#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:49:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179079 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/41/4304120.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_4304120
loop_
_publ_author_name
'Christiane Rotter'
'Michael Schuster'
'Mustafa Kidik'
'Oliver Schön'
'Thomas M. Klapötke'
'Konstantin Karaghiosoff'
_publ_section_title
;
Structural and NMR Spectroscopic Investigations of Chair and Twist
Conformers of the P2Se82- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1663
_journal_page_last               1673
_journal_paper_doi               10.1021/ic7015534
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C8 H12 Li N4, 0.5(p2 Se8)'
_chemical_formula_sum            'C8 H12 Li N4 P Se4'
_chemical_formula_weight         517.97
_chemical_melting_point          292
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Schoen, Oliver; Rotter, Christiane'
_audit_block_code                bx300
_audit_creation_date             28-Feb-2007
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0535(6)
_cell_length_b                   12.1200(5)
_cell_length_c                   15.0831(6)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.0000
_cell_measurement_theta_min      3.7552
_cell_volume                     3665.9(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    0.00  100.80   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000   70.0000    0.0000    0.0000    0.0000 144

  2 omega    0.00  100.80   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000   70.0000  120.0000    0.0000    0.0000 144

  3 omega    0.00  100.80   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000   70.0000  240.0000    0.0000    0.0000 144

  4 omega  -42.00   59.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -70.0000    0.0000    0.0000    0.0000 145

  5 omega  -42.00   59.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -70.0000  120.0000    0.0000    0.0000 145

  6 omega  -42.00   59.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -70.0000  240.0000    0.0000    0.0000 145

