 0.0179(3) Uani 1 1 d . . .
C51 C 0.03645(16) 0.40154(15) -0.24225(11) 0.0261(4) Uani 1 1 d . . .
H51 H 0.0608 0.4508 -0.2863 0.031 Uiso 1 1 calc R . .
C52 C -0.13379(15) 0.38312(13) -0.55839(10) 0.0176(3) Uani 1 1 d . . .
C53 C -0.59813(15) 0.78655(14) -0.40417(10) 0.0207(3) Uani 1 1 d . . .
H53 H -0.6486 0.8367 -0.3763 0.025 Uiso 1 1 calc R . .
C54 C 0.15426(15) 0.23685(13) -0.06946(10) 0.0197(3) Uani 1 1 d . . .
C55 C -0.23154(15) 0.44857(13) -0.58157(9) 0.0176(3) Uani 1 1 d . . .
C56 C -0.69517(16) 0.78097(15) -0.69352(11) 0.0257(4) Uani 1 1 d . . .
H56 H -0.7756 0.7828 -0.6908 0.031 Uiso 1 1 calc R . .
C57 C -0.10608(15) 0.39269(13) -0.36510(10) 0.0184(3) Uani 1 1 d . . .
C58 C -0.26383(16) 0.45913(14) -0.65645(10) 0.0220(4) Uani 1 1 d . . .
H58 H -0.2270 0.4189 -0.6959 0.026 Uiso 1 1 calc R . .
C59 C -0.52525(15) 0.72059(14) -0.63577(9) 0.0193(3) Uani 1 1 d . . .
C60 C -0.35524(16) 0.53608(14) -0.65988(10) 0.0225(4) Uani 1 1 d . . .
H60 H -0.3951 0.5603 -0.7021 0.027 Uiso 1 1 calc R . .
C61 C -0.58965(15) 0.78063(14) -0.48039(10) 0.0217(4) Uani 1 1 d . . .
H61 H -0.6330 0.8262 -0.5158 0.026 Uiso 1 1 calc R . .
C62 C -0.00377(17) 0.30435(15) -0.46044(11) 0.0273(4) Uani 1 1 d . . .
H62 H 0.0521 0.2582 -0.4897 0.033 Uiso 1 1 calc R . .
C63 C -0.64333(16) 0.72499(15) -0.63248(11) 0.0262(4) Uani 1 1 d . . .
H63 H -0.6887 0.6892 -0.5879 0.031 Uiso 1 1 calc R . .
C64 C -0.00680(17) 0.31554(15) -0.38640(11) 0.0290(4) Uani 1 1 d . . .
H64 H 0.0469 0.2791 -0.3543 0.035 Uiso 1 1 calc R . .


_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
Dy1 O5 2.2460(11) . ?
Dy1 O4 2.2641(11) 1_556 ?
Dy1 O8 2.3238(11) . ?
Dy1 O7 2.4152(12) 1_645 ?
Dy1 O12 2.4313(12) 1_646 ?
Dy1 O3 2.4390(11) 2_565 ?
Dy1 O9 2.4445(12) 1_646 ?
Dy1 O6 2.4737(11) 1_645 ?
Dy1 C19 2.7929(16) 1_646 ?
Dy1 C17 2.8178(16) 1_645 ?
Dy1 Na2 3.49450(13) 1_645 ?
Na2 O7 2.3028(11) . ?
Na2 O7 2.3028(11) 2_475 ?
Na2 O9 2.3639(12) 1_556 ?
Na2 O9 2.3640(12) 2_474 ?
Na2 O3 2.4100(11) . ?
Na2 O3 2.4100(11) 2_475 ?
Na2 Dy1 3.49447(13) 1_465 ?
Na2 Dy1 3.49448(13) 2_565 ?
O3 Dy1 2.4390(11) 2_565 ?
O4 C35 1.268(2) . ?
O4 Dy1 2.2640(11) 1_554 ?
O5 C54 1.277(2) . ?
O6 C17 1.2720(19) . ?
O6 Dy1 2.4737(11) 1_465 ?
O7 C17 1.264(2) . ?
O7 Dy1 2.4152(12) 1_465 ?
O9 C19 1.261(2) . ?
O9 Na2 2.3639(12) 1_554 ?
O9 Dy1 2.4444(12) 1_464 ?
O10 C35 1.244(2) . ?
O11 C54 1.242(2) . ?
O12 C19 1.263(2) . ?
O12 Dy1 2.4312(12) 1_464 ?
N13 C23 1.371(2) . ?
N13 C39 1.371(2) . ?
N14 C49 1.369(2) . ?
N14 C57 1.371(2) . ?
N15 C40 1.366(2) . ?
N15 C50 1.368(2) . ?
N16 C31 1.367(2) . ?
N16 C55 1.371(2) . ?
C17 C18 1.481(2) . ?
C17 Dy1 2.8178(16) 1_465 ?
C18 C30 1.398(2) . ?
C18 C27 1.403(2) . ?
C19 C33 1.491(2) . ?
C19 Dy1 2.7928(16) 1_464 ?
C20 C47 1.398(2) . ?
C20 C24 1.398(2) . ?
C20 C34 1.490(2) . ?
C21 C29 1.351(2) . ?
C21 C23 1.445(2) . ?
C22 C48 1.389(2) . ?
C22 C33 1.393(2) . ?
C23 C38 1.402(2) . ?
C24 C30 1.379(2) . ?
C25 C26 1.385(2) . ?
C25 C32 1.390(2) . ?
C26 C28 1.392(2) . ?
C27 C47 1.390(2) . ?
C28 C44 1.394(2) . ?
C28 C54 1.493(2) . ?
C29 C39 1.446(2) . ?
C31 C46 1.400(2) . ?
C31 C60 1.449(2) . ?
C32 C51 1.392(2) . ?
C32 C38 1.492(2) . ?
C33 C56 1.389(2) . ?
C34 C40 1.400(2) . ?
C34 C39 1.402(2) . ?
C35 C36 1.499(2) . ?
C36 C41 1.394(2) . ?
C36 C37 1.393(2) . ?
C37 C42 1.387(2) . ?
C38 C57 1.396(2) . ?
C40 C53 1.439(2) . ?
C41 C43 1.385(2) . ?
C42 C45 1.395(2) . ?
C43 C45 1.391(2) . ?
C44 C51 1.382(2) . ?
C45 C52 1.493(2) . ?
C46 C50 1.398(2) . ?
C46 C59 1.497(2) . ?
C48 C59 1.397(2) . ?
C49 C52 1.404(2) . ?
C49 C62 1.439(2) . ?
C50 C61 1.441(2) . ?
C52 C55 1.397(2) . ?
C53 C61 1.356(2) . ?
C55 C58 1.449(2) . ?
C56 C63 1.382(2) . ?
C57 C64 1.437(2) . ?
C58 C60 1.343(3) . ?
C59 C63 1.392(2) . ?
C62 C64 1.353(3) . ?

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 Dy1 O4 93.56(5) . 1_556 ?
O5 Dy1 O8 81.70(4) . . ?
O4 Dy1 O8 79.93(4) 1_556 . ?
