Synthesis, Structure, and Solution Behavior of a Phosphine−Borane-Stabilized 1,3-Dicarbanion†
Izod, Keith; Wills, Corinne; Clegg, William; Harrington, Ross W.; Organometallics 29 (2010) 4774–; doi:10.1021/om100454t

data_4066417
_publ_section_title
;
 Synthesis, Structure, and Solution Behavior of a
 Phosphine&#x2212;Borane-Stabilized 1,3-Dicarbanion&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4774
_journal_paper_doi               10.1021/om100454t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C34 H68 B Li2 O5 P Si2'
_chemical_formula_sum            'C34 H68 B Li2 O5 P Si2'
_chemical_formula_weight         668.72
_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                86.085(13)
_cell_angle_beta                 82.76(2)
_cell_angle_gamma                75.133(12)
_cell_formula_units_Z            2
_cell_length_a                   10.193(4)
_cell_length_b                   11.3220(14)
_cell_length_c                   19.021(4)
_cell_measurement_reflns_used    185
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.50
_cell_volume                     2103.2(10)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_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_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32091
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         9453
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1.1466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                7164
_reflns_number_total             9453
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100454t_si_001.cif
_cod_data_source_block           ki306_compound_3
_cod_original_cell_volume        2103.2(9)
_cod_database_code               4066417