Bis(12-crown-4)lithium(I) bis[(<i>N</i>,<i>N</i>-diisopropylamino)borohydride(1‒)]lithium(I)
Dornhaus, Franz; Bolte, Michael; Acta Crystallographica Section E 63 (2007) m41–m42; doi:10.1107/S1600536806051142

data_2211824
_publ_section_title
;
 Bis(12-crown-4)lithium(I)
 bis[(<i>N</i>,<i>N</i>-diisopropylamino)borohydride(1--)]lithium(I)
;
_journal_coeditor_code           HB2217
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m41
_journal_page_last               m42
_journal_paper_doi               10.1107/S1600536806051142
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Li (C8 H16 O4)2] [Li (C6 H17 B N)2]'
_chemical_formula_moiety         'C16 H32 Li1 O8 +, C12 H34 B2 Li1 N2 -'
_chemical_formula_sum            'C28 H66 B2 Li2 N2 O8'
_chemical_formula_weight         594.33
_chemical_name_systematic
;Bis(12-crown-4)lithium(I)
 bis[(N,N-diisopropylamino)borohydride(1-)]lithium(I)
;
_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                116.790(7)
_cell_angle_beta                 105.314(8)
_cell_angle_gamma                94.850(9)
_cell_formula_units_Z            2
_cell_length_a                   10.2918(12)
_cell_length_b                   14.5424(14)
_cell_length_c                   14.8057(13)
_cell_measurement_reflns_used    9247
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      3.6
_cell_volume                     1853.7(4)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Stoe IPDS-II two-circle'
_diffrn_measurement_method       \w
_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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.1814
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23964
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         3.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.324
_refine_ls_extinction_coef       0.0110(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                3312
_reflns_number_total             7468
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2217.cif
_cod_data_source_block           I
_cod_database_code               2211824
_cod_database_fobs_code          2211824