data_publication_text
_publ_requested_journal          'Dalton Trans.'
_publ_contact_author_name        'Tori Z. Forbes'
_publ_contact_author_address     
;W374 Chemistry Building
University of Iowa
Iowa City, IA 52242
;
_publ_contact_author_email       tori-forbes@uiowa.edu
_publ_contact_author_phone       3193841320
loop_
_publ_author_name
_publ_author_address
'Tori Z. Forbes'
;W374 Chemistry Building
University of Iowa
Iowa City, IA 52242
;
'Mikaela M. Pyrch'
;W374 Chemistry Building
University of Iowa
Iowa City, IA 52242
;

data_p6onm_b_pl_sq
 
_audit_creation_method            'SHELXL-2017/1'
_shelx_SHELXL_version_number      '2017/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'N6 Na Np3 O25' 
_chemical_formula_weight          1218.05

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'Np'  'Np' -11.4937   4.1493
 '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       hexagonal
_space_group_IT_number            191
_space_group_name_H-M_alt         'P 6/m m m'
_space_group_name_Hall            '-P 6 2'
 
_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'
 'x-y, x, z'
 '-y, x-y, z'
 '-x, -y, z'
 '-x+y, -x, z'
 'y, -x+y, z'
 '-y, -x, -z'
 'x-y, -y, -z'
 'x, x-y, -z'
 'y, x, -z'
 '-x+y, y, -z'
 '-x, -x+y, -z'
 '-x, -y, -z'
 '-x+y, -x, -z'
 'y, -x+y, -z'
 'x, y, -z'
 'x-y, x, -z'
 '-y, x-y, -z'
 'y, x, z'
 '-x+y, y, z'
 '-x, -x+y, z'
 '-y, -x, z'
 'x-y, -y, z'
 'x, x-y, z'
 
_cell_length_a                    8.1842(5)
_cell_length_b                    8.1842(5)
_cell_length_c                    11.2773(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      654.17(9)
_cell_formula_units_Z             1
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9970
_cell_measurement_theta_min       5.751
_cell_measurement_theta_max       50.895
 
_exptl_crystal_description        'plate'
_exptl_crystal_colour             'green'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     3.092          
_exptl_crystal_F_000              532
_exptl_transmission_factor_min    0.5905
_exptl_transmission_factor_max    0.7455
_exptl_crystal_size_max           0.45
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.3
_exptl_absorpt_coefficient_mu     11.946
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'sealed tube'
_diffrn_measurement_device_type   'Bruker D8 Quest'
_diffrn_measurement_method        'Phi and omega scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             20562
_diffrn_reflns_av_unetI/netI      0.0076
_diffrn_reflns_av_R_equivalents   0.0319
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          2.874
_diffrn_reflns_theta_max          27.157
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.989
_diffrn_measured_fraction_theta_full  0.986
_diffrn_reflns_Laue_measured_fraction_max    0.989
_diffrn_reflns_Laue_measured_fraction_full   0.986
_diffrn_reflns_point_group_measured_fraction_max   0.989
_diffrn_reflns_point_group_measured_fraction_full  0.986
_reflns_number_total              345
_reflns_number_gt                 345
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           
;
 Squeeze for disordered lattice solvent and diffuse electon 
density was used. total of 57 electons were found and removed
assigned to 2 Na atoms and disordered water
Specl A.L (2015) Acta Cryst C71 9-18
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0248P)²+0.4967P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          345
_refine_ls_number_parameters      32
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0132
_refine_ls_R_factor_gt            0.0132
_refine_ls_wR_factor_ref          0.0361
_refine_ls_wR_factor_gt           0.0361
_refine_ls_goodness_of_fit_ref    1.198
_refine_ls_restrained_S_all       1.198
_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
Np1 Np 0.500000 0.500000 0.500000 0.01591(12) Uani 1 8 d S T P . .
Na1 Na 0.000000 0.000000 0.500000 0.0424(16) Uani 1 24 d S T P . .
O1 O 0.4201(6) 0.1752(5) 0.500000 0.0269(13) Uani 0.5 2 d S T P . .
O2 O 0.500000 0.500000 0.1287(5) 0.097(4) Uani 1 4 d S T P . .
O3 O 0.3492(6) 0.4399(6) 0.2953(3) 0.0389(9) Uani 0.5 1 d . . P . .
O4 O 0.000000 0.000000 0.3240(19) 0.132(13) Uani 0.5 12 d S T P . .
N1 N 0.500000 0.500000 0.2381(6) 0.0489(18) Uani 1 4 d S T P . .
 
