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

#######################################################################
#
#                 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.
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data_dp

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
'[Ba₅(L)₃(H₂O)₆].25H₂O.10DMF.2Me₂NH₂⁺'
_chemical_melting_point          ?
_chemical_formula_moiety         'C154 H214 Ba5 N12 O65'
_chemical_formula_sum            'C154 H214 Ba5 N12 O65'
_chemical_formula_weight         3960.07

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'
Ba Ba -0.3244 2.2819 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 6/m'
_symmetry_space_group_name_Hall  '-P 6'

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

_cell_length_a                   15.0263(3)
_cell_length_b                   15.0263(3)
_cell_length_c                   17.6363(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3448.59(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2685
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.178
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2022
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker SMART APEX-II diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            25665
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2685
_reflns_number_gt                1973
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens SMART'
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_reduction        'Siemens XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
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
1 0.000 0.000 -0.010 1134.1 15.4
_platon_squeeze_details          
;
The unit cell contains twenty-five water and ten dmf molecules and two Me2NH2+ 
which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_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)+(0.1199P)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         2685
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1785
_refine_ls_wR_factor_gt          0.1651
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.5000 0.0000 0.0000 0.0317(3) Uani 1 4 d S . .
Ba2 Ba 0.6667 0.3333 0.0000 0.0280(3) Uani 1 6 d S . .
O1 O 0.5314(4) 0.1730(3) 0.0921(3) 0.0416(11) Uani 1 1 d . . .
O2 O 0.3966(4) 0.0235(4) 0.1245(3) 0.0601(16) Uani 1 1 d . . .
O1W O 0.7080(6) 0.1613(6) 0.0000 0.067(2) Uani 1 2 d S . .
H1WA H 0.7401 0.1608 -0.0395 0.080 Uiso 0.50 1 d PR . .
C1 C 0.4922(6) 0.4467(6) 0.5000 0.0246(16) Uani 1 2 d S . .
C2 C 0.4830(5) 0.3938(5) 0.4325(3) 0.0280(13) Uani 1 1 d . . .
H2A H 0.4867 0.4261 0.3867 0.034 Uiso 1 1 calc R . .
C3 C 0.4686(5) 0.2959(5) 0.4310(3) 0.0265(12) Uani 1 1 d . . .
C4 C 0.4610(7) 0.2465(6) 0.5000 0.0279(17) Uani 1 2 d S . .
H4A H 0.4507 0.1801 0.5000 0.034 Uiso 1 2 calc SR . .
C7 C 0.4633(5) 0.2463(4) 0.3564(3) 0.0265(12) Uani 1 1 d . . .
C8 C 0.4099(5) 0.1397(5) 0.3460(3) 0.0333(14) Uani 1 1 d . . .
H8A H 0.3754 0.0970 0.3867 0.040 Uiso 1 1 calc R . .
C9 C 0.4077(5) 0.0968(5) 0.2759(4) 0.0347(14) Uani 1 1 d . . .
H9A H 0.3721 0.0257 0.2701 0.042 Uiso 1 1 calc R . .
C10 C 0.4591(5) 0.1603(5) 0.2134(3) 0.0269(12) Uani 1 1 d . . .
C11 C 0.5117(5) 0.2652(5) 0.2237(3) 0.0307(13) Uani 1 1 d . . .
H11A H 0.5460 0.3079 0.1829 0.037 Uiso 1 1 calc R . .
C12 C 0.5146(5) 0.3083(5) 0.2940(3) 0.0310(13) Uani 1 1 d . . .
H12A H 0.5512 0.3793 0.2996 0.037 Uiso 1 1 calc R . .
C13 C 0.4611(5) 0.1159(5) 0.1382(3) 0.0319(13) Uani 1 1 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
Ba1 O2 2.812(5) 4_655 ?
Ba1 O2 2.812(5) 7_655 ?
Ba1 O2 2.812(5) 10 ?
Ba1 O2 2.812(5) . ?
Ba1 O1W 2.840(8) . ?
Ba1 O1W 2.840(8) 7_655 ?