O5 Dy1 O7 88.14(5) . 1_645 ?
O4 Dy1 O7 150.32(4) 1_556 1_645 ?
O8 Dy1 O7 129.51(4) . 1_645 ?
O5 Dy1 O12 160.66(5) . 1_646 ?
O4 Dy1 O12 80.08(5) 1_556 1_646 ?
O8 Dy1 O12 79.21(4) . 1_646 ?
O7 Dy1 O12 106.46(5) 1_645 1_646 ?
O5 Dy1 O3 77.50(4) . 2_565 ?
O4 Dy1 O3 80.36(4) 1_556 2_565 ?
O8 Dy1 O3 150.23(4) . 2_565 ?
O7 Dy1 O3 71.09(4) 1_645 2_565 ?
O12 Dy1 O3 118.80(4) 1_646 2_565 ?
O5 Dy1 O9 145.33(4) . 1_646 ?
O4 Dy1 O9 88.76(4) 1_556 1_646 ?
O8 Dy1 O9 132.56(4) . 1_646 ?
O7 Dy1 O9 73.75(4) 1_645 1_646 ?
O12 Dy1 O9 53.41(4) 1_646 1_646 ?
O3 Dy1 O9 68.80(4) 2_565 1_646 ?
O5 Dy1 O6 84.28(4) . 1_645 ?
O4 Dy1 O6 156.27(4) 1_556 1_645 ?
O8 Dy1 O6 76.38(4) . 1_645 ?
O7 Dy1 O6 53.38(4) 1_645 1_645 ?
O12 Dy1 O6 94.21(4) 1_646 1_645 ?
O3 Dy1 O6 121.83(4) 2_565 1_645 ?
O9 Dy1 O6 106.40(4) 1_646 1_645 ?
O5 Dy1 C19 169.72(5) . 1_646 ?
O4 Dy1 C19 81.05(5) 1_556 1_646 ?
O8 Dy1 C19 105.76(4) . 1_646 ?
O7 Dy1 C19 92.25(5) 1_645 1_646 ?
O12 Dy1 C19 26.85(4) 1_646 1_646 ?
O3 Dy1 C19 92.90(4) 2_565 1_646 ?
O9 Dy1 C19 26.82(4) 1_646 1_646 ?
O6 Dy1 C19 104.17(4) 1_645 1_646 ?
O5 Dy1 C17 86.14(5) . 1_645 ?
O4 Dy1 C17 176.85(4) 1_556 1_645 ?
O8 Dy1 C17 103.12(4) . 1_645 ?
O7 Dy1 C17 26.56(4) 1_645 1_645 ?
O12 Dy1 C17 101.18(5) 1_646 1_645 ?
O3 Dy1 C17 96.52(4) 2_565 1_645 ?
O9 Dy1 C17 89.71(4) 1_646 1_645 ?
O6 Dy1 C17 26.82(4) 1_645 1_645 ?
C19 Dy1 C17 98.75(5) 1_646 1_645 ?
O5 Dy1 Na2 105.70(3) . 1_645 ?
O4 Dy1 Na2 110.89(3) 1_556 1_645 ?
O8 Dy1 Na2 166.02(3) . 1_645 ?
O7 Dy1 Na2 40.99(3) 1_645 1_645 ?
O12 Dy1 Na2 93.62(3) 1_646 1_645 ?
O3 Dy1 Na2 43.56(3) 2_565 1_645 ?
O9 Dy1 Na2 42.49(3) 1_646 1_645 ?
O6 Dy1 Na2 92.36(3) 1_645 1_645 ?
C19 Dy1 Na2 68.59(3) 1_646 1_645 ?
C17 Dy1 Na2 66.24(3) 1_645 1_645 ?
O7 Na2 O7 180.0 . 2_475 ?
O7 Na2 O9 77.34(4) . 1_556 ?
O7 Na2 O9 102.66(4) 2_475 1_556 ?
O7 Na2 O9 102.66(4) . 2_474 ?
O7 Na2 O9 77.34(4) 2_475 2_474 ?
O9 Na2 O9 180.00(6) 1_556 2_474 ?
O7 Na2 O3 106.47(4) . . ?
O7 Na2 O3 73.53(4) 2_475 . ?
O9 Na2 O3 109.40(4) 1_556 . ?
O9 Na2 O3 70.61(4) 2_474 . ?
O7 Na2 O3 73.53(4) . 2_475 ?
O7 Na2 O3 106.47(4) 2_475 2_475 ?
O9 Na2 O3 70.60(4) 1_556 2_475 ?
O9 Na2 O3 109.40(4) 2_474 2_475 ?
O3 Na2 O3 180.0 . 2_475 ?
O7 Na2 Dy1 43.47(3) . 1_465 ?
O7 Na2 Dy1 136.53(3) 2_475 1_465 ?
O9 Na2 Dy1 44.30(3) 1_556 1_465 ?
O9 Na2 Dy1 135.70(3) 2_474 1_465 ?
O3 Na2 Dy1 135.78(3) . 1_465 ?
O3 Na2 Dy1 44.22(3) 2_475 1_465 ?
O7 Na2 Dy1 136.54(3) . 2_565 ?
O7 Na2 Dy1 43.46(3) 2_475 2_565 ?
O9 Na2 Dy1 135.70(3) 1_556 2_565 ?
O9 Na2 Dy1 44.30(3) 2_474 2_565 ?
O3 Na2 Dy1 44.22(3) . 2_565 ?
O3 Na2 Dy1 135.78(3) 2_475 2_565 ?
Dy1 Na2 Dy1 180.0 1_465 2_565 ?
Na2 O3 Dy1 92.22(4) . 2_565 ?
C35 O4 Dy1 136.98(11) . 1_554 ?
C54 O5 Dy1 139.50(11) . . ?
C17 O6 Dy1 91.85(9) . 1_465 ?
C17 O7 Na2 155.87(12) . . ?
C17 O7 Dy1 94.77(10) . 1_465 ?
Na2 O7 Dy1 95.55(4) . 1_465 ?
C19 O9 Na2 163.21(12) . 1_554 ?
C19 O9 Dy1 92.18(10) . 1_464 ?
Na2 O9 Dy1 93.21(4) 1_554 1_464 ?
C19 O12 Dy1 92.75(10) . 1_464 ?
C23 N13 C39 107.03(13) . . ?
C49 N14 C57 108.18(14) . . ?
C40 N15 C50 108.16(14) . . ?
C31 N16 C55 107.47(14) . . ?
O7 C17 O6 119.99(15) . . ?
O7 C17 C18 118.75(15) . . ?
O6 C17 C18 121.24(14) . . ?
O7 C17 Dy1 58.67(9) . 1_465 ?
O6 C17 Dy1 61.33(8) . 1_465 ?
C18 C17 Dy1 176.03(11) . 1_465 ?
C30 C18 C27 119.38(15) . . ?
C30 C18 C17 118.96(14) . . ?
C27 C18 C17 121.53(15) . . ?
O9 C19 O12 120.48(15) . . ?
O9 C19 C33 119.33(15) . . ?
O12 C19 C33 120.19(15) . . ?
