Synthesis and Structural Characterization of Phosphine‒Borane-Stabilized Dicarbanions with either Rigid or Flexible Spacers
Izod, Keith; Dixon, Casey M.; McMeekin, Emma; Rodgers, Lee; Harrington, Ross W.; Baisch, Ulrich; Organometallics 33 (2013) 378–; doi:10.1021/om4011142

data_4089651
_publ_section_title
;
 Synthesis and Structural Characterization of Phosphine--Borane-Stabilized
 Dicarbanions with either Rigid or Flexible Spacers
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              378
_journal_paper_doi               10.1021/om4011142
_journal_volume                  33
_journal_year                    2013
_chemical_formula_moiety         'C48 H76 B2 Li2 O4 P2 Si2'
_chemical_formula_sum            'C48 H76 B2 Li2 O4 P2 Si2'
_chemical_formula_weight         870.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                94.780(5)
_cell_angle_beta                 104.055(5)
_cell_angle_gamma                112.142(5)
_cell_formula_units_Z            1
_cell_length_a                   10.3857(6)
_cell_length_b                   10.5580(6)
_cell_length_c                   13.2588(8)
_cell_measurement_reflns_used    3496
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      28.5214
_cell_measurement_theta_min      2.9011
_cell_volume                     1281.35(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -21.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.1902   77.0000    0.0000 78

  2 omega   22.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9090 -116.0000   75.0000 36

  3 omega  -16.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9090   38.0000 -150.0000 92

  4 omega  -14.00   82.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9090   77.0000  -90.0000 96

  5 omega  -54.00  -28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9090  -38.0000  -90.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0215008000
_diffrn_orient_matrix_UB_12      -0.0685966000
_diffrn_orient_matrix_UB_13      -0.0276848000
_diffrn_orient_matrix_UB_21      0.0010094000
_diffrn_orient_matrix_UB_22      -0.0248244000
_diffrn_orient_matrix_UB_23      0.0481518000
_diffrn_orient_matrix_UB_31      -0.0741605000
_diffrn_orient_matrix_UB_32      -0.0120816000
_diffrn_orient_matrix_UB_33      -0.0087123000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9981
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.907
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+1.0284P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3627
_reflns_number_total             4504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4011142_si_001.cif
_cod_data_source_block           5b_ki503
_cod_original_cell_volume        1281.35(14)
_cod_database_code               4089651
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C32 H50 Li2 B2 P2 Si2'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H17A,H17B} of C17, {H18A,H18B} of C18, {H19A,H19B} of C19,
   {H20A,H20B} of C20, {H21A,H21B} of C21, {H22A,H22B} of C22, {H23A,H23B} of
  C23, {H24A,H24B} of C24
 At 1.5 times of:
  All C(H,H,H) groups, {H2AA,H2AB} of C2A, {H2A,H2B} of C2
2. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16)
3.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;