Hypervalent Sulfur-Functionalized Diphosphagermylene and Diphosphastannylene Compounds
Izod, Keith; Clark, Ewan R.; Clegg, William; Harrington, Ross W.; Organometallics 31 (2012) 246–; doi:10.1021/om2008327

data_4067855
_publ_section_title
;
 Hypervalent Sulfur-Functionalized Diphosphagermylene and
 Diphosphastannylene Compounds
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              246
_journal_paper_doi               10.1021/om2008327
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C28 H52 P2 S2 Si4 Sn,C4 H10 O'
_chemical_formula_sum            'C32 H62 O P2 S2 Si4 Sn'
_chemical_formula_weight         819.93
_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                90.00
_cell_angle_beta                 99.466(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9798(15)
_cell_length_b                   11.0771(10)
_cell_length_c                   23.0424(18)
_cell_measurement_reflns_used    7167
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.96
_cell_volume                     4275.0(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.1022
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25684
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.249
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0596
_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/[\s^2^(Fo^2^)+(0.0946P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                5104
_reflns_number_total             8243
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008327_si_001.cif
_cod_data_source_block           ki442_compound_11a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4067855
_computing_special_details
;
TITL ki442 in P2(1)/c
CELL 0.71073  16.9798  11.0771  23.0424  90.000  99.466  90.000
ZERR    4.00   0.0015   0.0010   0.0018   0.000   0.008   0.000
LATT  1
SYMM -X, 0.50000+Y, 0.50000-Z
SFAC    C   H   SI  P   S   SN O
UNIT   128 248  16   8   8   4 4

REM yellow block
SIZE 0.20 0.10 0.10
TEMP -123
OMIT -3 52
OMIT -1   2   7
OMIT -2   1  19
OMIT  0   5   5
OMIT  0   4   4
OMIT  0   4   7
OMIT -2   3  20

