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_4067854
_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 Ge P2 S2 Si4,0.5 C4 H10 O'
_chemical_formula_sum            'C30 H57 Ge O0.5 P2 S2 Si4'
_chemical_formula_weight         736.77
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.760(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.494(2)
_cell_length_b                   11.1789(7)
_cell_length_c                   22.9459(14)
_cell_measurement_reflns_used    1834
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.78
_cell_volume                     7818.3(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1209
_diffrn_reflns_av_sigmaI/netI    0.2203
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18342
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.878
_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            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                3160
_reflns_number_total             6872
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008327_si_001.cif
_cod_data_source_block           ki429_compound_10a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4067854
_computing_special_details
;
TITL ki429(erc278) in C2/c
CELL  0.71073   30.494  11.1789  22.9459    90.0000    91.760    90.0000
ZERR  8          0.002   0.0007   0.0014     0.0000     0.005     0.0000
LATT  7
SYMM  -X, Y, 0.5-Z
SFAC  C  H Ge  P  S Si O
UNIT   240    456   8  16  16  32 4

REM colourless block
SIZE 0.12 0.10 0.10
TEMP -123
OMIT -3 50

L.S. 8
BOND $H
ACTA
FMAP 2
PLAN 10
BIND GE S1
BIND GE S2
EQIV $1   -x, y, -z+1/2
DFIX 1.453 0.005 C29 C30
DFIX 1.423 0.005 O C29
DFIX 2.385 0.005 O C30
DFIX 2.394 0.005 C29 C29_$1