O9 C19 Dy1 61.00(8) . 1_464 ?
O12 C19 Dy1 60.40(8) . 1_464 ?
C33 C19 Dy1 169.62(12) . 1_464 ?
C47 C20 C24 118.60(15) . . ?
C47 C20 C34 123.31(15) . . ?
C24 C20 C34 118.02(15) . . ?
C29 C21 C23 107.13(14) . . ?
C48 C22 C33 120.16(16) . . ?
N13 C23 C38 125.84(14) . . ?
N13 C23 C21 109.31(14) . . ?
C38 C23 C21 124.75(14) . . ?
C30 C24 C20 121.32(15) . . ?
C26 C25 C32 120.75(16) . . ?
C25 C26 C28 120.34(15) . . ?
C47 C27 C18 120.01(16) . . ?
C26 C28 C44 119.07(15) . . ?
C26 C28 C54 120.80(15) . . ?
C44 C28 C54 120.09(15) . . ?
C21 C29 C39 107.24(14) . . ?
C24 C30 C18 119.95(15) . . ?
N16 C31 C46 126.70(15) . . ?
N16 C31 C60 109.01(15) . . ?
C46 C31 C60 124.27(15) . . ?
C25 C32 C51 118.73(15) . . ?
C25 C32 C38 121.29(15) . . ?
C51 C32 C38 119.97(15) . . ?
C56 C33 C22 119.31(15) . . ?
C56 C33 C19 120.32(15) . . ?
C22 C33 C19 120.37(15) . . ?
C40 C34 C39 125.04(15) . . ?
C40 C34 C20 118.40(14) . . ?
C39 C34 C20 116.31(14) . . ?
O10 C35 O4 124.68(15) . . ?
O10 C35 C36 118.64(15) . . ?
O4 C35 C36 116.67(15) . . ?
C41 C36 C37 119.18(15) . . ?
C41 C36 C35 118.97(15) . . ?
C37 C36 C35 121.83(15) . . ?
C42 C37 C36 120.49(16) . . ?
C57 C38 C23 125.63(15) . . ?
C57 C38 C32 116.67(15) . . ?
C23 C38 C32 117.69(14) . . ?
N13 C39 C34 126.39(14) . . ?
N13 C39 C29 109.21(14) . . ?
C34 C39 C29 124.35(15) . . ?
N15 C40 C34 125.71(15) . . ?
N15 C40 C53 108.82(14) . . ?
C34 C40 C53 125.42(15) . . ?
C43 C41 C36 120.06(16) . . ?
C37 C42 C45 120.39(16) . . ?
C45 C43 C41 121.00(15) . . ?
C51 C44 C28 120.28(16) . . ?
C43 C45 C42 118.74(15) . . ?
C43 C45 C52 119.07(15) . . ?
C42 C45 C52 122.13(15) . . ?
C50 C46 C31 125.28(15) . . ?
C50 C46 C59 117.31(15) . . ?
C31 C46 C59 117.40(14) . . ?
C27 C47 C20 120.61(15) . . ?
C22 C48 C59 120.43(16) . . ?
N14 C49 C52 125.69(16) . . ?
N14 C49 C62 108.35(15) . . ?
C52 C49 C62 125.79(16) . . ?
N15 C50 C46 125.82(15) . . ?
N15 C50 C61 108.33(14) . . ?
C46 C50 C61 125.84(15) . . ?
C44 C51 C32 120.83(16) . . ?
C55 C52 C49 125.25(15) . . ?
C55 C52 C45 117.60(14) . . ?
C49 C52 C45 116.97(15) . . ?
C61 C53 C40 107.07(15) . . ?
O11 C54 O5 124.47(16) . . ?
O11 C54 C28 119.46(15) . . ?
O5 C54 C28 116.06(15) . . ?
N16 C55 C52 125.85(15) . . ?
N16 C55 C58 108.70(14) . . ?
C52 C55 C58 125.29(15) . . ?
C63 C56 C33 120.60(16) . . ?
N14 C57 C38 126.10(15) . . ?
N14 C57 C64 108.42(15) . . ?
C38 C57 C64 125.18(15) . . ?
C60 C58 C55 107.53(15) . . ?
C63 C59 C48 118.96(15) . . ?
C63 C59 C46 121.09(15) . . ?
C48 C59 C46 119.95(15) . . ?
C58 C60 C31 107.19(15) . . ?
C53 C61 C50 107.61(15) . . ?
C64 C62 C49 107.53(16) . . ?
C56 C63 C59 120.53(16) . . ?
C62 C64 C57 107.51(16) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.037 0.000 0.500 538 133 ' '
2 -0.062 0.500 0.000 442 126 ' '
_platon_squeeze_details          
;

 Disordered DMA solvent located within the interstitial voids.
;

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        28.43
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 1021602'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_gt45sq

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N3 Na4 O10'
_chemical_formula_sum            'C32 H30 N3 Na4 O10'
_chemical_formula_weight         708.55

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'
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           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.4059(2)
_cell_length_b                   16.3502(5)
_cell_length_c                   17.8196(5)
_cell_angle_alpha                98.1090(10)
_cell_angle_beta                 94.0560(10)
_cell_angle_gamma                95.6510(10)
_cell_volume                     1831.95(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    4769
_cell_measurement_theta_min      1.16
_cell_measurement_theta_max      25.44

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             734
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9671
_exptl_absorpt_correction_T_max  0.9866
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. ω and φ scans'
_diffrn_detector_area_resol_mean 1.75
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24801
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.16
_diffrn_reflns_theta_max         25.44
_reflns_number_total             6709
_reflns_number_gt                4769
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2, Bruker-AXS'
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 

 The terminal Na-coordinated DMA residues are partly disordered.
 One of them was refined with restrained geometry.

 In addition, the crystal contains severely disordered DMA crystallization
 solvent residing in the intralattice channel voids, which could not be
 reliably modeled by discrete atoms. Its contribution was subtracted from
 the diffraction pattern by the Squeeze technique, using the PLATON software
 (Spek, 2009).
;

_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)+(0.0897P)²+2.2119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6709
_refine_ls_number_parameters     432
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1915
_refine_ls_wR_factor_gt          0.1793
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.014
_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
Na1 Na 0.57075(19) 0.39640(8) 0.51929(7) 0.0160(3) Uani 1 1 d . . .
Na2 Na 0.87431(19) 0.50879(8) 0.41351(7) 0.0176(3) Uani 1 1 d . . .
Na3 Na 0.8496(2) 0.41205(9) -0.27141(8) 0.0239(4) Uani 1 1 d . . .
Na4 Na 1.2734(2) 0.31100(10) 0.64102(8) 0.0274(4) Uani 1 1 d . . .
O5 O 0.2193(4) 0.51455(14) 0.37420(13) 0.0176(5) Uani 1 1 d . . .
O6 O 0.5123(3) 0.46547(15) 0.41404(13) 0.0181(5) Uani 1 1 d . . .
O7 O 0.9061(4) 0.39056(15) 0.46913(14) 0.0229(6) Uani 1 1 d . . .
