A Remarkable Isostructural Homologous Series of Mixed Lithium-Heavier Alkali Metaltert-Butoxides [(t-BuO)8Li4M4] (M = Na, K, Rb or Cs)
David R. Armstrong; William Clegg; Allison M. Drummond; Stephen T. Liddle; Robert E. Mulvey; Journal of the American Chemical Society 122 (2000) 11117–11124; doi:10.1021/ja002217z

data_4116234
_publ_section_title
;
 A Remarkable Isostructural Homologous Series of Mixed Lithium-Heavier
 Alkali Metaltert-Butoxides [(t-BuO)8Li4M4] (M = Na, K, Rb or Cs)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11117
_journal_page_last               11124
_journal_paper_doi               10.1021/ja002217z
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C32 H72 Cs4 Li4 O8'
_chemical_formula_weight         1144.30
_chemical_name_systematic
;
 ?
;
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_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 109.541(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.106(3)
_cell_length_b                   17.080(4)
_cell_length_c                   12.9130(17)
_cell_measurement_reflns_used    7886
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.39
_cell_volume                     2516.2(9)
_computing_cell_refinement       'Siemens saint'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0204
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21840
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_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.909
_exptl_absorpt_correction_T_max  0.1071
_exptl_absorpt_correction_T_min  0.0551
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.68
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_refine_diff_density_max         0.880
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6176
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_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.6298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                4750
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002217z_4.cif
_cod_data_source_block           rem282
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_cod_database_code               4116234