#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/74/2007483.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007483
loop_
_publ_author_name
'Rijnberk, Herme'
'Näther, Christian'
'Schur, Michael'
'Jeß, Inke'
'Bensch, Wolfgang'
_publ_section_title
;
 [Ph₄P]₂[Sb₂S₁₅]
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              920
_journal_page_last               923
_journal_paper_doi               10.1107/S0108270198001188
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C24 H20 P)2 [Sb2 S15]'
_chemical_formula_sum            'C48 H40 P2 S15 Sb2'
_chemical_formula_weight         1403.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.26(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.267(3)
_cell_length_b                   12.122(2)
_cell_length_c                   27.522(4)
_cell_measurement_reflns_used    82
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      15
_cell_volume                     5787.4(17)
_computing_cell_refinement       DIF-4
_computing_data_collection       ' DIF-4 (Stoe, 199?)'
_computing_data_reduction        'REDU-4 (Stoe, 199?)'
_computing_molecular_graphics    'SHELXTL/PC (Siemens, 1990)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE AED-II 4-circle diffractometer'
_diffrn_measurement_method       ω/θ
_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  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7493
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  120
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   'psi-scan (XEMP; Siemens, 1990)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_meas      ?
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    'H atoms: see text below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_obs          .0257
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0259P)²+4.0975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0629
_refine_ls_wR_factor_obs         .0577
_reflns_number_observed          5143
_reflns_number_total             6655
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1145.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0259P)^2^+4.0975P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0259P)^2^+4.0975P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5787.4(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2007483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Sb .468861(9) .679888(14) .180614(5) .04365(5) Uani d . 1 . Sb
S1 .5000 .81365(8) .2500 .0662(3) Uani d S 1 . S
S2 .59189(4) .55840(7) .23610(3) .0656(2) Uani d . 1 . S
S3 .52814(6) .41445(7) .22284(3) .0801(2) Uani d . 1 . S
S4 .34889(4) .81619(6) .14109(3) .0560(2) Uani d . 1 . S
S5 .32197(4) .75659(7) .06773(3) .0650(2) Uani d . 1 . S
S6 .40229(5) .82006(7) .03782(2) .0663(2) Uani d . 1 . S
S7 .50051(5) .72816(8) .06779(3) .0703(2) Uani d . 1 . S
S8 .55182(4) .78938(7) .14022(3) .0647(2) Uani d . 1 . S
P .29348(3) .19976(5) .12954(2) .03780(13) Uani d . 1 . P
C1 .31953(13) .1813(2) .19766(8) .0461(5) Uani d . 1 . C
C2 .2768(2) .2332(3) .22415(10) .0655(8) Uani d . 1 . C
H2 .2360(2) .2791(3) .20714(10) .079 Uiso calc R 1 . H
C3 .2950(2) .2162(4) .27658(11) .0837(11) Uani d . 1 . C
H3 .2669(2) .2517(4) .29492(11) .100 Uiso calc R 1 . H
C4 .3537(2) .1481(4) .30082(12) .0925(13) Uani d . 1 . C