L.S.      8
BOND $H
ACTA
FMAP      2
PLAN     10

BIND S1 Sn
BIND S2 Sn

REM EXTI    0.000000
WGHT    0.094600
FVAR       0.24927
SN    6    0.122483    0.057555    0.915014    11.00000    0.02650    0.02514 =
         0.02031   -0.00392   -0.00018    0.00270
P1    4    0.170542   -0.153911    0.885397    11.00000    0.02461    0.02585 =
         0.01214   -0.00095    0.00184   -0.00027
P2    4    0.251004    0.135435    0.982444    11.00000    0.02989    0.02157 =
         0.01404   -0.00155    0.00278    0.00014
S1    5    0.223533    0.095550    0.824518    11.00000    0.02970    0.02870 =
         0.01853    0.00339    0.00140   -0.00139
S2    5    0.126974   -0.055072    1.029388    11.00000    0.03825    0.02389 =
         0.01902   -0.00222    0.00905   -0.00228
SI1   3    0.013018   -0.225123    0.808316    11.00000    0.02826    0.02222 =
         0.02164   -0.00022   -0.00099   -0.00094
SI2   3    0.175308   -0.265481    0.760551    11.00000    0.03768    0.02768 =
         0.01686   -0.00642    0.00636   -0.00210
SI3   3    0.179383    0.382276    1.006156    11.00000    0.04291    0.02124 =
         0.02444    0.00233    0.00565    0.00110
SI4   3    0.279547    0.237339    1.110883    11.00000    0.03233    0.02949 =
         0.01640   -0.00545    0.00026    0.00078
C1    1    0.117937   -0.169832    0.807167    11.00000    0.02674    0.02547 =
         0.01005   -0.00212   -0.00078    0.00331
AFIX  13
H1A   2    0.113503   -0.087105    0.789558    11.00000   -1.20000
AFIX   0
C2    1   -0.055406   -0.193368    0.737196    11.00000    0.04701    0.05646 =
         0.03653    0.00843   -0.01691   -0.00693
AFIX 137
H2A   2   -0.046450   -0.253373    0.707713    11.00000   -1.50000
H2B   2   -0.044435   -0.112481    0.723254    11.00000   -1.50000
H2C   2   -0.111008   -0.197696    0.743538    11.00000   -1.50000
AFIX   0
C3    1    0.010453   -0.390633    0.821083    11.00000    0.04712    0.03536 =
         0.08783    0.01597    0.02663    0.00547
AFIX 137
H3A   2    0.046190   -0.410765    0.857669    11.00000   -1.50000
H3B   2    0.027949   -0.433136    0.788137    11.00000   -1.50000
H3C   2   -0.044135   -0.415274    0.824174    11.00000   -1.50000
AFIX   0
C4    1   -0.034194   -0.154198    0.866844    11.00000    0.02909    0.04836 =
         0.04205   -0.01838    0.00543   -0.01077
AFIX 137
H4A   2   -0.006803   -0.181203    0.905432    11.00000   -1.50000
H4B   2   -0.090545   -0.177705    0.861880    11.00000   -1.50000
H4C   2   -0.030201   -0.066178    0.864169    11.00000   -1.50000
AFIX   0
C5    1    0.260057   -0.184378    0.736328    11.00000    0.05336    0.05059 =
         0.02749   -0.00781    0.02323   -0.00090
AFIX 137
H5A   2    0.249513   -0.097360    0.735500    11.00000   -1.50000
H5B   2    0.266098   -0.211788    0.696862    11.00000   -1.50000
H5C   2    0.309250   -0.201216    0.763849    11.00000   -1.50000
AFIX   0
C6    1    0.109838   -0.309548    0.690677    11.00000    0.05355    0.05941 =
         0.02925   -0.01788    0.00955   -0.00830
AFIX 137
H6A   2    0.089024   -0.236771    0.669289    11.00000   -1.50000
H6B   2    0.065257   -0.358391    0.699677    11.00000   -1.50000
H6C   2    0.140829   -0.356640    0.666345    11.00000   -1.50000
AFIX   0
C7    1    0.214238   -0.408310    0.802307    11.00000    0.02990    0.02397 =
         0.03688   -0.01513    0.00108    0.01328
AFIX 137
H7A   2    0.237518   -0.462192    0.775946    11.00000   -1.50000
H7B   2    0.170033   -0.449498    0.816556    11.00000   -1.50000
H7C   2    0.255114   -0.386438    0.835818    11.00000   -1.50000
AFIX   0
C8    1    0.274567   -0.117462    0.881315    11.00000    0.02587    0.02854 =
         0.01485   -0.01103   -0.00076   -0.00180
C9    1    0.333837   -0.194740    0.903304    11.00000    0.03349    0.03014 =
         0.02187   -0.00201   -0.00137    0.00477
AFIX  43
H9A   2    0.319516   -0.268539    0.919810    11.00000   -1.20000
AFIX   0
C10   1    0.413951   -0.172607    0.903158    11.00000    0.03044    0.03999 =
         0.02842   -0.00161    0.00152    0.00576
AFIX  43
H10A  2    0.453091   -0.229753    0.919551    11.00000   -1.20000
AFIX   0
C11   1    0.436471   -0.066672    0.878960    11.00000    0.02545    0.05415 =
         0.04871   -0.01244    0.00879   -0.00497
AFIX  43
H11A  2    0.491300   -0.050938    0.878236    11.00000   -1.20000
AFIX   0
C12   1    0.379629    0.015837    0.855964    11.00000    0.03147    0.03463 =
         0.03869   -0.00453    0.00616   -0.00099
AFIX  43
H12A  2    0.395108    0.089457    0.839933    11.00000   -1.20000
AFIX   0
C13   1    0.299499   -0.008249    0.856121    11.00000    0.03171    0.03214 =
         0.01669   -0.00486    0.00012   -0.00088
C14   1    0.274783    0.238282    0.830312    11.00000    0.04056    0.03290 =
         0.03574    0.00793   -0.00140   -0.00621
AFIX 137
H14A  2    0.237343    0.302435    0.814952    11.00000   -1.50000
H14B  2    0.318598    0.235516    0.807465    11.00000   -1.50000
H14C  2    0.296326    0.254644    0.871676    11.00000   -1.50000
AFIX   0
C15   1    0.209233    0.228423    1.038536    11.00000    0.02492    0.02337 =
         0.01670    0.00204    0.00243   -0.00075
