#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:29:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179751 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/47/7004793.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_7004793
loop_
_publ_author_name
'Davies, Robert P.'
'Giménez, Maria A.'
'Patel, Laura'
'White, Andrew J. P.'
_publ_section_title
;
 Aluminium complexes with thio-phosphorus ligands: syntheses and
 characterisations of [Al2(CyPS3)2(CyPHS2)2] and [Al(S2PPh2)3]
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              5705
_journal_page_last               5707
_journal_paper_doi               10.1039/b813427h
_journal_year                    2008
_chemical_formula_moiety         'C24 H54 Li2 N4 P2 S4'
_chemical_formula_sum            'C24 H54 Li2 N4 P2 S4'
_chemical_formula_weight         602.77
_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                95.329(15)
_cell_angle_beta                 101.726(14)
_cell_angle_gamma                101.575(18)
_cell_formula_units_Z            2
_cell_length_a                   9.0103(17)
_cell_length_b                   10.680(2)
_cell_length_c                   18.826(3)
_cell_measurement_reflns_used    25117
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.6747
_cell_measurement_theta_min      2.4186
_cell_volume                     1720.8(6)
_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 8.2556
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54248
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36354
_diffrn_reflns_theta_full        71.33
_diffrn_reflns_theta_max         71.33
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    3.549
_exptl_absorpt_correction_T_max  1.10343
_exptl_absorpt_correction_T_min  0.90873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'blocky needles'
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0451
_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)+(0.0348P)²+3.1233P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5862
_reflns_number_total             6577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813427h.txt
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004793
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 0.1893(6) 0.4882(5) 0.1591(3) 0.0388(11) Uani 1 1 d . . .
Li2 Li 0.3148(6) 1.0336(5) 0.3453(3) 0.0385(11) Uani 1 1 d . . .
P1 P 0.27781(8) 0.71267(7) 0.30123(4) 0.02826(16) Uani 1 1 d . . .
P2 P 0.23216(8) 0.80091(7) 0.19746(4) 0.02886(16) Uani 1 1 d . . .
S1 S 0.37354(9) 0.56541(7) 0.27757(4) 0.03577(18) Uani 1 1 d . . .
S2 S 0.39866(9) 0.84672(7) 0.38499(4) 0.03636(18) Uani 1 1 d . . .
S3 S 0.06474(9) 0.66700(7) 0.12796(4) 0.03662(18) Uani 1 1 d . . .
S4 S 0.18896(9) 0.97538(7) 0.21589(4) 0.03646(18) Uani 1 1 d . . .
N1 N 0.3054(3) 0.3930(3) 0.09476(14) 0.0393(6) Uani 1 1 d . . .
N2 N 0.0112(3) 0.3212(2) 0.13616(14) 0.0386(6) Uani 1 1 d . . .
N3 N 0.4949(3) 1.2002(2) 0.37367(14) 0.0356(5) Uani 1 1 d . . .
N4 N 0.1925(3) 1.1286(2) 0.40869(14) 0.0355(5) Uani 1 1 d . . .
C1 C 0.0836(3) 0.6454(3) 0.31560(16) 0.0330(6) Uani 1 1 d . . .
H1A H 0.0250 0.5842 0.2706 0.040 Uiso 1 1 calc R . .
C2 C -0.0114(4) 0.7456(3) 0.32697(19) 0.0412(7) Uani 1 1 d . . .
H2A H -0.0233 0.7929 0.2841 0.049 Uiso 1 1 calc R . .
H2B H 0.0440 0.8086 0.3709 0.049 Uiso 1 1 calc R . .
C3 C -0.1721(4) 0.6808(4) 0.3368(2) 0.0523(9) Uani 1 1 d . . .
H3A H -0.2295 0.7478 0.3469 0.063 Uiso 1 1 calc R . .
H3B H -0.2316 0.6249 0.2908 0.063 Uiso 1 1 calc R . .
C4 C -0.1594(4) 0.6002(4) 0.3992(2) 0.0528(9) Uani 1 1 d . . .
H4A H -0.1112 0.6577 0.4461 0.063 Uiso 1 1 calc R . .
H4B H -0.2649 0.5549 0.4019 0.063 Uiso 1 1 calc R . .