O8 O 1.2011(4) 0.35814(16) 0.52434(14) 0.0232(6) Uani 1 1 d . . .
O9 O 0.1956(4) 0.45561(16) -0.29239(14) 0.0250(6) Uani 1 1 d . . .
O10 O 0.4910(4) 0.40385(17) -0.26124(16) 0.0301(6) Uani 1 1 d . . .
O11 O 0.9202(4) 0.27910(17) -0.32035(17) 0.0327(7) Uani 1 1 d . . .
O12 O 0.9231(5) 0.4205(2) -0.14234(17) 0.0516(9) Uani 1 1 d . . .
O13 O 1.1485(5) 0.1894(2) -0.3027(2) 0.0490(9) Uani 1 1 d . . .
O14 O 0.5782(4) 0.27503(16) 0.57860(15) 0.0293(6) Uani 1 1 d . . .
H14A H 0.6921 0.2798 0.6121 0.044 Uiso 1 1 d R . .
H14B H 0.5456 0.2271 0.5466 0.044 Uiso 1 1 d R . .
N15 N 0.1333(2) -0.04631(8) -0.09859(8) 0.0218(7) Uani 1 1 d . . .
H15 H 0.0757 -0.0263 -0.0573 0.026 Uiso 1 1 d R . .
N16 N 0.2346(2) 0.09506(8) 0.02316(8) 0.0221(7) Uani 1 1 d R . .
C17 C 0.3437(2) 0.45905(8) 0.37258(8) 0.0143(7) Uani 1 1 d R . .
C18 C 0.2869(2) 0.38064(8) 0.31548(8) 0.0164(7) Uani 1 1 d R . .
C19 C 1.0360(2) 0.34001(8) 0.47952(8) 0.0181(8) Uani 1 1 d R . .
C20 C 0.4249(2) 0.32026(8) 0.30693(8) 0.0214(8) Uani 1 1 d R . .
H20 H 0.5534 0.3270 0.3383 0.026 Uiso 1 1 calc R . .
C21 C 0.0469(6) 0.2984(2) 0.2168(2) 0.0218(8) Uani 1 1 d . . .
H21 H -0.0841 0.2907 0.1868 0.026 Uiso 1 1 calc R . .
C22 C 0.1870(5) 0.2389(2) 0.2064(2) 0.0205(8) Uani 1 1 d . . .
C23 C 0.2982(6) -0.0048(2) -0.1281(2) 0.0221(8) Uani 1 1 d . . .
C24 C 0.0968(6) 0.3693(2) 0.2709(2) 0.0206(8) Uani 1 1 d . . .
H24 H 0.0005 0.4098 0.2773 0.025 Uiso 1 1 calc R . .
C25 C 0.3640(5) 0.4569(2) -0.2511(2) 0.0219(8) Uani 1 1 d . . .
C26 C 0.3895(6) 0.1137(2) -0.0230(2) 0.0235(8) Uani 1 1 d . . .
C27 C 0.4181(6) 0.0687(2) -0.0937(2) 0.0237(8) Uani 1 1 d . . .
C28 C 0.0458(6) -0.1123(2) -0.1516(2) 0.0221(8) Uani 1 1 d . . .
C29 C 0.1338(6) 0.1657(2) 0.1451(2) 0.0210(8) Uani 1 1 d . . .
C30 C 0.3756(6) 0.2503(2) 0.2528(2) 0.0255(9) Uani 1 1 d . . .
H30 H 0.4713 0.2094 0.2472 0.031 Uiso 1 1 calc R . .
C31 C 0.1650(6) -0.1137(2) -0.2160(2) 0.0266(9) Uani 1 1 d . . .
H31 H 0.1415 -0.1534 -0.2610 0.032 Uiso 1 1 calc R . .
C32 C 0.2643(6) 0.1572(2) 0.0847(2) 0.0235(8) Uani 1 1 d . . .
C33 C 0.5724(6) 0.1077(2) -0.1415(2) 0.0253(9) Uani 1 1 d . . .
C34 C 0.3191(6) -0.0482(2) -0.2023(2) 0.0279(9) Uani 1 1 d . . .
H34 H 0.4213 -0.0341 -0.2358 0.034 Uiso 1 1 calc R . .
C35 C 0.9803(6) 0.2187(2) -0.2907(2) 0.0296(9) Uani 1 1 d . . .
C36 C 0.8401(6) 0.1799(2) -0.2377(2) 0.0281(9) Uani 1 1 d . . .
C37 C 0.5211(6) 0.1878(2) 0.0109(2) 0.0308(9) Uani 1 1 d . . .
H37 H 0.6403 0.2127 -0.0096 0.037 Uiso 1 1 calc R . .
C40 C 0.4444(6) 0.2153(2) 0.0768(2) 0.0317(10) Uani 1 1 d . . .
H40 H 0.4980 0.2635 0.1116 0.038 Uiso 1 1 calc R . .
C41 C 0.9947(7) 0.2535(3) 0.4358(3) 0.0374(10) Uani 1 1 d . . .
H41A H 0.8442 0.2344 0.4333 0.056 Uiso 1 1 calc R . .
H41B H 1.0753 0.2159 0.4615 0.056 Uiso 1 1 calc R . .
H41C H 1.0379 0.2537 0.3841 0.056 Uiso 1 1 calc R . .
C42 C 0.4114(7) 0.5267(3) -0.1846(2) 0.0357(10) Uani 1 1 d . . .
H42A H 0.3229 0.5155 -0.1438 0.054 Uiso 1 1 calc R . .
H42B H 0.3820 0.5793 -0.2013 0.054 Uiso 1 1 calc R . .
H42C H 0.5601 0.5304 -0.1658 0.054 Uiso 1 1 calc R . .
C43 C 0.7637(7) 0.0778(3) -0.1554(3) 0.0405(11) Uani 1 1 d . . .
H43 H 0.8042 0.0323 -0.1322 0.049 Uiso 1 1 calc R . .
C44 C 0.8959(7) 0.1137(3) -0.2029(3) 0.0427(12) Uani 1 1 d . . .
H44 H 1.0264 0.0926 -0.2117 0.051 Uiso 1 1 calc R . .
C45 C 0.6516(7) 0.2113(3) -0.2221(3) 0.0383(11) Uani 1 1 d . . .
H45 H 0.6130 0.2582 -0.2436 0.046 Uiso 1 1 calc R . .
C46 C 0.5202(7) 0.1745(3) -0.1753(3) 0.0377(11) Uani 1 1 d . . .
H46 H 0.3901 0.1959 -0.1662 0.045 Uiso 1 1 calc R . .
N47 N 0.8912(9) 0.3817(3) -0.0259(3) 0.074(3) Uani 1 1 d D . .
C48 C 0.7187(9) 0.4332(4) -0.0234(4) 0.0676(17) Uani 1 1 d D . .
H48A H 0.7727 0.4905 -0.0021 0.101 Uiso 1 1 calc R . .
H48B H 0.6138 0.4120 0.0086 0.101 Uiso 1 1 calc R . .
H48C H 0.6531 0.4318 -0.0750 0.101 Uiso 1 1 calc R . .
