#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:25:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179411 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/08/4330858.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_4330858
loop_
_publ_author_name
'Robert P. Davies'
'Laura Patel'
'Andrew J. P. White'
_publ_section_title
;
 Preparations of Metal Trichalcogenophosphonates from Organophosphonate
 Esters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11594
_journal_page_last               11601
_journal_paper_doi               10.1021/ic301504p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C24 H62 Li4 N6 P2 S6'
_chemical_formula_sum            'C24 H62 Li4 N6 P2 S6'
_chemical_formula_weight         716.86
_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                117.717(5)
_cell_angle_beta                 105.696(5)
_cell_angle_gamma                95.638(4)
_cell_formula_units_Z            1
_cell_length_a                   10.5462(5)
_cell_length_b                   10.7732(5)
_cell_length_c                   10.9125(6)
_cell_measurement_reflns_used    4351
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.3663
_cell_measurement_theta_min      2.6028
_cell_volume                     1019.47(11)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7877
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.45
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       blocks
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         5379
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0345
_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)+(0.0404P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                4044
_reflns_number_total             5379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301504p_si_003_3.cif
_cod_data_source_block           3
_cod_database_code               4330858
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
Li1 Li 0.3442(3) 0.5214(3) 0.6719(3) 0.0295(7) Uani 1 1 d . . .
Li2 Li 0.4223(3) 0.6807(3) 0.4657(3) 0.0303(7) Uani 1 1 d D . .
P1 P 0.29683(4) 0.36073(5) 0.27734(4) 0.02270(11) Uani 1 1 d . . .
S1 S 0.23032(4) 0.50157(5) 0.43409(4) 0.02606(11) Uani 1 1 d . A .
S2 S 0.41956(4) 0.47765(5) 0.23056(5) 0.02829(12) Uani 1 1 d . . .
S3 S 0.37266(5) 0.21426(5) 0.31856(5) 0.03286(13) Uani 1 1 d . . .
N1 N 0.22465(15) 0.36977(16) 0.69539(16) 0.0297(3) Uani 1 1 d . . .
C2 C 0.1501(2) 0.4549(2) 0.7844(2) 0.0451(5) Uani 1 1 d . . .
H2A H 0.1173 0.4044 0.8305 0.054 Uiso 1 1 calc R . .
H2B H 0.0695 0.4631 0.7195 0.054 Uiso 1 1 calc R . .
C3 C 0.2395(2) 0.6051(2) 0.9042(2) 0.0446(5) Uani 1 1 d . . .
H3A H 0.1855 0.6609 0.9610 0.054 Uiso 1 1 calc R . .
H3B H 0.3161 0.5969 0.9737 0.054 Uiso 1 1 calc R . .
N4 N 0.29405(16) 0.68369(16) 0.84312(16) 0.0333(4) Uani 1 1 d . . .
C5 C 0.1292(2) 0.2466(2) 0.5529(2) 0.0436(5) Uani 1 1 d . . .
H5A H 0.0768 0.1806 0.5709 0.065 Uiso 1 1 calc R . .
H5B H 0.1806 0.1944 0.4919 0.065 Uiso 1 1 calc R . .
H5C H 0.0666 0.2828 0.5011 0.065 Uiso 1 1 calc R . .
C6 C 0.3143(2) 0.3125(2) 0.7735(2) 0.0446(5) Uani 1 1 d . . .
H6A H 0.2586 0.2429 0.7846 0.067 Uiso 1 1 calc R . .
H6B H 0.3744 0.3928 0.8716 0.067 Uiso 1 1 calc R . .
H6C H 0.3697 0.2638 0.7161 0.067 Uiso 1 1 calc R . .
C7 C 0.4105(2) 0.8071(2) 0.9601(2) 0.0578(7) Uani 1 1 d . . .
H7A H 0.3793 0.8769 1.0346 0.087 Uiso 1 1 calc R . .
H7B H 0.4509 0.8545 0.9165 0.087 Uiso 1 1 calc R . .
H7C H 0.4791 0.7722 1.0071 0.087 Uiso 1 1 calc R . .
C8 C 0.1882(3) 0.7373(3) 0.7792(3) 0.0547(6) Uani 1 1 d . . .
