# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1056460'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'H[Na6(H2O)12Ce2(dipic)6(NO3)]?18H2O '
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H79 Ce2 N7 Na6 O57'
_chemical_formula_weight         2012.30

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   15.455(5)
_cell_length_b                   15.455(5)
_cell_length_c                   56.103(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11605(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8157
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      28.17

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_F_000             6108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.314
_shelx_estimated_absorpt_T_min   0.583
_shelx_estimated_absorpt_T_max   0.779
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42301
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_theta_min         1.686
_diffrn_reflns_theta_max         28.200
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3183
_reflns_number_gt                2881
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
all hydrogen atoms of lattice waters and coordinated waters could not be located. 
Maximum difference density  2.65  at  0.9042  0.1058  0.0220 (1.54 A from O10)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1119P)²+137.1359P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3183
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1766
_refine_ls_wR_factor_gt          0.1720
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce Ce 0.0000 0.0000 0.33525(2) 0.01277(18) Uani 1 3 d S T P . .
Na1 Na -0.21998(15) 0.0000 0.2500 0.0219(4) Uani 1 2 d S T P . .
Na2 Na -0.21657(16) -0.21657(16) 0.2500 0.0287(5) Uani 1 2 d S T P . .
O1 O -0.03256(19) -0.12884(19) 0.36657(4) 0.0200(5) Uani 1 1 d . . . . .
O2 O -0.1270(2) -0.2760(3) 0.38466(7) 0.0312(8) Uani 1 1 d . . . . .
O3 O -0.12920(19) -0.01783(19) 0.30525(4) 0.0203(5) Uani 1 1 d . . . . .
O4 O -0.2572(3) -0.1168(2) 0.28120(6) 0.0251(6) Uani 1 1 d . . . . .
O5 O -0.0485(4) -0.0929(5) 0.25188(13) 0.0271(14) Uani 0.5 1 d . . P . .
O6 O -0.1289(3) 0.1337(2) 0.27809(7) 0.0363(9) Uani 1 1 d . . . . .
O7 O -0.3674(4) 0.0000 0.2500 0.070(2) Uani 1 2 d S T P . .
O8 O -0.3628(4) -0.3628(4) 0.2500 0.076(3) Uani 1 2 d S T P . .
O9 O -0.2311(6) -0.4834(7) 0.3734(3) 0.177(6) Uani 1 1 d . . . . .
O10 O -0.2427(5) 0.2278(5) 0.2840(2) 0.121(4) Uani 1 1 d . . . . .
O11 O -0.4624(4) -0.2160(4) 0.26664(9) 0.0610(13) Uani 1 1 d . . . . .
N1 N -0.1725(2) -0.1665(2) 0.33472(5) 0.0163(6) Uani 1 1 d . . . . .
N2 N 0.0000 0.0000 0.2500 0.0240(19) Uani 1 6 d S T P . .
C1 C -0.1115(3) -0.2113(3) 0.36950(7) 0.0161(8) Uani 1 1 d . . . . .
C2 C -0.1947(3) -0.2356(3) 0.35158(6) 0.0189(6) Uani 1 1 d . . . . .
C3 C -0.2862(3) -0.3234(3) 0.35216(7) 0.0271(8) Uani 1 1 d . . . . .
H3 H -0.3017 -0.3705 0.3646 0.033 Uiso 1 1 calc R U . . .
C4 C -0.3545(4) -0.3409(3) 0.33412(7) 0.0304(10) Uani 1 1 d . . . . .
H4 H -0.4175 -0.4007 0.3341 0.037 Uiso 1 1 calc R U . . .
C5 C -0.3305(3) -0.2710(3) 0.31623(7) 0.0248(7) Uani 1 1 d . . . . .
H5 H -0.3755 -0.2824 0.3035 0.030 Uiso 1 1 calc R U . . .
C6 C -0.2384(3) -0.1835(3) 0.31747(6) 0.0182(6) Uani 1 1 d . . . . .
C7 C -0.2073(3) -0.1002(3) 0.29941(8) 0.0186(8) 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
Ce O1 2.511(3) 2 ?
Ce O1 2.511(3) . ?
Ce O1 2.511(3) 3 ?
Ce O3 2.519(3) 2 ?
Ce O3 2.519(3) . ?
Ce O3 2.519(3) 3 ?
Ce N1 2.621(3) 3 ?
Ce N1 2.621(3) 2 ?
Ce N1 2.621(3) . ?
Na1 O7 2.279(6) . ?
Na1 O4 2.370(3) 4 ?
Na1 O4 2.370(3) . ?
Na1 O6 2.414(4) . ?
Na1 O6 2.414(3) 4 ?
Na1 O5 2.428(6) 3 ?
Na1 O5 2.428(6) 6 ?
Na1 Na2 3.374(2) 3 ?
Na1 Na2 3.374(2) . ?
Na2 O8 2.259(6) . ?
Na2 O5 2.334(7) 6 ?
Na2 O5 2.334(7) . ?
Na2 O6 2.354(4) 2 ?
Na2 O6 2.354(4) 4 ?
Na2 O4 2.608(3) 6 ?
Na2 O4 2.608(3) . ?
Na2 Na1 3.374(2) 2 ?
O1 C1 1.259(5) . ?
O2 C1 1.242(5) . ?
O3 C7 1.284(5) . ?
O4 C7 1.228(6) . ?
O5 O5 1.209(11) 6 ?
O5 N2 1.249(7) . ?
O5 O5 1.314(11) 5 ?
O5 Na1 2.428(6) 2 ?
O6 Na2 2.354(4) 3 ?
N1 C6 1.332(4) . ?
N1 C2 1.337(4) . ?
N2 O5 1.249(7) 6 ?
N2 O5 1.249(7) 2 ?
N2 O5 1.249(7) 4 ?
N2 O5 1.249(7) 5 ?