C49 C 1.1688(9) 0.3248(4) -0.0986(4) 0.0703(18) Uani 1 1 d D . .
H49A H 1.2208 0.3198 -0.1493 0.105 Uiso 1 1 calc R . .
H49B H 1.1170 0.2696 -0.0879 0.105 Uiso 1 1 calc R . .
H49C H 1.2835 0.3496 -0.0604 0.105 Uiso 1 1 calc R . .
C50 C 0.9901(10) 0.3474(4) 0.0367(3) 0.078(2) Uani 1 1 d D . .
H50A H 1.0504 0.2968 0.0168 0.117 Uiso 1 1 calc R . .
H50B H 0.8846 0.3341 0.0717 0.117 Uiso 1 1 calc R . .
H50C H 1.1020 0.3883 0.0639 0.117 Uiso 1 1 calc R . .
C51 C 0.9922(9) 0.3793(4) -0.0958(3) 0.076(3) Uani 1 1 d D . .


_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
Na1 O6 2.348(3) . ?
Na1 O14 2.379(3) . ?
Na1 O7 2.390(3) . ?
Na1 O8 2.400(3) 1_455 ?
Na1 O5 2.450(3) 2_666 ?
Na1 O6 2.523(3) 2_666 ?
Na1 C17 2.8123(18) 2_666 ?
Na1 Na4 3.3466(19) 1_455 ?
Na1 Na2 3.3917(18) . ?
Na1 Na2 3.5769(17) 2_666 ?
Na1 Na1 3.734(3) 2_666 ?
Na1 Na2 3.7767(18) 2_766 ?
Na2 O7 2.313(3) . ?
Na2 O9 2.338(3) 2_665 ?
Na2 O6 2.358(3) . ?
Na2 O5 2.363(3) 1_655 ?
Na2 O8 2.407(3) 2_766 ?
Na2 O7 2.686(3) 2_766 ?
Na2 C19 2.8828(19) 2_766 ?
Na2 Na4 3.427(2) 2_766 ?
Na2 Na2 3.438(3) 2_766 ?
Na2 Na3 3.5104(18) 2_765 ?
Na2 Na1 3.5769(17) 2_666 ?
Na3 O12 2.297(3) . ?
Na3 O10 2.309(3) . ?
Na3 O11 2.325(3) . ?
Na3 O9 2.333(3) 1_655 ?
Na3 O5 2.366(3) 2_665 ?
Na3 Na2 3.5104(18) 2_765 ?
Na3 Na4 3.646(2) 1_554 ?
Na3 Na1 3.9830(19) 1_554 ?
Na3 Na4 4.006(2) 1_454 ?
Na4 O8 2.349(3) . ?
Na4 O14 2.397(3) 1_655 ?
Na4 O10 2.403(3) 1_656 ?
Na4 O13 2.440(3) 1_556 ?
Na4 O11 2.440(3) 1_556 ?
Na4 O9 2.602(3) 1_656 ?
Na4 C35 2.750(4) 1_556 ?
Na4 C25 2.828(4) 1_656 ?
Na4 Na1 3.3466(19) 1_655 ?
Na4 Na2 3.427(2) 2_766 ?
Na4 Na3 3.646(2) 1_556 ?
Na4 Na3 4.006(2) 1_656 ?
O5 C17 1.264(3) . ?
O5 Na2 2.363(3) 1_455 ?
O5 Na3 2.366(3) 2_665 ?
O5 Na1 2.450(3) 2_666 ?
O6 C17 1.251(3) . ?
O6 Na1 2.523(3) 2_666 ?
O7 C19 1.252(3) . ?
O7 Na2 2.687(3) 2_766 ?
O8 C19 1.263(3) . ?
O8 Na1 2.400(3) 1_655 ?
O8 Na2 2.408(3) 2_766 ?
O9 C25 1.259(4) . ?
O9 Na3 2.333(3) 1_455 ?
O9 Na2 2.338(3) 2_665 ?
O9 Na4 2.602(3) 1_454 ?
O10 C25 1.249(4) . ?
O10 Na4 2.403(3) 1_454 ?
O11 C35 1.264(5) . ?
O11 Na4 2.440(3) 1_554 ?
O12 C51 1.225(6) . ?
O13 C35 1.241(5) . ?
O13 Na4 2.440(3) 1_554 ?
O14 Na4 2.397(3) 1_455 ?
N15 C28 1.375(4) . ?
N15 C23 1.375(4) . ?
N16 C26 1.372(4) . ?
N16 C32 1.375(4) . ?
C17 C18 1.5162 . ?
C17 Na1 2.8123(18) 2_666 ?
C18 C20 1.3883 . ?
C18 C24 1.388(4) . ?
C19 C41 1.505(4) . ?
C19 Na2 2.8828(19) 2_766 ?
C20 C30 1.383(4) . ?
C21 C24 1.394(5) . ?
C21 C22 1.390(5) . ?
C22 C30 1.397(5) . ?
C22 C29 1.496(5) . ?
C23 C27 1.398(5) . ?
C23 C34 1.431(5) . ?
C25 C42 1.515(6) . ?
C25 Na4 2.828(4) 1_454 ?
C26 C27 1.399(5) . ?
C26 C37 1.437(5) . ?
C27 C33 1.503(5) . ?
C28 C29 1.397(5) 2 ?
C28 C31 1.421(5) . ?
C29 C28 1.397(5) 2 ?
C29 C32 1.409(5) . ?
C31 C34 1.365(5) . ?
C32 C40 1.448(5) . ?
C33 C46 1.377(6) . ?
C33 C43 1.389(5) . ?
C35 C36 1.509(6) . ?
C35 Na4 2.750(4) 1_554 ?
C36 C44 1.386(6) . ?
C36 C45 1.388(5) . ?
C37 C40 1.341(6) . ?
C43 C44 1.386(6) . ?
C45 C46 1.380(6) . ?
N47 C51 1.442(2) . ?
N47 C50 1.451(2) . ?
N47 C48 1.453(2) . ?
C49 C51 1.507(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Na1 O14 153.01(11) . . ?
O6 Na1 O7 80.77(9) . . ?
O14 Na1 O7 96.32(10) . . ?
O6 Na1 O8 92.44(9) . 1_455 ?
O14 Na1 O8 79.31(10) . 1_455 ?
O7 Na1 O8 155.97(10) . 1_455 ?
O6 Na1 O5 112.52(9) . 2_666 ?
O14 Na1 O5 93.50(10) . 2_666 ?
O7 Na1 O5 82.51(9) . 2_666 ?
O8 Na1 O5 121.16(9) 1_455 2_666 ?
O6 Na1 O6 79.96(9) . 2_666 ?
O14 Na1 O6 123.75(10) . 2_666 ?
O7 Na1 O6 117.85(9) . 2_666 ?
O8 Na1 O6 83.11(9) 1_455 2_666 ?
O5 Na1 O6 53.06(8) 2_666 2_666 ?
O6 Na1 C17 95.93(8) . 2_666 ?
O14 Na1 C17 110.95(8) . 2_666 ?
O7 Na1 C17 100.28(8) . 2_666 ?