Ba1 O1 2.896(4) . ?
Ba1 O1 2.896(4) 7_655 ?
Ba1 O1 2.896(4) 4_655 ?
Ba1 O1 2.896(4) 10 ?
Ba1 C13 3.214(6) 7_655 ?
Ba1 C13 3.214(6) . ?
Ba2 O1 2.771(4) 3_655 ?
Ba2 O1 2.771(4) 12_655 ?
Ba2 O1 2.771(4) 10 ?
Ba2 O1 2.771(4) . ?
Ba2 O1 2.771(4) 5_665 ?
Ba2 O1 2.771(4) 8_665 ?
Ba2 O1W 2.945(8) . ?
Ba2 O1W 2.945(8) 3_655 ?
Ba2 O1W 2.945(8) 8_665 ?
Ba2 Ba1 4.3377 3_655 ?
Ba2 Ba1 4.3377 2 ?
O1 C13 1.268(8) . ?
O2 C13 1.257(8) . ?
C1 C2 1.399(7) . ?
C1 C2 1.399(7) 10_556 ?
C1 C1 1.498(16) 7_666 ?
C2 C3 1.376(8) . ?
C3 C4 1.400(7) . ?
C3 C7 1.495(7) . ?
C4 C3 1.400(7) 10_556 ?
C7 C12 1.398(8) . ?
C7 C8 1.399(8) . ?
C8 C9 1.387(8) . ?
C9 C10 1.409(9) . ?
C10 C11 1.377(8) . ?
C10 C13 1.492(7) . ?
C11 C12 1.389(8) . ?

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
O2 Ba1 O2 102.6(3) 4_655 7_655 ?
O2 Ba1 O2 180.0(3) 4_655 10 ?
O2 Ba1 O2 77.4(3) 7_655 10 ?
O2 Ba1 O2 77.4(3) 4_655 . ?
O2 Ba1 O2 180.0(3) 7_655 . ?
O2 Ba1 O2 102.6(3) 10 . ?
O2 Ba1 O1W 70.47(14) 4_655 . ?
O2 Ba1 O1W 70.47(14) 7_655 . ?
O2 Ba1 O1W 109.53(14) 10 . ?
O2 Ba1 O1W 109.53(14) . . ?
O2 Ba1 O1W 109.53(14) 4_655 7_655 ?
O2 Ba1 O1W 109.53(14) 7_655 7_655 ?
O2 Ba1 O1W 70.47(14) 10 7_655 ?
O2 Ba1 O1W 70.47(14) . 7_655 ?
O1W Ba1 O1W 180.0(5) . 7_655 ?
O2 Ba1 O1 79.79(17) 4_655 . ?
O2 Ba1 O1 134.27(14) 7_655 . ?
O2 Ba1 O1 100.21(17) 10 . ?
O2 Ba1 O1 45.73(14) . . ?
O1W Ba1 O1 67.55(17) . . ?
O1W Ba1 O1 112.45(17) 7_655 . ?
O2 Ba1 O1 100.21(17) 4_655 7_655 ?
O2 Ba1 O1 45.73(14) 7_655 7_655 ?
O2 Ba1 O1 79.79(17) 10 7_655 ?
O2 Ba1 O1 134.27(14) . 7_655 ?
O1W Ba1 O1 112.45(17) . 7_655 ?
O1W Ba1 O1 67.55(17) 7_655 7_655 ?
O1 Ba1 O1 180.0(2) . 7_655 ?
O2 Ba1 O1 45.73(14) 4_655 4_655 ?
O2 Ba1 O1 100.21(17) 7_655 4_655 ?
O2 Ba1 O1 134.27(14) 10 4_655 ?
O2 Ba1 O1 79.79(17) . 4_655 ?
O1W Ba1 O1 112.45(17) . 4_655 ?
O1W Ba1 O1 67.55(17) 7_655 4_655 ?
O1 Ba1 O1 111.79(18) . 4_655 ?
O1 Ba1 O1 68.21(18) 7_655 4_655 ?
O2 Ba1 O1 134.27(14) 4_655 10 ?
