#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317638.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_4317638
loop_
_publ_author_name
'Wolfdieter A. Schenk'
'Katja Nielsen'
'Nicolai I. Burzlaff'
'Michael Hagel'
_publ_contact_author
;
              Prof. Dr. Wolfdieter A. Schenk
              Institut für Anorganische Chemie
              Universität Würzburg
              Am Hubland
              D-97074 Würzburg
              Germany
;
_publ_contact_author_email       wolfdieter.schenk@mail.uni-wuerzburg.de
_publ_contact_author_fax         '+49 931 8884605'
_publ_contact_author_phone       '+49 931 8885259'
_publ_section_title
;
 Molybdenum and Tungsten Complexes of Sulfene (Thioformaldehyde
 S,S-Dioxide)1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1079
_journal_page_last               1085
_journal_paper_doi               10.1021/ic010963e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[W(CO)3(dppe)(SO2)]'
_chemical_formula_sum            'C29 H24 O5 P2 S W'
_chemical_formula_weight         730.33
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 116.01(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.478(8)
_cell_length_b                   12.794(3)
_cell_length_c                   16.442(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2737(2)
_computing_cell_refinement       'SDP (ENRAF-NONIUS)'
_computing_data_collection       'ENRAF-NONIUS CAD4'
_computing_data_reduction        'SDP (ENRAF-NONIUS)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'ENRAF-NONIUS CAD4'
_diffrn_measurement_method       Omega-theta-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3960
_diffrn_reflns_theta_max         22.93
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        -0.7
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.7385
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_obs          0.0201
_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)+(0.0254P)²+1.8438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0502
_refine_ls_wR_factor_obs         0.0474
_reflns_number_observed          3361
_reflns_number_total             3786
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010963e_1.cif
_cod_data_source_block           Nielsen-1-8b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+1.8438P] 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^)+(0.0254P)^2^+1.8438P] 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        2737.3(22)
_cod_database_code               4317638
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W 0.400642(11) 0.131986(11) 0.134498(10) 0.02801(7) Uani 1 d . .
C1 C 0.2778(3) 0.1980(3) 0.0318(3) 0.0394(10) Uani 1 d . .
C2 C 0.4802(3) 0.1246(3) 0.0598(3) 0.0367(10) Uani 1 d . .
C3 C 0.5165(3) 0.0595(3) 0.2382(3) 0.0402(10) Uani 1 d . .
C11 C 0.1760(3) 0.1747(3) 0.1889(3) 0.0321(9) Uani 1 d . .
C12 C 0.1270(3) 0.2312(3) 0.2306(3) 0.0378(10) Uani 1 d . .
H12 H 0.1659(3) 0.2703(3) 0.2820(3) 0.045 Uiso 1 calc R .
C13 C 0.0214(3) 0.2303(3) 0.1969(3) 0.0448(11) Uani 1 d . .
H13 H -0.0106(3) 0.2704(3) 0.2244(3) 0.054 Uiso 1 calc R .
C14 C -0.0362(3) 0.1704(4) 0.1229(3) 0.0479(11) Uani 1 d . .
H14 H -0.1074(3) 0.1690(4) 0.1005(3) 0.057 Uiso 1 calc R .
C15 C 0.0111(3) 0.1126(4) 0.0819(3) 0.0566(13) Uani 1 d . .
H15 H -0.0281(3) 0.0718(4) 0.0317(3) 0.068 Uiso 1 calc R .
C16 C 0.1172(3) 0.1146(3) 0.1148(3) 0.0478(12) Uani 1 d . .
H16 H 0.1488(3) 0.0751(3) 0.0866(3) 0.057 Uiso 1 calc R .
C21 C 0.3508(3) 0.1052(3) 0.3407(3) 0.0350(9) Uani 1 d . .
C22 C 0.3507(3) 0.1498(4) 0.4179(3) 0.0471(11) Uani 1 d . .
H22 H 0.3427(3) 0.2217(4) 0.4204(3) 0.057 Uiso 1 calc R .
C23 C 0.3625(4) 0.0881(4) 0.4910(3) 0.0530(12) Uani 1 d . .
H23 H 0.3625(4) 0.1187(4) 0.5422(3) 0.064 Uiso 1 calc R .
C24 C 0.3743(3) -0.0181(4) 0.4880(3) 0.0494(12) Uani 1 d . .
H24 H 0.3800(3) -0.0597(4) 0.5365(3) 0.059 Uiso 1 calc R .
C25 C 0.3775(3) -0.0630(3) 0.4133(3) 0.0456(11) Uani 1 d . .
H25 H 0.3873(3) -0.1347(3) 0.4118(3) 0.055 Uiso 1 calc R .
