#------------------------------------------------------------------------------
#$Date: 2022-03-08 01:52:40 +0200 (Tue, 08 Mar 2022) $
#$Revision: 273516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/96/7709683.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_7709683
loop_
_publ_author_name
'Pyrch, Mikaela M.'
'Augustine, Logan J.'
'Williams, James M.'
'Mason, Sara E.'
'Forbes, Tori Z.'
_publ_section_title
;
 Use of vibrational spectroscopy to identify the formation of
 neptunyl--neptunyl interactions: a paired density functional theory and
 Raman spectroscopy study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00200K
_journal_year                    2022
_chemical_formula_sum            'N6 Na Np3 O25'
_chemical_formula_weight         1218.05
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   8.1842(5)
_cell_length_b                   8.1842(5)
_cell_length_c                   11.2773(8)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.895
_cell_measurement_theta_min      5.751
_cell_volume                     654.17(7)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'Phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0076
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20562
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.157
_diffrn_reflns_theta_min         2.874
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    11.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.092
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.5905
_refine_diff_density_max         0.647
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0132
_refine_ls_R_factor_gt           0.0132
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0248P)²+0.4967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                345
_reflns_number_total             345
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00200k1.cif
_cod_data_source_block           p6onm_b_pl_sq
_cod_original_cell_volume        654.17(9)
_cod_database_code               7709683
_shelx_shelxl_version_number     2017/1
_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'
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 . .
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'
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_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_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 . . . ?
