#------------------------------------------------------------------------------
#$Date: 2020-10-06 14:12:18 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257967 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/99/7239910.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_7239910
loop_
_publ_author_name
'Takao, Koichiro'
'März, Juliane'
'Matsuoka, Moe'
'Mashita, Takanori'
'Kazama, Hiroyuki'
'Tsushima, Satoru'
_publ_section_title
;
 Crystallization of colourless hexanitratoneptunate(iv) with anhydrous H+
 countercations trapped in a hydrogen bonded polymer with diamide linkers
;
_journal_issue                   10
_journal_name_full               'RSC Advances'
_journal_page_first              6082
_journal_page_last               6087
_journal_paper_doi               10.1039/C9RA10090C
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C28 H46 N10 Np O22'
_chemical_formula_sum            'C28 H46 N10 Np O22'
_chemical_formula_weight         1113.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-27 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.175(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8264(10)
_cell_length_b                   10.7164(11)
_cell_length_c                   19.517(2)
_cell_measurement_reflns_used    2678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3237
_cell_measurement_theta_min      2.1573
_cell_volume                     2001.1(4)
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'generic φ and ο scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53411
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.730
_diffrn_reflns_theta_min         2.182
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_T_max  0.6836
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.975
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0188
_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)+(0.0387P)²+0.1923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3596
_reflns_number_total             4249
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ra10090c2.cif
_cod_data_source_block           mo_kt_l2np_0m_a
_cod_depositor_comments
'Adding full bibliography for 7239909--7239910.cif.'
_cod_database_code               7239910
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C4(H4A,H4B), C14(H14A,H14B), C6(H6A,
 H6B), C12(H12A,H12B), C13(H13A,H13B), C2(H2A,H2B), C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Np1 Np 1.500000 1.000000 0.500000 0.00972(7) Uani 1 2 d S T P
O7 O 1.3046(2) 1.11046(17) 0.41681(10) 0.0175(4) Uani 1 1 d . . .
O9 O 1.1479(2) 1.22774(19) 0.44900(11) 0.0246(5) Uani 1 1 d . . .
O4 O 1.42122(19) 0.87544(18) 0.38875(10) 0.0170(4) Uani 1 1 d . . .
O6 O 1.5119(2) 0.8983(2) 0.29716(10) 0.0251(5) Uani 1 1 d . . .
O1 O 1.5588(2) 1.22231(17) 0.47883(10) 0.0178(4) Uani 1 1 d . . .
N3 N 1.2529(2) 1.1648(2) 0.46359(12) 0.0152(5) Uani 1 1 d . . .
N1 N 1.6919(3) 1.2084(2) 0.49348(12) 0.0168(5) Uani 1 1 d . . .
O5 O 1.5516(2) 1.0349(2) 0.38268(11) 0.0164(4) Uani 1 1 d . . .
O3 O 1.7715(2) 1.2938(2) 0.49168(11) 0.0277(5) Uani 1 1 d . . .
N2 N 1.4956(2) 0.9352(2) 0.35362(12) 0.0161(5) Uani 1 1 d . . .
O10 O 1.68170(19) 1.29844(17) 0.31019(10) 0.0169(4) Uani 1 1 d . . .
O11 O 1.6426(2) 1.68384(18) 0.23225(10) 0.0190(4) Uani 1 1 d . . .
H11 H 1.731(5) 1.745(4) 0.210(3) 0.096(17) Uiso 1 1 d . . .
N4 N 1.6446(3) 1.4797(2) 0.36190(14) 0.0146(5) Uani 1 1 d . . .
N5 N 1.4943(3) 1.5208(2) 0.21984(14) 0.0117(5) Uani 1 1 d . . .
C11 C 1.5892(3) 1.5873(2) 0.19887(14) 0.0122(5) Uani 1 1 d . . .
C9 C 1.2746(3) 1.5487(3) 0.25846(15) 0.0162(6) Uani 1 1 d . . .
H9A H 1.245206 1.463370 0.241984 0.019 Uiso 1 1 calc R . .
H9B H 1.239342 1.607274 0.219222 0.019 Uiso 1 1 calc R . .
C1 C 1.7279(3) 1.3965(2) 0.34430(14) 0.0133(6) Uani 1 1 d . . .
C10 C 1.4336(3) 1.5550(3) 0.27904(13) 0.0105(5) Uani 1 1 d . . .
H10 H 1.461188 1.642987 0.292656 0.013 Uiso 1 1 calc R . .
C8 C 1.2114(3) 1.5820(3) 0.32080(15) 0.0184(6) Uani 1 1 d . . .
H8A H 1.235020 1.669427 0.335206 0.022 Uiso 1 1 calc R . .
H8B H 1.108308 1.574929 0.306654 0.022 Uiso 1 1 calc R . .
C5 C 1.4916(3) 1.4704(3) 0.34282(15) 0.0123(6) Uani 1 1 d . . .
H5 H 1.466102 1.382224 0.328827 0.015 Uiso 1 1 calc R . .
C7 C 1.2671(4) 1.4954(2) 0.3822(2) 0.0230(8) Uani 1 1 d . . .