O2 Ba1 O1 79.79(17) 7_655 10 ?
O2 Ba1 O1 45.73(14) 10 10 ?
O2 Ba1 O1 100.21(17) . 10 ?
O1W Ba1 O1 67.55(17) . 10 ?
O1W Ba1 O1 112.45(17) 7_655 10 ?
O1 Ba1 O1 68.21(18) . 10 ?
O1 Ba1 O1 111.79(18) 7_655 10 ?
O1 Ba1 O1 180.00(19) 4_655 10 ?
O2 Ba1 C13 105.21(18) 4_655 7_655 ?
O2 Ba1 C13 22.85(15) 7_655 7_655 ?
O2 Ba1 C13 74.79(18) 10 7_655 ?
O2 Ba1 C13 157.15(15) . 7_655 ?
O1W Ba1 C13 92.39(16) . 7_655 ?
O1W Ba1 C13 87.61(16) 7_655 7_655 ?
O1 Ba1 C13 156.80(15) . 7_655 ?
O1 Ba1 C13 23.20(15) 7_655 7_655 ?
O1 Ba1 C13 86.06(15) 4_655 7_655 ?
O1 Ba1 C13 93.94(15) 10 7_655 ?
O2 Ba1 C13 74.79(18) 4_655 . ?
O2 Ba1 C13 157.15(15) 7_655 . ?
O2 Ba1 C13 105.21(18) 10 . ?
O2 Ba1 C13 22.85(15) . . ?
O1W Ba1 C13 87.61(16) . . ?
O1W Ba1 C13 92.39(16) 7_655 . ?
O1 Ba1 C13 23.20(15) . . ?
O1 Ba1 C13 156.80(15) 7_655 . ?
O1 Ba1 C13 93.94(15) 4_655 . ?
O1 Ba1 C13 86.06(15) 10 . ?
C13 Ba1 C13 180.0(3) 7_655 . ?
O1 Ba2 O1 71.75(19) 3_655 12_655 ?
O1 Ba2 O1 132.20(6) 3_655 10 ?
O1 Ba2 O1 89.13(14) 12_655 10 ?
O1 Ba2 O1 89.13(14) 3_655 . ?
O1 Ba2 O1 132.20(6) 12_655 . ?
O1 Ba2 O1 71.75(19) 10 . ?
O1 Ba2 O1 89.13(14) 3_655 5_665 ?
O1 Ba2 O1 132.20(6) 12_655 5_665 ?
O1 Ba2 O1 132.20(6) 10 5_665 ?
O1 Ba2 O1 89.13(14) . 5_665 ?
O1 Ba2 O1 132.20(6) 3_655 8_665 ?
O1 Ba2 O1 89.13(14) 12_655 8_665 ?
O1 Ba2 O1 89.13(14) 10 8_665 ?
O1 Ba2 O1 132.20(6) . 8_665 ?
O1 Ba2 O1 71.75(19) 5_665 8_665 ?
O1 Ba2 O1W 64.45(17) 3_655 . ?
O1 Ba2 O1W 64.45(17) 12_655 . ?
O1 Ba2 O1W 67.76(16) 10 . ?
O1 Ba2 O1W 67.76(16) . . ?
O1 Ba2 O1W 144.07(9) 5_665 . ?
O1 Ba2 O1W 144.07(9) 8_665 . ?
O1 Ba2 O1W 67.76(16) 3_655 3_655 ?
O1 Ba2 O1W 67.76(16) 12_655 3_655 ?
O1 Ba2 O1W 144.07(9) 10 3_655 ?
O1 Ba2 O1W 144.07(9) . 3_655 ?
O1 Ba2 O1W 64.45(17) 5_665 3_655 ?
O1 Ba2 O1W 64.45(17) 8_665 3_655 ?
O1W Ba2 O1W 120.0 . 3_655 ?
O1 Ba2 O1W 144.07(9) 3_655 8_665 ?
O1 Ba2 O1W 144.07(9) 12_655 8_665 ?
O1 Ba2 O1W 64.45(17) 10 8_665 ?
O1 Ba2 O1W 64.45(17) . 8_665 ?
