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_4067856
_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,0.5 C6 H14'
_chemical_formula_sum            'C31 H59 P2 S2 Si4 Sn'
_chemical_formula_weight         788.89
_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                 102.3116(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4746(2)
_cell_length_b                   21.3062(4)
_cell_length_c                   18.4807(3)
_cell_measurement_reflns_used    18544
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.75
_cell_volume                     4029.56(13)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.883
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38038
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00004(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         10038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                7460
_reflns_number_total             10038
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008327_si_001.cif
_cod_data_source_block           ki452_compound_11b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4067856
_computing_special_details
;
TITL ki452 in P2(1)/c
CELL 0.71073  10.4746  21.3062  18.4807  90.000 102.3116  90.000
ZERR    4.00   0.0002   0.0004   0.0003   0.000   0.0019   0.000
LATT  1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H SI P S SN
UNIT 124 236 16 8 8 4

REM yellow block
SIZE 0.24 0.10 0.10
TEMP -123

L.S. 8
ACTA 52
BOND $H
FMAP 2
PLAN 10
BIND SN S1

WGHT    0.023800
EXTI    0.000043
FVAR       0.10877
SN    6    0.235534    0.570736    0.494016    11.00000    0.02525    0.01675 =
         0.01583    0.00001    0.00523    0.00011
P1    4    0.304115    0.650303    0.602480    11.00000    0.01699    0.01860 =
         0.01769   -0.00102    0.00442    0.00038
P2    4    0.197190    0.653156    0.387715    11.00000    0.01623    0.01909 =
         0.01659    0.00039    0.00461   -0.00100
S1    5    0.515192    0.600181    0.506288    11.00000    0.01995    0.03120 =
         0.01964    0.00111    0.00674    0.00282
S2    5   -0.025318    0.621102    0.484195    11.00000    0.01884    0.02673 =
         0.02031   -0.00083    0.00720   -0.00197
SI1   3    0.328855    0.555323    0.729693    11.00000    0.02161    0.02292 =
         0.01752   -0.00053    0.00814   -0.00213
SI2   3    0.547343    0.658870    0.734798    11.00000    0.01904    0.02422 =
         0.01803   -0.00430    0.00376   -0.00233
SI3   3    0.159248    0.561732    0.258915    11.00000    0.01996    0.02566 =
         0.01788   -0.00270    0.00645   -0.00076
SI4   3   -0.051752    0.668976    0.257277    11.00000    0.01909    0.02952 =
         0.01950    0.00587    0.00312    0.00249
C1    1    0.423905    0.604937    0.674713    11.00000    0.01774    0.01999 =
         0.01461   -0.00098    0.00527    0.00136
AFIX  13
H1    2    0.473156    0.575854    0.648109    11.00000   -1.20000
AFIX   0
C2    1    0.431689    0.489623    0.778304    11.00000    0.03668    0.03179 =
         0.02910    0.00801    0.01077   -0.00051
AFIX 137
H2A   2    0.381381    0.465733    0.807964    11.00000   -1.50000
H2B   2    0.510096    0.506930    0.810773    11.00000   -1.50000
H2C   2    0.457348    0.461858    0.741587    11.00000   -1.50000
AFIX   0
C3    1    0.264380    0.603572    0.798279    11.00000    0.03378    0.03927 =
         0.03075   -0.00837    0.01731   -0.00455
AFIX 137
H3A   2    0.214062    0.576759    0.825062    11.00000   -1.50000
H3B   2    0.207753    0.636744    0.772300    11.00000   -1.50000
H3C   2    0.337475    0.622543    0.833481    11.00000   -1.50000
AFIX   0
C4    1    0.186111    0.515207    0.669617    11.00000    0.03046    0.03199 =
         0.02646   -0.00017    0.01164   -0.01063
AFIX 137
