Crystallization of colourless hexanitratoneptunate(iv) with anhydrous H+ countercations trapped in a hydrogen bonded polymer with diamide linkers
Takao, Koichiro; März, Juliane; Matsuoka, Moe; Mashita, Takanori; Kazama, Hiroyuki; Tsushima, Satoru; RSC Advances 10 (2020) 6082–6087; doi:10.1039/C9RA10090C

data_7239909
_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 Np1 O22'
_chemical_formula_sum            'C28 H46 N10 Np O22'
_chemical_formula_weight         1113.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
;
2019-06-18 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.931(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1413(10)
_cell_length_b                   10.9944(6)
_cell_length_c                   21.6888(12)
_cell_measurement_reflns_used    2189
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.4981
_cell_measurement_theta_min      2.1826
_cell_volume                     4066.8(4)
_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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'generic \f and \o scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57492
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.728
_diffrn_reflns_theta_min         2.245
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   'Numerical Mu Calculated'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00041(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4312
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0192
_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/[\s^2^(Fo^2^)+(0.0132P)^2^+13.0348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3582
_reflns_number_total             4312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra10090c2.cif
_cod_data_source_block           mo_kt_l1np_0m_a
_cod_depositor_comments
'Adding full bibliography for 7239909--7239910.cif.'
_cod_original_formula_sum        'C28 H46 N10 Np1 O22'
_cod_database_code               7239909
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 N5-C14 \\sim N5A-C14
 with sigma of 0.02
 N5-C11 \\sim N5A-C11
 with sigma of 0.02
 C7-C6 \\sim C7A-C6A
 with sigma of 0.02
 N4-C6 \\sim N4-C6A
 with sigma of 0.04
 N5-C7 \\sim N5A-C7A
 with sigma of 0.04
3. Others
 Sof(H5B)=Sof(H14C)=Sof(H14D)=Sof(H8B)=Sof(N5A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(N5)=Sof(H5A)=Sof(H14A)=Sof(H14B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H8A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C5(H5A), C5(H5B), C8(H8A), C8(H8B)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C10(H10A,H10B), C9(H9A,H9B), C14(H14A,
 H14B), C14(H14C,H14D), C13(H13A,H13B), C12(H12A,H12B), C7(H7A,H7B), C6(H6A,
 H6B), C7A(H7AA,H7AB), C6A(H6AA,H6AB)
;
_shelx_res_checksum              34873
_olex2_submission_special_instructions 'No special instructions were received'