#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:05:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178933 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/62/4116231.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4116231
loop_
_publ_author_name
'David R. Armstrong'
'William Clegg'
'Allison M. Drummond'
'Stephen T. Liddle'
'Robert E. Mulvey'
_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 K4 Li4 O8'
_chemical_formula_weight         769.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.166(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.5194(6)
_cell_length_b                   17.1506(10)
_cell_length_c                   13.0058(7)
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.90
_cell_volume                     2412.0(2)
_computing_cell_refinement       'local programs'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω 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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10325
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.7874
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0324
_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/[σ²(Fo²)+(0.0537P)²+0.0508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                3351
_reflns_number_total             4372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002217z_1.cif
_cod_data_source_block           rem218
_cod_database_code               4116231
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.80487(3) 0.36146(2) 0.43194(3) 0.03428(12) Uani 1 1 d . . .
K2 K 0.68029(3) 0.36129(2) 0.11477(3) 0.03899(12) Uani 1 1 d . . .
Li1 Li 0.9845(3) 0.2500 0.3781(3) 0.0318(9) Uani 1 2 d S . .
Li2 Li 0.9068(3) 0.2500 0.1792(3) 0.0320(9) Uani 1 2 d S . .
Li3 Li 0.5434(2) 0.32121(16) 0.2729(2) 0.0313(6) Uani 1 1 d . . .
O1 O 0.61094(13) 0.2500 0.39250(12) 0.0269(3) Uani 1 2 d S . .
C1 C 0.5641(2) 0.2500 0.47963(18) 0.0309(5) Uani 1 2 d S . .
C2 C 0.6073(2) 0.32187(13) 0.55121(16) 0.0548(5) Uani 1 1 d . . .
H2A H 0.6971 0.3193 0.5885 0.082 Uiso 1 1 calc R . .
H2B H 0.5662 0.3239 0.6058 0.082 Uiso 1 1 calc R . .
H2C H 0.5865 0.3688 0.5054 0.082 Uiso 1 1 calc R . .
C3 C 0.4225(2) 0.2500 0.4328(3) 0.0704(10) Uani 1 2 d S . .
H3A H 0.3940 0.2077 0.3793 0.106 Uiso 0.50 1 calc PR . .
H3B H 0.3933 0.3001 0.3969 0.106 Uiso 0.50 1 calc PR . .
H3C H 0.3898 0.2422 0.4923 0.106 Uiso 0.50 1 calc PR . .
O2 O 0.96947(13) 0.2500 0.51351(12) 0.0326(4) Uani 1 2 d S . .
C4 C 1.0564(2) 0.2500 0.61918(18) 0.0315(5) Uani 1 2 d S . .
C5 C 1.04014(18) 0.32249(12) 0.68139(15) 0.0498(5) Uani 1 1 d . . .
H5A H 1.0531 0.3693 0.6436 0.075 Uiso 1 1 calc R . .
H5B H 1.1005 0.3214 0.7560 0.075 Uiso 1 1 calc R . .
H5C H 0.9563 0.3232 0.6845 0.075 Uiso 1 1 calc R . .
C6 C 1.1872(2) 0.2500 0.6145(2) 0.0477(7) Uani 1 2 d S . .
H6A H 1.2470 0.2399 0.6878 0.072 Uiso 0.50 1 calc PR . .
H6B H 1.2045 0.3009 0.5887 0.072 Uiso 0.50 1 calc PR . .
H6C H 1.1939 0.2092 0.5641 0.072 Uiso 0.50 1 calc PR . .
O3 O 0.51308(13) 0.2500 0.15350(12) 0.0297(4) Uani 1 2 d S . .
C7 C 0.3987(2) 0.2500 0.06593(19) 0.0355(6) Uani 1 2 d S . .