N2 O5 1.249(7) 3 ?
C1 C2 1.524(5) . ?
C2 C3 1.386(5) . ?
C3 C4 1.388(6) . ?
C4 C5 1.382(5) . ?
C5 C6 1.391(5) . ?
C6 C7 1.515(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ce O1 76.42(9) 2 . ?
O1 Ce O1 76.42(9) 2 3 ?
O1 Ce O1 76.43(9) . 3 ?
O1 Ce O3 123.18(8) 2 2 ?
O1 Ce O3 88.44(9) . 2 ?
O1 Ce O3 151.99(9) 3 2 ?
O1 Ce O3 151.99(9) 2 . ?
O1 Ce O3 123.18(9) . . ?
O1 Ce O3 88.44(9) 3 . ?
O3 Ce O3 80.23(9) 2 . ?
O1 Ce O3 88.44(9) 2 3 ?
O1 Ce O3 151.99(9) . 3 ?
O1 Ce O3 123.18(8) 3 3 ?
O3 Ce O3 80.24(9) 2 3 ?
O3 Ce O3 80.23(9) . 3 ?
O1 Ce N1 77.91(8) 2 3 ?
O1 Ce N1 134.89(8) . 3 ?
O1 Ce N1 61.79(8) 3 3 ?
O3 Ce N1 136.64(8) 2 3 ?
O3 Ce N1 74.16(8) . 3 ?
O3 Ce N1 61.53(8) 3 3 ?
O1 Ce N1 61.79(8) 2 2 ?
O1 Ce N1 77.91(8) . 2 ?
O1 Ce N1 134.89(8) 3 2 ?
O3 Ce N1 61.53(8) 2 2 ?
O3 Ce N1 136.65(8) . 2 ?
O3 Ce N1 74.16(8) 3 2 ?
N1 Ce N1 119.987(3) 3 2 ?
O1 Ce N1 134.89(8) 2 . ?
O1 Ce N1 61.79(8) . . ?
O1 Ce N1 77.91(8) 3 . ?
O3 Ce N1 74.16(8) 2 . ?
O3 Ce N1 61.53(8) . . ?
O3 Ce N1 136.64(8) 3 . ?
N1 Ce N1 119.987(2) 3 . ?
N1 Ce N1 119.987(2) 2 . ?
O7 Na1 O4 97.96(10) . 4 ?
O7 Na1 O4 97.96(10) . . ?
O4 Na1 O4 164.1(2) 4 . ?
O7 Na1 O6 98.95(12) . . ?
O4 Na1 O6 88.37(11) 4 . ?
O4 Na1 O6 89.16(11) . . ?
O7 Na1 O6 98.94(12) . 4 ?
O4 Na1 O6 89.16(11) 4 4 ?
O4 Na1 O6 88.37(11) . 4 ?
O6 Na1 O6 162.1(2) . 4 ?
O7 Na1 O5 164.30(14) . 3 ?
O4 Na1 O5 73.89(19) 4 3 ?
O4 Na1 O5 90.62(19) . 3 ?
O6 Na1 O5 67.91(19) . 3 ?
O6 Na1 O5 94.4(2) 4 3 ?
O7 Na1 O5 164.30(14) . 6 ?
O4 Na1 O5 90.62(19) 4 6 ?
O4 Na1 O5 73.89(19) . 6 ?
O6 Na1 O5 94.4(2) . 6 ?
O6 Na1 O5 67.91(19) 4 6 ?
O5 Na1 O5 31.4(3) 3 6 ?
O7 Na1 Na2 120.77(4) . 3 ?
O4 Na1 Na2 50.37(9) 4 3 ?
O4 Na1 Na2 119.74(9) . 3 ?
O6 Na1 Na2 44.24(9) . 3 ?
O6 Na1 Na2 123.87(11) 4 3 ?
O5 Na1 Na2 43.77(14) 3 3 ?
O5 Na1 Na2 74.75(15) 6 3 ?
O7 Na1 Na2 120.77(4) . . ?
O4 Na1 Na2 119.74(9) 4 . ?
O4 Na1 Na2 50.38(9) . . ?
O6 Na1 Na2 123.87(11) . . ?
O6 Na1 Na2 44.24(9) 4 . ?
O5 Na1 Na2 74.75(15) 3 . ?
O5 Na1 Na2 43.77(15) 6 . ?
Na2 Na1 Na2 118.45(8) 3 . ?
O8 Na2 O5 164.99(15) . 6 ?
O8 Na2 O5 164.99(15) . . ?
O5 Na2 O5 30.0(3) 6 . ?
O8 Na2 O6 96.96(12) . 2 ?
O5 Na2 O6 95.7(2) 6 2 ?
O5 Na2 O6 70.5(2) . 2 ?
O8 Na2 O6 96.96(12) . 4 ?
O5 Na2 O6 70.5(2) 6 4 ?
O5 Na2 O6 95.7(2) . 4 ?
O6 Na2 O6 166.1(2) 2 4 ?
O8 Na2 O4 100.10(9) . 6 ?
O5 Na2 O4 89.09(19) 6 6 ?
O5 Na2 O4 71.17(19) . 6 ?
O6 Na2 O4 84.28(11) 2 6 ?
O6 Na2 O4 93.27(11) 4 6 ?
O8 Na2 O4 100.10(9) . . ?
O5 Na2 O4 71.17(19) 6 . ?
O5 Na2 O4 89.09(19) . . ?
O6 Na2 O4 93.27(11) 2 . ?
O6 Na2 O4 84.29(11) 4 . ?
O4 Na2 O4 159.81(18) 6 . ?
O8 Na2 Na1 119.23(4) . . ?
O5 Na2 Na1 46.04(15) 6 . ?
O5 Na2 Na1 75.58(15) . . ?
O6 Na2 Na1 125.47(12) 2 . ?
O6 Na2 Na1 45.68(9) 4 . ?
O4 Na2 Na1 122.89(9) 6 . ?
O4 Na2 Na1 44.43(7) . . ?
O8 Na2 Na1 119.23(4) . 2 ?
O5 Na2 Na1 75.58(15) 6 2 ?
O5 Na2 Na1 46.04(15) . 2 ?
O6 Na2 Na1 45.68(9) 2 2 ?
O6 Na2 Na1 125.47(12) 4 2 ?
O4 Na2 Na1 44.42(7) 6 2 ?
O4 Na2 Na1 122.89(9) . 2 ?
Na1 Na2 Na1 121.55(8) . 2 ?
C1 O1 Ce 127.1(2) . . ?
C7 O3 Ce 125.4(2) . . ?
C7 O4 Na1 124.6(3) . . ?
C7 O4 Na2 111.8(3) . . ?
Na1 O4 Na2 85.20(12) . . ?
O5 O5 N2 61.0(2) 6 . ?
O5 O5 O5 117.3(4) 6 5 ?
N2 O5 O5 58.2(2) . 5 ?
O5 O5 Na2 74.99(15) 6 . ?
N2 O5 Na2 136.0(3) . . ?
O5 O5 Na2 160.8(5) 5 . ?
O5 O5 Na1 160.9(6) 6 2 ?
N2 O5 Na1 132.5(3) . 2 ?
O5 O5 Na1 74.30(14) 5 2 ?
Na2 O5 Na1 90.2(2) . 2 ?
Na2 O6 Na1 90.09(16) 3 . ?
C6 N1 C2 119.4(3) . . ?
C6 N1 Ce 120.3(2) . . ?
C2 N1 Ce 120.3(2) . . ?
O5 N2 O5 57.9(4) . 6 ?
O5 N2 O5 119.29(10) . 2 ?
O5 N2 O5 177.2(4) 6 2 ?
O5 N2 O5 177.2(4) . 4 ?
O5 N2 O5 119.29(10) 6 4 ?
O5 N2 O5 63.5(4) 2 4 ?
O5 N2 O5 63.5(4) . 5 ?
O5 N2 O5 119.29(10) 6 5 ?
O5 N2 O5 57.9(4) 2 5 ?
O5 N2 O5 119.29(10) 4 5 ?
O5 N2 O5 119.29(10) . 3 ?
O5 N2 O5 63.5(4) 6 3 ?
O5 N2 O5 119.29(10) 2 3 ?
O5 N2 O5 57.9(4) 4 3 ?
O5 N2 O5 177.2(4) 5 3 ?
O2 C1 O1 127.2(4) . . ?
O2 C1 C2 117.0(4) . . ?
O1 C1 C2 115.8(3) . . ?
N1 C2 C3 121.8(3) . . ?
N1 C2 C1 115.0(3) . . ?
C3 C2 C1 123.2(3) . . ?
C2 C3 C4 118.5(4) . . ?
C5 C4 C3 119.8(4) . . ?
C4 C5 C6 117.9(4) . . ?
N1 C6 C5 122.5(3) . . ?
N1 C6 C7 115.5(3) . . ?
C5 C6 C7 121.9(3) . . ?
O4 C7 O3 126.9(4) . . ?
O4 C7 C6 118.7(4) . . ?
O3 C7 C6 114.5(4) . . ?

