#------------------------------------------------------------------------------
#$Date: 2015-06-05 05:23:31 +0300 (Fri, 05 Jun 2015) $
#$Revision: 138119 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/29/4342961.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_4342961
loop_
_publ_author_name
'Karhu, Aino J.'
'Pakkanen, Olli J.'
'Rautiainen, J. Mikko'
'Oilunkaniemi, Raija'
'Chivers, Tristram'
'Laitinen, Risto S.'
_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            'C2 H6 N2 Se10'
_chemical_formula_weight         847.69
_chemical_name_systematic
'dimethyl hexaselenium diimide-octaselenium(2/1)'
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-03-12 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90.07(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.000(2)
_cell_length_b                   5.6347(11)
_cell_length_c                   23.631(5)
_cell_measurement_reflns_used    1484
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.704
_cell_measurement_theta_min      3.095
_cell_volume                     1597.8(5)
_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 (Branderburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker Kappa CCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1529
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_laue_measured_fraction_full 0.919
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9346
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.704
_diffrn_reflns_theta_min         3.095
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.822
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_correction_T_min  0.5360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Sheldrick (2008)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    3.524
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         4.273
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1969
_refine_ls_R_factor_gt           0.1207
_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)+(0.1221P)²+61.0666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.3149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1484
_reflns_number_total             2661
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00582_si_003.cif
_cod_data_source_block           cmpd1bse8
_cod_depositor_comments
'Adding full bibliography for 4342961--4342962.cif.'
_cod_original_cell_volume        1597.9(5)
_cod_database_code               4342961
_publcif_datablock.id            {b8fcc229-79e3-42cd-9423-15048af5dff3}
_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.
;
_shelx_estimated_absorpt_t_min   0.170
_shelx_estimated_absorpt_t_max   0.263
_shelxl_version_number           2013-4
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.3649(3) 0.8055(7) 0.23862(15) 0.0786(11) Uani 1 1 d . . . . .
Se2 Se 0.6355(3) 0.8064(7) 0.23893(14) 0.0769(10) Uani 1 1 d . . . . .
Se3 Se 0.3215(3) 0.8748(6) 0.33388(15) 0.0760(10) Uani 1 1 d . . . . .
Se4 Se 0.6784(3) 0.8752(6) 0.33375(15) 0.0749(10) Uani 1 1 d . . . . .
Se5 Se 0.3677(3) 0.5220(6) 0.37892(18) 0.0929(13) Uani 1 1 d . . . . .
Se6 Se 0.6327(4) 0.5226(6) 0.37949(18) 0.0936(13) Uani 1 1 d . . . . .
N1 N 0.499(2) 0.925(5) 0.2220(9) 0.076(5) Uani 1 1 d D . . . .
N2 N 0.500(2) 0.573(5) 0.4183(8) 0.076(5) Uani 1 1 d D . . . .
C1 C 0.501(3) 1.173(5) 0.2337(11) 0.076(5) Uani 1 1 d D . . . .
H1A H 0.5698 1.2389 0.2201 0.114 Uiso 1 1 calc R U . . .
H1B H 0.4955 1.1977 0.2738 0.114 Uiso 1 1 calc R U . . .
H1C H 0.4396 1.2488 0.2150 0.114 Uiso 1 1 calc R U . . .
C2 C 0.500(2) 0.773(5) 0.4565(10) 0.076(5) Uani 1 1 d D . . . .
H2A H 0.4317 0.7744 0.4775 0.114 Uiso 1 1 calc R U . . .
H2B H 0.5069 0.9171 0.4353 0.114 Uiso 1 1 calc R U . . .
H2C H 0.5618 0.7590 0.4823 0.114 Uiso 1 1 calc R U . . .
Se1A Se 0.0895(7) 0.0731(17) 0.3970(3) 0.086(3) Uani 0.5 1 d D . P A 1
Se2A Se 0.2086(5) 0.1676(12) 0.4717(3) 0.0617(15) Uani 0.5 1 d . . P A 1
Se3A Se 0.2082(5) -0.1648(12) 0.5285(2) 0.0613(15) Uani 0.5 1 d . . P A 1
Se4A Se 0.0888(6) -0.0714(17) 0.6030(3) 0.082(2) Uani 0.5 1 d D . P A 1
Se1B Se 0.0698(13) 0.300(4) 0.4213(7) 0.261(13) Uani 0.5 1 d . . P B 2
Se2B Se 0.1590(7) -0.025(2) 0.4500(4) 0.123(4) Uani 0.5 1 d . . P B 2
Se3B Se 0.1590(7) 0.026(2) 0.5489(5) 0.123(4) Uani 0.5 1 d . . P B 2
Se4B Se 0.0681(12) -0.303(4) 0.5771(7) 0.238(11) Uani 0.5 1 d . . P B 2
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'
Se Se -0.0929 2.2259 '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
N1 Se1 Se3 110.4(7) .
N1 Se2 Se4 110.4(7) .
Se5 Se3 Se1 104.14(18) .
Se6 Se4 Se2 104.62(19) .
N2 Se5 Se3 107.4(8) .
N2 Se6 Se4 107.5(8) .
C1 N1 Se1 110(2) .
C1 N1 Se2 107(2) .
Se1 N1 Se2 128.7(15) .
C2 N2 Se5 115.5(19) .
C2 N2 Se6 115.5(19) .
Se5 N2 Se6 117.4(11) .
N1 C1 H1A 109.5 .
N1 C1 H1B 109.5 .
H1A C1 H1B 109.5 .
N1 C1 H1C 109.5 .
H1A C1 H1C 109.5 .
H1B C1 H1C 109.5 .
N2 C2 H2A 109.5 .
N2 C2 H2B 109.5 .
H2A C2 H2B 109.5 .
N2 C2 H2C 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
Se4A Se1A Se2A 127.9(4) 3_556
Se3A Se2A Se1A 104.7(4) .
Se2A Se3A Se4A 105.0(4) .
Se1A Se4A Se3A 127.8(4) 3_556
Se4B Se1B Se2B 118.7(11) 3_556
Se1B Se2B Se3B 101.5(7) .
Se4B Se3B Se2B 101.1(7) .
Se1B Se4B Se3B 118.9(12) 3_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 N1 1.79(2) .
Se1 Se3 2.344(5) .
Se2 N1 1.82(2) .
Se2 Se4 2.331(5) .
Se3 Se5 2.322(5) .
Se4 Se6 2.328(5) .
Se5 N2 1.87(2) .
Se6 N2 1.86(2) .
N1 C1 1.422(10) .
N2 C2 1.443(10) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
Se1A Se4A 2.139(11) 3_556
Se1A Se2A 2.331(10) .
Se2A Se3A 2.304(9) .
Se3A Se4A 2.332(9) .
Se4A Se1A 2.139(11) 3_556
Se1B Se4B 1.66(2) 3_556
Se1B Se2B 2.23(3) .
Se2B Se3B 2.353(15) .
Se3B Se4B 2.25(3) .
Se4B Se1B 1.66(2) 3_556
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
Se3 Se1 N1 C1 -58.0(19)
Se3 Se1 N1 Se2 76.9(17)
Se4 Se2 N1 C1 59.1(18)
Se4 Se2 N1 Se1 -76.7(18)
Se3 Se5 N2 C2 53.7(19)
Se3 Se5 N2 Se6 -88.0(14)
Se4 Se6 N2 C2 -54.2(19)
Se4 Se6 N2 Se5 87.5(14)
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{b8fcc229-79e3-42cd-9423-15048af5dff3} y y y
loop_
_publcif_info_cif.paper_type
E
