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_4067858
_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'
_chemical_formula_sum            'C28 H52 P2 S2 Si4'
_chemical_formula_weight         627.12
_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                 91.836(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6717(7)
_cell_length_b                   11.3658(4)
_cell_length_c                   15.8141(5)
_cell_measurement_reflns_used    7910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.99
_cell_volume                     3534.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17814
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.577
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0455P)^2^+8.8910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                4561
_reflns_number_total             5060
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008327_si_001.cif
_cod_data_source_block           ki496_compound_14
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4067858
_computing_special_details
;
TITL ki496 in P2(1)/c
CELL 0.71073  19.6717  11.3658  15.8141  90.000  91.836  90.000
ZERR    4.00   0.0007   0.0004   0.0005   0.000   0.003   0.000
LATT  1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H SI P S
UNIT 112 208 16 8 8

REM colourless block
SIZE 0.40 0.30 0.30
TEMP -123

L.S. 8
BOND $H
ACTA 52
SHEL 5.8 0.9
FMAP 2
PLAN 10

REM EXTI    0.000000
WGHT    0.045500    8.891002
FVAR       0.42320
P1    4    0.232995    0.368605    0.377761    11.00000    0.01788    0.01967 =
         0.02173    0.00009    0.00264   -0.00180
P2    4    0.244024    0.530982    0.300494    11.00000    0.02170    0.02040 =
         0.02167   -0.00006    0.00324   -0.00160
S1    5    0.370913    0.251090    0.446586    11.00000    0.03129    0.03819 =
         0.02578   -0.00347   -0.00629    0.00798
S2    5    0.213502    0.774051    0.226384    11.00000    0.04782    0.03011 =
         0.03340    0.00875    0.00658    0.00784
SI1   3    0.129176    0.224981    0.459240    11.00000    0.01934    0.02805 =
         0.03280    0.00410    0.00087   -0.00183
SI2   3    0.070453    0.377545    0.302417    11.00000    0.02520    0.02984 =
         0.02716    0.00132    0.00104    0.00220
SI3   3    0.373309    0.638241    0.412289    11.00000    0.03136    0.02745 =
         0.01947   -0.00244   -0.00029   -0.01092
SI4   3    0.381460    0.572480    0.215453    11.00000    0.02135    0.02433 =
         0.01936    0.00065    0.00531   -0.00363
C1    1    0.146331    0.303299    0.355783    11.00000    0.02054    0.02286 =
         0.02491   -0.00353    0.00453   -0.00421
AFIX  13
H1    2    0.156009    0.236846    0.316511    11.00000   -1.20000
AFIX   0
C2    1    0.047931    0.139860    0.454278    11.00000    0.03054    0.04925 =
         0.05669    0.02176   -0.00096   -0.01023
AFIX 137
H2A   2    0.009559    0.194215    0.446569    11.00000   -1.50000
H2B   2    0.043175    0.095880    0.507062    11.00000   -1.50000
H2C   2    0.048429    0.084822    0.406599    11.00000   -1.50000
AFIX   0
C3    1    0.125691    0.330276    0.549055    11.00000    0.04402    0.04022 =
         0.03005    0.00537    0.01074    0.00296
AFIX 137
H3A   2    0.090529    0.389479    0.536764    11.00000   -1.50000
H3B   2    0.169899    0.369176    0.556956    11.00000   -1.50000
H3C   2    0.114811    0.287644    0.600760    11.00000   -1.50000
