#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:49:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179079 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/41/4304117.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_4304117
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         'C20 H20 Li N4, 0.5(P2 Se8)'
_chemical_formula_sum            'C20 H20 Li N4 P Se4'
_chemical_formula_weight         670.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.271(6)
_cell_angle_beta                 94.847(6)
_cell_angle_gamma                114.219(7)
_cell_formula_units_Z            2
_cell_length_a                   10.1582(8)
_cell_length_b                   10.7716(8)
_cell_length_c                   12.7499(10)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.9968
_cell_measurement_theta_min      3.9728
_cell_volume                     1255.41(18)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.1587
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17142
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    5.922
_exptl_absorpt_correction_T_max  0.742656
_exptl_absorpt_correction_T_min  0.494912
_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            rod
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_gt           0.0481
_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)+(0.0083P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                2885
_reflns_number_total             7312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7015534-file001_1.cif
_cod_data_source_block           v1
_cod_original_cell_volume        1255.40(17)
_cod_database_code               4304117
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'
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
N1 N 0.2613(5) 0.2439(5) 0.0657(4) 0.0450(13) Uani 1 1 d . . .
N3 N 0.4880(5) 0.5020(5) 0.2567(4) 0.0425(13) Uani 1 1 d . . .
C13 C 0.2519(7) 0.6614(7) 0.0971(5) 0.0489(17) Uani 1 1 d . . .
H13 H 0.2626 0.6873 0.1717 0.059 Uiso 1 1 calc R . .
N2 N 0.1372(5) 0.3498(5) 0.2701(4) 0.0463(13) Uani 1 1 d . . .
N4 N 0.2621(5) 0.5458(5) 0.0637(4) 0.0435(13) Uani 1 1 d . . .
C6 C 0.0994(7) 0.2245(6) 0.2975(4) 0.0446(16) Uani 1 1 d . . .
H6 H 0.1503 0.1730 0.2730 0.054 Uiso 1 1 calc R . .
C4 C 0.3648(7) 0.1202(7) -0.0391(5) 0.0528(18) Uani 1 1 d . . .
H4 H 0.4460 0.1000 -0.0490 0.063 Uiso 1 1 calc R . .
C5 C 0.3719(7) 0.2103(6) 0.0469(5) 0.0474(17) Uani 1 1 d . . .
H5 H 0.4592 0.2510 0.0957 0.057 Uiso 1 1 calc R . .
C10 C 0.5888(7) 0.6233(7) 0.2448(5) 0.0456(16) Uani 1 1 d . . .
H10 H 0.5668 0.6684 0.1898 0.055 Uiso 1 1 calc R . .
C3 C 0.2414(8) 0.0602(6) -0.1099(5) 0.0573(19) Uani 1 1 d . . .
H3 H 0.2353 -0.0013 -0.1705 0.069 Uiso 1 1 calc R . .
C8 C 0.0672(7) 0.4208(6) 0.3088(5) 0.0505(18) Uani 1 1 d . . .
H8 H 0.0950 0.5121 0.2933 0.061 Uiso 1 1 calc R . .
C12 C 0.7532(7) 0.6272(7) 0.3862(5) 0.059(2) Uani 1 1 d . . .
H12 H 0.8442 0.6695 0.4307 0.070 Uiso 1 1 calc R . .
C2 C 0.1248(7) 0.0905(6) -0.0920(5) 0.0529(18) Uani 1 1 d . . .
H2 H 0.0364 0.0500 -0.1395 0.063 Uiso 1 1 calc R . .
C11 C 0.7233(7) 0.6896(6) 0.3055(5) 0.0482(17) Uani 1 1 d . . .
H11 H 0.7925 0.7756 0.2916 0.058 Uiso 1 1 calc R . .
C15 C 0.2093(7) 0.7109(6) -0.0756(6) 0.0550(18) Uani 1 1 d . . .
H15 H 0.1897 0.7661 -0.1230 0.066 Uiso 1 1 calc R . .
C1 C 0.1406(7) 0.1801(7) -0.0041(6) 0.0541(18) Uani 1 1 d . . .
