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_7017404
_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         'C20 H45 B N2 Na P S Si2'
_chemical_formula_sum            'C20 H45 B N2 Na P S Si2'
_chemical_formula_weight         466.59
_chemical_name_systematic
;
?
;
_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                93.397(7)
_cell_angle_beta                 104.760(7)
_cell_angle_gamma                97.552(6)
_cell_formula_units_Z            4
_cell_length_a                   11.3566(9)
_cell_length_b                   13.2652(10)
_cell_length_c                   21.1564(18)
_cell_measurement_reflns_used    3364
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      2.76
_cell_volume                     3040.9(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.2516
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26610
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.969
_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    1.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.698
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         10697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.698
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                4259
_reflns_number_total             10697
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1dt11368b.txt
_cod_data_source_block           ki385_compound_11
_cod_database_code               7017404
_computing_special_details
;
TITL ki385 in P-1
CELL 0.71073 11.3566 13.2652 21.1564 93.397 104.760 97.552
ZERR 4.00 0.0009 0.0010 0.0018 0.007 0.007 0.006
LATT 1
SFAC C H B N NA SI P S
UNIT 80 180 4 8 4 8 4 4

REM colourless block
SIZE 0.12 0.10 0.08
TEMP -123
OMIT -3 50

REM unidentified disordered solved treated by squeeze

L.S. 8
BOND $H
ACTA
FMAP 2
PLAN 10
EQIV $1 x, y+1, z
EQIV $2 x, y-1, z
FREE B1 NA2_$2
FREE B2 NA1
FREE NA2 B1_$1
BIND NA2 H1A_$1
BIND NA2 H1B_$1
BIND NA2 H1C_$1