H8A H 0.1656 0.8125 0.8587 0.082 Uiso 1 1 calc R . .
H8B H 0.1064 0.6568 0.7093 0.082 Uiso 1 1 calc R . .
H8C H 0.2218 0.7786 0.7271 0.082 Uiso 1 1 calc R . .
N9 N 0.3477(5) 0.8614(6) 0.4615(6) 0.0316(10) Uani 0.691(6) 1 d PD A 1
C10 C 0.4444(3) 1.0039(3) 0.5298(3) 0.0313(9) Uani 0.691(6) 1 d PD . 1
H10A H 0.4847 1.0448 0.6382 0.038 Uiso 0.691(6) 1 calc PR A 1
H10B H 0.3940 1.0708 0.5130 0.038 Uiso 0.691(6) 1 calc PR A 1
C11 C 0.2511(6) 0.8836(5) 0.5377(8) 0.079(2) Uani 0.691(6) 1 d PD A 1
H11A H 0.2120 0.9622 0.5370 0.119 Uiso 0.691(6) 1 calc PR A 1
H11B H 0.2981 0.9097 0.6404 0.119 Uiso 0.691(6) 1 calc PR A 1
H11C H 0.1779 0.7939 0.4872 0.119 Uiso 0.691(6) 1 calc PR A 1
C12 C 0.2732(4) 0.8034(5) 0.3025(5) 0.0698(15) Uani 0.691(6) 1 d PD A 1
H12A H 0.2373 0.8787 0.2895 0.105 Uiso 0.691(6) 1 calc PR A 1
H12B H 0.1975 0.7192 0.2643 0.105 Uiso 0.691(6) 1 calc PR A 1
H12C H 0.3354 0.7738 0.2481 0.105 Uiso 0.691(6) 1 calc PR A 1
N9' N 0.3497(14) 0.8382(13) 0.4325(13) 0.032(3) Uiso 0.309(6) 1 d PD A 2
C10' C 0.4369(5) 0.9527(6) 0.4295(7) 0.0264(17) Uiso 0.309(6) 1 d PD . 2
H10C H 0.3812 1.0163 0.4133 0.032 Uiso 0.309(6) 1 calc PR A 2
H10D H 0.4671 0.9059 0.3440 0.032 Uiso 0.309(6) 1 calc PR A 2
C11' C 0.2869(12) 0.9045(13) 0.5469(12) 0.057(3) Uiso 0.309(6) 1 d PD A 2
H11D H 0.2533 0.9842 0.5417 0.085 Uiso 0.309(6) 1 calc PR A 2
H11E H 0.3554 0.9422 0.6455 0.085 Uiso 0.309(6) 1 calc PR A 2
H11F H 0.2107 0.8307 0.5288 0.085 Uiso 0.309(6) 1 calc PR A 2
C12' C 0.2369(8) 0.7514(9) 0.2839(8) 0.039(2) Uiso 0.309(6) 1 d PD A 2
H12D H 0.1921 0.8170 0.2602 0.058 Uiso 0.309(6) 1 calc PR A 2
H12E H 0.1701 0.6833 0.2863 0.058 Uiso 0.309(6) 1 calc PR A 2
H12F H 0.2748 0.6970 0.2081 0.058 Uiso 0.309(6) 1 calc PR A 2
C13 C 0.14469(17) 0.25655(19) 0.10975(18) 0.0279(4) Uani 1 1 d . A .
H13A H 0.0746 0.2119 0.1325 0.033 Uiso 1 1 calc R . .
H13B H 0.1079 0.3241 0.0811 0.033 Uiso 1 1 calc R . .
C14 C 0.1684(2) 0.1377(2) -0.02133(18) 0.0358(5) Uani 1 1 d . . .
H14A H 0.1940 0.0631 0.0021 0.043 Uiso 1 1 calc R A .
H14B H 0.2458 0.1798 -0.0373 0.043 Uiso 1 1 calc R . .
C15 C 0.0429(2) 0.0650(2) -0.1642(2) 0.0452(6) Uani 1 1 d . A .
H15A H 0.0639 -0.0100 -0.2453 0.068 Uiso 1 1 calc R . .