H1 H 0.0591 0.1987 0.0085 0.065 Uiso 1 1 calc R . .
C9 C -0.0436(7) 0.3687(8) 0.3701(5) 0.0583(19) Uani 1 1 d . . .
H9 H -0.0925 0.4220 0.3947 0.070 Uiso 1 1 calc R . .
C7 C -0.0079(7) 0.1655(7) 0.3586(5) 0.0575(19) Uani 1 1 d . . .
H7 H -0.0310 0.0754 0.3755 0.069 Uiso 1 1 calc R . .
C14 C 0.2270(7) 0.7466(7) 0.0323(6) 0.0579(19) Uani 1 1 d . . .
H14 H 0.2221 0.8286 0.0617 0.069 Uiso 1 1 calc R . .
C16 C 0.2210(7) 0.5914(7) -0.1131(5) 0.0570(19) Uani 1 1 d . . .
H16 H 0.2114 0.5635 -0.1873 0.068 Uiso 1 1 calc R . .
C21 C 0.5191(7) 0.4426(7) 0.3361(5) 0.0568(19) Uani 1 1 d . . .
H21 H 0.4489 0.3558 0.3478 0.068 Uiso 1 1 calc R . .
C23 C 0.2466(7) 0.5149(7) -0.0416(5) 0.0536(18) Uani 1 1 d . . .
H23 H 0.2541 0.4332 -0.0687 0.064 Uiso 1 1 calc R . .
C20 C -0.0814(7) 0.2383(8) 0.3949(5) 0.059(2) Uani 1 1 d . . .
H20 H -0.1575 0.1993 0.4367 0.071 Uiso 1 1 calc R . .
C22 C 0.6513(8) 0.5035(7) 0.4026(5) 0.0571(19) Uani 1 1 d . . .
H22 H 0.6702 0.4589 0.4590 0.069 Uiso 1 1 calc R . .
Li1 Li 0.2866(11) 0.4132(10) 0.1685(8) 0.041(3) Uani 1 1 d . . .
Se1 Se 0.39812(7) 0.79177(6) 0.42476(5) 0.03835(17) Uani 1 1 d . . .
Se2 Se 0.64486(6) 0.89958(6) 0.49548(5) 0.03915(17) Uani 1 1 d . . .
Se3 Se 0.12860(7) 0.85599(7) 0.30692(5) 0.0536(2) Uani 1 1 d . . .
Se4 Se 0.51139(8) 1.07037(7) 0.26067(5) 0.0529(2) Uani 1 1 d . . .
P1 P 0.35797(16) 0.96413(16) 0.35825(12) 0.0346(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'
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
C1 N1 C5 115.3(6) . . ?
C1 N1 Li1 119.6(5) . . ?
C5 N1 Li1 123.3(5) . . ?
C10 N3 C21 116.4(5) . . ?
C10 N3 Li1 123.4(5) . . ?
C21 N3 Li1 120.0(5) . . ?
N4 C13 C14 125.1(6) . . ?
N4 C13 H13 117.5 . . ?
C14 C13 H13 117.5 . . ?
C8 N2 C6 116.4(5) . . ?
C8 N2 Li1 125.2(5) . . ?
C6 N2 Li1 118.3(5) . . ?
C13 N4 C23 114.9(5) . . ?
C13 N4 Li1 122.8(5) . . ?
C23 N4 Li1 122.2(5) . . ?
N2 C6 C7 124.0(6) . . ?
N2 C6 H6 118.0 . . ?
C7 C6 H6 118.0 . . ?
C3 C4 C5 119.7(6) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 123.3(6) . . ?
N1 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
N3 C10 C11 125.3(6) . . ?
N3 C10 H10 117.4 . . ?
C11 C10 H10 117.4 . . ?
C4 C3 C2 118.5(6) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
N2 C8 C9 123.4(6) . . ?
N2 C8 H8 118.3 . . ?
C9 C8 H8 118.3 . . ?
C11 C12 C22 119.2(6) . . ?