REM EXTI 0.000000
WGHT 0.031900
FVAR 2.19523
P1 7 1.005115 1.176837 0.200608 11.00000 0.02683 0.02065 =
0.02546 0.00254 0.00955 0.00565
P2 7 1.061880 1.699342 0.325368 11.00000 0.02381 0.01984 =
0.02657 -0.00123 0.00566 0.00455
S1 8 0.954540 1.372419 0.127818 11.00000 0.04497 0.02159 =
0.03117 0.00365 0.01503 0.01173
S2 8 1.081312 1.916421 0.401353 11.00000 0.04608 0.02177 =
0.03499 0.00137 0.00630 0.00817
SI1 6 0.725863 1.076624 0.119053 11.00000 0.03453 0.03614 =
0.03255 -0.00119 0.00935 -0.00088
SI2 6 0.801713 1.147433 0.272624 11.00000 0.02866 0.03684 =
0.02918 0.00334 0.01390 0.00734
SI3 6 0.852802 1.620346 0.398158 11.00000 0.03659 0.03144 =
0.03779 -0.00194 0.01454 0.00015
SI4 6 0.792593 1.641317 0.243524 11.00000 0.02371 0.03136 =
0.03718 -0.00349 0.00360 0.00768
B1 3 1.068976 1.053373 0.230387 11.00000 0.03607 0.02707 =
0.03558 0.00994 0.01656 0.01065
H1A 2 1.062394 1.048232 0.285381 11.00000 0.03536
H1B 2 1.170119 1.068148 0.230369 11.00000 0.03940
H1C 2 1.017367 0.980382 0.191006 11.00000 0.05954
B2 3 1.101318 1.568160 0.296137 11.00000 0.03182 0.01801 =
0.03976 0.00266 0.01281 0.00699
H2A 2 1.199986 1.582050 0.298099 11.00000 0.03148
H2B 2 1.047747 1.550644 0.239355 11.00000 0.03068
H2C 2 1.076191 1.502791 0.322685 11.00000 0.03178
NA1 5 1.142210 1.380395 0.260249 11.00000 0.02747 0.02335 =
0.03494 -0.00112 0.00867 0.00595
NA2 5 1.152285 1.885106 0.271532 11.00000 0.02916 0.02447 =
0.03767 0.00637 0.01282 0.00793
N1 4 1.316966 1.344496 0.354101 11.00000 0.02848 0.03070 =
0.03630 0.00183 0.00985 0.01258
N2 4 1.324416 1.387552 0.213956 11.00000 0.02701 0.03161 =
0.03468 0.00428 0.00697 0.00453
N3 4 1.380336 1.903507 0.325630 11.00000 0.02891 0.02839 =
0.03967 -0.00103 0.00705 0.00195
N4 4 1.245271 1.819258 0.183286 11.00000 0.03616 0.03321 =
0.03497 0.00559 0.01508 0.01258
C1 1 0.833518 1.161508 0.190694 11.00000 0.02005 0.01707 =
0.02193 0.00642 0.00339 0.00321
AFIX 13
H1 2 0.813565 1.231161 0.181106 11.00000 -1.20000
AFIX 0
C2 1 0.724610 1.128043 0.039632 11.00000 0.04165 0.06649 =
0.03261 -0.00098 -0.00430 -0.01198
AFIX 137
H2D 2 0.713385 1.200013 0.042468 11.00000 -1.50000
H2E 2 0.656795 1.089069 0.004990 11.00000 -1.50000
H2F 2 0.802987 1.122315 0.029320 11.00000 -1.50000
AFIX 0
C3 1 0.761442 0.943439 0.113295 11.00000 0.06283 0.03749 =
0.05532 -0.01651 0.00942 -0.00289
AFIX 137
H3A 2 0.704622 0.904299 0.074153 11.00000 -1.50000
H3B 2 0.752063 0.910972 0.152508 11.00000 -1.50000
H3C 2 0.846313 0.945147 0.110201 11.00000 -1.50000
AFIX 0
C4 1 0.562487 1.066987 0.123935 11.00000 0.04055 0.07696 =
0.05113 -0.01337 0.00635 -0.00305
AFIX 137
H4A 2 0.540022 1.135630 0.126838 11.00000 -1.50000
H4B 2 0.554053 1.033533 0.162962 11.00000 -1.50000
H4C 2 0.507883 1.026755 0.084560 11.00000 -1.50000
AFIX 0
C5 1 0.658814 1.203001 0.273566 11.00000 0.04238 0.06584 =
0.03958 0.00182 0.02179 0.01492
AFIX 137
H5A 2 0.656394 1.263706 0.249300 11.00000 -1.50000
H5B 2 0.659042 1.222147 0.319058 11.00000 -1.50000
H5C 2 0.586222 1.152230 0.252834 11.00000 -1.50000
AFIX 0
C6 1 0.780297 1.011072 0.290785 11.00000 0.03932 0.05687 =
0.04928 0.02133 0.02130 0.00566
AFIX 137
H6A 2 0.853826 0.980983 0.288951 11.00000 -1.50000
H6B 2 0.708391 0.973048 0.258188 11.00000 -1.50000
H6C 2 0.767443 1.007685 0.334738 11.00000 -1.50000
AFIX 0
C7 1 0.927638 1.219864 0.339305 11.00000 0.04737 0.06052 =
0.02440 -0.00279 0.01129 0.01247
AFIX 137
H7A 2 0.940766 1.291426 0.330133 11.00000 -1.50000
H7B 2 1.003412 1.190511 0.342114 11.00000 -1.50000
H7C 2 0.905579 1.216100 0.381062 11.00000 -1.50000