_refine_diff_density_max         2.645
_refine_diff_density_min         -2.296
_refine_diff_density_rms         0.190

_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1056461'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'H[Na6(H2O)12Pr2(dipic)6(NO3)]?18H2O '
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H79 N7 Na6 O57 Pr2'
_chemical_formula_weight         2013.88

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   15.4376(16)
_cell_length_b                   15.4376(16)
_cell_length_c                   56.468(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11654(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8680
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      26.07

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_F_000             6120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.391
_shelx_estimated_absorpt_T_min   0.657
_shelx_estimated_absorpt_T_max   0.778
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37596
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_theta_min         1.685
_diffrn_reflns_theta_max         26.083
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2567
_reflns_number_gt                2338
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 All hydrogen atoms of lattice waters and coordinated waters could not be located.
 Maximum difference density  2.81  at  0.7329  0.9496  0.0765  (1.29 A from O8).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0968P)²+450.1884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2567
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0717
_refine_ls_wR_factor_ref         0.1999
_refine_ls_wR_factor_gt          0.1955
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr Pr 0.0000 0.0000 0.33517(2) 0.0154(3) Uani 1 3 d S T P . .
Na1 Na -0.2205(3) 0.0000 0.2500 0.0300(9) Uani 1 2 d S T P . .
Na2 Na -0.2157(3) -0.2157(3) 0.2500 0.0472(12) Uani 1 2 d S T P . .
O1 O -0.0312(3) -0.1279(3) 0.36609(8) 0.0202(9) Uani 1 1 d . . . . .
O2 O -0.1261(4) -0.2733(4) 0.38462(9) 0.0312(12) Uani 1 1 d . . . . .
O3 O -0.1274(3) -0.0168(3) 0.30538(8) 0.0223(10) Uani 1 1 d . . . . .
O4 O -0.2572(4) -0.1143(4) 0.28161(9) 0.0312(12) Uani 1 1 d . . . . .
O5 O -0.0512(9) -0.0941(9) 0.2524(3) 0.041(3) Uani 0.5 1 d . . P . .
O6 O -0.1280(5) 0.1325(5) 0.27773(11) 0.0525(19) Uani 1 1 d . . . . .
O7 O -0.3689(6) 0.0000 0.2500 0.070(4) Uani 1 2 d S T P . .
O8 O -0.3619(7) -0.3619(7) 0.2500 0.074(4) Uani 1 2 d S T P . .
O9 O -0.5298(11) 0.2452(12) 0.2807(3) 0.155(7) Uani 1 1 d . . . . .
O10 O -0.4399(9) 0.1465(8) 0.2938(3) 0.123(5) Uani 1 1 d . . . . .
O11 O -0.4586(6) -0.2142(6) 0.26792(13) 0.062(2) Uani 1 1 d . . . . .
N1 N -0.1717(4) -0.1655(4) 0.33467(9) 0.0176(11) Uani 1 1 d . . . . .
N2 N 0.0000 0.0000 0.2500 0.044(5) Uani 1 6 d S T P . .
C1 C -0.1113(5) -0.2110(5) 0.36907(11) 0.0190(14) Uani 1 1 d . . . . .
C2 C -0.1939(5) -0.2348(5) 0.35117(11) 0.0213(13) Uani 1 1 d . . . . .
C3 C -0.2855(5) -0.3233(5) 0.35172(12) 0.0284(15) Uani 1 1 d . . . . .
H3 H -0.3010 -0.3709 0.3640 0.034 Uiso 1 1 calc R U . . .
C4 C -0.3532(6) -0.3398(6) 0.33386(13) 0.0346(18) Uani 1 1 d . . . . .
H4 H -0.4165 -0.3994 0.3338 0.042 Uiso 1 1 calc R U . . .
C5 C -0.3295(5) -0.2703(6) 0.31613(12) 0.0291(15) Uani 1 1 d . . . . .
H5 H -0.3745 -0.2819 0.3034 0.035 Uiso 1 1 calc R U . . .
C6 C -0.2376(5) -0.1827(5) 0.31743(11) 0.0218(13) Uani 1 1 d . . . . .
C7 C -0.2064(5) -0.0985(5) 0.29964(13) 0.0228(14) 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
Pr O1 2.496(4) 2 ?
Pr O1 2.496(4) 3 ?
Pr O1 2.496(4) . ?
Pr O3 2.501(4) . ?
Pr O3 2.501(4) 2 ?
Pr O3 2.501(4) 3 ?
Pr N1 2.604(5) 2 ?
Pr N1 2.604(6) . ?
Pr N1 2.604(5) 3 ?
Na1 O7 2.291(11) . ?
Na1 O4 2.371(5) . ?
Na1 O4 2.371(5) 4 ?
Na1 O6 2.399(6) . ?
Na1 O6 2.399(6) 4 ?
Na1 O5 2.448(12) 3 ?
Na1 O5 2.448(12) 6 ?
Na1 Na2 3.367(4) . ?
Na1 Na2 3.367(4) 3 ?
Na2 O8 2.258(12) . ?
Na2 O5 2.286(13) 6 ?
Na2 O5 2.286(13) . ?
Na2 O6 2.339(7) 2 ?
Na2 O6 2.339(7) 4 ?
Na2 O4 2.655(6) . ?
Na2 O4 2.655(6) 6 ?
Na2 Na1 3.367(4) 2 ?
O1 C1 1.272(8) . ?
O2 C1 1.237(9) . ?
O3 C7 1.283(9) . ?
O4 C7 1.233(9) . ?
O5 O5 1.18(2) 6 ?
O5 N2 1.267(12) . ?
O5 O5 1.39(2) 5 ?
O5 Na1 2.448(12) 2 ?
O6 Na2 2.339(7) 3 ?
N1 C2 1.328(8) . ?