C11 C12 H12 120.4 . . ?
C22 C12 H12 120.4 . . ?
C1 C2 C3 118.0(6) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C12 C11 C10 117.4(6) . . ?
C12 C11 H11 121.3 . . ?
C10 C11 H11 121.3 . . ?
C14 C15 C16 117.7(6) . . ?
C14 C15 H15 121.1 . . ?
C16 C15 H15 121.1 . . ?
N1 C1 C2 125.1(6) . . ?
N1 C1 H1 117.4 . . ?
C2 C1 H1 117.4 . . ?
C20 C9 C8 118.5(7) . . ?
C20 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C20 C7 C6 118.7(6) . . ?
C20 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C23 C16 C15 118.7(6) . . ?
C23 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
N3 C21 C22 122.1(6) . . ?
N3 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
N4 C23 C16 125.0(6) . . ?
N4 C23 H23 117.5 . . ?
C16 C23 H23 117.5 . . ?
C7 C20 C9 118.9(6) . . ?
C7 C20 H20 120.5 . . ?
C9 C20 H20 120.5 . . ?
C12 C22 C21 119.6(6) . . ?
C12 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
N2 Li1 N3 107.7(5) . . ?
N2 Li1 N1 107.9(5) . . ?
N3 Li1 N1 111.8(5) . . ?
N2 Li1 N4 116.4(5) . . ?
N3 Li1 N4 110.6(5) . . ?
N1 Li1 N4 102.4(5) . . ?
P1 Se1 Se2 102.99(5) . . ?
P1 Se2 Se1 101.98(5) 2_676 . ?
Se4 P1 Se3 124.28(8) . . ?
Se4 P1 Se2 113.26(7) . 2_676 ?
Se3 P1 Se2 99.69(6) . 2_676 ?
Se4 P1 Se1 113.65(7) . . ?
Se3 P1 Se1 98.89(7) . . ?
Se2 P1 Se1 104.33(6) 2_676 . ?
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
N1 C1 1.334(7) . ?
N1 C5 1.346(7) . ?
N1 Li1 2.056(11) . ?
N3 C10 1.320(7) . ?
N3 C21 1.329(7) . ?
N3 Li1 2.043(11) . ?
C13 N4 1.326(7) . ?
C13 C14 1.371(8) . ?
C13 H13 0.9500 . ?
N2 C8 1.330(7) . ?
N2 C6 1.332(7) . ?
N2 Li1 2.024(10) . ?
N4 C23 1.333(7) . ?
N4 Li1 2.115(11) . ?
C6 C7 1.366(7) . ?
C6 H6 0.9500 . ?
C4 C3 1.357(8) . ?
C4 C5 1.373(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C10 C11 1.376(7) . ?
C10 H10 0.9500 . ?
C3 C2 1.382(8) . ?
C3 H3 0.9500 . ?
C8 C9 1.380(8) . ?
C8 H8 0.9500 . ?
C12 C11 1.358(8) . ?
C12 C22 1.358(8) . ?
C12 H12 0.9500 . ?
C2 C1 1.364(8) . ?
C2 H2 0.9500 . ?
C11 H11 0.9500 . ?
C15 C14 1.370(8) . ?
C15 C16 1.386(8) . ?
C15 H15 0.9500 . ?
C1 H1 0.9500 . ?
C9 C20 1.371(8) . ?
C9 H9 0.9500 . ?
C7 C20 1.362(8) . ?
C7 H7 0.9500 . ?
C14 H14 0.9500 . ?
C16 C23 1.361(8) . ?
C16 H16 0.9500 . ?
C21 C22 1.391(8) . ?
C21 H21 0.9500 . ?
C23 H23 0.9500 . ?
C20 H20 0.9500 . ?
C22 H22 0.9500 . ?
Se1 P1 2.2769(16) . ?
Se1 Se2 2.3413(9) . ?
Se2 P1 2.2748(16) 2_676 ?
Se3 P1 2.1423(17) . ?
Se4 P1 2.1005(16) . ?