O8 Na1 C17 103.35(8) 1_455 2_666 ?
O5 Na1 C17 26.67(6) 2_666 2_666 ?
O6 Na1 C17 26.42(6) 2_666 2_666 ?
O6 Na1 Na4 136.30(8) . 1_455 ?
O14 Na1 Na4 45.73(7) . 1_455 ?
O7 Na1 Na4 141.02(8) . 1_455 ?
O8 Na1 Na4 44.58(7) 1_455 1_455 ?
O5 Na1 Na4 90.29(7) 2_666 1_455 ?
O6 Na1 Na4 86.12(7) 2_666 1_455 ?
C17 Na1 Na4 88.87(5) 2_666 1_455 ?
O6 Na1 Na2 44.01(6) . . ?
O14 Na1 Na2 139.27(8) . . ?
O7 Na1 Na2 42.96(7) . . ?
O8 Na1 Na2 136.38(8) 1_455 . ?
O5 Na1 Na2 83.07(7) 2_666 . ?
O6 Na1 Na2 85.99(7) 2_666 . ?
C17 Na1 Na2 83.00(5) 2_666 . ?
Na4 Na1 Na2 171.76(5) 1_455 . ?
O6 Na1 Na2 84.41(7) . 2_666 ?
O14 Na1 Na2 104.97(8) . 2_666 ?
O7 Na1 Na2 156.66(8) . 2_666 ?
O8 Na1 Na2 42.01(7) 1_455 2_666 ?
O5 Na1 Na2 86.68(7) 2_666 2_666 ?
O6 Na1 Na2 41.11(6) 2_666 2_666 ?
C17 Na1 Na2 63.36(4) 2_666 2_666 ?
Na4 Na1 Na2 59.23(4) 1_455 2_666 ?
Na2 Na1 Na2 115.26(4) . 2_666 ?
O6 Na1 Na1 41.70(6) . 2_666 ?
O14 Na1 Na1 159.34(9) . 2_666 ?
O7 Na1 Na1 102.40(8) . 2_666 ?
O8 Na1 Na1 86.89(8) 1_455 2_666 ?
O5 Na1 Na1 80.50(7) 2_666 2_666 ?
O6 Na1 Na1 38.26(6) 2_666 2_666 ?
C17 Na1 Na1 57.31(4) 2_666 2_666 ?
Na4 Na1 Na1 114.14(6) 1_455 2_666 ?
Na2 Na1 Na1 60.03(4) . 2_666 ?
Na2 Na1 Na1 55.23(4) 2_666 2_666 ?
O6 Na1 Na2 99.36(7) . 2_766 ?
O14 Na1 Na2 97.16(8) . 2_766 ?
O7 Na1 Na2 45.03(7) . 2_766 ?
O8 Na1 Na2 158.52(8) 1_455 2_766 ?
O5 Na1 Na2 37.49(6) 2_666 2_766 ?
O6 Na1 Na2 81.38(6) 2_666 2_766 ?
C17 Na1 Na2 57.82(4) 2_666 2_766 ?
Na4 Na1 Na2 119.28(5) 1_455 2_766 ?
Na2 Na1 Na2 57.01(4) . 2_766 ?
Na2 Na1 Na2 121.16(5) 2_666 2_766 ?
Na1 Na1 Na2 90.06(5) 2_666 2_766 ?
O7 Na2 O9 138.65(11) . 2_665 ?
O7 Na2 O6 82.17(9) . . ?
O9 Na2 O6 88.57(9) 2_665 . ?
O7 Na2 O5 93.74(9) . 1_655 ?
O9 Na2 O5 81.09(9) 2_665 1_655 ?
O6 Na2 O5 159.25(10) . 1_655 ?
O7 Na2 O8 126.68(10) . 2_766 ?
O9 Na2 O8 92.56(10) 2_665 2_766 ?
O6 Na2 O8 86.55(9) . 2_766 ?
O5 Na2 O8 111.71(10) 1_655 2_766 ?
O7 Na2 O7 93.47(9) . 2_766 ?
O9 Na2 O7 124.79(10) 2_665 2_766 ?
O6 Na2 O7 122.30(9) . 2_766 ?
O5 Na2 O7 78.13(8) 1_655 2_766 ?
O8 Na2 O7 51.15(8) 2_766 2_766 ?
O7 Na2 C19 113.01(8) . 2_766 ?
O9 Na2 C19 108.26(8) 2_665 2_766 ?
O6 Na2 C19 106.77(8) . 2_766 ?
O5 Na2 C19 93.59(7) 1_655 2_766 ?
O8 Na2 C19 25.66(6) 2_766 2_766 ?
O7 Na2 C19 25.66(6) 2_766 2_766 ?
O7 Na2 Na1 44.75(6) . . ?
O9 Na2 Na1 130.86(8) 2_665 . ?
O6 Na2 Na1 43.78(6) . . ?
O5 Na2 Na1 138.18(8) 1_655 . ?
O8 Na2 Na1 95.04(7) 2_766 . ?
O7 Na2 Na1 96.57(7) 2_766 . ?
C19 Na2 Na1 98.63(5) 2_766 . ?
O7 Na2 Na4 165.85(8) . 2_766 ?
O9 Na2 Na4 49.34(7) 2_665 2_766 ?
O6 Na2 Na4 86.85(7) . 2_766 ?
O5 Na2 Na4 99.64(7) 1_655 2_766 ?
O8 Na2 Na4 43.22(7) 2_766 2_766 ?
O7 Na2 Na4 84.86(7) 2_766 2_766 ?
C19 Na2 Na4 61.82(4) 2_766 2_766 ?
Na1 Na2 Na4 121.40(5) . 2_766 ?
O7 Na2 Na2 51.27(7) . 2_766 ?
O9 Na2 Na2 162.00(9) 2_665 2_766 ?
O6 Na2 Na2 109.02(8) . 2_766 ?
O5 Na2 Na2 83.29(7) 1_655 2_766 ?
O8 Na2 Na2 84.94(8) 2_766 2_766 ?
O7 Na2 Na2 42.20(6) 2_766 2_766 ?
C19 Na2 Na2 63.81(5) 2_766 2_766 ?
Na1 Na2 Na2 67.14(4) . 2_766 ?
Na4 Na2 Na2 125.63(6) 2_766 2_766 ?
O7 Na2 Na3 130.74(8) . 2_765 ?
O9 Na2 Na3 41.22(7) 2_665 2_765 ?
O6 Na2 Na3 129.77(8) . 2_765 ?
O5 Na2 Na3 42.11(6) 1_655 2_765 ?
O8 Na2 Na3 95.50(7) 2_766 2_765 ?
O7 Na2 Na3 95.76(7) 2_766 2_765 ?
C19 Na2 Na3 94.05(5) 2_766 2_765 ?
Na1 Na2 Na3 167.15(5) . 2_765 ?
Na4 Na2 Na3 63.39(4) 2_766 2_765 ?
Na2 Na2 Na3 121.18(6) 2_766 2_765 ?
O7 Na2 Na1 108.84(7) . 2_666 ?
O9 Na2 Na1 91.35(7) 2_665 2_666 ?