N1 C6 1.336(8) . ?
N2 O5 1.267(12) 6 ?
N2 O5 1.267(12) 2 ?
N2 O5 1.267(12) 4 ?
N2 O5 1.267(12) 3 ?
N2 O5 1.267(12) 5 ?
C1 C2 1.521(9) . ?
C2 C3 1.391(10) . ?
C3 C4 1.382(11) . ?
C4 C5 1.376(10) . ?
C5 C6 1.390(10) . ?
C6 C7 1.517(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
O1 Pr O1 76.48(16) 2 3 ?
O1 Pr O1 76.48(16) 2 . ?
O1 Pr O1 76.48(16) 3 . ?
O1 Pr O3 151.46(15) 2 . ?
O1 Pr O3 88.58(15) 3 . ?
O1 Pr O3 123.91(15) . . ?
O1 Pr O3 123.91(15) 2 2 ?
O1 Pr O3 151.46(16) 3 2 ?
O1 Pr O3 88.58(15) . 2 ?
O3 Pr O3 79.69(16) . 2 ?
O1 Pr O3 88.58(16) 2 3 ?
O1 Pr O3 123.91(15) 3 3 ?
O1 Pr O3 151.46(15) . 3 ?
O3 Pr O3 79.69(16) . 3 ?
O3 Pr O3 79.69(16) 2 3 ?
O1 Pr N1 62.10(15) 2 2 ?
O1 Pr N1 135.03(15) 3 2 ?
O1 Pr N1 77.49(15) . 2 ?
O3 Pr N1 136.37(15) . 2 ?
O3 Pr N1 61.92(15) 2 2 ?
O3 Pr N1 74.03(15) 3 2 ?
O1 Pr N1 135.03(15) 2 . ?
O1 Pr N1 77.49(15) 3 . ?
O1 Pr N1 62.11(15) . . ?
O3 Pr N1 61.92(15) . . ?
O3 Pr N1 74.03(16) 2 . ?
O3 Pr N1 136.36(15) 3 . ?
N1 Pr N1 119.989(4) 2 . ?
O1 Pr N1 77.49(15) 2 3 ?
O1 Pr N1 62.10(15) 3 3 ?
O1 Pr N1 135.03(15) . 3 ?
O3 Pr N1 74.03(15) . 3 ?
O3 Pr N1 136.37(15) 2 3 ?
O3 Pr N1 61.92(15) 3 3 ?
N1 Pr N1 119.988(5) 2 3 ?
N1 Pr N1 119.987(4) . 3 ?
O7 Na1 O4 97.65(17) . . ?
O7 Na1 O4 97.65(17) . 4 ?
O4 Na1 O4 164.7(3) . 4 ?
O7 Na1 O6 99.7(2) . . ?
O4 Na1 O6 87.8(2) . . ?
O4 Na1 O6 89.6(2) 4 . ?
O7 Na1 O6 99.7(2) . 4 ?
O4 Na1 O6 89.6(2) . 4 ?
O4 Na1 O6 87.8(2) 4 4 ?
O6 Na1 O6 160.6(5) . 4 ?
O7 Na1 O5 163.5(3) . 3 ?
O4 Na1 O5 90.6(4) . 3 ?
O4 Na1 O5 74.6(4) 4 3 ?
O6 Na1 O5 66.2(4) . 3 ?
O6 Na1 O5 94.6(4) 4 3 ?
O7 Na1 O5 163.5(3) . 6 ?
O4 Na1 O5 74.6(4) . 6 ?
O4 Na1 O5 90.6(4) 4 6 ?
O6 Na1 O5 94.6(4) . 6 ?
O6 Na1 O5 66.2(4) 4 6 ?
O5 Na1 O5 33.1(6) 3 6 ?
O7 Na1 Na2 121.10(9) . . ?
O4 Na1 Na2 51.63(15) . . ?
O4 Na1 Na2 118.89(16) 4 . ?
O6 Na1 Na2 123.0(2) . . ?
O6 Na1 Na2 43.99(17) 4 . ?
O5 Na1 Na2 75.2(3) 3 . ?
O5 Na1 Na2 42.7(3) 6 . ?
O7 Na1 Na2 121.10(9) . 3 ?
O4 Na1 Na2 118.89(16) . 3 ?
O4 Na1 Na2 51.64(15) 4 3 ?
O6 Na1 Na2 43.98(17) . 3 ?
O6 Na1 Na2 123.0(2) 4 3 ?
O5 Na1 Na2 42.7(3) 3 3 ?
O5 Na1 Na2 75.2(3) 6 3 ?
Na2 Na1 Na2 117.80(19) . 3 ?
O8 Na2 O5 165.0(3) . 6 ?
O8 Na2 O5 165.0(3) . . ?
O5 Na2 O5 29.9(6) 6 . ?
O8 Na2 O6 97.3(2) . 2 ?
O5 Na2 O6 95.8(4) 6 2 ?
O5 Na2 O6 69.8(4) . 2 ?
O8 Na2 O6 97.3(2) . 4 ?
O5 Na2 O6 69.8(4) 6 4 ?
O5 Na2 O6 95.8(4) . 4 ?
O6 Na2 O6 165.5(5) 2 4 ?
O8 Na2 O4 100.02(16) . . ?
O5 Na2 O4 72.0(4) 6 . ?
O5 Na2 O4 88.5(4) . . ?
O6 Na2 O4 93.1(2) 2 . ?
O6 Na2 O4 84.35(19) 4 . ?
O8 Na2 O4 100.02(16) . 6 ?
O5 Na2 O4 88.4(4) 6 6 ?
O5 Na2 O4 72.0(4) . 6 ?
O6 Na2 O4 84.35(19) 2 6 ?
O6 Na2 O4 93.1(2) 4 6 ?
O4 Na2 O4 160.0(3) . 6 ?
O8 Na2 Na1 118.90(9) . . ?
O5 Na2 Na1 46.6(3) 6 . ?
O5 Na2 Na1 75.7(3) . . ?
O6 Na2 Na1 125.4(2) 2 . ?
O6 Na2 Na1 45.42(17) 4 . ?
O4 Na2 Na1 44.44(12) . . ?
O4 Na2 Na1 123.08(17) 6 . ?
O8 Na2 Na1 118.90(9) . 2 ?
O5 Na2 Na1 75.7(3) 6 2 ?
O5 Na2 Na1 46.6(3) . 2 ?
O6 Na2 Na1 45.42(17) 2 2 ?
O6 Na2 Na1 125.4(2) 4 2 ?
O4 Na2 Na1 123.08(17) . 2 ?
O4 Na2 Na1 44.44(12) 6 2 ?
Na1 Na2 Na1 122.20(19) . 2 ?
C1 O1 Pr 126.6(4) . . ?
C7 O3 Pr 125.7(4) . . ?
C7 O4 Na1 125.7(5) . . ?
C7 O4 Na2 110.7(5) . . ?
Na1 O4 Na2 83.93(19) . . ?
O5 O5 N2 62.3(5) 6 . ?
O5 O5 O5 115.7(9) 6 5 ?
N2 O5 O5 56.6(5) . 5 ?
O5 O5 Na2 75.0(3) 6 . ?
N2 O5 Na2 137.3(7) . . ?
O5 O5 Na2 158.9(11) 5 . ?
O5 O5 Na1 158.7(13) 6 2 ?
N2 O5 Na1 130.1(7) . 2 ?
O5 O5 Na1 73.5(3) 5 2 ?
Na2 O5 Na1 90.6(4) . 2 ?
Na2 O6 Na1 90.6(3) 3 . ?
C2 N1 C6 119.2(6) . . ?
C2 N1 Pr 120.6(4) . . ?
C6 N1 Pr 120.2(4) . . ?
O5 N2 O5 55.5(10) . 6 ?
O5 N2 O5 118.9(2) . 2 ?
O5 N2 O5 174.3(10) 6 2 ?
O5 N2 O5 174.3(10) . 4 ?
O5 N2 O5 118.9(2) 6 4 ?
O5 N2 O5 66.8(10) 2 4 ?
O5 N2 O5 118.9(2) . 3 ?
O5 N2 O5 66.8(10) 6 3 ?
O5 N2 O5 118.9(2) 2 3 ?
O5 N2 O5 55.5(10) 4 3 ?
O5 N2 O5 66.8(10) . 5 ?
O5 N2 O5 118.9(2) 6 5 ?
O5 N2 O5 55.5(10) 2 5 ?
O5 N2 O5 118.9(2) 4 5 ?
O5 N2 O5 174.3(10) 3 5 ?
O2 C1 O1 125.9(6) . . ?
O2 C1 C2 118.5(6) . . ?
O1 C1 C2 115.6(6) . . ?
N1 C2 C3 122.2(6) . . ?
N1 C2 C1 115.1(6) . . ?
C3 C2 C1 122.7(6) . . ?
C4 C3 C2 117.9(7) . . ?
C5 C4 C3 120.4(7) . . ?
C4 C5 C6 117.7(7) . . ?
N1 C6 C5 122.5(6) . . ?
N1 C6 C7 115.4(6) . . ?
C5 C6 C7 122.1(6) . . ?
O4 C7 O3 126.9(6) . . ?
O4 C7 C6 118.6(6) . . ?
O3 C7 C6 114.4(6) . . ?