REM EXTI    0.000000
WGHT    0.000000
FVAR       0.15640
GE    3    0.177986    0.814584    0.100010    11.00000    0.03099    0.02846 =
         0.03204    0.00711   -0.00270   -0.00754
P1    4    0.152201    0.620305    0.131904    11.00000    0.02707    0.02320 =
         0.01687    0.00025   -0.00038   -0.00544
P2    4    0.113849    0.884897    0.044399    11.00000    0.03031    0.02501 =
         0.01985    0.00001    0.00290    0.00113
S1    5    0.128065    0.867107    0.196049    11.00000    0.03370    0.02895 =
         0.02316   -0.00081    0.00189    0.00071
S2    5    0.183659    0.701539   -0.009461    11.00000    0.03229    0.02589 =
         0.02327    0.00076    0.00620    0.00050
SI1   6    0.239633    0.548341    0.192334    11.00000    0.02824    0.02595 =
         0.02944    0.00290    0.00128   -0.00281
SI2   6    0.150897    0.502062    0.256255    11.00000    0.03307    0.02697 =
         0.02190    0.00280    0.00346    0.00084
SI3   6    0.152613    1.131049    0.013735    11.00000    0.06202    0.01746 =
         0.03420    0.00065    0.00858   -0.00131
SI4   6    0.099067    0.983116   -0.082796    11.00000    0.03885    0.03514 =
         0.02432    0.00746    0.00442    0.00657
C1    1    0.181804    0.601022    0.204809    11.00000    0.02919    0.00748 =
         0.01879   -0.00404   -0.00351    0.00369
AFIX  13
H1A   2    0.184021    0.681985    0.223197    11.00000   -1.20000
AFIX   0
C2    1    0.265382    0.627933    0.131185    11.00000    0.02960    0.06778 =
         0.06129    0.01487    0.00455    0.00469
AFIX 137
H2A   2    0.293688    0.590799    0.123225    11.00000   -1.50000
H2B   2    0.269947    0.712059    0.141742    11.00000   -1.50000
H2C   2    0.246108    0.622967    0.096299    11.00000   -1.50000
AFIX   0
C3    1    0.241128    0.385689    0.175717    11.00000    0.05503    0.03959 =
         0.10526   -0.01765    0.03643   -0.00763
AFIX 137
H3A   2    0.271565    0.360649    0.170589    11.00000   -1.50000
H3B   2    0.223878    0.369849    0.139806    11.00000   -1.50000
H3C   2    0.228728    0.340808    0.207993    11.00000   -1.50000
AFIX   0
C4    1    0.276599    0.575701    0.256825    11.00000    0.03975    0.07102 =
         0.04783    0.00857   -0.01181    0.00960
AFIX 137
H4A   2    0.304204    0.610482    0.244080    11.00000   -1.50000
H4B   2    0.282629    0.499869    0.276947    11.00000   -1.50000
H4C   2    0.262464    0.631185    0.283467    11.00000   -1.50000
AFIX   0
C5    1    0.102921    0.578263    0.288466    11.00000    0.05756    0.03316 =
         0.02868    0.00999    0.00558    0.00272
AFIX 137
H5A   2    0.093529    0.533205    0.322530    11.00000   -1.50000
H5B   2    0.078740    0.582125    0.259394    11.00000   -1.50000
H5C   2    0.111286    0.659495    0.300401    11.00000   -1.50000
AFIX   0
C6    1    0.130750    0.362179    0.219678    11.00000    0.04020    0.02354 =
         0.04819    0.00831    0.01754    0.00214
AFIX 137
H6A   2    0.111654    0.318595    0.245913    11.00000   -1.50000
H6B   2    0.155824    0.311751    0.210157    11.00000   -1.50000
H6C   2    0.114212    0.382869    0.183791    11.00000   -1.50000
AFIX   0
C7    1    0.186550    0.459515    0.321066    11.00000    0.04558    0.05927 =
         0.03765    0.01464    0.00245    0.00427
AFIX 137
H7A   2    0.168908    0.417169    0.349488    11.00000   -1.50000
H7B   2    0.199077    0.531856    0.339043    11.00000   -1.50000
H7C   2    0.210287    0.407298    0.308516    11.00000   -1.50000
AFIX   0
C8    1    0.096329    0.658614    0.149068    11.00000    0.03594    0.03110 =
         0.01169    0.00436   -0.00153   -0.01264
C9    1    0.062029    0.583961    0.134659    11.00000    0.01958    0.04342 =
         0.02492    0.01045    0.00119   -0.00072
AFIX  43
H9A   2    0.068628    0.510821    0.115756    11.00000   -1.20000
AFIX   0
C10   1    0.018740    0.607195    0.145568    11.00000    0.04592    0.04966 =
         0.03335    0.01125   -0.01611   -0.02219
AFIX  43
H10A  2   -0.003482    0.550390    0.135895    11.00000   -1.20000
AFIX   0
C11   1    0.008316    0.716303    0.171198    11.00000    0.01466    0.06459 =
         0.04398    0.01428    0.00456   -0.00348
AFIX  43
H11A  2   -0.021386    0.735296    0.178466    11.00000   -1.20000
AFIX   0
C12   1    0.040926    0.796039    0.185879    11.00000    0.03433    0.03828 =
         0.03718    0.00264    0.00209   -0.01393
AFIX  43
H12A  2    0.033600    0.870171    0.203330    11.00000   -1.20000
AFIX   0
C13   1    0.084565    0.770020    0.175608    11.00000    0.02502    0.04157 =
         0.01545    0.01483   -0.00246    0.00275
C14   1    0.101639    1.011112    0.194654    11.00000    0.05351    0.03950 =
         0.03729   -0.01194    0.00508    0.00257
AFIX 137
H14A  2    0.123608    1.073814    0.201827    11.00000   -1.50000
