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_4067857
_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         'C12 H24 Li O5 +,Cl3 Sn -'
_chemical_formula_sum            'C12 H24 Cl3 Li O5 Sn'
_chemical_formula_weight         480.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.973(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6864(4)
_cell_length_b                   8.3921(3)
_cell_length_c                   23.1898(12)
_cell_measurement_reflns_used    6731
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.99
_cell_volume                     1877.99(14)
_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 0.855
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10803
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.533
_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            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                3578
_reflns_number_total             4509
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008327_si_001.cif
_cod_data_source_block           ki454
_cod_original_cell_volume        1877.98(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4067857
_computing_special_details
;
TITL ki454 in P2(1)/n
CELL 0.71073   9.6864   8.3921  23.1898  90.000  94.973  90.000
ZERR    4.00   0.0004   0.0003   0.0012   0.000   0.004   0.000
LATT  1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H  CL SN O Li
UNIT 48 96 12 4 20 4

REM colourless slab
SIZE 0.40 0.20 0.10
TEMP -123

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

REM EXTI    0.000604
WGHT    0.030400
FVAR       0.11166
LI    6    0.271668    0.751445    0.427230    11.00000    0.02709    0.03033 =
         0.02083   -0.00091    0.00690   -0.00080
O1    5    0.159669    0.730323    0.352336    11.00000    0.02331    0.03284 =
         0.02363   -0.00335    0.00285   -0.00086
O2    5    0.266601    0.995130    0.400894    11.00000    0.02551    0.02970 =
         0.01977   -0.00215    0.00208    0.00222
O3    5    0.476382    0.807298    0.447975    11.00000    0.02387    0.02423 =
         0.01963    0.00065    0.00333    0.00055
O4    5    0.358507    0.537820    0.399917    11.00000    0.02427    0.02847 =
         0.02572   -0.00019    0.00568   -0.00227
O5    5    0.157614    0.726117    0.489093    11.00000    0.02226    0.05297 =
         0.01750    0.00746    0.00526    0.00192
C1    1    0.116778    0.880513    0.327636    11.00000    0.02593    0.03610 =
         0.02696   -0.00003   -0.00409    0.00607
AFIX  23
H1A   2    0.032553    0.918037    0.344829    11.00000   -1.20000
H1B   2    0.094502    0.868821    0.285372    11.00000   -1.20000
AFIX   0
C2    1    0.231949    0.999557    0.339394    11.00000    0.03521    0.02653 =
         0.02161    0.00086   -0.00156    0.00712
AFIX  23
H2A   2    0.313079    0.969966    0.318497    11.00000   -1.20000
H2B   2    0.200799    1.107509    0.326939    11.00000   -1.20000
AFIX   0
C3    1    0.399081    1.063735    0.418969    11.00000    0.03061    0.02127 =
         0.02505   -0.00293   -0.00046   -0.00219
AFIX  23
H3A   2    0.399952    1.100482    0.459566    11.00000   -1.20000
H3B   2    0.415804    1.157113    0.394431    11.00000   -1.20000
AFIX   0
C4    1    0.512364    0.941796    0.414040    11.00000    0.02574    0.02548 =
         0.02758    0.00289    0.00142   -0.00564
AFIX  23
H4A   2    0.517527    0.910333    0.373138    11.00000   -1.20000
H4B   2    0.603265    0.985757    0.429104    11.00000   -1.20000
AFIX   0
C5    1    0.559869    0.668121    0.439339    11.00000    0.02178    0.02604 =
         0.02436    0.00163    0.00124    0.00509
AFIX  23
H5A   2    0.564945    0.600841    0.474526    11.00000   -1.20000
H5B   2    0.655190    0.701351    0.432565    11.00000   -1.20000
AFIX   0
C6    1    0.498403    0.573659    0.388385    11.00000    0.02384    0.02556 =
         0.02963    0.00059    0.00566    0.00392
AFIX  23
H6A   2    0.499639    0.636595    0.352325    11.00000   -1.20000
H6B   2    0.551564    0.474243    0.384081    11.00000   -1.20000
AFIX   0
C7    1    0.272317    0.484852    0.349925    11.00000    0.02874    0.02510 =
         0.03165   -0.00665    0.00384   -0.00975
AFIX  23
H7A   2    0.193045    0.423468    0.362576    11.00000   -1.20000
H7B   2    0.326415    0.413484    0.326414    11.00000   -1.20000
AFIX   0
C8    1    0.219029    0.624045    0.313533    11.00000    0.02500    0.03240 =
         0.02293   -0.00526    0.00282   -0.00727
AFIX  23
H8A   2    0.295666    0.676475    0.295201    11.00000   -1.20000
H8B   2    0.148424    0.588560    0.282792    11.00000   -1.20000
AFIX   0
C9    1    0.011656    0.761745    0.479536    11.00000    0.02515    0.04998 =
         0.02572    0.00079    0.00090    0.00650
AFIX  23
H9A   2   -0.033075    0.693185    0.448583    11.00000   -1.20000
H9B   2   -0.002702    0.874676    0.468217    11.00000   -1.20000
AFIX   0
C10   1   -0.047180    0.728907    0.536216    11.00000    0.03252    0.05665 =
         0.03839    0.00281    0.01628    0.01347
AFIX  23
H10A  2   -0.079581    0.617333    0.538276    11.00000   -1.20000
H10B  2   -0.125119    0.801641    0.542216    11.00000   -1.20000
AFIX   0
C11   1    0.075420    0.759796    0.580230    11.00000    0.06261    0.04624 =
         0.01767    0.00239    0.01006    0.01717
AFIX  23
H11A  2    0.086987    0.874978    0.588519    11.00000   -1.20000
H11B  2    0.065721    0.701878    0.616851    11.00000   -1.20000
AFIX   0
C12   1    0.193555    0.695418    0.549308    11.00000    0.03373    0.03808 =
         0.02353    0.00801    0.00041   -0.00022
AFIX  23
H12A  2    0.281185    0.749875    0.562701    11.00000   -1.20000
H12B  2    0.204894    0.579626    0.556379    11.00000   -1.20000
AFIX   0
SN    4   -0.237907    0.501031    0.242941    11.00000    0.01705    0.01860 =
         0.01892   -0.00035    0.00019   -0.00120
CL1   3   -0.095488    0.710811    0.193049    11.00000    0.03146    0.02184 =
         0.02139    0.00273    0.00833   -0.00278
CL2   3   -0.029357    0.312954    0.256751    11.00000    0.01815    0.02058 =
         0.02253   -0.00139    0.00283    0.00213
CL3   3   -0.178490    0.624958    0.338992    11.00000    0.02396    0.02928 =
         0.01803   -0.00149    0.00248   -0.00187

HKLF 4

REM  ki454 in P2(1)/n
REM R1 =  0.0232 for   3578 Fo > 4sig(Fo)  and  0.0342 for all   4509 data
REM    199 parameters refined using      0 restraints

END
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