_refine_diff_density_max         2.813
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.212

_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1056462'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'H[Na6(H2O)12Nd2(dipic)6(NO3)]?18H2O '
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H79 N7 Na6 Nd2 O57'
_chemical_formula_weight         2020.54

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   15.4030(7)
_cell_length_b                   15.4030(7)
_cell_length_c                   56.461(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11600.9(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8392
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      26.04

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_F_000             6132
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.480
_shelx_estimated_absorpt_T_min   0.556
_shelx_estimated_absorpt_T_max   0.737
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.694766
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27595
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         26.066
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.928
_reflns_number_total             2374
_reflns_number_gt                2143
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 All hydrogen atoms of lattice waters and coordinated waters could not be located.
 Maximum difference density 2.09  at  0.7317  0.9515  0.0766  (1.24 A from O8)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0965P)²+377.1892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2374
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.1916
_refine_ls_wR_factor_gt          0.1882
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd Nd 0.0000 0.0000 0.33513(2) 0.0170(3) Uani 1 3 d S T P . .
Na1 Na -0.2209(3) 0.0000 0.2500 0.0313(9) Uani 1 2 d S T P . .
Na2 Na -0.2158(3) -0.2158(3) 0.2500 0.0476(11) Uani 1 2 d S T P . .
O1 O -0.0300(3) -0.1267(3) 0.36605(7) 0.0222(9) Uani 1 1 d . . . . .
O2 O -0.1252(4) -0.2723(4) 0.38459(9) 0.0344(12) Uani 1 1 d . . . . .
O3 O -0.1265(3) -0.0156(3) 0.30542(7) 0.0241(10) Uani 1 1 d . . . . .
O4 O -0.2565(4) -0.1135(4) 0.28164(9) 0.0333(12) Uani 1 1 d . . . . .
O5 O -0.0506(8) -0.0947(8) 0.2523(2) 0.038(3) Uani 0.5 1 d . . P . .
O6 O -0.1278(5) 0.1331(5) 0.27784(11) 0.0513(18) Uani 1 1 d . . . . .
O7 O -0.3695(6) 0.0000 0.2500 0.078(4) Uani 1 2 d S T P . .
O8 O -0.3629(7) -0.3629(7) 0.2500 0.085(4) Uani 1 2 d S T P . .
O9 O -0.2473(19) 0.2267(11) 0.2806(4) 0.258(15) Uani 1 1 d . . . . .
O10 O -0.4404(10) 0.1459(9) 0.2939(3) 0.143(6) Uani 1 1 d . . . . .
O11 O -0.4586(6) -0.2141(7) 0.26782(14) 0.070(2) Uani 1 1 d . . . . .
N1 N -0.1708(4) -0.1644(4) 0.33470(8) 0.0199(11) Uani 1 1 d . . . . .
N2 N 0.0000 0.0000 0.2500 0.041(4) Uani 1 6 d S T P . .
C1 C -0.1104(5) -0.2102(6) 0.36911(12) 0.0224(14) Uani 1 1 d . . . . .
C2 C -0.1930(5) -0.2343(5) 0.35129(11) 0.0245(13) Uani 1 1 d . . . . .
C3 C -0.2845(6) -0.3227(5) 0.35170(12) 0.0308(15) Uani 1 1 d . . . . .
H3 H -0.3001 -0.3706 0.3639 0.037 Uiso 1 1 calc R U . . .
C4 C -0.3526(7) -0.3394(6) 0.33387(12) 0.0366(19) Uani 1 1 d . . . . .
H4 H -0.4160 -0.3992 0.3339 0.044 Uiso 1 1 calc R U . . .
C5 C -0.3292(5) -0.2700(6) 0.31615(11) 0.0316(15) Uani 1 1 d . . . . .
H5 H -0.3743 -0.2816 0.3035 0.038 Uiso 1 1 calc R U . . .
C6 C -0.2368(5) -0.1820(5) 0.31747(11) 0.0236(13) Uani 1 1 d . . . . .
C7 C -0.2053(5) -0.0978(5) 0.29956(13) 0.0251(15) 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
Nd O1 2.484(4) 2 ?
Nd O1 2.484(4) 3 ?
Nd O1 2.484(4) . ?
Nd O3 2.490(4) . ?
Nd O3 2.490(4) 2 ?
Nd O3 2.490(4) 3 ?
Nd N1 2.584(6) . ?
Nd N1 2.584(5) 3 ?
Nd N1 2.584(5) 2 ?
Na1 O7 2.290(11) . ?
Na1 O4 2.364(5) . ?
Na1 O4 2.364(5) 4 ?
Na1 O6 2.406(6) . ?
Na1 O6 2.406(6) 4 ?
Na1 O5 2.432(11) 3 ?
Na1 O5 2.432(11) 6 ?
Na1 Na2 3.363(4) . ?
Na1 Na2 3.363(4) 3 ?
Na2 O8 2.267(13) . ?
Na2 O5 2.285(12) 6 ?
Na2 O5 2.285(12) . ?
Na2 O6 2.337(7) 2 ?
Na2 O6 2.337(7) 4 ?
Na2 O4 2.657(6) . ?
Na2 O4 2.657(6) 6 ?
Na2 Na1 3.363(4) 2 ?
O1 C1 1.275(9) . ?
O2 C1 1.230(9) . ?
O3 C7 1.284(9) . ?
O4 C7 1.230(9) . ?
O5 O5 1.20(2) 6 ?
O5 N2 1.271(11) . ?
O5 O5 1.37(2) 5 ?
O5 Na1 2.432(11) 2 ?
O6 Na2 2.337(7) 3 ?
N1 C2 1.336(8) . ?
