#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179334 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323145.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_4323145
loop_
_publ_author_name
'Scott Flanagan'
'Henry A. Luten'
'William S. Rees'
_publ_section_title
;
 Reaction of β-Diketones with P4S10 To Produce Novel
 Alkyl-Phosphorus-Sulfur Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6093
_journal_page_last               6095
_journal_paper_doi               10.1021/ic9709234
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C11 H20 P2 S5'
_chemical_formula_weight         374.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.96430(10)
_cell_length_b                   16.08700(10)
_cell_length_c                   17.86810(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.28
_cell_volume                     3439.07(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART/CCD'
_diffrn_measurement_method       '15 second frames'
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13873
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0.01
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0063(3)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_obs          0.0238
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0304P)²+2.1046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0672
_refine_ls_wR_factor_obs         0.0627
_reflns_number_observed          2228
_reflns_number_total             2454
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9709234_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+2.1046P] 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^)+(0.0304P)^2^+2.1046P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323145
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
S4 S 0.09255(4) 0.83930(3) 0.48247(3) 0.0359(2) Uani 1 d . .
P1 P 0.13334(4) 0.87706(3) 0.59040(3) 0.0314(2) Uani 1 d . .
S3 S 0.22231(5) 0.99548(3) 0.43290(3) 0.0395(2) Uani 1 d . .
P2 P 0.24845(5) 1.01450(3) 0.54708(3) 0.0358(2) Uani 1 d . .
S1 S 0.32899(7) 1.11540(4) 0.56986(4) 0.0587(2) Uani 1 d . .
S2 S 0.07091(5) 0.80593(4) 0.66651(3) 0.0509(2) Uani 1 d . .
S5 S 0.09383(5) 1.00368(4) 0.60297(4) 0.0473(2) Uani 1 d . .
C4 C 0.2388(2) 0.84105(13) 0.35999(12) 0.0381(5) Uani 1 d . .
C3 C 0.2242(2) 0.87977(12) 0.43983(11) 0.0300(5) Uani 1 d . .
C8 C 0.3692(2) 0.88815(13) 0.63737(12) 0.0363(5) Uani 1 d . .
C2 C 0.3156(2) 0.85985(12) 0.49715(11) 0.0309(5) Uani 1 d . .
C7 C 0.3442(2) 0.8763(2) 0.32230(13) 0.0525(6) Uani 1 d . .
C6 C 0.1363(2) 0.8622(2) 0.31147(13) 0.0491(6) Uani 1 d . .
C9 C 0.3797(2) 0.79493(14) 0.65276(13) 0.0445(6) Uani 1 d . .
C10 C 0.3306(2) 0.9325(2) 0.70887(13) 0.0500(6) Uani 1 d . .
C5 C 0.2499(2) 0.74612(14) 0.36645(14) 0.0506(6) Uani 1 d . .
C11 C 0.4850(2) 0.9203(2) 0.6149(2) 0.0596(7) Uani 1 d . .
C1 C 0.2854(2) 0.90275(12) 0.57097(11) 0.0291(4) Uani 1 d . .
H6A H 0.1189 0.9248 0.3107 0.050 Uiso 1 d . .
H7A H 0.4101 0.8620 0.3507 0.050 Uiso 1 d . .
H10A H 0.3826 0.9209 0.7507 0.050 Uiso 1 d . .
H9A H 0.4236 0.7852 0.7005 0.050 Uiso 1 d . .
H11A H 0.5340 0.9185 0.6500 0.050 Uiso 1 d . .
H2A H 0.3237 0.7988 0.5108 0.050 Uiso 1 d . .
H11B H 0.5233 0.8871 0.5700 0.050 Uiso 1 d . .
H11C H 0.4874 0.9648 0.6100 0.050 Uiso 1 d . .
H7B H 0.3424 0.9398 0.3108 0.050 Uiso 1 d . .
H10B H 0.3281 0.9957 0.7009 0.050 Uiso 1 d . .
H7C H 0.3540 0.8481 0.2708 0.050 Uiso 1 d . .
H9B H 0.4091 0.7632 0.6106 0.050 Uiso 1 d . .
H2B H 0.3925 0.8787 0.4807 0.050 Uiso 1 d . .
H5A H 0.3236 0.7229 0.3909 0.050 Uiso 1 d . .
H5B H 0.1814 0.7189 0.4009 0.050 Uiso 1 d . .
H6B H 0.1468 0.8371 0.2608 0.050 Uiso 1 d . .
H6C H 0.0659 0.8364 0.3306 0.050 Uiso 1 d . .
H10C H 0.2579 0.9131 0.7310 0.050 Uiso 1 d . .
H9C H 0.3137 0.7675 0.6608 0.050 Uiso 1 d . .
H5C H 0.2442 0.7179 0.3110 0.050 Uiso 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'
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
C3 S4 P1 94.50(7) . . ?
C1 P1 S2 129.03(7) . . ?
C1 P1 S4 96.84(6) . . ?
S2 P1 S4 112.94(4) . . ?
C1 P1 S5 91.39(6) . . ?
S2 P1 S5 114.35(4) . . ?
S4 P1 S5 109.22(3) . . ?
C3 S3 P2 94.57(7) . . ?
C1 P2 S1 129.18(7) . . ?
C1 P2 S3 96.65(6) . . ?
S1 P2 S3 113.85(4) . . ?
C1 P2 S5 91.13(6) . . ?
S1 P2 S5 114.03(4) . . ?
S3 P2 S5 108.63(4) . . ?
P1 S5 P2 80.34(3) . . ?
C5 C4 C7 109.1(2) . . ?
C5 C4 C6 109.3(2) . . ?
C7 C4 C6 109.0(2) . . ?
C5 C4 C3 109.7(2) . . ?
C7 C4 C3 110.1(2) . . ?
C6 C4 C3 109.6(2) . . ?
C2 C3 C4 116.5(2) . . ?
C2 C3 S3 105.18(13) . . ?
C4 C3 S3 109.74(14) . . ?
C2 C3 S4 104.85(13) . . ?
C4 C3 S4 109.08(13) . . ?
S3 C3 S4 111.39(10) . . ?
C9 C8 C11 107.7(2) . . ?
C9 C8 C10 109.3(2) . . ?
C11 C8 C10 109.5(2) . . ?
C9 C8 C1 109.5(2) . . ?
C11 C8 C1 109.2(2) . . ?
C10 C8 C1 111.6(2) . . ?
C1 C2 C3 108.3(2) . . ?
C2 C1 C8 115.6(2) . . ?
C2 C1 P1 106.57(13) . . ?
C8 C1 P1 116.17(14) . . ?
C2 C1 P2 106.72(13) . . ?
C8 C1 P2 117.37(14) . . ?
P1 C1 P2 91.37(9) . . ?
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
S4 C3 1.867(2) . ?
S4 P1 2.0799(8) . ?
P1 C1 1.898(2) . ?
P1 S2 1.9280(8) . ?
P1 S5 2.1031(8) . ?
S3 C3 1.866(2) . ?
S3 P2 2.0865(8) . ?
P2 C1 1.900(2) . ?
P2 S1 1.9310(8) . ?
P2 S5 2.1095(9) . ?
C4 C5 1.537(3) . ?
C4 C7 1.538(3) . ?
C4 C6 1.540(3) . ?
C4 C3 1.566(3) . ?
C3 C2 1.532(3) . ?
C8 C9 1.530(3) . ?
C8 C11 1.532(3) . ?
C8 C10 1.534(3) . ?
C8 C1 1.571(3) . ?
C2 C1 1.532(3) . ?
