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_7017405
_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         'C46 H104 B2 K2 N6 P2 S2 Si4'
_chemical_formula_sum            'C46 H104 B2 K2 N6 P2 S2 Si4'
_chemical_formula_weight         1079.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.977(4)
_cell_angle_beta                 108.829(5)
_cell_angle_gamma                105.691(5)
_cell_formula_units_Z            1
_cell_length_a                   11.1081(6)
_cell_length_b                   12.0772(7)
_cell_length_c                   14.3398(7)
_cell_measurement_reflns_used    5761
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.21
_cell_measurement_theta_min      3.44
_cell_volume                     1658.67(19)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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 Ultra optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8950
_diffrn_reflns_theta_full        62.29
_diffrn_reflns_theta_max         62.29
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.443
_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    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00075(18)
_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   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0465P)^2^+0.5734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                4426
_reflns_number_total             5133
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1dt11368b.txt
_cod_data_source_block           ki450_compound_12
_cod_original_cell_volume        1658.67(15)
_cod_database_code               7017405
_computing_special_details
;
TITL ki450 in P-1
CELL 1.54178 11.1081 12.0772 14.3398 101.977 108.829 105.691
ZERR 1.00 0.0006 0.0007 0.0007 0.004 0.005 0.005
LATT 1
SFAC C H B N SI P S K
UNIT 46 104 2 6 4 2 2 2

REM colourless block
SIZE 0.30 0.20 0.20
TEMP -123

L.S. 8
ACTA
BOND $H
FMAP 2
PLAN 10
EQIV $1 -x+1, -y+1, -z+1
BIND K H1A_$1
BIND K H1B_$1
BIND K H1C_$1
FREE K B
FREE K B_$1
FREE B K_$1