;
_diffrn_measurement_device_type  'Oxford diffraction X-calibur'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1607
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35613
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    8.081
_exptl_absorpt_correction_T_max  0.1971
_exptl_absorpt_correction_T_min  0.0948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.364
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.364
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0175P)²+16.8724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                3427
_reflns_number_total             3732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7015534-file001_4.cif
_cod_data_source_block           v1
_cod_database_code               4304120
loop_
_publ_contact_author_name
_publ_contact_author_address
_publ_contact_author_email
_publ_contact_author_fax
_publ_contact_author_phone
'Konstantin Karaghiosoff'
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;
klk@cup.uni-muenchen.de '+49 89 2180 77492' '+49 89 2180 77426'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.01700(5) 0.90835(9) 0.14700(7) 0.0351(3) Uani 1 1 d . . .
Se2 Se -0.05419(5) 0.96616(9) 0.36307(7) 0.0385(3) Uani 1 1 d . . .
Se3 Se -0.15397(5) 0.82853(10) 0.22018(8) 0.0471(3) Uani 1 1 d . . .
Se4 Se 0.00258(5) 0.68840(10) 0.28115(8) 0.0472(3) Uani 1 1 d . . .
P5 P -0.05086(12) 0.8358(2) 0.25337(17) 0.0326(6) Uani 1 1 d . . .
N1 N 0.0597(7) 0.6406(13) 0.0000 0.057(4) Uani 1 2 d S . .
N2 N 0.1802(4) 0.7566(9) 0.1123(6) 0.054(3) Uani 1 1 d . . .
N3 N 0.2229(7) 0.5442(13) 0.0000 0.059(4) Uani 1 2 d S . .
N4 N 0.1967(7) 0.9072(14) 0.5000 0.063(4) Uani 1 2 d S . .
N5 N 0.3144(5) 1.0279(10) 0.3847(7) 0.070(3) Uani 1 1 d . . .
N6 N 0.2042(8) 1.1728(15) 0.5000 0.071(5) Uani 1 2 d S . .
Li1 Li 0.1591(12) 0.671(3) 0.0000 0.051(7) Uani 1 2 d S . .
Li2 Li 0.2612(16) 1.037(4) 0.5000 0.083(11) Uani 1 2 d S . .
C1 C 0.0046(9) 0.6502(13) 0.0000 0.046(4) Uani 1 2 d S . .
C2 C -0.0693(7) 0.6583(15) 0.0000 0.054(5) Uani 1 2 d S . .
H2A H -0.0849 0.6763 0.0598 0.065 Uiso 0.50 1 calc PR . .
H2B H -0.0885 0.5876 -0.0186 0.065 Uiso 0.50 1 calc PR . .
H2C H -0.0833 0.7163 -0.0412 0.065 Uiso 0.50 1 calc PR . .
C3 C 0.1837(5) 0.7923(10) 0.1805(8) 0.044(3) Uani 1 1 d . . .
C4 C 0.1863(5) 0.8367(10) 0.2692(7) 0.053(3) Uani 1 1 d . . .
H4A H 0.1442 0.8213 0.2996 0.063 Uiso 1 1 calc R . .
H4B H 0.1934 0.9166 0.2663 0.063 Uiso 1 1 calc R . .
H4C H 0.2231 0.8022 0.3017 0.063 Uiso 1 1 calc R . .
C5 C 0.2788(8) 0.5265(12) 0.0000 0.036(3) Uani 1 2 d S . .
C6 C 0.3505(6) 0.5102(14) 0.0000 0.045(4) Uani 1 2 d S . .
H6A H 0.3676 0.5183 0.0605 0.054 Uiso 0.50 1 calc PR . .
H6B H 0.3715 0.5653 -0.0385 0.054 Uiso 0.50 1 calc PR . .
H6C H 0.3608 0.4361 -0.0220 0.054 Uiso 0.50 1 calc PR . .
C8 C 0.1550(9) 0.8460(15) 0.5000 0.046(4) Uani 1 2 d S . .
C9 C 0.0996(8) 0.7667(14) 0.5000 0.056(5) Uani 1 2 d S . .
H9A H 0.0898 0.7443 0.5611 0.067 Uiso 0.50 1 calc PR . .
H9B H 0.1121 0.7016 0.4651 0.067 Uiso 0.50 1 calc PR . .
H9C H 0.0600 0.8012 0.4738 0.067 Uiso 0.50 1 calc PR . .
C10 C 0.3312(6) 1.0155(11) 0.3145(9) 0.053(3) Uani 1 1 d . . .
C11 C 0.3524(6) 0.9986(10) 0.2235(7) 0.056(3) Uani 1 1 d . . .
H11A H 0.3164 1.0201 0.1831 0.068 Uiso 1 1 calc R . .
H11B H 0.3633 0.9206 0.2145 0.068 Uiso 1 1 calc R . .
H11C H 0.3920 1.0437 0.2116 0.068 Uiso 1 1 calc R . .
C15 C 0.1610(9) 1.2290(16) 0.5000 0.050(5) Uani 1 2 d S . .