C5 C -0.0627(4) 0.5020(3) 0.3887(2) 0.0518(9) Uani 1 1 d . . .
H5A H -0.1168 0.4386 0.3447 0.062 Uiso 1 1 calc R . .
H5B H -0.0513 0.4547 0.4316 0.062 Uiso 1 1 calc R . .
C6 C 0.0980(4) 0.5671(3) 0.37966(18) 0.0417(7) Uani 1 1 d . . .
H6A H 0.1571 0.5008 0.3707 0.050 Uiso 1 1 calc R . .
H6B H 0.1559 0.6248 0.4253 0.050 Uiso 1 1 calc R . .
C7 C 0.4124(3) 0.8120(3) 0.16442(16) 0.0333(6) Uani 1 1 d . . .
H7A H 0.4288 0.7223 0.1571 0.040 Uiso 1 1 calc R . .
C8 C 0.5592(4) 0.8937(3) 0.21735(18) 0.0429(7) Uani 1 1 d . . .
H8A H 0.5480 0.9838 0.2262 0.052 Uiso 1 1 calc R . .
H8B H 0.5729 0.8597 0.2648 0.052 Uiso 1 1 calc R . .
C9 C 0.7011(4) 0.8911(4) 0.1857(2) 0.0533(9) Uani 1 1 d . . .
H9A H 0.7938 0.9485 0.2193 0.064 Uiso 1 1 calc R . .
H9B H 0.7186 0.8024 0.1823 0.064 Uiso 1 1 calc R . .
C10 C 0.6823(4) 0.9341(4) 0.1105(2) 0.0559(9) Uani 1 1 d . . .
H10A H 0.7733 0.9244 0.0903 0.067 Uiso 1 1 calc R . .
H10B H 0.6789 1.0265 0.1149 0.067 Uiso 1 1 calc R . .
C11 C 0.5344(4) 0.8553(4) 0.05822(19) 0.0500(8) Uani 1 1 d . . .
H11A H 0.5438 0.7648 0.0487 0.060 Uiso 1 1 calc R . .
H11B H 0.5213 0.8901 0.0110 0.060 Uiso 1 1 calc R . .
C12 C 0.3918(4) 0.8583(3) 0.08947(17) 0.0417(7) Uani 1 1 d . . .
H12A H 0.2985 0.8022 0.0556 0.050 Uiso 1 1 calc R . .
H12B H 0.3756 0.9475 0.0941 0.050 Uiso 1 1 calc R . .
C13 C 0.4733(4) 0.4066(4) 0.1217(2) 0.0552(9) Uani 1 1 d . . .
H13A H 0.5131 0.3569 0.0864 0.083 Uiso 1 1 calc R . .
H13B H 0.4928 0.3741 0.1690 0.083 Uiso 1 1 calc R . .
H13C H 0.5263 0.4978 0.1278 0.083 Uiso 1 1 calc R . .
C14 C 0.2776(4) 0.4427(4) 0.02476(18) 0.0482(8) Uani 1 1 d . . .
H14A H 0.3296 0.4014 -0.0087 0.072 Uiso 1 1 calc R . .
H14B H 0.3191 0.5362 0.0325 0.072 Uiso 1 1 calc R . .
H14C H 0.1655 0.4237 0.0034 0.072 Uiso 1 1 calc R . .
C15 C 0.2236(5) 0.2573(3) 0.0877(2) 0.0545(9) Uani 1 1 d . . .
H15A H 0.2640 0.2208 0.1322 0.065 Uiso 1 1 calc R . .
H15B H 0.2453 0.2079 0.0453 0.065 Uiso 1 1 calc R . .
C16 C 0.0510(5) 0.2415(3) 0.07746(19) 0.0540(9) Uani 1 1 d . . .
H16A H 0.0081 0.2664 0.0295 0.065 Uiso 1 1 calc R . .
H16B H 0.0024 0.1496 0.0771 0.065 Uiso 1 1 calc R . .
C17 C -0.1471(4) 0.3399(4) 0.1132(3) 0.0618(11) Uani 1 1 d . . .
H17A H -0.2213 0.2562 0.1040 0.093 Uiso 1 1 calc R . .
H17B H -0.1564 0.3801 0.0682 0.093 Uiso 1 1 calc R . .
H17C H -0.1697 0.3960 0.1519 0.093 Uiso 1 1 calc R . .