AFIX   0
C4    1    0.198584    0.117522    0.483091    11.00000    0.03495    0.03066 =
         0.04199    0.00611   -0.00179   -0.00087
AFIX 137
H4A   2    0.185671    0.066786    0.530040    11.00000   -1.50000
H4B   2    0.240453    0.159998    0.498851    11.00000   -1.50000
H4C   2    0.206168    0.069211    0.432938    11.00000   -1.50000
AFIX   0
C5    1    0.013435    0.258559    0.259548    11.00000    0.03660    0.04973 =
         0.04474    0.00211   -0.01024   -0.00603
AFIX 137
H5A   2   -0.018443    0.291759    0.217045    11.00000   -1.50000
H5B   2   -0.012037    0.224172    0.305719    11.00000   -1.50000
H5C   2    0.040909    0.197398    0.233417    11.00000   -1.50000
AFIX   0
C6    1    0.020461    0.469098    0.376420    11.00000    0.03839    0.05061 =
         0.04116   -0.00058    0.00292    0.01515
AFIX 137
H6A   2   -0.020050    0.500140    0.346419    11.00000   -1.50000
H6B   2    0.048610    0.534591    0.397535    11.00000   -1.50000
H6C   2    0.006609    0.420566    0.424107    11.00000   -1.50000
AFIX   0
C7    1    0.091505    0.469762    0.209535    11.00000    0.03373    0.04251 =
         0.03198    0.00758   -0.00734    0.00211
AFIX 137
H7A   2    0.050134    0.484231    0.174926    11.00000   -1.50000
H7B   2    0.124889    0.428629    0.175602    11.00000   -1.50000
H7C   2    0.110573    0.544964    0.229189    11.00000   -1.50000
AFIX   0
C8    1    0.337642    0.551465    0.319520    11.00000    0.01842    0.02168 =
         0.01546    0.00150    0.00052   -0.00415
AFIX  13
H8    2    0.352197    0.469804    0.335150    11.00000   -1.20000
AFIX   0
C9    1    0.343004    0.580317    0.514604    11.00000    0.04975    0.05342 =
         0.02061   -0.00259   -0.00248   -0.01901
AFIX 137
H9A   2    0.375367    0.602125    0.560341    11.00000   -1.50000
H9B   2    0.339391    0.494419    0.511498    11.00000   -1.50000
H9C   2    0.298308    0.613926    0.525811    11.00000   -1.50000
AFIX   0
C10   1    0.355263    0.799092    0.406013    11.00000    0.05756    0.02987 =
         0.03620   -0.01185    0.00304   -0.01203
AFIX 137
H10A  2    0.385881    0.841249    0.445615    11.00000   -1.50000
H10B  2    0.308000    0.813650    0.420799    11.00000   -1.50000
H10C  2    0.362422    0.826928    0.348326    11.00000   -1.50000
AFIX   0
C11   1    0.467896    0.616525    0.416009    11.00000    0.03239    0.05641 =
         0.03846   -0.00112   -0.00854   -0.01491
AFIX 137
H11A  2    0.487209    0.649576    0.468735    11.00000   -1.50000
H11B  2    0.487698    0.656400    0.367678    11.00000   -1.50000
H11C  2    0.478189    0.532254    0.413558    11.00000   -1.50000
AFIX   0
C12   1    0.452972    0.464218    0.213685    11.00000    0.02767    0.03402 =
         0.03603   -0.00138    0.00991   -0.00056
AFIX 137
H12A  2    0.477221    0.472915    0.160872    11.00000   -1.50000
H12B  2    0.434766    0.384188    0.217388    11.00000   -1.50000
H12C  2    0.484409    0.478809    0.261870    11.00000   -1.50000
AFIX   0
C14   1    0.414737    0.724826    0.201538    11.00000    0.03747    0.03073 =
         0.03192    0.00545    0.00924   -0.00624
AFIX 137
H14D  2    0.377344    0.781319    0.205557    11.00000   -1.50000
H14E  2    0.434957    0.731663    0.145915    11.00000   -1.50000
H14F  2    0.449381    0.741476    0.245835    11.00000   -1.50000
AFIX   0
