#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:29:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179751 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/47/7004792.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_7004792
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 H46 Al2 P4 S10, C7 H8'
_chemical_formula_sum            'C31 H54 Al2 P4 S10'
_chemical_formula_weight         925.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90.7425(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8035(3)
_cell_length_b                   13.4034(3)
_cell_length_c                   11.7729(2)
_cell_measurement_reflns_used    15125
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.5803
_cell_measurement_theta_min      3.7168
_cell_volume                     2177.97(8)
_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 15.9863
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.936
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21647
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.65
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubes
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         7459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_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+1.8704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                5860
_reflns_number_total             7459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813427h.txt
_cod_data_source_block           Compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/c
_cod_database_code               7004792
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al 0.52274(5) 0.45331(4) 0.35396(5) 0.03564(13) Uani 1 1 d . . .
P1 P 0.33388(4) 0.43993(4) 0.48502(4) 0.03309(11) Uani 1 1 d . . .
S1 S 0.46553(4) 0.38390(3) 0.54130(4) 0.03286(10) Uani 1 1 d . . .
S2 S 0.35300(4) 0.47480(4) 0.32009(4) 0.04212(13) Uani 1 1 d . . .
S3 S 0.31261(4) 0.56064(4) 0.58419(4) 0.03966(12) Uani 1 1 d . . .
P2 P 0.56130(5) 0.37213(4) 0.12645(4) 0.04198(14) Uani 1 1 d . . .
H2 H 0.4962(19) 0.353(2) 0.048(2) 0.054(8) Uiso 1 1 d . . .
S4 S 0.53094(5) 0.29284(4) 0.26711(4) 0.04700(15) Uani 1 1 d . . .
S5 S 0.55858(4) 0.51809(4) 0.16904(4) 0.03947(12) Uani 1 1 d . . .
C1 C 0.23925(14) 0.34639(14) 0.50147(15) 0.0327(4) Uani 1 1 d . . .
H1A H 0.1782 0.3739 0.4672 0.039 Uiso 1 1 calc R . .
C2 C 0.26418(17) 0.25044(16) 0.43757(17) 0.0420(5) Uani 1 1 d . . .
H2A H 0.2738 0.2658 0.3562 0.050 Uiso 1 1 calc R . .
H2B H 0.3253 0.2223 0.4686 0.050 Uiso 1 1 calc R . .
C3 C 0.18300(19) 0.17394(17) 0.44923(18) 0.0472(5) Uani 1 1 d . . .
H3A H 0.1239 0.1992 0.4104 0.057 Uiso 1 1 calc R . .
H3B H 0.2022 0.1111 0.4116 0.057 Uiso 1 1 calc R . .
C4 C 0.16070(18) 0.15300(16) 0.57278(18) 0.0443(5) Uani 1 1 d . . .
H4A H 0.1045 0.1073 0.5770 0.053 Uiso 1 1 calc R . .
H4B H 0.2170 0.1195 0.6092 0.053 Uiso 1 1 calc R . .
C5 C 0.13838(18) 0.24814(17) 0.63648(19) 0.0459(5) Uani 1 1 d . . .
H5A H 0.1283 0.2323 0.7176 0.055 Uiso 1 1 calc R . .
H5B H 0.0776 0.2774 0.6058 0.055 Uiso 1 1 calc R . .
C6 C 0.22003(17) 0.32436(16) 0.62661(16) 0.0407(4) Uani 1 1 d . . .
H6A H 0.2796 0.2979 0.6634 0.049 Uiso 1 1 calc R . .
H6B H 0.2018 0.3867 0.6660 0.049 Uiso 1 1 calc R . .
C7 C 0.67432(19) 0.33470(17) 0.06265(18) 0.0470(5) Uani 1 1 d . . .
H7A H 0.6687 0.2624 0.0425 0.056 Uiso 1 1 calc R . .
C8 C 0.69260(19) 0.3923(2) -0.04707(19) 0.0541(6) Uani 1 1 d . . .
H8A H 0.6382 0.3809 -0.1012 0.065 Uiso 1 1 calc R . .
H8B H 0.6959 0.4646 -0.0304 0.065 Uiso 1 1 calc R . .
C9 C 0.7869(2) 0.3587(3) -0.1005(2) 0.0650(7) Uani 1 1 d . . .
H9A H 0.7804 0.2883 -0.1250 0.078 Uiso 1 1 calc R . .
H9B H 0.7991 0.3996 -0.1689 0.078 Uiso 1 1 calc R . .
C10 C 0.8722(2) 0.3680(2) -0.0192(3) 0.0626(7) Uani 1 1 d . . .
H10A H 0.9310 0.3410 -0.0555 0.075 Uiso 1 1 calc R . .
H10B H 0.8839 0.4393 -0.0018 0.075 Uiso 1 1 calc R . .
C11 C 0.8537(3) 0.3121(2) 0.0894(3) 0.0715(8) Uani 1 1 d . . .
H11A H 0.9086 0.3230 0.1429 0.086 Uiso 1 1 calc R . .
H11B H 0.8499 0.2398 0.0729 0.086 Uiso 1 1 calc R . .
C12 C 0.7599(2) 0.3457(2) 0.1451(2) 0.0549(6) Uani 1 1 d . . .
H12A H 0.7484 0.3049 0.2137 0.066 Uiso 1 1 calc R . .
H12B H 0.7660 0.4163 0.1688 0.066 Uiso 1 1 calc R . .