AFIX 0
C8 1 1.024469 1.185508 0.117616 11.00000 0.01621 0.02569 =
0.02691 0.00257 0.00367 0.00750
C9 1 1.068086 1.109983 0.086352 11.00000 0.03152 0.02218 =
0.03332 0.00289 0.01332 0.00424
AFIX 43
H9 2 1.078084 1.048110 0.106124 11.00000 -1.20000
AFIX 0
C10 1 1.097793 1.120747 0.027455 11.00000 0.03619 0.03131 =
0.03683 -0.00135 0.01551 0.01226
AFIX 43
H10 2 1.128503 1.067573 0.007465 11.00000 -1.20000
AFIX 0
C11 1 1.082072 1.210248 -0.001923 11.00000 0.04412 0.03369 =
0.02378 0.00222 0.01709 0.00353
AFIX 43
H11 2 1.102785 1.219359 -0.042190 11.00000 -1.20000
AFIX 0
C12 1 1.036167 1.286241 0.027523 11.00000 0.03406 0.02319 =
0.02995 0.00320 0.00784 0.00259
AFIX 43
H12 2 1.023433 1.346864 0.006663 11.00000 -1.20000
AFIX 0
C13 1 1.008653 1.275450 0.086530 11.00000 0.02158 0.02001 =
0.02437 -0.00284 0.00645 0.00406
C14 1 0.958664 1.477270 0.078176 11.00000 0.06179 0.02252 =
0.04570 0.00701 0.01945 0.01274
AFIX 137
H14A 2 0.906978 1.455520 0.033537 11.00000 -1.50000
H14B 2 1.043672 1.499409 0.076761 11.00000 -1.50000
H14C 2 0.927592 1.534135 0.097122 11.00000 -1.50000
AFIX 0
C15 1 1.327838 1.475663 0.176266 11.00000 0.05256 0.05099 =
0.05171 0.01511 0.01621 0.00740
AFIX 137
H15A 2 1.406436 1.486941 0.164656 11.00000 -1.50000
H15B 2 1.319485 1.536245 0.202655 11.00000 -1.50000
H15C 2 1.259899 1.463137 0.136103 11.00000 -1.50000
AFIX 0
C16 1 1.334851 1.296862 0.173725 11.00000 0.03832 0.04484 =
0.04230 -0.00537 0.01010 0.00512
AFIX 137
H16A 2 1.417851 1.303081 0.167273 11.00000 -1.50000
H16B 2 1.274028 1.291200 0.130986 11.00000 -1.50000
H16C 2 1.319642 1.235740 0.196047 11.00000 -1.50000
AFIX 0
C17 1 1.425389 1.407402 0.273599 11.00000 0.02134 0.03801 =
0.04363 -0.00606 0.00864 0.00125
AFIX 23
H17A 2 1.426994 1.476677 0.294278 11.00000 -1.20000
H17B 2 1.504121 1.406400 0.261716 11.00000 -1.20000
AFIX 0
C18 1 1.416121 1.331446 0.322728 11.00000 0.02740 0.03989 =
0.03689 -0.00416 0.00034 0.01273
AFIX 23
H18A 2 1.400827 1.261436 0.300369 11.00000 -1.20000
H18B 2 1.495465 1.339410 0.356916 11.00000 -1.20000
AFIX 0
C19 1 1.356346 1.428511 0.406354 11.00000 0.04581 0.04425 =
0.03649 -0.00154 0.00872 0.01872
AFIX 137
H19A 2 1.429410 1.414944 0.439024 11.00000 -1.50000
H19B 2 1.289752 1.434553 0.427417 11.00000 -1.50000
H19C 2 1.376287 1.492383 0.387663 11.00000 -1.50000
AFIX 0
C20 1 1.285177 1.250291 0.383728 11.00000 0.04386 0.04302 =
0.04491 0.00901 0.01584 0.01418
AFIX 137
H20A 2 1.358104 1.236274 0.416310 11.00000 -1.50000
H20B 2 1.256597 1.192993 0.349389 11.00000 -1.50000
H20C 2 1.219703 1.258996 0.405176 11.00000 -1.50000
AFIX 0
C21 1 0.895792 1.684166 0.328117 11.00000 0.01822 0.01367 =
0.03501 -0.00404 0.00742 0.00067
AFIX 13
H21 2 0.881615 1.756130 0.335961 11.00000 -1.20000
AFIX 0
C22 1 0.917076 1.699537 0.477747 11.00000 0.06042 0.05672 =
0.03041 -0.00764 0.01871 -0.00749
AFIX 137
H22A 2 0.900128 1.769569 0.472565 11.00000 -1.50000
H22B 2 1.006296 1.699959 0.492087 11.00000 -1.50000
H22C 2 0.878793 1.670962 0.510678 11.00000 -1.50000
AFIX 0
C23 1 0.900534 1.491424 0.407090 11.00000 0.06381 0.03737 =
0.05084 0.00457 0.02901 0.00323
AFIX 137
H23A 2 0.990093 1.497549 0.414673 11.00000 -1.50000
H23B 2 0.859935 1.446404 0.366883 11.00000 -1.50000
H23C 2 0.876634 1.462632 0.444404 11.00000 -1.50000
AFIX 0
C24 1 0.682826 1.603148 0.387416 11.00000 0.04719 0.08239 =
0.05340 -0.00489 0.02204 -0.00052
AFIX 137
H24A 2 0.653550 1.669063 0.381140 11.00000 -1.50000
H24B 2 0.664036 1.576636 0.426573 11.00000 -1.50000
H24C 2 0.641656 1.554714 0.348894 11.00000 -1.50000