O6 Na2 Na1 44.70(6) . 2_666 ?
O5 Na2 Na1 152.51(8) 1_655 2_666 ?
O8 Na2 Na1 41.85(6) 2_766 2_666 ?
O7 Na2 Na1 84.87(6) 2_766 2_666 ?
C19 Na2 Na1 63.60(4) 2_766 2_666 ?
Na1 Na2 Na1 64.74(4) . 2_666 ?
Na4 Na2 Na1 57.03(4) 2_766 2_666 ?
Na2 Na2 Na1 98.48(5) 2_766 2_666 ?
Na3 Na2 Na1 120.12(5) 2_765 2_666 ?
O12 Na3 O10 92.59(12) . . ?
O12 Na3 O11 104.32(13) . . ?
O10 Na3 O11 106.22(11) . . ?
O12 Na3 O9 93.77(11) . 1_655 ?
O10 Na3 O9 164.03(11) . 1_655 ?
O11 Na3 O9 86.35(10) . 1_655 ?
O12 Na3 O5 146.36(13) . 2_665 ?
O10 Na3 O5 85.49(10) . 2_665 ?
O11 Na3 O5 108.45(10) . 2_665 ?
O9 Na3 O5 81.11(9) 1_655 2_665 ?
O12 Na3 Na2 132.71(10) . 2_765 ?
O10 Na3 Na2 127.14(9) . 2_765 ?
O11 Na3 Na2 89.37(8) . 2_765 ?
O9 Na3 Na2 41.33(7) 1_655 2_765 ?
O5 Na3 Na2 42.03(6) 2_665 2_765 ?
O12 Na3 Na4 106.09(10) . 1_554 ?
O10 Na3 Na4 145.17(9) . 1_554 ?
O11 Na3 Na4 41.26(7) . 1_554 ?
O9 Na3 Na4 45.31(7) 1_655 1_554 ?
O5 Na3 Na4 93.83(7) 2_665 1_554 ?
Na2 Na3 Na4 57.20(4) 2_765 1_554 ?
O12 Na3 Na1 165.30(10) . 1_554 ?
O10 Na3 Na1 72.72(8) . 1_554 ?
O11 Na3 Na1 80.90(8) . 1_554 ?
O9 Na3 Na1 100.33(8) 1_655 1_554 ?
O5 Na3 Na1 34.90(6) 2_665 1_554 ?
Na2 Na3 Na1 60.14(3) 2_765 1_554 ?
Na4 Na3 Na1 86.98(4) 1_554 1_554 ?
O12 Na3 Na4 117.24(10) . 1_454 ?
O10 Na3 Na4 32.50(8) . 1_454 ?
O11 Na3 Na4 79.44(8) . 1_454 ?
O9 Na3 Na4 148.17(8) 1_655 1_454 ?
O5 Na3 Na4 76.71(7) 2_665 1_454 ?
Na2 Na3 Na4 109.65(5) 2_765 1_454 ?
Na4 Na3 Na4 113.61(5) 1_554 1_454 ?
Na1 Na3 Na4 49.53(3) 1_554 1_454 ?
O8 Na4 O14 79.98(10) . 1_655 ?
O8 Na4 O10 117.60(11) . 1_656 ?
O14 Na4 O10 90.67(10) 1_655 1_656 ?
O8 Na4 O13 134.97(13) . 1_556 ?
O14 Na4 O13 105.89(11) 1_655 1_556 ?
O10 Na4 O13 107.06(12) 1_656 1_556 ?
O8 Na4 O11 101.83(10) . 1_556 ?
O14 Na4 O11 152.88(12) 1_655 1_556 ?
O10 Na4 O11 111.46(11) 1_656 1_556 ?
O13 Na4 O11 53.79(10) 1_556 1_556 ?
O8 Na4 O9 87.54(9) . 1_656 ?
O14 Na4 O9 128.70(10) 1_655 1_656 ?
O10 Na4 O9 52.33(9) 1_656 1_656 ?
O13 Na4 O9 117.40(11) 1_556 1_656 ?
O11 Na4 O9 78.34(10) 1_556 1_656 ?
O8 Na4 C35 123.45(12) . 1_556 ?
O14 Na4 C35 131.88(12) 1_655 1_556 ?
O10 Na4 C35 108.34(12) 1_656 1_556 ?
O13 Na4 C35 26.83(10) 1_556 1_556 ?
O11 Na4 C35 27.35(10) 1_556 1_556 ?
O9 Na4 C35 96.26(11) 1_656 1_556 ?
O8 Na4 C25 105.05(11) . 1_656 ?
O14 Na4 C25 111.81(11) 1_655 1_656 ?
O10 Na4 C25 26.04(9) 1_656 1_656 ?
O13 Na4 C25 113.09(12) 1_556 1_656 ?
O11 Na4 C25 94.02(11) 1_556 1_656 ?
O9 Na4 C25 26.39(9) 1_656 1_656 ?
C35 Na4 C25 102.00(12) 1_556 1_656 ?
O8 Na4 Na1 45.83(7) . 1_655 ?
O14 Na4 Na1 45.30(7) 1_655 1_655 ?
O10 Na4 Na1 85.57(8) 1_656 1_655 ?
O13 Na4 Na1 149.72(9) 1_556 1_655 ?
O11 Na4 Na1 147.12(9) 1_556 1_655 ?
O9 Na4 Na1 92.25(7) 1_656 1_655 ?
C35 Na4 Na1 166.09(11) 1_556 1_655 ?
C25 Na4 Na1 90.49(8) 1_656 1_655 ?
O8 Na4 Na2 44.58(7) . 2_766 ?
O14 Na4 Na2 109.03(8) 1_655 2_766 ?
O10 Na4 Na2 83.75(8) 1_656 2_766 ?
O13 Na4 Na2 143.26(9) 1_556 2_766 ?
O11 Na4 Na2 89.48(8) 1_556 2_766 ?
O9 Na4 Na2 42.97(6) 1_656 2_766 ?
C35 Na4 Na2 116.52(9) 1_556 2_766 ?
C25 Na4 Na2 63.27(8) 1_656 2_766 ?
Na1 Na4 Na2 63.73(4) 1_655 2_766 ?
O8 Na4 Na3 93.12(8) . 1_556 ?
O14 Na4 Na3 167.29(9) 1_655 1_556 ?
O10 Na4 Na3 83.04(7) 1_656 1_556 ?
O13 Na4 Na3 86.56(8) 1_556 1_556 ?
O11 Na4 Na3 38.93(7) 1_556 1_556 ?
O9 Na4 Na3 39.60(6) 1_656 1_556 ?
C35 Na4 Na3 60.80(9) 1_556 1_556 ?
C25 Na4 Na3 59.45(8) 1_656 1_556 ?
Na1 Na4 Na3 122.83(5) 1_655 1_556 ?
Na2 Na4 Na3 59.42(4) 2_766 1_556 ?
O8 Na4 Na3 108.44(8) . 1_656 ?
O14 Na4 Na3 59.59(8) 1_655 1_656 ?
O10 Na4 Na3 31.09(7) 1_656 1_656 ?