C20 C -0.0150(9) 0.5126(9) 0.6857(10) 0.102(7) Uani 0.50 1 d P A -1
H20A H -0.0841 0.5095 0.7035 0.153 Uiso 0.50 1 calc PR A -1
H20B H 0.0116 0.5767 0.7115 0.153 Uiso 0.50 1 calc PR A -1
H20C H 0.0193 0.4581 0.7245 0.153 Uiso 0.50 1 calc PR A -1
C21 C -0.0023(3) 0.5030(4) 0.5611(4) 0.0572(13) Uani 0.50 1 d PG A -1
C22 C -0.0607(3) 0.4375(4) 0.4994(5) 0.079(5) Uani 0.50 1 d PG A -1
H22A H -0.1085 0.3991 0.5370 0.095 Uiso 0.50 1 calc PR A -1
C23 C -0.0492(4) 0.4280(4) 0.3828(5) 0.104(3) Uani 0.50 1 d PG A -1
H23A H -0.0891 0.3832 0.3407 0.125 Uiso 0.50 1 calc PR A -1
C24 C 0.0208(5) 0.4841(5) 0.3278(4) 0.087(6) Uani 0.50 1 d PG A -1
H24A H 0.0286 0.4776 0.2481 0.105 Uiso 0.50 1 calc PR A -1
C25 C 0.0791(4) 0.5497(4) 0.3894(4) 0.077(2) Uani 0.50 1 d PG A -1
H25A H 0.1269 0.5880 0.3519 0.092 Uiso 0.50 1 calc PR A -1
C26 C 0.0676(3) 0.5591(3) 0.5061(4) 0.079(4) Uani 0.50 1 d PG A -1
H26A H 0.1075 0.6039 0.5482 0.094 Uiso 0.50 1 calc PR A -1
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'
Al Al 0.0645 0.0514 '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
_geom_angle_publ_flag
S3 Al S4 90.57(3) 3_666 . ?
S3 Al S2 171.53(3) 3_666 . ?
S4 Al S2 95.11(3) . . ?
S3 Al S5 95.65(3) 3_666 . ?
S4 Al S5 85.75(3) . . ?
S2 Al S5 91.04(3) . . ?
S3 Al S1 82.13(2) 3_666 3_666 ?
S4 Al S1 172.45(4) . 3_666 ?
S2 Al S1 91.95(3) . 3_666 ?
S5 Al S1 96.80(2) . 3_666 ?
S3 Al S1 90.68(2) 3_666 . ?
S4 Al S1 93.39(2) . . ?
S2 Al S1 82.72(3) . . ?
S5 Al S1 173.61(3) . . ?
S1 Al S1 84.85(2) 3_666 . ?
C1 P1 S2 111.38(6) . . ?
C1 P1 S3 112.33(7) . . ?
S2 P1 S3 113.12(3) . . ?
C1 P1 S1 110.14(7) . . ?
S2 P1 S1 105.50(3) . . ?
S3 P1 S1 103.86(3) . . ?
P1 S1 Al 83.83(3) . 3_666 ?
P1 S1 Al 82.53(2) . . ?
Al S1 Al 95.15(2) 3_666 . ?
P1 S2 Al 87.23(3) . . ?
P1 S3 Al 88.20(3) . 3_666 ?
C7 P2 S4 112.58(8) . . ?
C7 P2 S5 112.96(7) . . ?
S4 P2 S5 107.57(3) . . ?
P2 S4 Al 83.58(3) . . ?
P2 S5 Al 83.08(3) . . ?
C6 C1 C2 110.74(16) . . ?
C6 C1 P1 111.64(13) . . ?
C2 C1 P1 111.07(14) . . ?
C3 C2 C1 110.49(18) . . ?
C4 C3 C2 111.64(17) . . ?
C5 C4 C3 111.37(18) . . ?
C4 C5 C6 111.78(18) . . ?
C5 C6 C1 109.88(16) . . ?
C12 C7 C8 110.7(2) . . ?
C12 C7 P2 111.93(16) . . ?
C8 C7 P2 111.30(18) . . ?
C9 C8 C7 110.6(2) . . ?
C10 C9 C8 112.2(2) . . ?
C11 C10 C9 110.9(3) . . ?
C10 C11 C12 111.8(2) . . ?
C7 C12 C11 110.6(2) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 C20 119.7(6) . . ?
C26 C21 C20 120.3(6) . . ?
C23 C22 C21 120.0 . . ?
C24 C23 C22 120.0 . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C26 120.0 . . ?
C25 C26 C21 120.0 . . ?
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
Al S3 2.3849(8) 3_666 ?
Al S4 2.3849(8) . ?
Al S2 2.3890(9) . ?
Al S5 2.4012(7) . ?
Al S1 2.5105(7) 3_666 ?
Al S1 2.5296(7) . ?
P1 C1 1.8226(18) . ?
P1 S2 2.0178(6) . ?
P1 S3 2.0189(7) . ?
P1 S1 2.0674(7) . ?
S1 Al 2.5105(7) 3_666 ?
S3 Al 2.3849(8) 3_666 ?
P2 C7 1.811(3) . ?
P2 S4 2.0162(7) . ?
P2 S5 2.0201(8) . ?
C1 C6 1.529(3) . ?
C1 C2 1.531(3) . ?
C2 C3 1.526(3) . ?
C3 C4 1.517(3) . ?
C4 C5 1.513(3) . ?
C5 C6 1.527(3) . ?
C7 C12 1.526(3) . ?
C7 C8 1.528(3) . ?
C8 C9 1.521(4) . ?
C9 C10 1.514(4) . ?
C10 C11 1.506(4) . ?
C11 C12 1.526(4) . ?
C20 C21 1.486(10) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