AFIX  13
H15A  2    0.159463    0.187485    1.046196    11.00000   -1.20000
AFIX   0
C16   1    0.129777    0.374661    0.927649    11.00000    0.08437    0.03049 =
         0.04025    0.00975    0.00194    0.00925
AFIX 137
H16A  2    0.122318    0.456562    0.911604    11.00000   -1.50000
H16B  2    0.077717    0.335111    0.925271    11.00000   -1.50000
H16C  2    0.163265    0.328312    0.904877    11.00000   -1.50000
AFIX   0
C17   1    0.104720    0.453713    1.047223    11.00000    0.05652    0.03087 =
         0.04678    0.00425    0.01360    0.01829
AFIX 137
H17A  2    0.076157    0.517946    1.023163    11.00000   -1.50000
H17B  2    0.132491    0.487974    1.084205    11.00000   -1.50000
H17C  2    0.066532    0.392514    1.055740    11.00000   -1.50000
AFIX   0
C18   1    0.267621    0.484117    1.006940    11.00000    0.06018    0.03020 =
         0.05563    0.00371    0.01457   -0.00904
AFIX 137
H18A  2    0.249322    0.564135    0.992385    11.00000   -1.50000
H18B  2    0.303118    0.450291    0.981599    11.00000   -1.50000
H18C  2    0.296586    0.491204    1.047247    11.00000   -1.50000
AFIX   0
C19   1    0.278733    0.097547    1.156645    11.00000    0.04808    0.04786 =
         0.01738    0.00306   -0.00499    0.00502
AFIX 137
H19A  2    0.224289    0.065404    1.152045    11.00000   -1.50000
H19B  2    0.297332    0.117240    1.198097    11.00000   -1.50000
H19C  2    0.314154    0.036923    1.143715    11.00000   -1.50000
AFIX   0
C20   1    0.383690    0.264510    1.098790    11.00000    0.03481    0.04788 =
         0.03935   -0.01760   -0.00251   -0.00190
AFIX 137
H20A  2    0.399116    0.201867    1.072798    11.00000   -1.50000
H20B  2    0.419784    0.262095    1.136618    11.00000   -1.50000
H20C  2    0.387059    0.343889    1.080579    11.00000   -1.50000
AFIX   0
C21   1    0.253430    0.364029    1.158999    11.00000    0.05891    0.05380 =
         0.01908   -0.01797    0.00196   -0.00039
AFIX 137
H21A  2    0.198959    0.352559    1.166917    11.00000   -1.50000
H21B  2    0.256893    0.441301    1.138861    11.00000   -1.50000
H21C  2    0.290869    0.364057    1.196221    11.00000   -1.50000
AFIX   0
C22   1    0.283112   -0.007740    1.021239    11.00000    0.03404    0.02608 =
         0.01163   -0.00649    0.00105   -0.00092
C23   1    0.364010   -0.034937    1.030367    11.00000    0.03811    0.02544 =
         0.02050   -0.00408   -0.00172    0.00095
AFIX  43
H23A  2    0.400469    0.018626    1.016499    11.00000   -1.20000
AFIX   0
C24   1    0.392561   -0.142127    1.060252    11.00000    0.04413    0.03463 =
         0.02966   -0.00603   -0.00798    0.01104
AFIX  43
H24A  2    0.448210   -0.158597    1.068005    11.00000   -1.20000
AFIX   0
C25   1    0.341069   -0.219549    1.077391    11.00000    0.06860    0.02498 =
         0.02936   -0.00156   -0.01006    0.00588
AFIX  43
H25A  2    0.360833   -0.291905    1.096623    11.00000   -1.20000
AFIX   0
C26   1    0.259434   -0.198128    1.068108    11.00000    0.05788    0.02585 =
         0.01722   -0.00424    0.00085    0.00446
AFIX  43
H26A  2    0.223777   -0.255567    1.080084    11.00000   -1.20000
AFIX   0
C27   1    0.230273   -0.089305    1.040513    11.00000    0.03857    0.02965 =
         0.01428   -0.00055    0.00188   -0.00551
C28   1    0.079131   -0.199838    1.023891    11.00000    0.05783    0.02808 =
         0.02714   -0.00963    0.01537   -0.01102
AFIX 137
H28A  2    0.087769   -0.238992    1.062556    11.00000   -1.50000
H28B  2    0.101741   -0.250166    0.995754    11.00000   -1.50000
H28C  2    0.021729   -0.189495    1.010358    11.00000   -1.50000
AFIX   0
O     7    0.517428   -0.318868    1.164763    11.00000    0.05361    0.05533 =
         0.06833   -0.00307    0.00811   -0.00046
C31   1    0.492764   -0.321832    1.219613    11.00000    0.05641    0.09252 =
         0.05248    0.02690   -0.00452   -0.01606
AFIX  23
H31A  2    0.534481   -0.361218    1.248501    11.00000   -1.20000
H31B  2    0.443371   -0.370474    1.216823    11.00000   -1.20000
AFIX   0
C32   1    0.477895   -0.201292    1.239999    11.00000    0.07479    0.08386 =
         0.05672   -0.02253    0.01726   -0.01329
AFIX 137
H32A  2    0.444245   -0.206373    1.270629    11.00000   -1.50000
H32B  2    0.450628   -0.153261    1.206981    11.00000   -1.50000
H32C  2    0.528770   -0.162847    1.256153    11.00000   -1.50000
AFIX   0
C30   1    0.534157   -0.438145    1.144119    11.00000    0.07402    0.04881 =
         0.13508   -0.01676    0.00280    0.00976
AFIX  23
H30A  2    0.489346   -0.493442    1.147542    11.00000   -1.20000
H30B  2    0.583228   -0.470903    1.168114    11.00000   -1.20000
AFIX   0
C29   1    0.545132   -0.427572    1.080253    11.00000    0.09735    0.10208 =
         0.14527   -0.06518    0.04276   -0.02595
AFIX 137
H29A  2    0.558079   -0.507038    1.065670    11.00000   -1.50000
H29B  2    0.588730   -0.371171    1.077203    11.00000   -1.50000
H29C  2    0.495672   -0.397680    1.056655    11.00000   -1.50000

HKLF      4

REM  ki442 in P2(1)/c
REM R1 =  0.0596 for   5104 Fo > 4sig(Fo)  and  0.1001 for all   8243 data
REM    395 parameters refined using      0 restraints

END

;