Experimental and Computational (77)Se NMR Investigations of the Cyclic Eight-Membered Selenium Imides 1,3,5,7-Se4(NR)4 (R = Me, (t)Bu) and 1,5-Se6(NMe)2.
Karhu, Aino J.; Pakkanen, Olli J.; Rautiainen, J. Mikko; Oilunkaniemi, Raija; Chivers, Tristram; Laitinen, Risto S.; Inorganic chemistry 54 (2015) 4990–4997; doi:10.1021/acs.inorgchem.5b00582

data_4342962
_publ_section_title
;
 Experimental and Computational (77)Se NMR Investigations of the Cyclic
 Eight-Membered Selenium Imides 1,3,5,7-Se4(NR)4 (R = Me, (t)Bu) and
 1,5-Se6(NMe)2.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4990
_journal_page_last               4997
_journal_paper_doi               10.1021/acs.inorgchem.5b00582
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C4 H12 N4 Se4'
_chemical_formula_weight         432.02
_chemical_name_systematic
;
methyl tetraselenium tetraimide
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2015-03-12 # Formatted by publCIF

;
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_cell_measurement_theta_min      2.818
_cell_volume                     1172.1(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Bruker, 2008)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
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_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7907
_diffrn_reflns_point_group_measured_fraction_full 0.969
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_crystal_colour            yellow
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_exptl_crystal_description       needle
_exptl_crystal_F_000             800
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_exptl_crystal_size_mid          0.100
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_refine_diff_density_min         -1.337
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_refine_ls_extinction_coef       0.013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2059
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0676
_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/[\s^2^(Fo^2^)+(0.0984P)^2^+6.4664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1686
_reflns_number_total             2059
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {92544c27-b2fd-4739-9d53-3b3d8c9a6a17}
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_cod_data_source_block           cmpd5b
_cod_depositor_comments
'Adding full bibliography for 4342961--4342962.cif.'
_cod_database_code               4342962
_shelx_estimated_absorpt_t_min   0.118
_shelx_estimated_absorpt_t_max   0.574
_shelxl_version_number           2013-4
_shelx_res_checksum              69185
_shelx_hkl_checksum              4027