#------------------------------------------------------------------------------
#$Date: 2017-03-02 19:20:33 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192782 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/86/4308646.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_4308646
loop_
_publ_author_name
'Wolfgang Petz'
'Christian Kutschera'
'Maya Heitbaum'
'Gernot Frenking'
'Ralf Tonner'
'Bernhard Neumüller'
_publ_contact_author
;
        Gernot Frenking
        Fachbereich Chemie
        Universität Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany
;
_publ_contact_author_email       frenking@chemie.uni-marburg.de
_publ_contact_author_fax         'int. 6421-28-25566'
_publ_contact_author_phone       'int. 6421-28-25563'
_publ_section_title
;
Experimental and Theoretical Studies of Carbodiphosphorane-CX2 Adducts
with Unusual Bonding Situations: Preparation, Crystal Structures, and
Bonding Analyses of S2CC(PPh3)2, O2CC(PPh3)2, and [(CO)4MS2CC(PPh3)2] (M =
Cr, Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1263
_journal_page_last               1274
_journal_paper_doi               10.1021/ic048397l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[S~2~CC(PPh~3~)~2~]'
_chemical_formula_sum            'C38 H30 P2 S2'
_chemical_formula_weight         612.68
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.83(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.752(2)
_cell_length_b                   14.617(3)
_cell_length_c                   16.266(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.12
_cell_volume                     3025.1(10)
_computing_cell_refinement       'IPDS II (Stoe)'
_computing_data_collection       'IPDS II (Stoe)'
_computing_data_reduction        'IPDS II (Stoe)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PLATON-98 (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'IPDS II (Stoe)'
_diffrn_measurement_method       'IPDS II (Stoe)'
_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  0.1105
_diffrn_reflns_av_sigmaI/netI    0.0875
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10797
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0515
_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)+(0.0758P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                1925
_reflns_number_total             3047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048397lsi20041124_051054_1.cif
_cod_data_source_block           pe30
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        3025(1)
_cod_database_code               4308646
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_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
P1 P 0.11011(6) 0.21088(5) 0.21238(4) 0.0398(2) Uani 1 1 d . . .
S1 S 0.11708(7) 0.00360(6) 0.24583(5) 0.0554(2) Uani 1 1 d . . .
C1 C 0.0000 0.1577(3) 0.2500 0.0406(9) Uani 1 2 d S . .
C2 C 0.0000 0.0572(3) 0.2500 0.0446(9) Uani 1 2 d S . .
C3 C 0.2239(2) 0.2197(2) 0.28515(17) 0.0433(6) Uani 1 1 d . . .
C4 C 0.3135(3) 0.2693(2) 0.26950(18) 0.0483(7) Uani 1 1 d . . .
H41 H 0.3181 0.2983 0.2176 0.053(2) Uiso 1 1 calc R . .
C5 C 0.3965(3) 0.2769(2) 0.3293(2) 0.0550(8) Uani 1 1 d . . .
H51 H 0.4579 0.3101 0.3179 0.053(2) Uiso 1 1 calc R . .
C6 C 0.3892(3) 0.2361(2) 0.40485(19) 0.0562(8) Uani 1 1 d . . .
H61 H 0.4455 0.2419 0.4458 0.053(2) Uiso 1 1 calc R . .
C7 C 0.3006(3) 0.1868(2) 0.42173(18) 0.0530(8) Uani 1 1 d . . .
H71 H 0.2959 0.1591 0.4742 0.053(2) Uiso 1 1 calc R . .
C8 C 0.2191(3) 0.1779(2) 0.36240(17) 0.0462(7) Uani 1 1 d . . .
H81 H 0.1589 0.1431 0.3739 0.053(2) Uiso 1 1 calc R . .
C9 C 0.0760(2) 0.32774(19) 0.18106(16) 0.0409(6) Uani 1 1 d . . .
C10 C 0.1263(2) 0.4040(2) 0.21626(17) 0.0445(7) Uani 1 1 d . . .
H101 H 0.1793 0.3966 0.2596 0.053(2) Uiso 1 1 calc R . .
C11 C 0.0992(3) 0.4908(2) 0.18808(18) 0.0498(7) Uani 1 1 d . . .
H111 H 0.1346 0.5426 0.2116 0.053(2) Uiso 1 1 calc R . .
C12 C 0.0210(3) 0.5025(2) 0.12595(18) 0.0515(7) Uani 1 1 d . . .
H121 H 0.0025 0.5622 0.1071 0.053(2) Uiso 1 1 calc R . .
