A triclinic polymorph of octa-<i>tert</i>-butoxytetralithiumtetrasodium
Clegg, William; Drummond, Allison M.; Liddle, Stephen T.; Mulvey, Robert E.; Acta Crystallographica Section E 59 (2003) m64–m66; doi:10.1107/S1600536803001193

data_2201791
_publ_section_title
;
 A triclinic polymorph of
 octa-<i>tert</i>-butoxytetralithiumtetrasodium
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m64
_journal_page_last               m66
_journal_paper_doi               10.1107/S1600536803001193
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Li4 Na4 (C4 H9 O)8]'
_chemical_formula_moiety         'C32 H72 Li4 Na4 O8'
_chemical_formula_sum            'C32 H72 Li4 Na4 O8'
_chemical_formula_weight         704.62
_chemical_name_systematic
;
tetra-\m~3~-tert-butoxy-tetra-\m~4~-tert-butoxy-tetralithiumtetrasodium
;
_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                82.560(2)
_cell_angle_beta                 89.492(2)
_cell_angle_gamma                82.033(2)
_cell_formula_units_Z            6
_cell_length_a                   11.1917(8)
_cell_length_b                   21.0007(14)
_cell_length_c                   29.450(2)
_cell_measurement_reflns_used    28018
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.3
_cell_volume                     6796.9(8)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       'fine-slice \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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32571
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.80
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.198
_refine_ls_extinction_coef       0.00064(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1370
_refine_ls_number_reflns         22410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0515P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                15221
_reflns_number_total             22410
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6229.cif
_cod_data_source_block           I
_cod_original_cell_volume        6796.8(8)
_cod_database_code               2201791
_cod_database_fobs_code          2201791