WGHT 0.046500 0.573400
EXTI 0.000748
FVAR 0.24898
K 8 0.336992 0.364815 0.364082 11.00000 0.02765 0.02629 =
0.02278 0.00592 0.00661 0.00755
P 6 0.369206 0.642568 0.293321 11.00000 0.02119 0.02160 =
0.02097 0.00856 0.00994 0.00823
S 7 0.081508 0.514482 0.287531 11.00000 0.02707 0.02642 =
0.05235 0.01195 0.02036 0.00724
SI1 5 0.295360 0.720788 0.099670 11.00000 0.03528 0.03887 =
0.02338 0.01560 0.01057 0.01852
SI2 5 0.593227 0.712614 0.208454 11.00000 0.02716 0.03378 =
0.02883 0.01368 0.01680 0.01204
B 3 0.511000 0.651095 0.423221 11.00000 0.02758 0.02800 =
0.02115 0.01136 0.00867 0.01242
H1A 2 0.570314 0.591523 0.405756 11.00000 0.03956
H1B 2 0.585784 0.748683 0.471517 11.00000 0.03596
H1C 2 0.445659 0.613418 0.464500 11.00000 0.02904
N1 4 0.072851 0.182196 0.311990 11.00000 0.03492 0.03579 =
0.03525 0.01855 0.01953 0.01429
N2 4 0.195441 0.194177 0.154818 11.00000 0.02723 0.02463 =
0.02448 0.00700 0.01039 0.00768
N3 4 0.483597 0.230302 0.284156 11.00000 0.02750 0.03364 =
0.03091 0.01379 0.01289 0.01195
C1 1 0.440996 0.740751 0.223205 11.00000 0.02656 0.02381 =
0.02181 0.00920 0.01178 0.01056
AFIX 13
H1 2 0.474224 0.827094 0.268337 11.00000 -1.20000
AFIX 0
C2 1 0.347865 0.832919 0.033403 11.00000 0.06486 0.06171 =
0.04504 0.03599 0.02790 0.03626
AFIX 137
H2A 2 0.266212 0.837327 -0.016487 11.00000 -1.50000
H2B 2 0.400918 0.806554 -0.003438 11.00000 -1.50000
H2C 2 0.403807 0.913265 0.085625 11.00000 -1.50000
AFIX 0
C3 1 0.229297 0.564116 0.006152 11.00000 0.05890 0.04887 =
0.02893 0.00704 0.00120 0.01881
AFIX 137
H3A 2 0.148894 0.553621 -0.054413 11.00000 -1.50000
H3B 2 0.203945 0.504634 0.040284 11.00000 -1.50000
H3C 2 0.300335 0.551762 -0.016559 11.00000 -1.50000
AFIX 0
C4 1 0.149184 0.747773 0.124890 11.00000 0.03992 0.08057 =
0.03796 0.03285 0.01288 0.03460
AFIX 137
H4A 2 0.083061 0.749627 0.061102 11.00000 -1.50000
H4B 2 0.182960 0.825688 0.180047 11.00000 -1.50000
H4C 2 0.104848 0.682161 0.146752 11.00000 -1.50000
AFIX 0
C5 1 0.636303 0.766963 0.105721 11.00000 0.05019 0.06619 =
0.04931 0.03147 0.03523 0.02532
AFIX 137
H5A 2 0.720686 0.756106 0.105959 11.00000 -1.50000
H5B 2 0.649058 0.853242 0.120155 11.00000 -1.50000
H5C 2 0.561678 0.719943 0.037360 11.00000 -1.50000
AFIX 0
C6 1 0.748251 0.797111 0.332295 11.00000 0.02692 0.05437 =
0.04252 0.01603 0.01476 0.00909
AFIX 137
H6A 2 0.736550 0.764702 0.387352 11.00000 -1.50000
H6B 2 0.761159 0.883528 0.352365 11.00000 -1.50000
H6C 2 0.828439 0.787468 0.322190 11.00000 -1.50000
AFIX 0
C7 1 0.562701 0.546490 0.171563 11.00000 0.04107 0.04073 =
0.04080 0.01244 0.02124 0.02159
AFIX 137
H7A 2 0.542170 0.514442 0.224362 11.00000 -1.50000
H7B 2 0.644563 0.534092 0.167124 11.00000 -1.50000
H7C 2 0.485370 0.503865 0.103866 11.00000 -1.50000
AFIX 0
C8 1 0.287962 0.733054 0.354034 11.00000 0.02222 0.02781 =
0.01924 0.01157 0.00824 0.01161
C9 1 0.347528 0.858658 0.402115 11.00000 0.02231 0.02818 =
0.02632 0.01093 0.00963 0.00866
AFIX 43
H9 2 0.432894 0.901187 0.401868 11.00000 -1.20000
AFIX 0
C10 1 0.286388 0.923391 0.450174 11.00000 0.03528 0.02628 =
0.02922 0.00850 0.01140 0.01493
AFIX 43
H10 2 0.328202 1.009250 0.480722 11.00000 -1.20000
AFIX 0
C11 1 0.164420 0.862323 0.453356 11.00000 0.04078 0.03760 =
0.03832 0.01523 0.02423 0.02426
AFIX 43
H11 2 0.122738 0.906018 0.487412 11.00000 -1.20000
AFIX 0
C12 1 0.102588 0.738081 0.407337 11.00000 0.03362 0.03688 =
0.04486 0.01983 0.02604 0.01760
AFIX 43
H12 2 0.018939 0.696381 0.410490 11.00000 -1.20000
AFIX 0
C13 1 0.162201 0.673054 0.356056 11.00000 0.02795 0.02664 =
0.02953 0.01401 0.01420 0.01216
C14 1 -0.084157 0.480989 0.292836 11.00000 0.03153 0.04249 =
0.07772 0.01961 0.02819 0.00867
AFIX 137
H14A 2 -0.142417 0.396817 0.249563 11.00000 -1.50000
H14B 2 -0.126161 0.536193 0.266831 11.00000 -1.50000
H14C 2 -0.073862 0.491768 0.364996 11.00000 -1.50000
AFIX 0
C15 1 0.011944 0.234403 0.376859 11.00000 0.07332 0.06966 =
0.05273 0.03477 0.04271 0.04256
AFIX 137
H15A 2 0.064223 0.244728 0.449757 11.00000 -1.50000
H15B 2 -0.082603 0.180031 0.354758 11.00000 -1.50000
H15C 2 0.013162 0.313639 0.369784 11.00000 -1.50000
AFIX 0
C16 1 0.082777 0.071518 0.331520 11.00000 0.06071 0.05117 =
0.05982 0.03326 0.02907 0.02939
AFIX 137
H16A 2 0.129048 0.088090 0.406572 11.00000 -1.50000
H16B 2 0.135082 0.041415 0.295844 11.00000 -1.50000
H16C 2 -0.009076 0.010067 0.305376 11.00000 -1.50000
AFIX 0
C17 1 -0.005163 0.163188 0.202628 11.00000 0.02601 0.03664 =
0.04078 0.01624 0.01367 0.00991
AFIX 23
H17A 2 -0.011806 0.241286 0.195276 11.00000 -1.20000
H17B 2 -0.099009 0.105146 0.181004 11.00000 -1.20000
AFIX 0
C18 1 0.055684 0.115151 0.130009 11.00000 0.02781 0.03209 =
0.02937 0.00554 0.00764 0.00382
AFIX 23
H18A 2 0.055512 0.033961 0.133038 11.00000 -1.20000
H18B 2 -0.002948 0.105060 0.057821 11.00000 -1.20000
AFIX 0
C19 1 0.193768 0.293025 0.111081 11.00000 0.03431 0.03360 =
0.03600 0.01416 0.01423 0.01264
AFIX 7
H19A 2 0.287477 0.349934 0.134473 11.00000 -1.50000
H19B 2 0.140045 0.335802 0.134542 11.00000 -1.50000
H19C 2 0.152657 0.259650 0.034887 11.00000 -1.50000
AFIX 0
C20 1 0.272691 0.127096 0.119148 11.00000 0.03772 0.03043 =
0.02536 0.00915 0.01464 0.01364
AFIX 23
H20A 2 0.242036 0.108405 0.042824 11.00000 -1.20000
H20B 2 0.251709 0.048910 0.133442 11.00000 -1.20000
AFIX 0
C21 1 0.425936 0.195009 0.170176 11.00000 0.03652 0.03245 =
0.03366 0.01575 0.02089 0.01702
AFIX 23
H21A 2 0.470589 0.143148 0.143132 11.00000 -1.20000
H21B 2 0.447609 0.269133 0.149927 11.00000 -1.20000
AFIX 0
C22 1 0.628650 0.303834 0.326513 11.00000 0.02928 0.05166 =
0.05143 0.02037 0.01367 0.01535
AFIX 137
H22A 2 0.666493 0.326146 0.402600 11.00000 -1.50000
H22B 2 0.640715 0.377686 0.306626 11.00000 -1.50000
H22C 2 0.676277 0.257112 0.298794 11.00000 -1.50000
AFIX 0
C23 1 0.466710 0.124137 0.319307 11.00000 0.04840 0.04597 =
0.03906 0.02473 0.01902 0.01741
AFIX 137
H23A 2 0.510432 0.150720 0.395506 11.00000 -1.50000
H23B 2 0.509195 0.072864 0.290037 11.00000 -1.50000
H23C 2 0.369171 0.077580 0.295968 11.00000 -1.50000

HKLF 4

REM ki450 in P-1
REM R1 = 0.0315 for 4426 Fo > 4sig(Fo) and 0.0388 for all 5133 data
REM 314 parameters refined using 0 restraints

END
;