Synthesis and structural characterisation of alkali metal complexes of heteroatom-stabilised 1,4- and 1,6-dicarbanions
Izod, Keith; Bowman, Lyndsey J.; Wills, Corinne; Clegg, William; Harrington, Ross W.; Dalton Transactions  (2009) 3340–3347; doi:10.1039/b822054a

data_7001125
_publ_section_title
;
 Synthesis and structural characterisation of alkali metal complexes of
 heteroatom-stabilised 1,4- and 1,6-dicarbanions
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              3340
_journal_page_last               3347
_journal_paper_doi               10.1039/b822054a
_journal_year                    2009
_chemical_formula_moiety         'C18 H54 B2 P2 Si4'
_chemical_formula_sum            'C18 H54 B2 P2 Si4'
_chemical_formula_weight         466.53
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.709(2)
_cell_angle_beta                 86.352(2)
_cell_angle_gamma                77.554(2)
_cell_formula_units_Z            1
_cell_length_a                   6.6106(1)
_cell_length_b                   8.7160(2)
_cell_length_c                   13.3995(4)
_cell_measurement_reflns_used    4476
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.4671
_cell_measurement_theta_min      3.0244
_cell_volume                     745.61(3)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.833
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6863
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Scalepack/CrysAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             258
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                2720
_reflns_number_total             3477
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b822054a.txt
_cod_data_source_block           ki338_compound6
_cod_database_code               7001125