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_7001124
_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         'C58 H96 B2 Li2 O6 P2 Si2, 2 C4 H8 O'
_chemical_formula_sum            'C66 H112 B2 Li2 O8 P2 Si2'
_chemical_formula_weight         1187.18
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.405(8)
_cell_angle_beta                 108.263(7)
_cell_angle_gamma                99.787(9)
_cell_formula_units_Z            1
_cell_length_a                   10.3298(12)
_cell_length_b                   13.2276(13)
_cell_length_c                   15.0800(15)
_cell_measurement_reflns_used    582
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.75
_cell_volume                     1799.9(4)
_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      180(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         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39378
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.107(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6322
_refine_ls_number_restraints     347
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0681
_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^)+(0.1314P)^2^+0.4330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                4956
_reflns_number_total             6322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b822054a.txt
_cod_data_source_block           ki202_compound5
_cod_original_cell_volume        1799.9(3)
_cod_database_code               7001124