 
_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
Np1 O1 1.850(4) 21_665 ?
Np1 O1 1.850(4) 9_556 ?
Np1 O1 1.850(4) 14_666 ?
Np1 O1 1.850(4) 2 ?
Np1 O1 2.399(4) . ?
Np1 O1 2.399(4) 13_666 ?
Np1 O1 2.399(4) 19 ?
Np1 O1 2.399(4) 7_666 ?
Np1 O3 2.547(4) 19 ?
Np1 O3 2.547(4) 7_666 ?
Np1 O3 2.547(4) 13_666 ?
Np1 O3 2.547(4) 22_665 ?
Na1 O4 1.99(2) 13_556 ?
Na1 O4 1.99(2) . ?
Na1 O1 2.991(4) 21 ?
Na1 O1 2.991(4) 9_556 ?
Na1 O1 2.991(4) 14_556 ?
Na1 O1 2.991(4) 2 ?
Na1 O1 2.991(4) 19 ?
Na1 O1 2.991(4) 7_556 ?
Na1 O1 2.991(4) 13_556 ?
Na1 O1 2.991(4) 20 ?
Na1 O1 2.991(4) 8_556 ?
Na1 O1 2.991(4) 15_556 ?
O1 O1 0.570(7) 9_556 ?
O2 N1 1.234(9) . ?
O3 N1 1.255(5) . ?
O3 O3 1.286(8) 19 ?
O3 O3 1.726(9) 22_665 ?
 