C26 C 0.3663(3) -0.0020(3) 0.3407(3) 0.0407(10) Uani 1 d . .
H26 H 0.3690(3) -0.0330(3) 0.2907(3) 0.049 Uiso 1 calc R .
C31 C 0.4346(3) 0.4169(3) 0.1141(3) 0.0363(9) Uani 1 d . .
C32 C 0.4316(4) 0.5171(4) 0.1432(3) 0.0510(12) Uani 1 d . .
H32 H 0.4517(4) 0.5300(4) 0.2043(3) 0.061 Uiso 1 calc R .
C33 C 0.3985(4) 0.5992(4) 0.0816(4) 0.0640(14) Uani 1 d . .
H33 H 0.3976(4) 0.6668(4) 0.1020(4) 0.077 Uiso 1 calc R .
C34 C 0.3674(4) 0.5816(4) -0.0080(4) 0.0634(14) Uani 1 d . .
H34 H 0.3454(4) 0.6369(4) -0.0488(4) 0.076 Uiso 1 calc R .
C35 C 0.3686(4) 0.4818(4) -0.0383(3) 0.0589(13) Uani 1 d . .
H35 H 0.3466(4) 0.4695(4) -0.0998(3) 0.071 Uiso 1 calc R .
C36 C 0.4024(3) 0.3994(4) 0.0221(3) 0.0459(11) Uani 1 d . .
H36 H 0.4036(3) 0.3321(4) 0.0013(3) 0.055 Uiso 1 calc R .
C41 C 0.6237(3) 0.3183(3) 0.2381(3) 0.0391(10) Uani 1 d . .
C42 C 0.6713(4) 0.4088(4) 0.2835(3) 0.0562(13) Uani 1 d . .
H42 H 0.6324(4) 0.4638(4) 0.2889(3) 0.067 Uiso 1 calc R .
C43 C 0.7780(4) 0.4166(5) 0.3207(4) 0.068(2) Uani 1 d . .
H43 H 0.8101(4) 0.4765(5) 0.3525(4) 0.081 Uiso 1 calc R .
C44 C 0.8360(4) 0.3380(5) 0.3115(4) 0.066(2) Uani 1 d . .
H44 H 0.9069(4) 0.3453(5) 0.3352(4) 0.080 Uiso 1 calc R .
C45 C 0.7897(4) 0.2485(5) 0.2672(4) 0.0671(15) Uani 1 d . .
H45 H 0.8290(4) 0.1940(5) 0.2617(4) 0.080 Uiso 1 calc R .
C46 C 0.6836(3) 0.2393(4) 0.2305(3) 0.0548(13) Uani 1 d . .
H46 H 0.6524(3) 0.1783(4) 0.2001(3) 0.066 Uiso 1 calc R .
C51 C 0.3486(3) 0.3146(3) 0.2692(3) 0.0385(10) Uani 1 d . .
H51A H 0.3039(3) 0.3598(3) 0.2205(3) 0.046 Uiso 1 calc R .
H51B H 0.3375(3) 0.3293(3) 0.3221(3) 0.046 Uiso 1 calc R .
C52 C 0.4598(3) 0.3369(3) 0.2903(3) 0.0368(9) Uani 1 d . .
H52A H 0.5048(3) 0.2954(3) 0.3419(3) 0.044 Uiso 1 calc R .
H52B H 0.4748(3) 0.4101(3) 0.3058(3) 0.044 Uiso 1 calc R .
O1 O 0.3818(3) -0.1238(2) 0.1226(2) 0.0729(11) Uani 1 d . .
O2 O 0.2352(3) -0.0427(3) 0.0053(3) 0.102(2) Uani 1 d . .
O3 O 0.2062(3) 0.2328(3) -0.0256(2) 0.0654(10) Uani 1 d . .
O4 O 0.5270(3) 0.1202(3) 0.0203(2) 0.0675(10) Uani 1 d . .
O5 O 0.5809(3) 0.0152(3) 0.2952(2) 0.0689(10) Uani 1 d . .
P1 P 0.31657(7) 0.17745(8) 0.23585(7) 0.0308(2) Uani 1 d . .
P2 P 0.48326(8) 0.30535(8) 0.19182(7) 0.0325(2) Uani 1 d . .
S1 S 0.33127(9) -0.02669(8) 0.08325(8) 0.0448(3) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
W W -1.4210 6.8720 '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 W1 C2 90.4(2) . . ?
C3 W1 C1 176.1(2) . . ?
C2 W1 C1 92.3(2) . . ?
C3 W1 S1 88.34(13) . . ?
C2 W1 S1 90.56(12) . . ?
C1 W1 S1 88.83(12) . . ?
C3 W1 P2 90.35(13) . . ?