AFIX 0
C25 1 0.861820 1.695421 0.179764 11.00000 0.04267 0.04698 =
0.03602 0.00708 0.00742 0.01410
AFIX 137
H25D 2 0.938688 1.668487 0.181198 11.00000 -1.50000
H25E 2 0.879129 1.770046 0.188176 11.00000 -1.50000
H25F 2 0.804116 1.676237 0.136324 11.00000 -1.50000
AFIX 0
C26 1 0.758173 1.499967 0.225328 11.00000 0.03326 0.04454 =
0.04210 -0.01152 0.01033 0.00057
AFIX 137
H26A 2 0.835418 1.472028 0.230457 11.00000 -1.50000
H26B 2 0.706975 1.482626 0.180143 11.00000 -1.50000
H26C 2 0.713996 1.470795 0.255800 11.00000 -1.50000
AFIX 0
C27 1 0.642902 1.692104 0.233122 11.00000 0.03615 0.04929 =
0.05776 -0.00457 -0.00025 0.01338
AFIX 137
H25A 2 0.593675 1.654906 0.258643 11.00000 -1.50000
H25B 2 0.597499 1.682996 0.186593 11.00000 -1.50000
H25C 2 0.659344 1.764938 0.248698 11.00000 -1.50000
AFIX 0
C28 1 1.152018 1.729217 0.411386 11.00000 0.02182 0.01984 =
0.02734 -0.00155 0.00497 -0.00088
C29 1 1.220873 1.660188 0.443931 11.00000 0.02756 0.02446 =
0.03391 -0.00075 0.00367 0.00042
AFIX 43
H29 2 1.212781 1.593230 0.423139 11.00000 -1.20000
AFIX 0
C30 1 1.301526 1.685499 0.506049 11.00000 0.03926 0.03591 =
0.03990 0.00668 0.00286 0.00870
AFIX 43
H30 2 1.346904 1.636146 0.527346 11.00000 -1.20000
AFIX 0
C31 1 1.315144 1.782152 0.536370 11.00000 0.04521 0.04256 =
0.02990 0.00382 -0.00464 -0.00026
AFIX 43
H31 2 1.371311 1.800185 0.578468 11.00000 -1.20000
AFIX 0
C32 1 1.247186 1.853843 0.505816 11.00000 0.05045 0.02620 =
0.02571 -0.00679 0.00341 -0.00016
AFIX 43
H32 2 1.255478 1.920181 0.527527 11.00000 -1.20000
AFIX 0
C33 1 1.167520 1.828862 0.443888 11.00000 0.02360 0.02486 =
0.02895 0.00213 0.00494 0.00292
C34 1 1.131841 2.034092 0.454960 11.00000 0.06685 0.01609 =
0.05440 -0.00667 0.01833 0.00165
AFIX 137
H34A 2 1.115533 2.023396 0.497569 11.00000 -1.50000
H34B 2 1.086968 2.087601 0.435170 11.00000 -1.50000
H34C 2 1.220385 2.055000 0.461168 11.00000 -1.50000
AFIX 0
C35 1 1.180354 1.718806 0.150024 11.00000 0.04617 0.04143 =
0.05347 -0.00257 0.01618 0.01184
AFIX 137
H35A 2 1.225636 1.693276 0.120284 11.00000 -1.50000
H35B 2 1.097071 1.725926 0.124810 11.00000 -1.50000
H35C 2 1.175274 1.670552 0.182902 11.00000 -1.50000
AFIX 0
C36 1 1.243667 1.891343 0.133265 11.00000 0.05678 0.04688 =
0.04258 0.01468 0.02495 0.02223
AFIX 137
H36A 2 1.292162 1.870591 0.103855 11.00000 -1.50000
H36B 2 1.279244 1.960063 0.154675 11.00000 -1.50000
H36C 2 1.158522 1.891562 0.107828 11.00000 -1.50000
AFIX 0
C37 1 1.370738 1.809481 0.218855 11.00000 0.03511 0.05680 =
0.05475 0.00629 0.01945 0.02323
AFIX 23
H37A 2 1.420249 1.802836 0.186916 11.00000 -1.20000
H37B 2 1.368922 1.746054 0.241233 11.00000 -1.20000
AFIX 0
C38 1 1.432449 1.897650 0.268693 11.00000 0.02817 0.05213 =
0.06100 0.00568 0.01233 0.00402
AFIX 23
H38A 2 1.521088 1.892298 0.284452 11.00000 -1.20000
H38B 2 1.425716 1.961797 0.247290 11.00000 -1.20000
AFIX 0
C39 1 1.419945 1.825213 0.367997 11.00000 0.03649 0.06183 =
0.05882 0.01479 0.00988 0.00847
AFIX 137
H39A 2 1.509842 1.830406 0.378567 11.00000 -1.50000
H39B 2 1.382141 1.757622 0.345386 11.00000 -1.50000
H39C 2 1.394561 1.834816 0.408608 11.00000 -1.50000
AFIX 0
C40 1 1.424310 2.003650 0.363410 11.00000 0.04976 0.05019 =
0.07278 -0.01322 0.00955 -0.00329
AFIX 137
H40A 2 1.514447 2.013792 0.378655 11.00000 -1.50000
H40B 2 1.389760 2.006770 0.401341 11.00000 -1.50000
H40C 2 1.398119 2.057329 0.335491 11.00000 -1.50000

HKLF 4

REM ki385 in P-1
REM R1 = 0.0476 for 4259 Fo > 4sig(Fo) and 0.1302 for all 10697 data
REM 551 parameters refined using 0 restraints

END
;