H14B  2    0.079722    1.014178    0.224973    11.00000   -1.50000
H14C  2    0.087201    1.023744    0.156404    11.00000   -1.50000
AFIX   0
C15   1    0.137067    0.979721   -0.015503    11.00000    0.03004    0.02861 =
         0.01825    0.01544    0.00639    0.00470
AFIX  13
H15A  2    0.164839    0.940203   -0.027318    11.00000   -1.20000
AFIX   0
C16   1    0.191071    1.208320   -0.035517    11.00000    0.09059    0.03104 =
         0.04424   -0.00682    0.01181   -0.01703
AFIX 137
H16A  2    0.204692    1.276345   -0.015000    11.00000   -1.50000
H16B  2    0.174830    1.237005   -0.070288    11.00000   -1.50000
H16C  2    0.213895    1.152204   -0.047136    11.00000   -1.50000
AFIX   0
C17   1    0.103227    1.224406    0.024300    11.00000    0.09714    0.03326 =
         0.05686   -0.00790    0.02173    0.01012
AFIX 137
H17A  2    0.111446    1.296185    0.046590    11.00000   -1.50000
H17B  2    0.081560    1.178484    0.045670    11.00000   -1.50000
H17C  2    0.090573    1.247888   -0.013775    11.00000   -1.50000
AFIX   0
C18   1    0.183673    1.121781    0.085251    11.00000    0.09770    0.03561 =
         0.04297   -0.01068   -0.00446   -0.01828
AFIX 137
H18A  2    0.187826    1.202419    0.101240    11.00000   -1.50000
H18B  2    0.212348    1.084814    0.079428    11.00000   -1.50000
H18C  2    0.167103    1.073260    0.112517    11.00000   -1.50000
AFIX   0
C19   1    0.113263    1.108808   -0.133554    11.00000    0.07449    0.03836 =
         0.02695    0.00660    0.00752    0.01642
AFIX 137
H19A  2    0.110145    1.185495   -0.113407    11.00000   -1.50000
H19B  2    0.093424    1.106829   -0.167961    11.00000   -1.50000
H19C  2    0.143604    1.099482   -0.145700    11.00000   -1.50000
AFIX   0
C20   1    0.103204    0.843546   -0.127957    11.00000    0.04474    0.04689 =
         0.01342    0.00988   -0.00262    0.00190
AFIX 137
H20A  2    0.088836    0.777250   -0.108132    11.00000   -1.50000
H20B  2    0.134168    0.823963   -0.133120    11.00000   -1.50000
H20C  2    0.088764    0.856647   -0.166169    11.00000   -1.50000
AFIX   0
C21   1    0.041350    1.007129   -0.062082    11.00000    0.04302    0.05816 =
         0.03956    0.01315    0.00413    0.00953
AFIX 137
H21A  2    0.039897    1.075592   -0.035536    11.00000   -1.50000
H21B  2    0.030535    0.935400   -0.042610    11.00000   -1.50000
H21C  2    0.023151    1.023070   -0.097167    11.00000   -1.50000
AFIX   0
C22   1    0.097615    0.746002    0.008187    11.00000    0.02795    0.02233 =
         0.01705    0.01237   -0.00400   -0.00201
C23   1    0.053466    0.718420    0.004311    11.00000    0.03424    0.03349 =
         0.01705    0.01389    0.00011   -0.00873
AFIX  43
H23A  2    0.032731    0.773366    0.018922    11.00000   -1.20000
AFIX   0
C24   1    0.038766    0.611309   -0.020679    11.00000    0.03155    0.04075 =
         0.04757    0.02345   -0.01558   -0.01342
AFIX  43
H24A  2    0.008256    0.594270   -0.023582    11.00000   -1.20000
AFIX   0
C25   1    0.068801    0.530144   -0.041181    11.00000    0.06618    0.02868 =
         0.03900    0.01214   -0.02577   -0.01460
AFIX  43
H25A  2    0.058968    0.456551   -0.057647    11.00000   -1.20000
AFIX   0
C26   1    0.113064    0.555901   -0.037758    11.00000    0.04422    0.03169 =
         0.02014   -0.00594   -0.00504    0.00147
AFIX  43
H26A  2    0.133641    0.500766   -0.052585    11.00000   -1.20000
AFIX   0
C27   1    0.127343    0.661000   -0.012973    11.00000    0.03237    0.01514 =
         0.01654    0.00496   -0.00744    0.00061
C28   1    0.211757    0.559917   -0.012217    11.00000    0.04377    0.03673 =
         0.03345   -0.00554    0.00445    0.02265
AFIX 137
H28A  2    0.243457    0.573039   -0.007746    11.00000   -1.50000
H28B  2    0.205159    0.521254   -0.049802    11.00000   -1.50000
H28C  2    0.201933    0.508447    0.019398    11.00000   -1.50000
AFIX   0
O     7    0.000000    0.223041    0.250000    10.50000    0.11680    0.36743 =
         0.08329    0.00000    0.00556    0.00000
C29   1    0.001921    0.296611    0.198576    11.00000    0.05426    0.18176 =
         0.12865   -0.05219   -0.01489    0.01334
AFIX  23
H29A  2   -0.027996    0.324261    0.187317    11.00000   -1.20000
H29B  2    0.020176    0.368013    0.207288    11.00000   -1.20000
AFIX   0
C30   1    0.019992    0.232333    0.151077    11.00000    0.13961    0.20555 =
         0.24554   -0.12372   -0.02206    0.06921
AFIX  33
H30A  2    0.020946    0.284558    0.116836    11.00000   -1.50000
H30B  2    0.001637    0.162466    0.141900    11.00000   -1.50000
H30C  2    0.049778    0.205923    0.161942    11.00000   -1.50000

HKLF 4

REM  ki429(erc278) in C2/c
REM R1 =  0.0614 for   3160 Fo > 4sig(Fo)  and  0.1688 for all   6872 data
REM    371 parameters refined using      4 restraints

END

;