H4 .3657(2) .1374(4) .33591(12) .111 Uiso calc R 1 . H
C5 .3952(2) .0953(4) .27491(12) .0951(13) Uani d . 1 . C
H5 .4348(2) .0478(4) .29214(12) .114 Uiso calc R 1 . H
C6 .3788(2) .1120(3) .22267(10) .0733(9) Uani d . 1 . C
H6 .4076(2) .0766(3) .20482(10) .088 Uiso calc R 1 . H
C11 .25044(12) .3328(2) .11322(8) .0386(5) Uani d . 1 . C
C12 .28480(15) .4241(2) .14202(9) .0508(6) Uani d . 1 . C
H12 .32640(15) .4147(2) .17157(9) .061 Uiso calc R 1 . H
C13 .2575(2) .5279(2) .12693(11) .0579(7) Uani d . 1 . C
H13 .2807(2) .5888(2) .14615(11) .069 Uiso calc R 1 . H
C14 .1957(2) .5422(2) .08334(11) .0579(7) Uani d . 1 . C
H14 .1778(2) .6129(2) .07292(11) .070 Uiso calc R 1 . H
C15 .1604(2) .4524(2) .05516(10) .0573(7) Uani d . 1 . C
H15 .1180(2) .4625(2) .02614(10) .069 Uiso calc R 1 . H
C16 .18739(13) .3478(2) .06966(9) .0457(6) Uani d . 1 . C
H16 .16358(13) .2872(2) .05039(9) .055 Uiso calc R 1 . H
C21 .37557(12) .1940(2) .10645(8) .0401(5) Uani d . 1 . C
C22 .39690(15) .2872(2) .08500(11) .0547(6) Uani d . 1 . C
H22 .37117(15) .3536(2) .08455(11) .066 Uiso calc R 1 . H
C23 .4566(2) .2810(3) .06430(12) .0654(8) Uani d . 1 . C
H23 .4700(2) .3429(3) .04900(12) .078 Uiso calc R 1 . H
C24 .4959(2) .1848(3) .06614(11) .0617(7) Uani d . 1 . C
H24 .5369(2) .1821(3) .05290(11) .074 Uiso calc R 1 . H
C25 .47558(15) .0913(2) .08745(10) .0557(6) Uani d . 1 . C
H25 .50275(15) .0260(2) .08866(10) .067 Uiso calc R 1 . H
C26 .41430(14) .0955(2) .10708(9) .0484(6) Uani d . 1 . C
H26 .39928(14) .0323(2) .12063(9) .058 Uiso calc R 1 . H
C31 .22737(13) .0942(2) .09791(9) .0419(5) Uani d . 1 . C
C32 .2214(2) .0634(2) .04798(10) .0541(6) Uani d . 1 . C
H32 .2531(2) .0957(2) .03136(10) .065 Uiso calc R 1 . H
C33 .1681(2) -.0150(3) .02348(12) .0667(8) Uani d . 1 . C
H33 .1639(2) -.0358(3) -.00983(12) .080 Uiso calc R 1 . H
C34 .1216(2) -.0624(3) .04787(14) .0830(10) Uani d . 1 . C
H34 .0856(2) -.1151(3) .03098(14) .100 Uiso calc R 1 . H
C35 .1275(2) -.0330(3) .09731(14) .0831(11) Uani d . 1 . C
H35 .0958(2) -.0662(3) .11371(14) .100 Uiso calc R 1 . H
C36 .1805(2) .0459(2) .12256(11) .0593(7) Uani d . 1 . C
H36 .1845(2) .0661(2) .15589(11) .071 Uiso calc R 1 . H
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'
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'
Sb Sb -0.5866 1.5461 '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_site_symmetry_1
_geom_angle
_geom_angle_publ_flag
S1 Sb S8 . 88.30(3) y
S1 Sb S4 . 82.44(3) y
S8 Sb S4 . 91.40(3) y
S1 Sb S2 . 88.36(3) y
S8 Sb S2 . 91.58(3) y
S4 Sb S2 . 170.24(2) y
Sb S1 Sb 2_655 96.41(4) y
S3 S2 Sb . 92.14(4) y
S3 S3 S2 2_655 104.68(4) y
S5 S4 Sb . 95.47(4) y
S6 S5 S4 . 106.41(5) y
S5 S6 S7 . 106.33(5) y
S6 S7 S8 . 105.61(5) y
S7 S8 Sb . 94.76(4) y
C31 P C11 . 110.28(11) n
C31 P C1 . 109.64(11) n
C11 P C1 . 109.04(12) n
C31 P C21 . 108.05(11) n
C11 P C21 . 107.16(10) n
C1 P C21 . 112.64(11) n
C6 C1 C2 . 120.2(2) n
C6 C1 P . 120.6(2) n
C2 C1 P . 119.1(2) n
C1 C2 C3 . 119.4(3) n
C4 C3 C2 . 119.8(3) n
C3 C4 C5 . 121.1(3) n
C4 C5 C6 . 120.1(3) n
C1 C6 C5 . 119.3(3) n
C16 C11 C12 . 119.4(2) n
C16 C11 P . 121.0(2) n
C12 C11 P . 119.3(2) n
C13 C12 C11 . 120.1(2) n
C12 C13 C14 . 120.1(3) n
C15 C14 C13 . 120.3(3) n
C16 C15 C14 . 120.3(2) n
C15 C16 C11 . 119.8(2) n
C26 C21 C22 . 119.8(2) n
