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_4089650
_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         'C12 H38 B2 P2 Si2'
_chemical_formula_sum            'C12 H38 B2 P2 Si2'
_chemical_formula_weight         322.16
_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                93.414(9)
_cell_angle_beta                 90.514(8)
_cell_angle_gamma                117.629(13)
_cell_formula_units_Z            1
_cell_length_a                   6.1097(7)
_cell_length_b                   6.3338(9)
_cell_length_c                   15.3651(14)
_cell_measurement_reflns_used    1444
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      66.5590
_cell_measurement_theta_min      2.8811
_cell_volume                     525.41(12)
_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 0.925
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
  1 omega   89.00  118.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3405   77.0000  150.0000 29

  2 omega   10.00   85.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3405   77.0000  150.0000 75

  3 omega   19.00   87.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3405 -125.0000   60.0000 68

  4 omega   34.00  114.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3405   38.0000  -90.0000 80

  5 omega -132.00 -102.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  147.0000   16.0000 30

  6 omega   21.00   77.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 56

  7 omega   19.00   72.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 53

  8 omega   89.00  173.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -30.0000 84

  9 omega   77.00  115.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  -30.0000 38

 10 omega  135.00  166.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 31

 11 omega   62.00   94.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -124.0000  -31.0000 32

 12 omega   77.00  117.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  -90.0000 40

 13 omega   64.00  110.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 46

 14 omega   31.00   71.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 40

 15 omega   15.00   45.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 30

 16 omega   44.00   70.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 26

 17 omega   23.00   55.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 32

 18 omega  101.00  127.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 26

 19 omega   42.00   74.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -30.0000 32

 20 omega   26.00   67.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 41

 21 omega   75.00  100.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -82.0000    0.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0344549000
_diffrn_orient_matrix_UB_12      -0.0644703000
_diffrn_orient_matrix_UB_13      -0.0991706000
_diffrn_orient_matrix_UB_21      0.0129542000
_diffrn_orient_matrix_UB_22      -0.2328138000
_diffrn_orient_matrix_UB_23      0.0140718000
_diffrn_orient_matrix_UB_31      -0.2824604000
_diffrn_orient_matrix_UB_32      -0.1319193000
_diffrn_orient_matrix_UB_33      0.0085492000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3048
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.663
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74529
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_description       plate
_exptl_crystal_F_000             178
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0455P)^2^+0.2052P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1568
_reflns_number_total             1774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4011142_si_001.cif
_cod_data_source_block           4a_ki505
_cod_database_code               4089650
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C12 H36 B2 Li2 P2 Si2'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.692
_reflns_odcompleteness_completeness 98.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
 C1(H1D,H1E,H1F), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;