#------------------------------------------------------------------------------
#$Date: 2015-12-09 14:56:32 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171066 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/17/7221757.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7221757
loop_
_publ_author_name
'Elahi, Syed Meheboob'
'Rajasekharan, M. V.'
_publ_section_title
;
 Spherical octanuclear clusters in a Na--Ln--dipic system -- encapsulation
 of a nitrate ion and incorporation of water nonamers and dodecamers
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7191
_journal_paper_doi               10.1039/C5CE00843C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C42 H79 Ce2 N7 Na6 O57'
_chemical_formula_weight         2012.30
_chemical_name_systematic        'H[Na6(H2O)12Ce2(dipic)6(NO3)]?18H2O '
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.455(5)
_cell_length_b                   15.455(5)
_cell_length_c                   56.103(4)
_cell_measurement_reflns_used    8157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.64
_cell_volume                     11605(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            42301
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.200
_diffrn_reflns_theta_min         1.686
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             6108
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.645
_refine_diff_density_min         -2.296
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1119P)²+137.1359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2881
_reflns_number_total             3183
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00843c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7221757--7221760.cif.'
_cod_original_cell_volume        11605(8)
_cod_database_code               7221757
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.583
_shelx_estimated_absorpt_t_max   0.779
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'
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
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 . . .
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