C2 W1 P2 87.98(12) . . ?
C1 W1 P2 92.54(12) . . ?
S1 W1 P2 178.03(4) . . ?
C3 W1 P1 90.62(12) . . ?
C2 W1 P1 168.51(11) . . ?
C1 W1 P1 87.29(13) . . ?
S1 W1 P1 100.90(4) . . ?
P2 W1 P1 80.58(4) . . ?
O3 C1 W1 177.5(4) . . ?
O4 C2 W1 178.2(4) . . ?
O5 C3 W1 177.5(4) . . ?
C16 C11 C12 118.5(4) . . ?
C16 C11 P1 121.7(3) . . ?
C12 C11 P1 119.7(3) . . ?
C13 C12 C11 121.0(4) . . ?
C14 C13 C12 119.9(4) . . ?
C13 C14 C15 119.9(4) . . ?
C14 C15 C16 120.4(4) . . ?
C11 C16 C15 120.3(4) . . ?
C26 C21 C22 118.0(4) . . ?
C26 C21 P1 118.6(3) . . ?
C22 C21 P1 123.1(3) . . ?
C23 C22 C21 120.6(4) . . ?
C24 C23 C22 120.3(4) . . ?
C23 C24 C25 119.8(4) . . ?
C26 C25 C24 120.1(4) . . ?
C25 C26 C21 121.2(4) . . ?
C32 C31 C36 118.7(4) . . ?
C32 C31 P2 122.9(3) . . ?
C36 C31 P2 118.3(3) . . ?
C31 C32 C33 120.3(5) . . ?
C34 C33 C32 120.6(5) . . ?
C33 C34 C35 119.8(5) . . ?
C34 C35 C36 120.3(5) . . ?
C35 C36 C31 120.2(4) . . ?
C46 C41 C42 118.7(4) . . ?
C46 C41 P2 121.6(3) . . ?
C42 C41 P2 119.7(3) . . ?
C41 C42 C43 119.3(5) . . ?
C44 C43 C42 121.2(5) . . ?
C43 C44 C45 119.8(5) . . ?
C44 C45 C46 119.6(5) . . ?
C41 C46 C45 121.4(5) . . ?
C52 C51 P1 110.6(3) . . ?
C51 C52 P2 110.1(3) . . ?
C21 P1 C11 100.4(2) . . ?
C21 P1 C51 105.9(2) . . ?
C11 P1 C51 103.5(2) . . ?
C21 P1 W1 119.81(14) . . ?
C11 P1 W1 119.00(14) . . ?
C51 P1 W1 106.57(14) . . ?
C31 P2 C52 106.2(2) . . ?
C31 P2 C41 103.6(2) . . ?
C52 P2 C41 102.3(2) . . ?
C31 P2 W1 116.92(14) . . ?
C52 P2 W1 106.50(13) . . ?
C41 P2 W1 119.68(14) . . ?
O2 S1 O1 112.3(2) . . ?
O2 S1 W1 124.1(2) . . ?
O1 S1 W1 123.5(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
W1 C3 2.017(5) . ?
W1 C2 2.021(4) . ?
W1 C1 2.024(4) . ?
W1 S1 2.2580(12) . ?
W1 P2 2.5000(11) . ?
W1 P1 2.5250(14) . ?
C1 O3 1.142(5) . ?
C2 O4 1.126(5) . ?
C3 O5 1.142(5) . ?
C11 C16 1.375(6) . ?
C11 C12 1.387(5) . ?
C11 P1 1.833(4) . ?
C12 C13 1.378(6) . ?
C13 C14 1.369(6) . ?
C14 C15 1.369(7) . ?
C15 C16 1.388(6) . ?
C21 C26 1.389(6) . ?
C21 C22 1.393(6) . ?
C21 P1 1.822(4) . ?
C22 C23 1.384(6) . ?
C23 C24 1.374(7) . ?
C24 C25 1.376(6) . ?
C25 C26 1.375(6) . ?
C31 C32 1.376(6) . ?
C31 C36 1.391(6) . ?
C31 P2 1.837(4) . ?
C32 C33 1.390(7) . ?
C33 C34 1.358(7) . ?
C34 C35 1.373(7) . ?
C35 C36 1.382(6) . ?
C41 C46 1.372(6) . ?
C41 C42 1.386(6) . ?
C41 P2 1.840(4) . ?
C42 C43 1.393(7) . ?
C43 C44 1.361(8) . ?
C44 C45 1.365(8) . ?
C45 C46 1.387(6) . ?
C51 C52 1.517(5) . ?
C51 P1 1.836(4) . ?
C52 P2 1.840(4) . ?
O1 S1 1.443(4) . ?
O2 S1 1.434(4) . ?