P1 Se2 2.2748(16) 2_676 ?
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
C14 C13 N4 C23 0.2(10) . . . . ?
C14 C13 N4 Li1 -175.8(6) . . . . ?
C8 N2 C6 C7 2.2(9) . . . . ?
Li1 N2 C6 C7 -174.7(6) . . . . ?
C1 N1 C5 C4 1.9(9) . . . . ?
Li1 N1 C5 C4 -163.1(6) . . . . ?
C3 C4 C5 N1 -0.2(10) . . . . ?
C21 N3 C10 C11 2.1(9) . . . . ?
Li1 N3 C10 C11 176.9(6) . . . . ?
C5 C4 C3 C2 -1.0(10) . . . . ?
C6 N2 C8 C9 -2.9(9) . . . . ?
Li1 N2 C8 C9 173.8(6) . . . . ?
C4 C3 C2 C1 0.4(10) . . . . ?
C22 C12 C11 C10 0.6(10) . . . . ?
N3 C10 C11 C12 -2.0(10) . . . . ?
C5 N1 C1 C2 -2.6(9) . . . . ?
Li1 N1 C1 C2 163.0(6) . . . . ?
C3 C2 C1 N1 1.5(10) . . . . ?
N2 C8 C9 C20 1.7(10) . . . . ?
N2 C6 C7 C20 -0.4(10) . . . . ?
C16 C15 C14 C13 -1.4(10) . . . . ?
N4 C13 C14 C15 0.8(11) . . . . ?
C14 C15 C16 C23 1.2(10) . . . . ?
C10 N3 C21 C22 -0.8(9) . . . . ?
Li1 N3 C21 C22 -175.8(6) . . . . ?
C13 N4 C23 C16 -0.5(10) . . . . ?
Li1 N4 C23 C16 175.5(6) . . . . ?
C15 C16 C23 N4 -0.2(11) . . . . ?
C6 C7 C20 C9 -0.9(10) . . . . ?
C8 C9 C20 C7 0.3(10) . . . . ?
C11 C12 C22 C21 0.5(10) . . . . ?
N3 C21 C22 C12 -0.5(10) . . . . ?
C8 N2 Li1 N3 95.3(7) . . . . ?
C6 N2 Li1 N3 -88.1(6) . . . . ?
C8 N2 Li1 N1 -143.9(6) . . . . ?
C6 N2 Li1 N1 32.7(7) . . . . ?
C8 N2 Li1 N4 -29.6(8) . . . . ?
C6 N2 Li1 N4 147.0(5) . . . . ?
C10 N3 Li1 N2 -131.0(5) . . . . ?
C21 N3 Li1 N2 43.7(7) . . . . ?
C10 N3 Li1 N1 110.7(6) . . . . ?
C21 N3 Li1 N1 -74.6(7) . . . . ?
C10 N3 Li1 N4 -2.7(8) . . . . ?
C21 N3 Li1 N4 172.0(5) . . . . ?
C1 N1 Li1 N2 67.2(7) . . . . ?
C5 N1 Li1 N2 -128.4(5) . . . . ?
C1 N1 Li1 N3 -174.6(5) . . . . ?
C5 N1 Li1 N3 -10.2(8) . . . . ?
C1 N1 Li1 N4 -56.1(6) . . . . ?
C5 N1 Li1 N4 108.3(6) . . . . ?
C13 N4 Li1 N2 53.7(8) . . . . ?
C23 N4 Li1 N2 -122.1(6) . . . . ?
C13 N4 Li1 N3 -69.7(7) . . . . ?
C23 N4 Li1 N3 114.6(6) . . . . ?
C13 N4 Li1 N1 171.1(5) . . . . ?
C23 N4 Li1 N1 -4.7(7) . . . . ?
P1 Se1 Se2 P1 72.02(7) . . . 2_676 ?
Se2 Se1 P1 Se4 50.02(7) . . . . ?
Se2 Se1 P1 Se3 -176.28(5) . . . . ?
Se2 Se1 P1 Se2 -73.82(6) . . . 2_676 ?
