#------------------------------------------------------------------------------
#$Date: 2015-12-09 13:56:32 +0100 (Wed 09 de Dec de 2015) $
#$Revision: 171066 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/17/7221759.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_7221759
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 N7 Na6 Nd2 O57'
_chemical_formula_weight         2020.54
_chemical_name_systematic        'H[Na6(H2O)12Nd2(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                   15.4030(7)
_cell_length_b                   15.4030(7)
_cell_length_c                   56.461(5)
_cell_measurement_reflns_used    8392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.64
_cell_volume                     11600.9(13)
_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 0.928
_diffrn_measured_fraction_theta_max 0.930
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_laue_measured_fraction_full 0.928
_diffrn_reflns_laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            27595
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.066
_diffrn_reflns_theta_min         1.688
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.694766
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             6132
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.220
_refine_diff_density_max         2.092
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0965P)²+377.1892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2143
_reflns_number_total             2374
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00843c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7221757--7221760.cif.'
_cod_original_cell_volume        11600.9(15)
_cod_database_code               7221759
_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   0.556
_shelx_estimated_absorpt_t_max   0.737
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
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 . . .
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'
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 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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