N1 C6 1.333(8) . ?
N2 O5 1.271(11) 6 ?
N2 O5 1.271(11) 2 ?
N2 O5 1.271(11) 4 ?
N2 O5 1.271(11) 3 ?
N2 O5 1.271(11) 5 ?
C1 C2 1.515(9) . ?
C2 C3 1.386(10) . ?
C3 C4 1.382(11) . ?
C4 C5 1.374(10) . ?
C5 C6 1.393(10) . ?
C6 C7 1.520(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
O1 Nd O1 76.05(15) 2 3 ?
O1 Nd O1 76.04(15) 2 . ?
O1 Nd O1 76.04(15) 3 . ?
O1 Nd O3 150.91(15) 2 . ?
O1 Nd O3 88.76(15) 3 . ?
O1 Nd O3 124.64(15) . . ?
O1 Nd O3 124.64(15) 2 2 ?
O1 Nd O3 150.91(16) 3 2 ?
O1 Nd O3 88.77(15) . 2 ?
O3 Nd O3 79.58(16) . 2 ?
O1 Nd O3 88.77(15) 2 3 ?
O1 Nd O3 124.64(15) 3 3 ?
O1 Nd O3 150.91(15) . 3 ?
O3 Nd O3 79.58(16) . 3 ?
O3 Nd O3 79.57(16) 2 3 ?
O1 Nd N1 134.78(15) 2 . ?
O1 Nd N1 77.15(15) 3 . ?
O1 Nd N1 62.49(15) . . ?
O3 Nd N1 62.27(15) . . ?
O3 Nd N1 73.83(15) 2 . ?
O3 Nd N1 136.43(15) 3 . ?
O1 Nd N1 77.15(15) 2 3 ?
O1 Nd N1 62.49(15) 3 3 ?
O1 Nd N1 134.77(15) . 3 ?
O3 Nd N1 73.83(15) . 3 ?
O3 Nd N1 136.44(15) 2 3 ?
O3 Nd N1 62.27(15) 3 3 ?
N1 Nd N1 119.991(4) . 3 ?
O1 Nd N1 62.49(15) 2 2 ?
O1 Nd N1 134.77(15) 3 2 ?
O1 Nd N1 77.15(15) . 2 ?
O3 Nd N1 136.44(15) . 2 ?
O3 Nd N1 62.27(15) 2 2 ?
O3 Nd N1 73.83(15) 3 2 ?
N1 Nd N1 119.991(4) . 2 ?
N1 Nd N1 119.991(5) 3 2 ?
O7 Na1 O4 97.89(17) . . ?
O7 Na1 O4 97.89(17) . 4 ?
O4 Na1 O4 164.2(3) . 4 ?
O7 Na1 O6 99.8(2) . . ?
O4 Na1 O6 87.45(19) . . ?
O4 Na1 O6 89.9(2) 4 . ?
O7 Na1 O6 99.8(2) . 4 ?
O4 Na1 O6 89.9(2) . 4 ?
O4 Na1 O6 87.45(19) 4 4 ?
O6 Na1 O6 160.5(4) . 4 ?
O7 Na1 O5 163.6(3) . 3 ?
O4 Na1 O5 90.3(3) . 3 ?
O4 Na1 O5 74.4(3) 4 3 ?
O6 Na1 O5 66.3(3) . 3 ?
O6 Na1 O5 94.4(4) 4 3 ?
O7 Na1 O5 163.6(3) . 6 ?
O4 Na1 O5 74.4(3) . 6 ?
O4 Na1 O5 90.3(3) 4 6 ?
O6 Na1 O5 94.4(4) . 6 ?
O6 Na1 O5 66.3(3) 4 6 ?
O5 Na1 O5 32.8(5) 3 6 ?
O7 Na1 Na2 121.16(9) . . ?
O4 Na1 Na2 51.76(15) . . ?
O4 Na1 Na2 118.48(16) 4 . ?
O6 Na1 Na2 122.9(2) . . ?
O6 Na1 Na2 44.02(17) 4 . ?
O5 Na1 Na2 75.0(3) 3 . ?
O5 Na1 Na2 42.8(3) 6 . ?
O7 Na1 Na2 121.16(9) . 3 ?
O4 Na1 Na2 118.49(16) . 3 ?
O4 Na1 Na2 51.76(15) 4 3 ?
O6 Na1 Na2 44.01(17) . 3 ?
O6 Na1 Na2 122.9(2) 4 3 ?
O5 Na1 Na2 42.8(3) 3 3 ?
O5 Na1 Na2 75.0(3) 6 3 ?
Na2 Na1 Na2 117.68(18) . 3 ?
O8 Na2 O5 164.7(3) . 6 ?
O8 Na2 O5 164.7(3) . . ?
O5 Na2 O5 30.6(5) 6 . ?
O8 Na2 O6 97.1(2) . 2 ?
O5 Na2 O6 96.1(4) 6 2 ?
O5 Na2 O6 69.8(4) . 2 ?
O8 Na2 O6 97.1(2) . 4 ?
O5 Na2 O6 69.8(4) 6 4 ?
O5 Na2 O6 96.1(4) . 4 ?
O6 Na2 O6 165.8(5) 2 4 ?
O8 Na2 O4 100.27(16) . . ?
O5 Na2 O4 71.4(3) 6 . ?
O5 Na2 O4 88.6(3) . . ?
O6 Na2 O4 92.85(19) 2 . ?
O6 Na2 O4 84.62(18) 4 . ?
O8 Na2 O4 100.27(16) . 6 ?
O5 Na2 O4 88.6(3) 6 6 ?
O5 Na2 O4 71.4(3) . 6 ?
O6 Na2 O4 84.62(18) 2 6 ?
O6 Na2 O4 92.85(19) 4 6 ?
O4 Na2 O4 159.5(3) . 6 ?
O8 Na2 Na1 118.84(9) . 2 ?
O5 Na2 Na1 76.1(3) 6 2 ?
O5 Na2 Na1 46.3(3) . 2 ?
O6 Na2 Na1 45.68(16) 2 2 ?
O6 Na2 Na1 125.4(2) 4 2 ?
O4 Na2 Na1 122.91(17) . 2 ?
O4 Na2 Na1 44.34(12) 6 2 ?
O8 Na2 Na1 118.84(9) . . ?
O5 Na2 Na1 46.3(3) 6 . ?
O5 Na2 Na1 76.1(3) . . ?
O6 Na2 Na1 125.4(2) 2 . ?
O6 Na2 Na1 45.68(16) 4 . ?
O4 Na2 Na1 44.33(12) . . ?
O4 Na2 Na1 122.91(17) 6 . ?
Na1 Na2 Na1 122.32(18) 2 . ?
C1 O1 Nd 126.4(4) . . ?
C7 O3 Nd 125.3(4) . . ?
C7 O4 Na1 126.0(5) . . ?
C7 O4 Na2 110.5(5) . . ?
Na1 O4 Na2 83.91(19) . . ?
O5 O5 N2 61.7(5) 6 . ?
O5 O5 O5 116.0(7) 6 5 ?
N2 O5 O5 57.3(5) . 5 ?
O5 O5 Na2 74.7(3) 6 . ?
N2 O5 Na2 136.4(7) . . ?
O5 O5 Na2 159.4(10) 5 . ?
O5 O5 Na1 159.3(11) 6 2 ?
N2 O5 Na1 130.8(7) . 2 ?
O5 O5 Na1 73.6(3) 5 2 ?
Na2 O5 Na1 90.9(4) . 2 ?
Na2 O6 Na1 90.3(3) 3 . ?
C2 N1 C6 119.1(6) . . ?
C2 N1 Nd 120.5(4) . . ?
C6 N1 Nd 120.3(4) . . ?
O5 N2 O5 56.6(10) . 6 ?
O5 N2 O5 119.0(2) . 2 ?
O5 N2 O5 175.5(9) 6 2 ?
O5 N2 O5 175.5(9) . 4 ?
O5 N2 O5 119.0(2) 6 4 ?
O5 N2 O5 65.5(9) 2 4 ?
O5 N2 O5 119.0(2) . 3 ?
O5 N2 O5 65.5(9) 6 3 ?
O5 N2 O5 119.0(2) 2 3 ?
O5 N2 O5 56.6(10) 4 3 ?
O5 N2 O5 65.5(9) . 5 ?
O5 N2 O5 119.0(2) 6 5 ?
O5 N2 O5 56.6(10) 2 5 ?
O5 N2 O5 119.0(2) 4 5 ?
O5 N2 O5 175.5(10) 3 5 ?
O2 C1 O1 126.1(6) . . ?
O2 C1 C2 118.4(6) . . ?
O1 C1 C2 115.5(6) . . ?
N1 C2 C3 121.8(6) . . ?
N1 C2 C1 115.0(6) . . ?
C3 C2 C1 123.1(6) . . ?
C4 C3 C2 118.4(6) . . ?
C5 C4 C3 120.4(7) . . ?
C4 C5 C6 117.4(7) . . ?
N1 C6 C5 122.8(6) . . ?
N1 C6 C7 115.3(6) . . ?
C5 C6 C7 121.9(6) . . ?
O4 C7 O3 127.1(6) . . ?
O4 C7 C6 118.7(6) . . ?
O3 C7 C6 114.2(6) . . ?