O1 Ba2 O1W 67.76(16) 5_665 8_665 ?
O1 Ba2 O1W 67.76(16) 8_665 8_665 ?
O1W Ba2 O1W 120.0 . 8_665 ?
O1W Ba2 O1W 120.0 3_655 8_665 ?
O1 Ba2 Ba1 96.77(11) 3_655 . ?
O1 Ba2 Ba1 96.77(11) 12_655 . ?
O1 Ba2 Ba1 41.13(9) 10 . ?
O1 Ba2 Ba1 41.13(9) . . ?
O1 Ba2 Ba1 129.44(12) 5_665 . ?
O1 Ba2 Ba1 129.44(12) 8_665 . ?
O1W Ba2 Ba1 40.52(16) . . ?
O1W Ba2 Ba1 160.52(16) 3_655 . ?
O1W Ba2 Ba1 79.48(16) 8_665 . ?
O1 Ba2 Ba1 41.13(9) 3_655 3_655 ?
O1 Ba2 Ba1 41.13(9) 12_655 3_655 ?
O1 Ba2 Ba1 129.44(12) 10 3_655 ?
O1 Ba2 Ba1 129.44(12) . 3_655 ?
O1 Ba2 Ba1 96.77(11) 5_665 3_655 ?
O1 Ba2 Ba1 96.77(11) 8_665 3_655 ?
O1W Ba2 Ba1 79.48(16) . 3_655 ?
O1W Ba2 Ba1 40.52(16) 3_655 3_655 ?
O1W Ba2 Ba1 160.52(16) 8_665 3_655 ?
Ba1 Ba2 Ba1 120.0 . 3_655 ?
O1 Ba2 Ba1 129.44(12) 3_655 2 ?
O1 Ba2 Ba1 129.44(12) 12_655 2 ?
O1 Ba2 Ba1 96.77(11) 10 2 ?
O1 Ba2 Ba1 96.77(11) . 2 ?
O1 Ba2 Ba1 41.13(9) 5_665 2 ?
O1 Ba2 Ba1 41.13(9) 8_665 2 ?
O1W Ba2 Ba1 160.52(16) . 2 ?
O1W Ba2 Ba1 79.48(16) 3_655 2 ?
O1W Ba2 Ba1 40.52(16) 8_665 2 ?
Ba1 Ba2 Ba1 120.0 . 2 ?
Ba1 Ba2 Ba1 120.0 3_655 2 ?
C13 O1 Ba2 164.9(4) . . ?
C13 O1 Ba1 92.6(3) . . ?
Ba2 O1 Ba1 99.87(14) . . ?
C13 O2 Ba1 96.8(4) . . ?
Ba1 O1W Ba2 97.1(3) . . ?
C2 C1 C2 116.5(7) . 10_556 ?
C2 C1 C1 121.7(4) . 7_666 ?
C2 C1 C1 121.7(4) 10_556 7_666 ?
C3 C2 C1 122.9(5) . . ?
C2 C3 C4 118.5(5) . . ?
C2 C3 C7 119.4(5) . . ?
C4 C3 C7 122.1(5) . . ?
C3 C4 C3 120.7(7) . 10_556 ?
C12 C7 C8 118.0(5) . . ?
C12 C7 C3 119.1(5) . . ?
C8 C7 C3 122.9(5) . . ?
C9 C8 C7 121.1(5) . . ?
C8 C9 C10 120.3(6) . . ?
C11 C10 C9 118.6(5) . . ?
C11 C10 C13 120.1(5) . . ?
C9 C10 C13 121.3(5) . . ?
C10 C11 C12 121.2(5) . . ?
C11 C12 C7 120.9(6) . . ?
O2 C13 O1 123.1(5) . . ?
O2 C13 C10 119.2(6) . . ?
O1 C13 C10 117.6(5) . . ?
O2 C13 Ba1 60.3(3) . . ?
O1 C13 Ba1 64.2(3) . . ?
C10 C13 Ba1 165.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.429
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.169
_database_code_depnum_ccdc_archive 'CCDC 1001306'