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 Np1 O1 180.0 21_665 9_556 ?
O1 Np1 O1 84.3(3) 21_665 14_666 ?
O1 Np1 O1 95.7(3) 9_556 14_666 ?
O1 Np1 O1 95.7(3) 21_665 2 ?
O1 Np1 O1 84.3(3) 9_556 2 ?
O1 Np1 O1 180.0 14_666 2 ?
O1 Np1 O1 175.83(6) 21_665 . ?
O1 Np1 O1 4.17(6) 9_556 . ?
O1 Np1 O1 91.5(2) 14_666 . ?
O1 Np1 O1 88.5(2) 2 . ?
O1 Np1 O1 4.17(6) 21_665 13_666 ?
O1 Np1 O1 175.83(6) 9_556 13_666 ?
O1 Np1 O1 88.5(2) 14_666 13_666 ?
O1 Np1 O1 91.5(2) 2 13_666 ?
O1 Np1 O1 180.0 . 13_666 ?
O1 Np1 O1 91.5(2) 21_665 19 ?
O1 Np1 O1 88.5(2) 9_556 19 ?
O1 Np1 O1 175.83(6) 14_666 19 ?
O1 Np1 O1 4.17(6) 2 19 ?
O1 Np1 O1 92.7(2) . 19 ?
O1 Np1 O1 87.3(2) 13_666 19 ?
O1 Np1 O1 88.5(2) 21_665 7_666 ?
O1 Np1 O1 91.5(2) 9_556 7_666 ?
O1 Np1 O1 4.17(6) 14_666 7_666 ?
O1 Np1 O1 175.83(6) 2 7_666 ?
O1 Np1 O1 87.3(2) . 7_666 ?
O1 Np1 O1 92.7(2) 13_666 7_666 ?
O1 Np1 O1 180.0 19 7_666 ?
O1 Np1 O3 114.87(10) 21_665 19 ?
O1 Np1 O3 65.13(10) 9_556 19 ?
O1 Np1 O3 94.69(11) 14_666 19 ?
O1 Np1 O3 85.31(11) 2 19 ?
O1 Np1 O3 65.38(10) . 19 ?
O1 Np1 O3 114.62(10) 13_666 19 ?
O1 Np1 O3 87.06(10) 19 19 ?
O1 Np1 O3 92.94(10) 7_666 19 ?
O1 Np1 O3 65.13(10) 21_665 7_666 ?
O1 Np1 O3 114.87(10) 9_556 7_666 ?
O1 Np1 O3 85.31(11) 14_666 7_666 ?
O1 Np1 O3 94.69(11) 2 7_666 ?
O1 Np1 O3 114.62(10) . 7_666 ?
O1 Np1 O3 65.38(10) 13_666 7_666 ?
O1 Np1 O3 92.94(10) 19 7_666 ?
O1 Np1 O3 87.06(10) 7_666 7_666 ?
O3 Np1 O3 180.0 19 7_666 ?
O1 Np1 O3 85.31(11) 21_665 13_666 ?
O1 Np1 O3 94.69(11) 9_556 13_666 ?
O1 Np1 O3 65.13(10) 14_666 13_666 ?
O1 Np1 O3 114.87(10) 2 13_666 ?
O1 Np1 O3 92.94(10) . 13_666 ?
O1 Np1 O3 87.06(10) 13_666 13_666 ?
O1 Np1 O3 114.62(10) 19 13_666 ?
O1 Np1 O3 65.38(10) 7_666 13_666 ?
O3 Np1 O3 150.76(18) 19 13_666 ?
O3 Np1 O3 29.24(18) 7_666 13_666 ?
O1 Np1 O3 65.13(10) 21_665 22_665 ?
O1 Np1 O3 114.87(10) 9_556 22_665 ?
O1 Np1 O3 85.31(11) 14_666 22_665 ?
O1 Np1 O3 94.69(11) 2 22_665 ?
O1 Np1 O3 114.62(10) . 22_665 ?
O1 Np1 O3 65.38(10) 13_666 22_665 ?
O1 Np1 O3 92.94(10) 19 22_665 ?
O1 Np1 O3 87.06(10) 7_666 22_665 ?
O3 Np1 O3 49.99(19) 19 22_665 ?
O3 Np1 O3 130.01(19) 7_666 22_665 ?
O3 Np1 O3 140.4(2) 13_666 22_665 ?
O4 Na1 O4 180.0 13_556 . ?
O4 Na1 O1 90.000(2) 13_556 21 ?
O4 Na1 O1 90.000(2) . 21 ?
O4 Na1 O1 90.000(2) 13_556 9_556 ?
O4 Na1 O1 90.000(2) . 9_556 ?
O1 Na1 O1 180.0 21 9_556 ?
O4 Na1 O1 90.000(2) 13_556 14_556 ?
O4 Na1 O1 90.000(2) . 14_556 ?
O1 Na1 O1 49.06(13) 21 14_556 ?
O1 Na1 O1 130.94(13) 9_556 14_556 ?
O4 Na1 O1 90.000(2) 13_556 2 ?
O4 Na1 O1 90.000(2) . 2 ?
O1 Na1 O1 130.94(13) 21 2 ?
O1 Na1 O1 49.06(13) 9_556 2 ?
O1 Na1 O1 180.00(12) 14_556 2 ?
O4 Na1 O1 90.000(2) 13_556 19 ?
O4 Na1 O1 90.000(2) . 19 ?
O1 Na1 O1 120.0 21 19 ?
O1 Na1 O1 60.000(1) 9_556 19 ?
O1 Na1 O1 169.06(13) 14_556 19 ?