_refine_diff_density_max         2.092
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.184

_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1056463'
_audit_update_record             
;
2015-08-05 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Na6(H2O)12Ce2(dipic)6]?21H2O '
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H90 Ce2 N6 Na6 O60'
_chemical_formula_weight         2057.37

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   15.4098(6)
_cell_length_b                   15.4098(6)
_cell_length_c                   55.880(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11491.7(12)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7304
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      25.94

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             6276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.332
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.777
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.787581
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36178
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_theta_min         1.691
_diffrn_reflns_theta_max         25.957
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2508
_reflns_number_gt                2045
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 All hydrogen atoms of lattice waters and coordinated waters could not be located
 Maximum difference density  7.13  at  0.3333  0.6667  0.0037 (0.01 A from CE).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2508
_refine_ls_number_parameters     151
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.1037
_refine_ls_wR_factor_ref         0.4227
_refine_ls_wR_factor_gt          0.3783
_refine_ls_goodness_of_fit_ref   2.066
_refine_ls_restrained_S_all      2.179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce Ce 0.0000 0.0000 0.33727(2) 0.0356(6) Uani 1 3 d S T P . .
Na1 Na -0.2177(4) 0.0000 0.2500 0.0691(14) Uani 1 2 d S T P . .
Na2 Na -0.2083(6) -0.2083(6) 0.2500 0.109(2) Uani 1 2 d S T P . .
O1 O -0.03502(17) -0.13125(18) 0.36808(4) 0.0518(11) Uani 1 1 d G . . . .
O2 O -0.13053(19) -0.2774(2) 0.38598(4) 0.0562(15) Uani 1 1 d G . . . .
O3 O -0.12580(15) -0.01784(14) 0.30632(4) 0.0520(11) Uani 1 1 d G . . . .
O4 O -0.2579(2) -0.11174(16) 0.28261(4) 0.0747(18) Uani 1 1 d G . . . .
O5 O -0.0438(3) 0.0483(3) 0.26125(5) 0.141(11) Uani 0.5 1 d G . P . .
O6 O -0.1261(2) 0.13049(17) 0.27797(6) 0.101(4) Uani 1 1 d G . . . .
O7 O -0.3502(3) 0.0000(3) 0.25000(7) 0.118(4) Uani 1 2 d G T P . .
O8 O -0.3240(5) -0.3239(3) 0.25000(6) 0.157(7) Uani 1 2 d DG T P . .
O9 O -0.2287(3) 0.2229(3) 0.23378(8) 0.083(3) Uani 1 1 d G . . . .
O10 O -0.4108(4) 0.1697(4) 0.27955(11) 0.36(2) Uani 1 1 d G . . . .
O11 O -0.2173(4) 0.2391(2) 0.28978(8) 0.244(11) Uani 1 1 d G . . . .
N1 N -0.17328(14) -0.16777(13) 0.33611(3) 0.0452(12) Uani 1 1 d G . . . .
C1 C -0.11179(17) -0.21334(18) 0.37105(4) 0.038(2) Uani 1 1 d G . . . .
C2 C -0.19466(15) -0.23886(15) 0.35230(4) 0.0476(14) Uani 1 1 d G . . . .
C3 C -0.28189(18) -0.32884(17) 0.35189(6) 0.0598(16) Uani 1 1 d G . . . .
H3 H -0.2958 -0.3782 0.3638 0.072 Uiso 1 1 calc R U . . .
C4 C -0.3497(8) -0.3461(9) 0.33354(10) 0.065(3) Uani 1 1 d . . . . .
H4 H -0.4109 -0.4080 0.3327 0.077 Uiso 1 1 calc R U . . .
C5 C -0.3276(5) -0.2729(5) 0.31658(11) 0.0569(16) Uani 1 1 d . . . . .
H5 H -0.3727 -0.2831 0.3039 0.068 Uiso 1 1 calc R U . . .
C6 C -0.2387(4) -0.1851(4) 0.31866(10) 0.0505(14) Uani 1 1 d . . . . .
C7 C -0.2073(7) -0.1000(5) 0.30126(16) 0.045(2) Uani 1 1 d . . . . .
O12 O -0.3805(6) -0.4671(6) 0.25942(14) 0.124(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
Ce O1 2.501(2) . ?
Ce O1 2.501(2) 2 ?
Ce O1 2.501(2) 3 ?
Ce O3 2.5082(18) . ?
Ce O3 2.508(3) 2 ?
Ce O3 2.508(3) 3 ?
Ce N1 2.629(3) 3 ?
Ce N1 2.629(3) 2 ?
Ce N1 2.6295(19) . ?
Na1 O7 2.041(7) . ?
Na1 O4 2.367(2) 4 ?
Na1 O4 2.367(2) . ?
Na1 O6 2.375(3) . ?
Na1 O6 2.375(3) 4 ?
Na1 O5 2.478(7) . ?
Na1 O5 2.478(8) 4 ?
Na1 Na2 3.285(6) . ?
Na1 Na2 3.285(7) 3 ?
Na2 O8 1.782(10) . ?
Na2 O5 2.296(9) 2 ?
Na2 O5 2.296(9) 4 ?
Na2 O6 2.308(5) 2 ?
Na2 O6 2.308(6) 4 ?
