#------------------------------------------------------------------------------
#$Date: 2015-12-09 14:56:32 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171066 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/17/7221758.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_7221758
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 O57 Pr2'
_chemical_formula_weight         2013.88
_chemical_name_systematic        'H[Na6(H2O)12Pr2(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                   15.4376(16)
_cell_length_b                   15.4376(16)
_cell_length_c                   56.468(5)
_cell_measurement_reflns_used    8680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.64
_cell_volume                     11654(2)
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            37596
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.083
_diffrn_reflns_theta_min         1.685
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS absorption correction - V2.10'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             6120
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.813
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0717
_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)+(0.0968P)²+450.1884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.1999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2338
_reflns_number_total             2567
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00843c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7221757--7221760.cif.'
_cod_original_cell_volume        11654(3)
_cod_database_code               7221758
_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   0.657
_shelx_estimated_absorpt_t_max   0.778
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
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 . . .
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'
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 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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