C26 C21 P . 120.4(2) n
C22 C21 P . 119.6(2) n
C23 C22 C21 . 119.6(3) n
C24 C23 C22 . 120.5(3) n
C23 C24 C25 . 120.6(2) n
C24 C25 C26 . 119.6(3) n
C21 C26 C25 . 119.8(2) n
C36 C31 C32 . 120.2(2) n
C36 C31 P . 119.6(2) n
C32 C31 P . 120.2(2) n
C33 C32 C31 . 119.5(2) n
C34 C33 C32 . 120.3(3) n
C33 C34 C35 . 120.6(3) n
C34 C35 C36 . 120.1(3) n
C31 C36 C35 . 119.4(3) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sb S1 . 2.4328(7) y
Sb S8 . 2.5200(8) y
Sb S4 . 2.6874(8) y
Sb S2 . 2.7205(9) y
S1 Sb 2_655 2.4328(7) y
S2 S3 . 2.0659(13) y
S3 S3 2_655 2.063(2) y
S4 S5 . 2.0538(11) y
S5 S6 . 2.0441(12) y
S6 S7 . 2.0526(13) y
S7 S8 . 2.0570(11) y
P C31 . 1.788(2) n
P C11 . 1.789(2) n
P C1 . 1.798(2) n
P C21 . 1.804(2) n
C1 C6 . 1.373(4) n
C1 C2 . 1.377(4) n
C2 C3 . 1.391(4) n
C3 C4 . 1.351(5) n
C4 C5 . 1.354(5) n
C5 C6 . 1.389(4) n
C11 C16 . 1.390(3) n
C11 C12 . 1.391(3) n
C12 C13 . 1.369(4) n
C13 C14 . 1.376(4) n
C14 C15 . 1.374(4) n
C15 C16 . 1.374(4) n
C21 C26 . 1.385(3) n
C21 C22 . 1.386(3) n
C22 C23 . 1.382(4) n
C23 C24 . 1.362(4) n
C24 C25 . 1.379(4) n
C25 C26 . 1.388(3) n
C31 C36 . 1.378(3) n
C31 C32 . 1.395(3) n
C32 C33 . 1.376(4) n
C33 C34 . 1.364(4) n
C34 C35 . 1.378(5) n
C35 C36 . 1.383(4) n
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_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
S8 Sb S1 Sb 2_655 -132.86(2) n
S4 Sb S1 Sb 2_655 135.50(2) n
S2 Sb S1 Sb 2_655 -41.23(2) n
S1 Sb S2 S3 . 133.13(4) n
S8 Sb S2 S3 . -138.62(4) n
S4 Sb S2 S3 . 113.66(14) n
Sb S2 S3 S3 2_655 -83.21(6) n
S1 Sb S4 S5 . 163.01(4) n
S8 Sb S4 S5 . 74.92(4) n
S2 Sb S4 S5 . -177.36(13) n
Sb S4 S5 S6 . -76.09(5) n
S4 S5 S6 S7 . 77.87(6) n
S5 S6 S7 S8 . -79.82(6) n
S6 S7 S8 Sb . 82.21(5) n
S1 Sb S8 S7 . -158.53(4) n
S4 Sb S8 S7 . -76.14(4) n
S2 Sb S8 S7 . 113.16(4) n
C31 P C1 C6 . 85.9(3) n
C11 P C1 C6 . -153.3(2) n
C21 P C1 C6 . -34.5(3) n
C31 P C1 C2 . -90.9(2) n
C11 P C1 C2 . 29.9(3) n
C21 P C1 C2 . 148.8(2) n
C6 C1 C2 C3 . 1.1(5) n
P C1 C2 C3 . 177.9(3) n
C1 C2 C3 C4 . -0.9(6) n
C2 C3 C4 C5 . -0.2(6) n
C3 C4 C5 C6 . 1.1(7) n
C2 C1 C6 C5 . -0.2(5) n
P C1 C6 C5 . -176.9(3) n
C4 C5 C6 C1 . -0.9(6) n
C31 P C11 C16 . -20.0(2) n
C1 P C11 C16 . -140.5(2) n
C21 P C11 C16 . 97.3(2) n
C31 P C11 C12 . 165.8(2) n
C1 P C11 C12 . 45.3(2) n
C21 P C11 C12 . -76.9(2) n
C16 C11 C12 C13 . -1.2(4) n
P C11 C12 C13 . 173.1(2) n
C11 C12 C13 C14 . 0.3(4) n
C12 C13 C14 C15 . 1.0(4) n
C13 C14 C15 C16 . -1.3(4) n
C14 C15 C16 C11 . 0.4(4) n
C12 C11 C16 C15 . 0.8(4) n
P C11 C16 C15 . -173.4(2) n
C31 P C21 C26 . -52.1(2) n
C11 P C21 C26 . -170.9(2) n
C1 P C21 C26 . 69.2(2) n
C31 P C21 C22 . 123.9(2) n
C11 P C21 C22 . 5.0(2) n
C1 P C21 C22 . -114.9(2) n
C26 C21 C22 C23 . 0.2(4) n
P C21 C22 C23 . -175.8(2) n
C21 C22 C23 C24 . -1.9(4) n
C22 C23 C24 C25 . 1.7(5) n
C23 C24 C25 C26 . 0.1(4) n
C22 C21 C26 C25 . 1.7(4) n
P C21 C26 C25 . 177.6(2) n
C24 C25 C26 C21 . -1.8(4) n
C11 P C31 C36 . -93.1(2) n
C1 P C31 C36 . 27.0(2) n
C21 P C31 C36 . 150.1(2) n
C11 P C31 C32 . 84.8(2) n
C1 P C31 C32 . -155.1(2) n
C21 P C31 C32 . -32.0(2) n
C36 C31 C32 C33 . 0.3(4) n
P C31 C32 C33 . -177.5(2) n
C31 C32 C33 C34 . 0.0(5) n
C32 C33 C34 C35 . -0.3(6) n
C33 C34 C35 C36 . 0.5(6) n
C32 C31 C36 C35 . -0.2(4) n
P C31 C36 C35 . 177.7(2) n
C34 C35 C36 C31 . -0.2(5) n