Na2 O4 2.694(3) 6 ?
Na2 O4 2.694(4) . ?
Na2 Na1 3.285(6) 2 ?
O1 C1 1.2373 . ?
O2 C1 1.2116 . ?
O3 C7 1.292(9) . ?
O4 C7 1.259(8) . ?
O5 O5 1.716(5) 5 ?
O5 O5 1.800(8) 4 ?
O5 Na2 2.296(9) 3 ?
O6 Na2 2.308(3) 3 ?
N1 C2 1.3291 . ?
N1 C6 1.330(6) . ?
C1 C2 1.5430 . ?
C2 C3 1.3661 . ?
C3 C4 1.392(8) . ?
C4 C5 1.379(12) . ?
C5 C6 1.366(9) . ?
C6 C7 1.505(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
O1 Ce O1 77.82(10) . 2 ?
O1 Ce O1 77.82(10) . 3 ?
O1 Ce O1 77.81(10) 2 3 ?
O1 Ce O3 122.93(8) . . ?
O1 Ce O3 153.03(7) 2 . ?
O1 Ce O3 89.39(8) 3 . ?
O1 Ce O3 89.4 . 2 ?
O1 Ce O3 122.93(10) 2 2 ?
O1 Ce O3 153.03(8) 3 2 ?
O3 Ce O3 77.70(7) . 2 ?
O1 Ce O3 153.03(9) . 3 ?
O1 Ce O3 89.39(10) 2 3 ?
O1 Ce O3 122.93(8) 3 3 ?
O3 Ce O3 77.70(14) . 3 ?
O3 Ce O3 77.70(10) 2 3 ?
O1 Ce N1 136.25(11) . 3 ?
O1 Ce N1 78.98(9) 2 3 ?
O1 Ce N1 61.28(8) 3 3 ?
O3 Ce N1 74.05(9) . 3 ?
O3 Ce N1 134.26(11) 2 3 ?
O3 Ce N1 61.71(5) 3 3 ?
O1 Ce N1 78.98(9) . 2 ?
O1 Ce N1 61.28(8) 2 2 ?
O1 Ce N1 136.25(15) 3 2 ?
O3 Ce N1 134.27(12) . 2 ?
O3 Ce N1 61.71(9) 2 2 ?
O3 Ce N1 74.05(6) 3 2 ?
N1 Ce N1 119.9 3 2 ?
O1 Ce N1 61.3 . . ?
O1 Ce N1 136.26(9) 2 . ?
O1 Ce N1 78.99(7) 3 . ?
O3 Ce N1 61.7 . . ?
O3 Ce N1 74.05(10) 2 . ?
O3 Ce N1 134.26(12) 3 . ?
N1 Ce N1 119.94(9) 3 . ?
N1 Ce N1 119.94(9) 2 . ?
O7 Na1 O4 95.87(18) . 4 ?
O7 Na1 O4 95.9(2) . . ?
O4 Na1 O4 168.3(4) 4 . ?
O7 Na1 O6 99.8(2) . . ?
O4 Na1 O6 91.56(17) 4 . ?
O4 Na1 O6 86.44(8) . . ?
O7 Na1 O6 99.84(17) . 4 ?
O4 Na1 O6 86.44(8) 4 4 ?
O4 Na1 O6 91.56(14) . 4 ?
O6 Na1 O6 160.3(4) . 4 ?
O7 Na1 O5 158.70(19) . . ?
O4 Na1 O5 86.4(2) 4 . ?
O4 Na1 O5 82.72(16) . . ?
O6 Na1 O5 58.89(11) . . ?
O6 Na1 O5 101.4(3) 4 . ?
O7 Na1 O5 158.71(13) . 4 ?
O4 Na1 O5 82.72(18) 4 4 ?
O4 Na1 O5 86.35(19) . 4 ?
O6 Na1 O5 101.4(3) . 4 ?
O6 Na1 O5 58.9(2) 4 4 ?
O5 Na1 O5 42.6(2) . 4 ?
O7 Na1 Na2 122.18(15) . . ?
O4 Na1 Na2 118.61(16) 4 . ?
O4 Na1 Na2 54.01(12) . . ?
O6 Na1 Na2 121.98(15) . . ?
O6 Na1 Na2 44.63(16) 4 . ?
O5 Na1 Na2 73.96(15) . . ?
O5 Na1 Na2 44.26(15) 4 . ?
O7 Na1 Na2 122.18(15) . 3 ?
O4 Na1 Na2 54.01(17) 4 3 ?
O4 Na1 Na2 118.60(13) . 3 ?
O6 Na1 Na2 44.63(12) . 3 ?
O6 Na1 Na2 121.98(18) 4 3 ?
O5 Na1 Na2 44.26(14) . 3 ?
O5 Na1 Na2 73.96(16) 4 3 ?
Na2 Na1 Na2 115.6(2) . 3 ?
O8 Na2 O5 158.06(13) . 2 ?
O8 Na2 O5 158.1(2) . 4 ?
O5 Na2 O5 43.9(2) 2 4 ?
O8 Na2 O6 95.7(2) . 2 ?
O5 Na2 O6 62.46(15) 2 2 ?
O5 Na2 O6 106.2(3) 4 2 ?
O8 Na2 O6 95.7(3) . 4 ?
O5 Na2 O6 106.2(3) 2 4 ?
O5 Na2 O6 62.46(16) 4 4 ?
O6 Na2 O6 168.7(5) 2 4 ?
O8 Na2 O4 97.7(2) . 6 ?
O5 Na2 O4 82.9(2) 2 6 ?
O5 Na2 O4 82.8(3) 4 6 ?
O6 Na2 O4 85.2(2) 2 6 ?
O6 Na2 O4 93.2(2) 4 6 ?
O8 Na2 O4 97.7(3) . . ?
O5 Na2 O4 82.8(2) 2 . ?
O5 Na2 O4 82.9(2) 4 . ?
O6 Na2 O4 93.25(15) 2 . ?
O6 Na2 O4 85.23(11) 4 . ?
O4 Na2 O4 164.5(4) 6 . ?
O8 Na2 Na1 117.8(2) . 2 ?
O5 Na2 Na1 48.87(15) 2 2 ?
O5 Na2 Na1 78.0(2) 4 2 ?
O6 Na2 Na1 46.29(13) 2 2 ?
O6 Na2 Na1 126.8(2) 4 2 ?
O4 Na2 Na1 45.32(13) 6 2 ?
O4 Na2 Na1 125.28(18) . 2 ?
O8 Na2 Na1 117.8(2) . . ?
O5 Na2 Na1 78.00(19) 2 . ?
O5 Na2 Na1 48.87(16) 4 . ?
O6 Na2 Na1 126.8(2) 2 . ?
O6 Na2 Na1 46.29(13) 4 . ?
O4 Na2 Na1 125.3(2) 6 . ?
O4 Na2 Na1 45.32(9) . . ?
Na1 Na2 Na1 124.4(2) 2 . ?
C1 O1 Ce 128.9 . . ?
C7 O3 Ce 125.3(3) . . ?
C7 O4 Na1 127.9(4) . . ?
C7 O4 Na2 108.2(4) . . ?
Na1 O4 Na2 80.66(19) . . ?
O5 O5 O5 74.4(2) 5 4 ?
O5 O5 Na2 68.06(15) 5 3 ?
O5 O5 Na2 118.34(15) 4 3 ?
O5 O5 Na1 116.9(3) 5 . ?
O5 O5 Na1 68.71(11) 4 . ?
Na2 O5 Na1 86.88(13) 3 . ?
Na2 O6 Na1 89.1(2) 3 . ?
C2 N1 C6 118.9(3) . . ?
C2 N1 Ce 120.3 . . ?
C6 N1 Ce 120.7(3) . . ?
O2 C1 O1 129.9 . . ?
O2 C1 C2 115.5 . . ?
O1 C1 C2 114.6 . . ?
N1 C2 C3 122.5 . . ?
N1 C2 C1 114.8 . . ?
C3 C2 C1 122.6 . . ?
C2 C3 C4 118.0(5) . . ?
C5 C4 C3 119.7(8) . . ?
C6 C5 C4 117.8(7) . . ?
N1 C6 C5 123.1(5) . . ?
N1 C6 C7 114.7(5) . . ?
C5 C6 C7 122.3(6) . . ?
O4 C7 O3 123.4(6) . . ?
O4 C7 C6 120.2(6) . . ?
O3 C7 C6 116.4(6) . . ?

_refine_diff_density_max         7.129
_refine_diff_density_min         -2.198
_refine_diff_density_rms         0.268


#===END

#=====================================================================


_chemical_properties_physical    Efflorescent
