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_4066416
_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         'C14 H30 B P Si2'
_chemical_formula_sum            'C14 H30 B P Si2'
_chemical_formula_weight         296.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.447(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.792(3)
_cell_length_b                   10.686(3)
_cell_length_c                   13.1277(15)
_cell_measurement_reflns_used    95
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     1933.0(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27151
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0390P)^2^+0.7445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                3332
_reflns_number_total             4411
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100454t_si_001.cif
_cod_data_source_block           ki305_compound_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4066416