C13 C -0.0299(3) 0.4273(2) 0.09149(17) 0.0498(7) Uani 1 1 d . . .
H131 H -0.0841 0.4352 0.0492 0.053(2) Uiso 1 1 calc R . .
C14 C -0.0025(2) 0.3404(2) 0.11809(16) 0.0454(7) Uani 1 1 d . . .
H141 H -0.0373 0.2888 0.0934 0.053(2) Uiso 1 1 calc R . .
C15 C 0.1470(2) 0.1588(2) 0.11679(16) 0.0449(7) Uani 1 1 d . . .
C16 C 0.2509(3) 0.1560(2) 0.09581(19) 0.0551(8) Uani 1 1 d . . .
H161 H 0.3054 0.1781 0.1333 0.053(2) Uiso 1 1 calc R . .
C17 C 0.2751(3) 0.1207(3) 0.0198(2) 0.0629(9) Uani 1 1 d . . .
H171 H 0.3462 0.1185 0.0060 0.053(2) Uiso 1 1 calc R . .
C18 C 0.1969(3) 0.0891(2) -0.03555(19) 0.0584(9) Uani 1 1 d . . .
H181 H 0.2142 0.0657 -0.0875 0.053(2) Uiso 1 1 calc R . .
C19 C 0.0938(3) 0.0914(2) -0.01539(18) 0.0568(8) Uani 1 1 d . . .
H191 H 0.0399 0.0691 -0.0533 0.053(2) Uiso 1 1 calc R . .
C20 C 0.0683(3) 0.1263(2) 0.06007(18) 0.0511(7) Uani 1 1 d . . .
H201 H -0.0031 0.1281 0.0734 0.053(2) 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 0.0033 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
C1 P1 C3 115.39(10) . . ?
C1 P1 C15 111.84(13) . . ?
C3 P1 C15 110.23(14) . . ?
C1 P1 C9 109.31(14) . . ?
C3 P1 C9 106.29(14) . . ?
C15 P1 C9 102.88(12) . . ?
C2 C1 P1 116.35(12) . . ?
C2 C1 P1 116.35(12) . 2 ?
P1 C1 P1 127.3(2) . 2 ?
C1 C2 S1 117.59(13) . . ?
C1 C2 S1 117.59(13) . 2 ?
S1 C2 S1 124.8(3) . 2 ?
C4 C3 C8 118.5(3) . . ?
C4 C3 P1 123.3(2) . . ?
C8 C3 P1 118.2(2) . . ?
C3 C4 C5 120.6(3) . . ?
C6 C5 C4 119.7(3) . . ?
C5 C6 C7 120.6(3) . . ?
C8 C7 C6 119.9(3) . . ?
C7 C8 C3 120.7(3) . . ?
C10 C9 C14 119.0(3) . . ?
C10 C9 P1 122.7(2) . . ?
C14 C9 P1 118.3(2) . . ?
C11 C10 C9 120.0(3) . . ?
C12 C11 C10 120.5(3) . . ?
C13 C12 C11 119.7(3) . . ?
C12 C13 C14 120.3(3) . . ?
C13 C14 C9 120.4(3) . . ?
C16 C15 C20 118.7(3) . . ?
C16 C15 P1 121.8(2) . . ?
C20 C15 P1 119.3(2) . . ?
C15 C16 C17 119.9(3) . . ?
C18 C17 C16 120.8(3) . . ?
C19 C18 C17 119.8(3) . . ?
C18 C19 C20 120.2(3) . . ?
C19 C20 C15 120.5(3) . . ?
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
P1 C1 1.7506(19) . ?
P1 C3 1.815(3) . ?
P1 C15 1.821(3) . ?
P1 C9 1.827(3) . ?
S1 C2 1.691(2) . ?
C1 C2 1.470(6) . ?
C1 P1 1.7506(19) 2 ?
C2 S1 1.691(2) 2 ?
C3 C4 1.390(4) . ?
C3 C8 1.402(4) . ?
C4 C5 1.394(5) . ?
C5 C6 1.374(5) . ?
C6 C7 1.384(5) . ?
C7 C8 1.376(5) . ?
C9 C10 1.391(4) . ?
C9 C14 1.396(4) . ?
C10 C11 1.384(4) . ?
C11 C12 1.382(5) . ?
C12 C13 1.378(5) . ?
C13 C14 1.379(4) . ?
C15 C16 1.391(4) . ?
C15 C20 1.400(4) . ?
C16 C17 1.392(4) . ?
C17 C18 1.378(5) . ?
C18 C19 1.377(5) . ?
C19 C20 1.388(4) . ?