H7A H 1.239254 1.408502 0.368571 0.028 Uiso 1 1 calc R . .
H7B H 1.226246 1.518434 0.422411 0.028 Uiso 1 1 calc R . .
C4 C 1.7220(3) 1.5839(3) 0.40277(16) 0.0221(6) Uani 1 1 d . . .
H4A H 1.718461 1.578466 0.452974 0.027 Uiso 1 1 calc R . .
H4B H 1.683759 1.665461 0.383756 0.027 Uiso 1 1 calc R . .
C14 C 1.4496(3) 1.4110(3) 0.17395(14) 0.0156(6) Uani 1 1 d . . .
H14A H 1.355856 1.424278 0.142996 0.019 Uiso 1 1 calc R . .
H14B H 1.447978 1.334495 0.202156 0.019 Uiso 1 1 calc R . .
C6 C 1.4260(4) 1.5040(2) 0.40433(18) 0.0204(7) Uani 1 1 d . . .
H6A H 1.460953 1.446214 0.444035 0.024 Uiso 1 1 calc R . .
H6B H 1.453557 1.589792 0.420484 0.024 Uiso 1 1 calc R . .
C12 C 1.6208(3) 1.5366(3) 0.13310(16) 0.0183(6) Uani 1 1 d . . .
H12A H 1.722564 1.536088 0.135706 0.022 Uiso 1 1 calc R . .
H12B H 1.573023 1.585241 0.091402 0.022 Uiso 1 1 calc R . .
C13 C 1.5621(3) 1.4028(3) 0.13103(16) 0.0204(6) Uani 1 1 d . . .
H13A H 1.520947 1.376567 0.082054 0.025 Uiso 1 1 calc R . .
H13B H 1.636200 1.342895 0.152578 0.025 Uiso 1 1 calc R . .
C2 C 1.8787(3) 1.4326(3) 0.36921(16) 0.0184(6) Uani 1 1 d . . .
H2A H 1.928329 1.427565 0.330488 0.022 Uiso 1 1 calc R . .
H2B H 1.926711 1.378403 0.408396 0.022 Uiso 1 1 calc R . .
C3 C 1.8709(4) 1.5658(4) 0.3936(2) 0.0451(11) Uani 1 1 d . . .
H3A H 1.890997 1.624788 0.358104 0.054 Uiso 1 1 calc R . .
H3B H 1.939302 1.579897 0.438662 0.054 Uiso 1 1 calc R . .
O2 O 1.7344(2) 1.09750(18) 0.50967(10) 0.0157(4) Uani 1 1 d . . .
O8 O 1.3206(2) 1.14732(19) 0.52660(10) 0.0167(4) 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'
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
O7 Np1 O7 180.00(7) . 3_876
O7 Np1 O4 110.33(6) 3_876 .
O7 Np1 O4 110.34(6) . 3_876
O7 Np1 O4 69.66(6) . .
O7 Np1 O4 69.66(6) 3_876 3_876
O4 Np1 O4 180.0 . 3_876
O1 Np1 O7 67.45(6) . .
O1 Np1 O7 112.55(6) 3_876 .
O1 Np1 O7 112.55(6) . 3_876
O1 Np1 O7 67.44(6) 3_876 3_876
O1 Np1 O4 113.52(6) . .
O1 Np1 O4 66.49(6) . 3_876
O1 Np1 O4 113.51(6) 3_876 3_876
O1 Np1 O4 66.48(6) 3_876 .
O1 Np1 O1 180.0 . 3_876
O5 Np1 O7 112.35(7) . 3_876
O5 Np1 O7 112.35(7) 3_876 .
O5 Np1 O7 67.65(7) . .
O5 Np1 O7 67.65(7) 3_876 3_876
O5 Np1 O4 51.07(7) . .
O5 Np1 O4 51.07(7) 3_876 3_876
O5 Np1 O4 128.94(7) . 3_876
O5 Np1 O4 128.93(7) 3_876 .
O5 Np1 O1 66.55(7) 3_876 3_876
O5 Np1 O1 66.55(7) . .
O5 Np1 O1 113.45(7) 3_876 .
O5 Np1 O1 113.45(7) . 3_876
O5 Np1 O5 180.00(14) . 3_876
O5 Np1 O2 68.16(7) . .
O5 Np1 O2 111.84(7) 3_876 .
O5 Np1 O2 68.16(7) 3_876 3_876
O5 Np1 O2 111.84(7) . 3_876
O5 Np1 O8 113.40(7) . .
O5 Np1 O8 66.60(7) . 3_876
O5 Np1 O8 66.60(7) 3_876 .
O5 Np1 O8 113.40(7) 3_876 3_876
O2 Np1 O7 114.07(6) 3_876 3_876
O2 Np1 O7 114.07(6) . .
O2 Np1 O7 65.93(6) 3_876 .
O2 Np1 O7 65.93(6) . 3_876
O2 Np1 O4 112.61(6) . .
O2 Np1 O4 67.39(6) . 3_876
O2 Np1 O4 67.39(6) 3_876 .
O2 Np1 O4 112.60(6) 3_876 3_876
O2 Np1 O1 51.08(6) . .