C18 C 0.0226(4) 0.2606(3) 0.20272(18) 0.0428(7) Uani 1 1 d . . .
H18A H -0.0590 0.1813 0.1943 0.064 Uiso 1 1 calc R . .
H18B H 0.0095 0.3202 0.2427 0.064 Uiso 1 1 calc R . .
H18C H 0.1248 0.2397 0.2159 0.064 Uiso 1 1 calc R . .
C19 C 0.5025(4) 1.2629(3) 0.30843(18) 0.0426(7) Uani 1 1 d . . .
H19A H 0.5862 1.3411 0.3208 0.064 Uiso 1 1 calc R . .
H19B H 0.4032 1.2859 0.2900 0.064 Uiso 1 1 calc R . .
H19C H 0.5233 1.2037 0.2706 0.064 Uiso 1 1 calc R . .
C20 C 0.6471(4) 1.1745(3) 0.4039(2) 0.0503(9) Uani 1 1 d . . .
H20A H 0.7258 1.2558 0.4161 0.075 Uiso 1 1 calc R . .
H20B H 0.6742 1.1165 0.3675 0.075 Uiso 1 1 calc R . .
H20C H 0.6431 1.1338 0.4482 0.075 Uiso 1 1 calc R . .
C21 C 0.4485(4) 1.2808(3) 0.42933(18) 0.0436(7) Uani 1 1 d . . .
H21A H 0.4980 1.3726 0.4300 0.052 Uiso 1 1 calc R . .
H21B H 0.4852 1.2566 0.4783 0.052 Uiso 1 1 calc R . .
C22 C 0.2746(4) 1.2639(3) 0.41332(19) 0.0428(7) Uani 1 1 d . . .
H22A H 0.2467 1.3170 0.4524 0.051 Uiso 1 1 calc R . .
H22B H 0.2397 1.2957 0.3664 0.051 Uiso 1 1 calc R . .
C23 C 0.2142(4) 1.0841(3) 0.48050(18) 0.0443(7) Uani 1 1 d . . .
H23A H 0.1581 1.1271 0.5111 0.066 Uiso 1 1 calc R . .
H23B H 0.3253 1.1048 0.5041 0.066 Uiso 1 1 calc R . .
H23C H 0.1738 0.9905 0.4744 0.066 Uiso 1 1 calc R . .
C24 C 0.0263(4) 1.1153(4) 0.3790(2) 0.0500(8) Uani 1 1 d . . .
H24A H -0.0168 1.1634 0.4136 0.075 Uiso 1 1 calc R . .
H24B H -0.0266 1.0239 0.3713 0.075 Uiso 1 1 calc R . .
H24C H 0.0110 1.1496 0.3322 0.075 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 0.0181 0.0091 '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 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
N1 Li1 N2 87.9(2) . . ?
N1 Li1 S1 106.0(2) . . ?
N2 Li1 S1 125.3(3) . . ?
N1 Li1 S3 126.4(3) . . ?
N2 Li1 S3 106.4(2) . . ?
S1 Li1 S3 106.29(19) . . ?
N3 Li2 N4 87.5(2) . . ?
N3 Li2 S2 112.1(2) . . ?
N4 Li2 S2 118.7(2) . . ?
N3 Li2 S4 116.6(2) . . ?
N4 Li2 S4 115.1(2) . . ?
S2 Li2 S4 106.5(2) . . ?
N3 Li2 C22 58.18(16) . . ?
N4 Li2 C22 31.17(12) . . ?
S2 Li2 C22 136.0(2) . . ?
S4 Li2 C22 116.0(2) . . ?
C1 P1 S2 110.39(10) . . ?
C1 P1 S1 107.85(10) . . ?
S2 P1 S1 116.99(5) . . ?
C1 P1 P2 104.60(10) . . ?
S2 P1 P2 110.67(4) . . ?
S1 P1 P2 105.53(4) . . ?
C7 P2 S4 110.51(10) . . ?
C7 P2 S3 107.86(10) . . ?
S4 P2 S3 116.85(5) . . ?
C7 P2 P1 104.44(10) . . ?
S4 P2 P1 111.60(4) . . ?
S3 P2 P1 104.70(4) . . ?
P1 S1 Li1 94.19(13) . . ?