H4A   2    0.140328    0.490024    0.700504    11.00000   -1.50000
H4B   2    0.216856    0.487820    0.634278    11.00000   -1.50000
H4C   2    0.126277    0.546733    0.642559    11.00000   -1.50000
AFIX   0
C5    1    0.467896    0.732021    0.760486    11.00000    0.03101    0.03029 =
         0.03307   -0.01007    0.00658   -0.00297
AFIX 137
H5A   2    0.514598    0.746494    0.809313    11.00000   -1.50000
H5B   2    0.376720    0.723078    0.761981    11.00000   -1.50000
H5C   2    0.470843    0.764724    0.723589    11.00000   -1.50000
AFIX   0
C6    1    0.683700    0.676994    0.687311    11.00000    0.02295    0.03618 =
         0.02827   -0.00598    0.00636   -0.00813
AFIX 137
H6A   2    0.763151    0.686423    0.724448    11.00000   -1.50000
H6B   2    0.660072    0.713375    0.654763    11.00000   -1.50000
H6C   2    0.699367    0.640688    0.657824    11.00000   -1.50000
AFIX   0
C7    1    0.630920    0.620795    0.824040    11.00000    0.02859    0.03947 =
         0.02217   -0.00509    0.00116   -0.00072
AFIX 137
H7A   2    0.694925    0.649958    0.852400    11.00000   -1.50000
H7B   2    0.675588    0.582607    0.813257    11.00000   -1.50000
H7C   2    0.565849    0.609956    0.853020    11.00000   -1.50000
AFIX   0
C8    1    0.408953    0.702269    0.559807    11.00000    0.02288    0.02220 =
         0.01827    0.00353    0.00001   -0.00225
C9    1    0.397279    0.766890    0.569503    11.00000    0.03496    0.02387 =
         0.03298    0.00310    0.00283    0.00194
AFIX  43
H9    2    0.336273    0.782107    0.596677    11.00000   -1.20000
AFIX   0
C10   1    0.473322    0.809283    0.540102    11.00000    0.05392    0.02234 =
         0.04958    0.00808    0.00704   -0.00680
AFIX  43
H10   2    0.464457    0.853021    0.547735    11.00000   -1.20000
AFIX   0
C11   1    0.560378    0.788504    0.500455    11.00000    0.04900    0.03854 =
         0.03994    0.01585    0.00535   -0.01885
AFIX  43
H11   2    0.612872    0.817877    0.481288    11.00000   -1.20000
AFIX   0
C12   1    0.573339    0.725191    0.487740    11.00000    0.03084    0.04381 =
         0.02626    0.00685    0.00640   -0.01083
AFIX  43
H12   2    0.632639    0.710908    0.458948    11.00000   -1.20000
AFIX   0
C13   1    0.497707    0.682395    0.517951    11.00000    0.02178    0.02655 =
         0.01967    0.00299    0.00061   -0.00258
C14   1    0.579950    0.595403    0.423480    11.00000    0.02917    0.05422 =
         0.02532   -0.00449    0.01457   -0.00262
AFIX 137
H14A  2    0.576858    0.551761    0.406447    11.00000   -1.50000
H14B  2    0.670666    0.610136    0.434247    11.00000   -1.50000
H14C  2    0.527501    0.621717    0.384767    11.00000   -1.50000
AFIX   0
C15   1    0.068742    0.612759    0.314963    11.00000    0.01652    0.02089 =
         0.01613    0.00055    0.00531   -0.00196
AFIX  13
H15   2    0.018065    0.584272    0.341424    11.00000   -1.20000
AFIX   0
C16   1    0.237477    0.611054    0.197220    11.00000    0.03558    0.04112 =
         0.02979    0.00413    0.01839    0.00414
AFIX 137
H16A  2    0.292757    0.584627    0.173133    11.00000   -1.50000
H16B  2    0.291145    0.643528    0.226665    11.00000   -1.50000
H16C  2    0.169659    0.630939    0.159424    11.00000   -1.50000
AFIX   0
C17   1    0.052138    0.500672    0.202698    11.00000    0.03376    0.04341 =
         0.03677   -0.01875    0.00769   -0.00387
AFIX 137
H17A  2    0.100249    0.479893    0.169419    11.00000   -1.50000
H17B  2   -0.026212    0.520784    0.173429    11.00000   -1.50000
H17C  2    0.026536    0.469508    0.235936    11.00000   -1.50000
AFIX   0
C18   1    0.288611    0.514466    0.320516    11.00000    0.03186    0.02958 =
         0.02626   -0.00359    0.00794    0.00776
AFIX 137