O2 Np1 O1 128.92(6) . 3_876
O2 Np1 O1 128.92(6) 3_876 .
O2 Np1 O1 51.08(6) 3_876 3_876
O2 Np1 O2 180.0 . 3_876
O2 Np1 O8 113.63(6) . .
O2 Np1 O8 113.63(6) 3_876 3_876
O2 Np1 O8 66.37(6) 3_876 .
O2 Np1 O8 66.37(6) . 3_876
O8 Np1 O7 129.29(6) . 3_876
O8 Np1 O7 129.29(6) 3_876 .
O8 Np1 O7 50.71(6) 3_876 3_876
O8 Np1 O7 50.72(6) . .
O8 Np1 O4 114.84(6) 3_876 3_876
O8 Np1 O4 65.16(6) 3_876 .
O8 Np1 O4 114.84(6) . .
O8 Np1 O4 65.16(6) . 3_876
O8 Np1 O1 68.60(6) . .
O8 Np1 O1 111.40(6) 3_876 .
O8 Np1 O1 111.40(6) . 3_876
O8 Np1 O1 68.60(6) 3_876 3_876
O8 Np1 O8 180.00(6) 3_876 .
N3 O7 Np1 97.03(15) . .
N2 O4 Np1 95.50(15) . .
N1 O1 Np1 96.57(15) . .
O7 N3 Np1 57.48(12) . .
O9 N3 Np1 177.07(19) . .
O9 N3 O7 122.7(2) . .
O9 N3 O8 122.6(2) . .
O8 N3 Np1 57.28(12) . .
O8 N3 O7 114.7(2) . .
O1 N1 Np1 57.79(12) . .
O3 N1 Np1 179.2(2) . .
O3 N1 O1 122.6(2) . .
O3 N1 O2 122.4(2) . .
O2 N1 Np1 57.25(13) . .
O2 N1 O1 115.0(2) . .
N2 O5 Np1 97.21(15) . .
O4 N2 Np1 58.70(12) . .
O6 N2 Np1 170.17(18) . .
O6 N2 O4 122.1(2) . .
O6 N2 O5 122.9(2) . .
O5 N2 Np1 57.23(13) . .
O5 N2 O4 115.0(2) . .
C1 N4 C5 123.6(2) . .
C1 N4 C4 112.4(3) . .
C5 N4 C4 124.0(2) . .
C11 N5 C10 123.9(2) . .
C11 N5 C14 112.1(2) . .
C10 N5 C14 123.9(2) . .
O11 C11 N5 121.5(2) . .
O11 C11 C12 126.6(2) . .
N5 C11 C12 111.9(2) . .
C10 C9 C8 111.0(2) . .
O10 C1 N4 122.1(3) . .
O10 C1 C2 126.2(2) . .
N4 C1 C2 111.7(2) . .
N5 C10 C9 111.0(2) . .
N5 C10 C5 110.4(2) . .
C9 C10 C5 110.8(2) . .
C7 C8 C9 110.3(2) . .
N4 C5 C10 109.5(2) . .
N4 C5 C6 112.1(3) . .
C6 C5 C10 110.6(2) . .
C8 C7 C6 110.4(3) . .
N4 C4 C3 103.3(2) . .
N5 C14 C13 103.0(2) . .
C7 C6 C5 110.6(3) . .
C11 C12 C13 102.2(2) . .
C14 C13 C12 104.1(2) . .
C1 C2 C3 103.2(2) . .
C2 C3 C4 106.0(3) . .
N1 O2 Np1 97.31(15) . .
N3 O8 Np1 97.47(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Np1 O7 2.5107(19) .
Np1 O7 2.5107(19) 3_876
Np1 O4 2.5158(19) 3_876
Np1 O4 2.5158(19) .
Np1 O1 2.5077(19) .
Np1 O1 2.5078(19) 3_876
Np1 O5 2.484(2) 3_876
Np1 O5 2.484(2) .
Np1 O2 2.4966(19) 3_876
Np1 O2 2.4966(19) .
Np1 O8 2.5075(19) .
Np1 O8 2.5075(19) 3_876
O7 N3 1.282(3) .
O9 N3 1.211(3) .
O4 N2 1.281(3) .
O6 N2 1.215(3) .
O1 N1 1.283(3) .
N3 O8 1.272(3) .
N1 O3 1.209(3) .
N1 O2 1.275(3) .
O5 N2 1.274(3) .
O10 C1 1.271(3) .
O11 C11 1.271(3) .
N4 C1 1.308(4) .
N4 C5 1.467(4) .
N4 C4 1.478(4) .
N5 C11 1.311(3) .
N5 C10 1.463(3) .
N5 C14 1.483(3) .
C11 C12 1.490(4) .
C9 C10 1.523(4) .
C9 C8 1.530(4) .
C1 C2 1.501(4) .
C10 C5 1.540(4) .
C8 C7 1.517(4) .
C5 C6 1.530(4) .
C7 C6 1.525(5) .
C4 C3 1.526(5) .
C14 C13 1.534(4) .
C12 C13 1.542(4) .
C2 C3 1.512(5) .