O13 Na4 Na3 112.80(10) 1_556 1_656 ?
O11 Na4 Na3 140.63(9) 1_556 1_656 ?
O9 Na4 Na3 78.43(7) 1_656 1_656 ?
C35 Na4 Na3 127.66(10) 1_556 1_656 ?
C25 Na4 Na3 54.47(8) 1_656 1_656 ?
Na1 Na4 Na3 64.88(4) 1_655 1_656 ?
Na2 Na4 Na3 94.68(5) 2_766 1_656 ?
Na3 Na4 Na3 113.61(5) 1_556 1_656 ?
C17 O5 Na2 128.05(16) . 1_455 ?
C17 O5 Na3 123.46(16) . 2_665 ?
Na2 O5 Na3 95.86(9) 1_455 2_665 ?
C17 O5 Na1 92.85(14) . 2_666 ?
Na2 O5 Na1 103.37(9) 1_455 2_666 ?
Na3 O5 Na1 111.55(10) 2_665 2_666 ?
C17 O6 Na1 125.70(16) . . ?
C17 O6 Na2 140.53(17) . . ?
Na1 O6 Na2 92.22(9) . . ?
C17 O6 Na1 89.81(14) . 2_666 ?
Na1 O6 Na1 100.04(9) . 2_666 ?
Na2 O6 Na1 94.19(9) . 2_666 ?
C19 O7 Na2 140.40(17) . . ?
C19 O7 Na1 127.16(17) . . ?
Na2 O7 Na1 92.29(9) . . ?
C19 O7 Na2 85.97(14) . 2_766 ?
Na2 O7 Na2 86.54(9) . 2_766 ?
Na1 O7 Na2 95.96(9) . 2_766 ?
C19 O8 Na4 127.51(17) . . ?
C19 O8 Na1 139.03(17) . 1_655 ?
Na4 O8 Na1 89.59(9) . 1_655 ?
C19 O8 Na2 98.69(15) . 2_766 ?
Na4 O8 Na2 92.20(10) . 2_766 ?
Na1 O8 Na2 96.14(10) 1_655 2_766 ?
C25 O9 Na3 130.1(2) . 1_455 ?
C25 O9 Na2 132.5(2) . 2_665 ?
Na3 O9 Na2 97.45(10) 1_455 2_665 ?
C25 O9 Na4 86.9(2) . 1_454 ?
Na3 O9 Na4 95.09(10) 1_455 1_454 ?
Na2 O9 Na4 87.70(9) 2_665 1_454 ?
C25 O10 Na3 133.6(2) . . ?
C25 O10 Na4 96.3(2) . 1_454 ?
Na3 O10 Na4 116.42(12) . 1_454 ?
C35 O11 Na3 133.8(3) . . ?
C35 O11 Na4 90.1(2) . 1_554 ?
Na3 O11 Na4 99.80(11) . 1_554 ?
C51 O12 Na3 139.8(4) . . ?
C35 O13 Na4 90.6(2) . 1_554 ?
Na1 O14 Na4 88.97(10) . 1_455 ?
C28 N15 C23 109.0(2) . . ?
C26 N16 C32 105.5(2) . . ?
O6 C17 O5 124.15(18) . . ?
O6 C17 C18 118.09(12) . . ?
O5 C17 C18 117.75(12) . . ?
O6 C17 Na1 63.77(12) . 2_666 ?
O5 C17 Na1 60.48(12) . 2_666 ?
C18 C17 Na1 177.3 . 2_666 ?
C20 C18 C24 119.62(16) . . ?
C20 C18 C17 120.4 . . ?
C24 C18 C17 119.95(16) . . ?
O7 C19 O8 123.3(2) . . ?
O7 C19 C41 118.4(2) . . ?
O8 C19 C41 118.3(2) . . ?
O7 C19 Na2 68.37(13) . 2_766 ?
O8 C19 Na2 55.64(13) . 2_766 ?
C41 C19 Na2 169.9(2) . 2_766 ?
C30 C20 C18 120.15(16) . . ?
C24 C21 C22 120.6(3) . . ?
C30 C22 C21 118.6(3) . . ?
C30 C22 C29 122.1(3) . . ?
C21 C22 C29 119.3(3) . . ?
N15 C23 C27 126.4(3) . . ?
N15 C23 C34 107.7(3) . . ?
C27 C23 C34 125.9(3) . . ?
C18 C24 C21 120.1(3) . . ?
O10 C25 O9 123.9(4) . . ?
O10 C25 C42 118.8(3) . . ?
O9 C25 C42 117.2(3) . . ?
O10 C25 Na4 57.6(2) . 1_454 ?
O9 C25 Na4 66.7(2) . 1_454 ?
C42 C25 Na4 171.7(3) . 1_454 ?
N16 C26 C27 126.0(3) . . ?
N16 C26 C37 110.3(3) . . ?
C27 C26 C37 123.6(3) . . ?
C23 C27 C26 125.8(3) . . ?
C23 C27 C33 116.3(3) . . ?
C26 C27 C33 117.4(3) . . ?
N15 C28 C29 126.3(3) . 2 ?
N15 C28 C31 107.5(3) . . ?
C29 C28 C31 126.1(3) 2 . ?
C28 C29 C32 125.2(3) 2 . ?
C28 C29 C22 116.8(3) 2 . ?
C32 C29 C22 117.9(3) . . ?
C20 C30 C22 120.9(3) . . ?
C34 C31 C28 108.4(3) . . ?
N16 C32 C29 125.3(3) . . ?
N16 C32 C40 110.0(3) . . ?
C29 C32 C40 124.6(3) . . ?
C46 C33 C43 118.1(4) . . ?
C46 C33 C27 119.0(3) . . ?
C43 C33 C27 122.9(3) . . ?
C31 C34 C23 107.3(3) . . ?
O13 C35 O11 123.6(4) . . ?
O13 C35 C36 118.2(3) . . ?
O11 C35 C36 118.2(3) . . ?
O13 C35 Na4 62.5(2) . 1_554 ?
O11 C35 Na4 62.5(2) . 1_554 ?
C36 C35 Na4 167.6(3) . 1_554 ?
C44 C36 C45 118.5(4) . . ?
C44 C36 C35 121.5(3) . . ?
C45 C36 C35 120.0(3) . . ?
C40 C37 C26 107.3(3) . . ?
C37 C40 C32 106.8(3) . . ?
C44 C43 C33 120.6(4) . . ?
C36 C44 C43 120.8(4) . . ?
C46 C45 C36 120.1(4) . . ?
C33 C46 C45 121.8(4) . . ?
C51 N47 C50 118.8(5) . . ?
C51 N47 C48 112.8(4) . . ?
C50 N47 C48 127.3(6) . . ?
N47 C51 O12 116.5(5) . . ?
N47 C51 C49 112.6(5) . . ?
O12 C51 C49 130.9(5) . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.021 0.000 0.500 289 52 ' '
_platon_squeeze_details          
;
 Disordered DMA solvent included in the intralattice channel voids
;

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.44
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.093
_database_code_depnum_ccdc_archive 'CCDC 1021603'