H18A  2    0.333817    0.488385    0.290185    11.00000   -1.50000
H18B  2    0.248374    0.487496    0.352378    11.00000   -1.50000
H18C  2    0.351518    0.542717    0.351306    11.00000   -1.50000
AFIX   0
C19   1   -0.138919    0.632455    0.167970    11.00000    0.02821    0.05045 =
         0.02712    0.00670   -0.00141   -0.00029
AFIX 137
H19A  2   -0.201760    0.662522    0.140388    11.00000   -1.50000
H19B  2   -0.185287    0.594741    0.178558    11.00000   -1.50000
H19C  2   -0.075237    0.621028    0.138318    11.00000   -1.50000
AFIX   0
C20   1   -0.184829    0.689205    0.306212    11.00000    0.02463    0.04989 =
         0.03275    0.01279    0.00791    0.01605
AFIX 137
H20A  2   -0.261463    0.704071    0.270165    11.00000   -1.50000
H20B  2   -0.154519    0.722283    0.342678    11.00000   -1.50000
H20C  2   -0.208372    0.651883    0.331484    11.00000   -1.50000
AFIX   0
C21   1    0.031429    0.741103    0.232149    11.00000    0.03588    0.03328 =
         0.03471    0.01332    0.00508    0.00349
AFIX 137
H21A  2   -0.014946    0.756379    0.183622    11.00000   -1.50000
H21B  2    0.121886    0.730984    0.230163    11.00000   -1.50000
H21C  2    0.030866    0.773679    0.269516    11.00000   -1.50000
AFIX   0
C22   1    0.108109    0.713209    0.429913    11.00000    0.02098    0.02077 =
         0.01741   -0.00090    0.00148    0.00202
C23   1    0.139020    0.775913    0.419969    11.00000    0.03401    0.02302 =
         0.02788    0.00041    0.00783   -0.00137
AFIX  43
H23   2    0.202777    0.785437    0.391961    11.00000   -1.20000
AFIX   0
C24   1    0.079277    0.824702    0.449827    11.00000    0.05926    0.02068 =
         0.03924   -0.00258    0.01002    0.00346
AFIX  43
H24   2    0.101842    0.867020    0.442254    11.00000   -1.20000
AFIX   0
C25   1   -0.013328    0.811129    0.490668    11.00000    0.05760    0.02752 =
         0.03744   -0.00641    0.01238    0.01599
AFIX  43
H25   2   -0.055925    0.844425    0.510270    11.00000   -1.20000
AFIX   0
C26   1   -0.044745    0.749829    0.503355    11.00000    0.03378    0.03524 =
         0.02594   -0.00344    0.01174    0.00813
AFIX  43
H26   2   -0.107124    0.740874    0.532459    11.00000   -1.20000
AFIX   0
C27   1    0.015951    0.701018    0.473039    11.00000    0.02096    0.02270 =
         0.02031   -0.00097    0.00238    0.00281
C28   1   -0.082843    0.621862    0.569220    11.00000    0.03465    0.03932 =
         0.02888    0.00219    0.01843    0.00162
AFIX 137
H28A  2   -0.165221    0.645202    0.561916    11.00000   -1.50000
H28B  2   -0.017596    0.642127    0.608102    11.00000   -1.50000
H28C  2   -0.097047    0.578673    0.583961    11.00000   -1.50000
AFIX   0
C29   1    0.563211    0.516387    1.001031    11.00000    0.05808    0.03660 =
         0.03065    0.00625    0.01447    0.00519
AFIX  23
H29A  2    0.547791    0.550196    0.963426    11.00000   -1.20000
H29B  2    0.590810    0.536634    1.050097    11.00000   -1.20000
AFIX   0
C30   1    0.673227    0.476888    0.987774    11.00000    0.06147    0.04681 =
         0.04414    0.00574    0.01255    0.00524
AFIX  23
H30A  2    0.646923    0.457612    0.938081    11.00000   -1.20000
H30B  2    0.687425    0.442398    1.024515    11.00000   -1.20000
AFIX   0
C31   1    0.802190    0.510820    0.992133    11.00000    0.05246    0.06287 =
         0.03942    0.00051    0.00629   -0.00463
AFIX 137
H31A  2    0.867142    0.481339    0.980925    11.00000   -1.50000
H31B  2    0.832759    0.527759    1.042131    11.00000   -1.50000
H31C  2    0.789868    0.545253    0.956153    11.00000   -1.50000

HKLF 4

REM  ki452 in P2(1)/c
REM R1 =  0.0230 for   7460 Fo > 4sig(Fo)  and  0.0387 for all  10038 data
REM    377 parameters refined using      0 restraints

END
;