C13   1    0.324532    0.539747    0.122157    11.00000    0.03832    0.04380 =
         0.01702   -0.00083    0.00409   -0.00491
AFIX 137
H13A  2    0.284927    0.592034    0.122449    11.00000   -1.50000
H13B  2    0.309359    0.457736    0.124749    11.00000   -1.50000
H13C  2    0.349332    0.552235    0.070146    11.00000   -1.50000
AFIX   0
C15   1    0.285195    0.276195    0.308380    11.00000    0.02380    0.01851 =
         0.02370   -0.00203    0.00300   -0.00023
C16   1    0.266726    0.258458    0.223146    11.00000    0.02538    0.02262 =
         0.02199    0.00125    0.00059    0.00188
AFIX  43
H16   2    0.227261    0.296285    0.200078    11.00000   -1.20000
AFIX   0
C17   1    0.304474    0.187366    0.171882    11.00000    0.03153    0.03121 =
         0.02011   -0.00750    0.00525   -0.00371
AFIX  43
H17   2    0.291216    0.176827    0.114085    11.00000   -1.20000
AFIX   0
C18   1    0.361322    0.131925    0.204879    11.00000    0.02903    0.03614 =
         0.03397   -0.01184    0.00888    0.00394
AFIX  43
H18   2    0.386964    0.081825    0.169902    11.00000   -1.20000
AFIX   0
C19   1    0.381593    0.148254    0.288375    11.00000    0.02052    0.02976 =
         0.03556   -0.00341    0.00164    0.00590
AFIX  43
H19   2    0.420900    0.109042    0.310586    11.00000   -1.20000
AFIX   0
C20   1    0.344706    0.221946    0.340255    11.00000    0.02433    0.02208 =
         0.02313   -0.00058    0.00056   -0.00120
C21   1    0.433842    0.140035    0.468384    11.00000    0.03380    0.03672 =
         0.03647    0.00899   -0.00317    0.00504
AFIX 137
H21A  2    0.448024    0.143205    0.528314    11.00000   -1.50000
H21B  2    0.473312    0.153841    0.433437    11.00000   -1.50000
H21C  2    0.414572    0.062380    0.455311    11.00000   -1.50000
AFIX   0
C22   1    0.201147    0.640178    0.366997    11.00000    0.02651    0.02274 =
         0.02923   -0.00408    0.00502   -0.00067
C23   1    0.178225    0.617507    0.447853    11.00000    0.04130    0.02801 =
         0.03179   -0.00256    0.01174    0.00163
AFIX  43
H23A  2    0.186489    0.542542    0.472684    11.00000   -1.20000
AFIX   0
C24   1    0.143683    0.701809    0.492782    11.00000    0.04257    0.03668 =
         0.03933   -0.00625    0.01910   -0.00250
AFIX  43
H24   2    0.128605    0.685055    0.547970    11.00000   -1.20000
AFIX   0
C25   1    0.131383    0.810577    0.456466    11.00000    0.03685    0.02858 =
         0.05295   -0.01323    0.01694   -0.00024
AFIX  43
H25   2    0.108759    0.869705    0.487371    11.00000   -1.20000
AFIX   0
C26   1    0.151701    0.833573    0.375952    11.00000    0.03156    0.02564 =
         0.04714   -0.00214    0.00574    0.00147
AFIX  43
H26   2    0.142155    0.908141    0.351166    11.00000   -1.20000
AFIX   0
C27   1    0.186053    0.749265    0.330173    11.00000    0.02519    0.02478 =
         0.03546    0.00032    0.00143    0.00170
C28   1    0.205771    0.930220    0.214434    11.00000    0.08618    0.03641 =
         0.05730    0.01624    0.01774    0.00529
AFIX 137
H28A  2    0.224872    0.954171    0.160606    11.00000   -1.50000
H28B  2    0.230557    0.969496    0.261180    11.00000   -1.50000
H28C  2    0.157653    0.952446    0.214976    11.00000   -1.50000

HKLF 4

REM  ki496 in P2(1)/c
REM R1 =  0.0477 for   4561 Fo > 4sig(Fo)  and  0.0533 for all   5060 data
REM    339 parameters refined using      0 restraints

END
;