Synthesis, structures and stabilities of thioanisole-functionalised phosphido-borane complexes of the alkali metals.
Izod, Keith; Watson, James M.; Clegg, William; Harrington, Ross W.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 11712–11718; doi:10.1039/c1dt11368b

data_7017403
_publ_section_title
;
 Synthesis, structures and stabilities of thioanisole-functionalised
 phosphido-borane complexes of the alkali metals.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11712
_journal_page_last               11718
_journal_paper_doi               10.1039/c1dt11368b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C36 H74 B2 Li2 O2 P2 S2 Si4'
_chemical_formula_sum            'C36 H74 B2 Li2 O2 P2 S2 Si4'
_chemical_formula_weight         812.87
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.733(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4504(5)
_cell_length_b                   16.2605(5)
_cell_length_c                   11.2638(4)
_cell_measurement_reflns_used    7105
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.94
_cell_volume                     2393.08(15)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_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 0.870
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15640
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                4054
_reflns_number_total             5823
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1dt11368b.txt
_cod_data_source_block           ki397_compound_10
_cod_original_cell_volume        2393.08(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017403
_computing_special_details
;
TITL ki397 in P2(1)/c
CELL 0.71073 13.4504 16.2605 11.2638 90.0000 103.733 90.0000
ZERR 2.00 0.0005 0.0005 0.0004 0.0000 0.004 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H O S Si Li B P
UNIT 72 148 4 4 8 4 4 4

REM colourless block
SIZE 0.32 0.30 0.30
TEMP -123

L.S. 8
ACTA 52
BOND $H
EQIV $1 -x+1, -y+1, -z+1
BIND LI H1A_$1
BIND LI H1B_$1
FREE LI B_$1
FREE B LI_$1
BIND H1A LI_$1
BIND H1B LI_$1
FMAP 2
PLAN 10