P1 S2 Li2 100.24(13) . . ?
P2 S3 Li1 93.93(13) . . ?
P2 S4 Li2 100.21(13) . . ?
C14 N1 C13 109.1(3) . . ?
C14 N1 C15 111.3(3) . . ?
C13 N1 C15 110.2(3) . . ?
C14 N1 Li1 105.1(3) . . ?
C13 N1 Li1 117.9(3) . . ?
C15 N1 Li1 103.1(2) . . ?
C18 N2 C17 108.7(3) . . ?
C18 N2 C16 110.9(3) . . ?
C17 N2 C16 110.7(3) . . ?
C18 N2 Li1 106.7(2) . . ?
C17 N2 Li1 116.0(3) . . ?
C16 N2 Li1 103.7(2) . . ?
C19 N3 C20 109.2(3) . . ?
C19 N3 C21 111.3(2) . . ?
C20 N3 C21 110.0(3) . . ?
C19 N3 Li2 108.5(2) . . ?
C20 N3 Li2 113.5(2) . . ?
C21 N3 Li2 104.3(2) . . ?
C24 N4 C23 108.9(3) . . ?
C24 N4 C22 109.6(3) . . ?
C23 N4 C22 111.7(3) . . ?
C24 N4 Li2 117.5(3) . . ?
C23 N4 Li2 108.0(2) . . ?
C22 N4 Li2 101.1(2) . . ?
C2 C1 C6 110.5(3) . . ?
C2 C1 P1 114.3(2) . . ?
C6 C1 P1 109.7(2) . . ?
C1 C2 C3 110.7(3) . . ?
C4 C3 C2 111.3(3) . . ?
C5 C4 C3 111.4(3) . . ?
C4 C5 C6 111.1(3) . . ?
C5 C6 C1 110.5(3) . . ?
C12 C7 C8 110.9(3) . . ?
C12 C7 P2 110.1(2) . . ?
C8 C7 P2 115.1(2) . . ?
C9 C8 C7 110.4(3) . . ?
C10 C9 C8 112.0(3) . . ?
C9 C10 C11 111.4(3) . . ?
C10 C11 C12 111.5(3) . . ?
C11 C12 C7 110.5(3) . . ?
N1 C15 C16 112.4(3) . . ?
N2 C16 C15 111.8(3) . . ?
N3 C21 C22 110.9(3) . . ?
N4 C22 C21 112.6(3) . . ?
N4 C22 Li2 47.77(17) . . ?
C21 C22 Li2 76.6(2) . . ?
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
Li1 N1 2.075(6) . ?
Li1 N2 2.091(6) . ?
Li1 S1 2.452(5) . ?
Li1 S3 2.459(5) . ?
Li2 N3 2.097(6) . ?
Li2 N4 2.105(6) . ?
Li2 S2 2.402(5) . ?
Li2 S4 2.433(5) . ?
Li2 C22 2.789(6) . ?
P1 C1 1.837(3) . ?
P1 S2 1.9948(11) . ?
P1 S1 1.9966(11) . ?
P1 P2 2.2460(10) . ?
P2 C7 1.840(3) . ?
P2 S4 1.9924(11) . ?
P2 S3 2.0044(11) . ?
N1 C14 1.459(4) . ?
N1 C13 1.468(4) . ?
N1 C15 1.469(4) . ?
N2 C18 1.457(4) . ?
N2 C17 1.464(4) . ?
N2 C16 1.477(4) . ?
N3 C19 1.459(4) . ?
N3 C20 1.464(4) . ?
N3 C21 1.472(4) . ?
N4 C24 1.461(4) . ?
N4 C23 1.463(4) . ?
N4 C22 1.471(4) . ?
C1 C2 1.524(4) . ?
C1 C6 1.529(4) . ?
C2 C3 1.529(5) . ?
C3 C4 1.519(5) . ?
C4 C5 1.516(5) . ?
C5 C6 1.525(5) . ?
C7 C12 1.526(4) . ?
C7 C8 1.531(4) . ?
C8 C9 1.520(5) . ?
C9 C10 1.517(5) . ?
C10 C11 1.522(5) . ?
C11 C12 1.523(5) . ?
C15 C16 1.500(6) . ?
C21 C22 1.504(5) . ?