O1 Na1 O1 10.94(13) 2 19 ?
O4 Na1 O1 90.000(2) 13_556 7_556 ?
O4 Na1 O1 90.000(2) . 7_556 ?
O1 Na1 O1 60.0 21 7_556 ?
O1 Na1 O1 120.0 9_556 7_556 ?
O1 Na1 O1 10.94(13) 14_556 7_556 ?
O1 Na1 O1 169.06(14) 2 7_556 ?
O1 Na1 O1 180.0 19 7_556 ?
O4 Na1 O1 90.000(2) 13_556 13_556 ?
O4 Na1 O1 90.000(2) . 13_556 ?
O1 Na1 O1 10.94(13) 21 13_556 ?
O1 Na1 O1 169.06(14) 9_556 13_556 ?
O1 Na1 O1 60.0 14_556 13_556 ?
O1 Na1 O1 120.0 2 13_556 ?
O1 Na1 O1 109.06(13) 19 13_556 ?
O1 Na1 O1 70.94(14) 7_556 13_556 ?
O4 Na1 O1 90.0 13_556 20 ?
O4 Na1 O1 90.0 . 20 ?
O1 Na1 O1 60.0 21 20 ?
O1 Na1 O1 120.000(1) 9_556 20 ?
O1 Na1 O1 109.06(14) 14_556 20 ?
O1 Na1 O1 70.94(14) 2 20 ?
O1 Na1 O1 60.0 19 20 ?
O1 Na1 O1 120.000(1) 7_556 20 ?
O1 Na1 O1 49.06(14) 13_556 20 ?
O4 Na1 O1 90.0 13_556 8_556 ?
O4 Na1 O1 90.0 . 8_556 ?
O1 Na1 O1 120.000(1) 21 8_556 ?
O1 Na1 O1 60.0 9_556 8_556 ?
O1 Na1 O1 70.94(14) 14_556 8_556 ?
O1 Na1 O1 109.06(14) 2 8_556 ?
O1 Na1 O1 120.000(1) 19 8_556 ?
O1 Na1 O1 60.0 7_556 8_556 ?
O1 Na1 O1 130.94(14) 13_556 8_556 ?
O1 Na1 O1 180.0 20 8_556 ?
O4 Na1 O1 90.0 13_556 15_556 ?
O4 Na1 O1 90.0 . 15_556 ?
O1 Na1 O1 109.06(14) 21 15_556 ?
O1 Na1 O1 70.94(14) 9_556 15_556 ?
O1 Na1 O1 60.0 14_556 15_556 ?
O1 Na1 O1 120.000(1) 2 15_556 ?
O1 Na1 O1 130.94(14) 19 15_556 ?
O1 Na1 O1 49.06(13) 7_556 15_556 ?
O1 Na1 O1 120.000(1) 13_556 15_556 ?
O1 Na1 O1 169.06(14) 20 15_556 ?
O1 Na1 O1 10.94(14) 8_556 15_556 ?
O1 O1 Np1 162.17(13) 9_556 3_655 ?
O1 O1 Np1 13.66(11) 9_556 . ?
Np1 O1 Np1 148.5(2) 3_655 . ?
O1 O1 Na1 84.53(7) 9_556 . ?
Np1 O1 Na1 113.30(18) 3_655 . ?
Np1 O1 Na1 98.19(12) . . ?
N1 O3 O3 59.2(2) . 19 ?
N1 O3 O3 46.6(2) . 22_665 ?
O3 O3 O3 90.000(2) 19 22_665 ?
N1 O3 Np1 96.0(3) . . ?
O3 O3 Np1 75.38(9) 19 . ?
O3 O3 Np1 70.19(10) 22_665 . ?
O2 N1 O3 121.0(3) . . ?
O2 N1 O3 121.0(3) . 22_665 ?
O3 N1 O3 86.9(5) . 22_665 ?
O2 N1 O3 121.0(3) . 4_665 ?
O3 N1 O3 118.1(6) . 4_665 ?
O3 N1 O3 61.6(4) 22_665 4_665 ?
O2 N1 O3 121.0(3) . 19 ?
O3 N1 O3 61.6(4) . 19 ?
O3 N1 O3 118.1(6) 22_665 19 ?
O3 N1 O3 86.9(5) 4_665 19 ?
O2 N1 Np1 180.0 . . ?
O3 N1 Np1 59.0(3) . . ?
O3 N1 Np1 59.0(3) 22_665 . ?
O3 N1 Np1 59.0(3) 4_665 . ?
O3 N1 Np1 59.0(3) 19 . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
O3 O3 N1 O2 111.0(2) 19 . . . ?
O3 O3 N1 O2 -124.6(3) 22_665 . . . ?
Np1 O3 N1 O2 180.000(1) . . . . ?
O3 O3 N1 O3 -124.4(4) 19 . . 22_665 ?
Np1 O3 N1 O3 -55.4(3) . . . 22_665 ?
O3 O3 N1 O3 -69.0(2) 19 . . 4_665 ?
O3 O3 N1 O3 55.4(3) 22_665 . . 4_665 ?
Np1 O3 N1 O3 0.001(1) . . . 4_665 ?
O3 O3 N1 O3 124.4(4) 22_665 . . 19 ?
Np1 O3 N1 O3 69.0(2) . . . 19 ?
O3 O3 N1 Np1 -69.0(2) 19 . . . ?
O3 O3 N1 Np1 55.4(3) 22_665 . . . ?
 
_refine_diff_density_max    0.647
_refine_diff_density_min   -1.449
_refine_diff_density_rms    0.132