H15B H 0.0178 0.1380 -0.1887 0.068 Uiso 1 1 calc R . .
H15C H -0.0333 0.0203 -0.1501 0.068 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 '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
N1 Li1 N4 86.08(13) . .
N1 Li1 S2 106.82(13) . 2_666
N4 Li1 S2 109.51(12) . 2_666
N1 Li1 S1 109.98(13) . .
N4 Li1 S1 111.00(13) . .
S2 Li1 S1 126.06(13) 2_666 .
N9' Li2 S3 111.6(3) . 2_666
N9 Li2 S3 106.73(18) . 2_666
N9' Li2 S2 110.6(3) . .
N9 Li2 S2 118.2(2) . .
S3 Li2 S2 118.64(13) 2_666 .
N9' Li2 S1 109.7(4) . .
N9 Li2 S1 108.64(17) . .
S3 Li2 S1 119.59(12) 2_666 .
S2 Li2 S1 83.80(9) . .
C13 P1 S3 106.01(6) . .
C13 P1 S2 105.46(6) . .
S3 P1 S2 115.50(3) . .
C13 P1 S1 105.03(6) . .
S3 P1 S1 115.40(3) . .
S2 P1 S1 108.40(3) . .
P1 S1 Li1 109.83(8) . .
P1 S1 Li2 81.83(7) . .
Li1 S1 Li2 94.04(10) . .
P1 S2 Li1 110.52(8) . 2_666
P1 S2 Li2 82.28(8) . .
Li1 S2 Li2 95.19(10) 2_666 .
P1 S3 Li2 114.01(8) . 2_666
C2 N1 C5 110.50(16) . .
C2 N1 C6 110.90(16) . .
C5 N1 C6 108.48(15) . .
C2 N1 Li1 103.95(14) . .
C5 N1 Li1 113.24(14) . .
C6 N1 Li1 109.76(14) . .
N1 C2 C3 111.15(17) . .
N4 C3 C2 111.95(16) . .
C3 N4 C8 110.03(18) . .
C3 N4 C7 110.11(16) . .
C8 N4 C7 109.30(17) . .
C3 N4 Li1 103.16(14) . .
C8 N4 Li1 109.73(14) . .
C7 N4 Li1 114.36(15) . .
C11 N9 C10 106.9(4) . .
C11 N9 C12 109.2(5) . .
C10 N9 C12 111.0(4) . .
C11 N9 Li2 105.7(3) . .
C10 N9 Li2 119.9(3) . .
C12 N9 Li2 103.7(3) . .
N9 C10 C10 113.0(3) . 2_676
C10' N9' C11' 110.6(9) . .
C10' N9' C12' 107.2(9) . .
C11' N9' C12' 108.0(10) . .
C10' N9' Li2 122.7(9) . .
C11' N9' Li2 104.3(9) . .
C12' N9' Li2 103.2(7) . .
N9' C10' C10' 114.4(7) . 2_676
C14 C13 P1 114.43(12) . .
C13 C14 C15 112.78(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Li1 N1 2.117(3) .
Li1 N4 2.123(3) .
Li1 S2 2.427(3) 2_666
Li1 S1 2.444(3) .
Li2 N9' 2.067(16) .
Li2 N9 2.185(6) .
Li2 S3 2.405(3) 2_666
Li2 S2 2.469(3) .
Li2 S1 2.486(3) .
P1 C13 1.8242(16) .
P1 S3 2.0113(6) .
P1 S2 2.0391(6) .
P1 S1 2.0406(6) .
S2 Li1 2.427(3) 2_666
S3 Li2 2.405(3) 2_666
N1 C2 1.459(3) .
N1 C5 1.471(2) .
N1 C6 1.472(2) .
C2 C3 1.511(3) .
C3 N4 1.459(3) .
N4 C8 1.465(2) .
N4 C7 1.469(2) .
N9 C11 1.452(6) .
N9 C10 1.473(5) .
N9 C12 1.475(6) .
C10 C10 1.478(5) 2_676
N9' C10' 1.483(12) .
N9' C11' 1.490(12) .
N9' C12' 1.499(12) .
C10' C10' 1.531(10) 2_676
C13 C14 1.517(2) .
C14 C15 1.530(2) .