C16 C 0.1059(9) 1.3074(15) 0.5000 0.063(5) Uani 1 2 d S . .
H16A H 0.0855 1.3095 0.5590 0.076 Uiso 0.50 1 calc PR . .
H16B H 0.0725 1.2844 0.4563 0.076 Uiso 0.50 1 calc PR . .
H16C H 0.1226 1.3809 0.4847 0.076 Uiso 0.50 1 calc PR . .
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'
Li Li -0.0003 0.0001 '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'
P P 0.1023 0.0942 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P5 Se1 Se1 101.17(8) . 2_575 ?
P5 Se2 Se2 102.50(8) . 2_575 ?
Se4 P5 Se3 120.10(13) . . ?
Se4 P5 Se1 99.33(11) . . ?
Se3 P5 Se1 115.47(12) . . ?
Se4 P5 Se2 116.91(12) . . ?
Se3 P5 Se2 99.79(11) . . ?
Se1 P5 Se2 105.05(11) . . ?
C1 N1 Li1 163.3(18) . . ?
C3 N2 Li1 168.1(13) . . ?
C5 N3 Li1 140.5(17) . . ?
C8 N4 Li2 171.1(18) . . ?
C10 N5 Li2 165.3(14) . . ?
C15 N6 Li2 163(2) . . ?
N3 Li1 N2 105.0(9) . 6 ?
N3 Li1 N2 105.0(9) . . ?
N2 Li1 N2 113.3(16) 6 . ?
N3 Li1 N1 119.1(16) . . ?
N2 Li1 N1 107.3(9) 6 . ?
N2 Li1 N1 107.3(9) . . ?
N6 Li2 N4 105.8(16) . . ?
N6 Li2 N5 110.0(14) . 6_556 ?
N4 Li2 N5 106.9(14) . 6_556 ?
N6 Li2 N5 110.0(14) . . ?
N4 Li2 N5 106.9(14) . . ?
N5 Li2 N5 116.6(16) 6_556 . ?
N1 C1 C2 177.8(19) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C4 178.1(13) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 C6 177.0(17) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C8 C9 179.2(19) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C10 C11 179.5(17) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C15 C16 178(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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
Se1 P5 2.280(3) . ?
Se1 Se1 2.324(2) 2_575 ?
Se2 P5 2.289(3) . ?
Se2 Se2 2.323(2) 2_575 ?
Se3 P5 2.129(3) . ?
Se4 P5 2.125(3) . ?
N1 C1 1.111(18) . ?
N1 Li1 2.03(3) . ?
N2 C3 1.119(13) . ?
N2 Li1 2.028(19) . ?
N3 C5 1.141(17) . ?
N3 Li1 2.00(3) . ?
N4 C8 1.12(2) . ?
N4 Li2 2.04(4) . ?
N5 C10 1.122(14) . ?
N5 Li2 2.04(2) . ?
N6 C15 1.10(2) . ?
N6 Li2 2.00(4) . ?
Li1 N2 2.028(19) 6 ?
Li2 N5 2.04(2) 6_556 ?
C1 C2 1.49(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.442(15) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.451(19) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 C9 1.47(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.451(16) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C15 C16 1.46(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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
Se1 Se1 P5 Se4 -161.91(8) 2_575 . . . ?
Se1 Se1 P5 Se3 68.21(13) 2_575 . . . ?
Se1 Se1 P5 Se2 -40.65(10) 2_575 . . . ?
Se2 Se2 P5 Se4 71.72(12) 2_575 . . . ?
Se2 Se2 P5 Se3 -157.11(9) 2_575 . . . ?
Se2 Se2 P5 Se1 -37.22(11) 2_575 . . . ?
C5 N3 Li1 N2 59.8(9) . . . 6 ?
C5 N3 Li1 N2 -59.8(9) . . . . ?
C5 N3 Li1 N1 180.0 . . . . ?
C3 N2 Li1 N3 -91(6) . . . . ?
C3 N2 Li1 N2 155(5) . . . 6 ?
C3 N2 Li1 N1 37(6) . . . . ?
C1 N1 Li1 N3 180.0 . . . . ?
C1 N1 Li1 N2 -61.0(11) . . . 6 ?
C1 N1 Li1 N2 61.0(11) . . . . ?
C15 N6 Li2 N4 0.0 . . . . ?
C15 N6 Li2 N5 -115.1(14) . . . 6_556 ?
C15 N6 Li2 N5 115.1(14) . . . . ?
C8 N4 Li2 N6 0.0 . . . . ?
C8 N4 Li2 N5 117.2(12) . . . 6_556 ?
C8 N4 Li2 N5 -117.2(12) . . . . ?
C10 N5 Li2 N6 -78(7) . . . . ?
C10 N5 Li2 N4 37(7) . . . . ?
C10 N5 Li2 N5 156(5) . . . 6_556 ?
Li1 N1 C1 C2 180.0 . . . . ?
Li1 N2 C3 C4 -14(46) . . . . ?
Li1 N3 C5 C6 0.0 . . . . ?
Li2 N4 C8 C9 0.0 . . . . ?
Li2 N5 C10 C11 -41(100) . . . . ?
Li2 N6 C15 C16 180.0 . . . . ?