REM EXTI 0.000000
WGHT 0.040400
FVAR 2.85744
P 8 0.686417 0.533735 0.555606 11.00000 0.01758 0.01354 =
0.01600 0.00064 0.00411 -0.00028
S 4 0.578705 0.671164 0.686702 11.00000 0.02861 0.02567 =
0.03153 -0.01102 0.01379 -0.00699
SI1 5 0.900415 0.488698 0.725528 11.00000 0.02002 0.02593 =
0.02142 0.00103 -0.00007 0.00226
SI2 5 0.782814 0.364208 0.525002 11.00000 0.03178 0.01599 =
0.02267 -0.00125 0.00471 0.00448
O 3 0.607358 0.476186 0.860216 11.00000 0.03366 0.03179 =
0.01519 0.00259 0.00154 -0.00888
B 7 0.608583 0.530930 0.384662 11.00000 0.02167 0.02029 =
0.01811 0.00069 0.00142 -0.00218
H1A 2 0.541629 0.576179 0.378290 11.00000 0.02332
H1B 2 0.576693 0.466876 0.362423 11.00000 0.02040
H1C 2 0.656754 0.552544 0.320431 11.00000 0.03252
LI 6 0.565871 0.511258 0.693894 11.00000 0.02457 0.02977 =
0.01836 0.00256 0.00409 -0.00354
C1 1 0.808587 0.475557 0.570916 11.00000 0.01974 0.01737 =
0.01864 0.00186 0.00602 0.00240
AFIX 13
H1 2 0.843252 0.500045 0.509925 11.00000 -1.20000
AFIX 0
C2 1 1.033549 0.474881 0.705496 11.00000 0.02271 0.05981 =
0.05163 0.00331 0.00374 0.00441
AFIX 137
H2A 2 1.082721 0.484993 0.783492 11.00000 -1.50000
H2B 2 1.045786 0.513841 0.644118 11.00000 -1.50000
H2C 2 1.041881 0.418573 0.678384 11.00000 -1.50000
AFIX 0
C3 1 0.873157 0.413643 0.839793 11.00000 0.04696 0.03564 =
0.02230 0.00435 0.00382 0.00474
AFIX 137
H3A 2 0.912119 0.429027 0.921788 11.00000 -1.50000
H3B 2 0.893245 0.358306 0.820087 11.00000 -1.50000
H3C 2 0.799838 0.414304 0.837323 11.00000 -1.50000
AFIX 0
C4 1 0.900564 0.591847 0.799110 11.00000 0.03982 0.03143 =
0.02649 -0.00504 -0.00820 -0.00285
AFIX 137
H4A 2 0.947227 0.590911 0.880441 11.00000 -1.50000
H4B 2 0.831236 0.604997 0.806700 11.00000 -1.50000
H4C 2 0.923305 0.633670 0.748736 11.00000 -1.50000
AFIX 0
C5 1 0.751849 0.351753 0.355711 11.00000 0.05867 0.03316 =
0.02844 -0.00965 0.00709 0.00709
AFIX 137
H5A 2 0.735636 0.294009 0.334765 11.00000 -1.50000
H5B 2 0.810860 0.368535 0.324512 11.00000 -1.50000
H5C 2 0.692767 0.386165 0.318838 11.00000 -1.50000
AFIX 0
C6 1 0.897857 0.296524 0.578704 11.00000 0.05432 0.03383 =
0.05140 -0.00870 0.00369 0.02073
AFIX 137
H6A 2 0.881014 0.240181 0.550004 11.00000 -1.50000
H6B 2 0.918147 0.297031 0.668213 11.00000 -1.50000
H6C 2 0.954442 0.317041 0.545916 11.00000 -1.50000
AFIX 0
C7 1 0.675886 0.323362 0.586172 11.00000 0.04938 0.02043 =
0.04069 0.00149 0.01078 -0.00707
AFIX 137
H7A 2 0.667396 0.264492 0.567947 11.00000 -1.50000
H7B 2 0.612548 0.352438 0.547969 11.00000 -1.50000
H7C 2 0.691338 0.331621 0.674852 11.00000 -1.50000
AFIX 0
C8 1 0.729942 0.641732 0.567707 11.00000 0.01824 0.01473 =
0.01658 0.00168 -0.00033 0.00032
C9 1 0.807529 0.668208 0.513755 11.00000 0.02541 0.01935 =
0.03214 0.00290 0.01070 0.00234
AFIX 43
H9 2 0.834791 0.630782 0.464966 11.00000 -1.20000
AFIX 0
C10 1 0.846017 0.747636 0.529313 11.00000 0.02595 0.02315 =
0.04629 0.00819 0.01396 -0.00166
AFIX 43
H10 2 0.899107 0.764177 0.491917 11.00000 -1.20000
AFIX 0
C11 1 0.806474 0.802348 0.599581 11.00000 0.03119 0.01487 =
0.04349 0.00255 0.00415 -0.00594
AFIX 43
H11 2 0.834524 0.856087 0.613575 11.00000 -1.20000
AFIX 0
C12 1 0.726601 0.779624 0.649611 11.00000 0.02782 0.01808 =
0.02783 -0.00369 0.00346 0.00033
AFIX 43
H12 2 0.698295 0.818301 0.695604 11.00000 -1.20000
AFIX 0
C13 1 0.687150 0.700139 0.633034 11.00000 0.01785 0.01814 =
0.01766 0.00083 0.00009 0.00027
C14 1 0.582472 0.736156 0.815864 11.00000 0.04425 0.02670 =
0.03153 -0.00874 0.01802 -0.00077
AFIX 137
H14A 2 0.572941 0.793515 0.788853 11.00000 -1.50000
H14B 2 0.648845 0.730223 0.874288 11.00000 -1.50000
H14C 2 0.527696 0.720328 0.855202 11.00000 -1.50000
AFIX 0
C15 1 0.672738 0.523708 0.956144 11.00000 0.02932 0.03601 =
0.02181 -0.00197 0.00339 -0.00925
AFIX 23
H15A 2 0.636096 0.572784 0.975744 11.00000 -1.20000
H15B 2 0.734851 0.541990 0.930889 11.00000 -1.20000
AFIX 0
C16 1 0.700913 0.467178 1.065321 11.00000 0.02800 0.04590 =
0.02008 -0.00084 0.00158 0.00185
AFIX 23
H16A 2 0.714446 0.498400 1.142961 11.00000 -1.20000
H16B 2 0.761547 0.433296 1.062870 11.00000 -1.20000
AFIX 0
C17 1 0.605107 0.414718 1.049352 11.00000 0.03784 0.02801 =
0.02038 0.00439 0.00791 0.00399
AFIX 23
H17A 2 0.620398 0.361296 1.091933 11.00000 -1.20000
H17B 2 0.551436 0.443425 1.080306 11.00000 -1.20000
AFIX 0
C18 1 0.573037 0.403249 0.912419 11.00000 0.04194 0.02640 =
0.02078 0.00296 0.00522 -0.00514
AFIX 23
H18A 2 0.605332 0.353467 0.887560 11.00000 -1.20000
H18B 2 0.497772 0.397578 0.885127 11.00000 -1.20000

HKLF 4

REM ki397 in P2(1)/c
REM R1 = 0.0324 for 4054 Fo > 4sig(Fo) and 0.0539 for all 5823 data
REM 245 parameters refined using 0 restraints

END
;