C8 C 0.4187(7) 0.2612(15) -0.0428(7) 0.083(7) Uani 0.325(9) 1 d P A -1
H8A H 0.4758 0.2212 -0.0509 0.125 Uiso 0.325(9) 1 calc PR A -1
H8B H 0.4538 0.3130 -0.0447 0.125 Uiso 0.325(9) 1 calc PR A -1
H8C H 0.3394 0.2565 -0.1030 0.125 Uiso 0.325(9) 1 calc PR A -1
C9 C 0.3361(18) 0.1665(10) 0.058(2) 0.081(6) Uani 0.325(9) 1 d P A -1
H9A H 0.3912 0.1267 0.0457 0.121 Uiso 0.325(9) 1 calc PR A -1
H9B H 0.2573 0.1660 -0.0036 0.121 Uiso 0.325(9) 1 calc PR A -1
H9C H 0.3211 0.1553 0.1260 0.121 Uiso 0.325(9) 1 calc PR A -1
C10 C 0.3052(19) 0.2998(14) 0.0803(18) 0.137(15) Uani 0.325(9) 1 d P A -1
H10A H 0.2983 0.2900 0.1523 0.206 Uiso 0.325(9) 1 calc PR A -1
H10B H 0.2256 0.2889 0.0229 0.206 Uiso 0.325(9) 1 calc PR A -1
H10C H 0.3277 0.3544 0.0756 0.206 Uiso 0.325(9) 1 calc PR A -1
C11 C 0.3047(13) 0.2500 0.125(2) 0.138(15) Uani 0.350(17) 2 d SP A 2
H11A H 0.3118 0.2988 0.1664 0.207 Uiso 0.175(9) 1 calc PR A 2
H11B H 0.3213 0.2058 0.1763 0.207 Uiso 0.175(9) 1 calc PR A 2
H11C H 0.2209 0.2454 0.0718 0.207 Uiso 0.175(9) 1 calc PR A 2
C12 C 0.3891(8) 0.1785(5) 0.0004(7) 0.078(7) Uani 0.350(17) 1 d P A 2
H12A H 0.3991 0.1327 0.0477 0.117 Uiso 0.350(17) 1 calc PR A 2
H12B H 0.4540 0.1786 -0.0324 0.117 Uiso 0.350(17) 1 calc PR A 2
H12C H 0.3079 0.1767 -0.0578 0.117 Uiso 0.350(17) 1 calc PR A 2
O4 O 0.79008(14) 0.2500 0.04232(12) 0.0361(4) Uani 1 2 d S . .
C13 C 0.8064(2) 0.2500 -0.05929(19) 0.0426(7) Uani 1 2 d S . .
C14 C 0.7504(3) 0.32273(18) -0.12288(19) 0.0887(9) Uani 1 1 d . . .
H14A H 0.6606 0.3221 -0.1401 0.133 Uiso 1 1 calc R . .
H14B H 0.7687 0.3243 -0.1911 0.133 Uiso 1 1 calc R . .
H14C H 0.7856 0.3689 -0.0787 0.133 Uiso 1 1 calc R . .
C15 C 0.9446(3) 0.2500 -0.0429(3) 0.0719(10) Uani 1 2 d S . .
H15A H 0.9816 0.2007 -0.0092 0.108 Uiso 0.50 1 calc PR . .
H15B H 0.9852 0.2934 0.0049 0.108 Uiso 0.50 1 calc PR . .
H15C H 0.9555 0.2559 -0.1140 0.108 Uiso 0.50 1 calc PR . .
O5 O 0.61011(10) 0.41721(6) 0.27385(9) 0.0340(3) Uani 1 1 d . . .
C16 C 0.56607(15) 0.49229(10) 0.27788(15) 0.0397(4) Uani 1 1 d . . .
C17 C 0.6519(2) 0.53493(13) 0.3800(2) 0.0781(8) Uani 1 1 d . . .
H17A H 0.6547 0.5062 0.4460 0.117 Uiso 1 1 calc R . .
H17B H 0.6204 0.5877 0.3827 0.117 Uiso 1 1 calc R . .
H17C H 0.7354 0.5380 0.3764 0.117 Uiso 1 1 calc R . .
C18 C 0.43669(16) 0.48985(12) 0.28637(17) 0.0476(5) Uani 1 1 d . . .
H18A H 0.3799 0.4628 0.2224 0.071 Uiso 1 1 calc R . .
H18B H 0.4073 0.5432 0.2890 0.071 Uiso 1 1 calc R . .
H18C H 0.4402 0.4620 0.3532 0.071 Uiso 1 1 calc R . .
C19 C 0.5597(3) 0.53742(15) 0.1758(2) 0.0912(10) Uani 1 1 d . . .
H19A H 0.6420 0.5393 0.1696 0.137 Uiso 1 1 calc R . .
H19B H 0.5309 0.5906 0.1807 0.137 Uiso 1 1 calc R . .
H19C H 0.5021 0.5115 0.1112 0.137 Uiso 1 1 calc R . .
O6 O 0.92621(9) 0.33529(6) 0.27820(9) 0.0291(3) Uani 1 1 d . . .
C20 C 1.00458(14) 0.39845(10) 0.27798(14) 0.0344(4) Uani 1 1 d . . .
C21 C 1.0304(2) 0.44769(12) 0.38119(17) 0.0544(5) Uani 1 1 d . . .
H21A H 0.9537 0.4727 0.3806 0.082 Uiso 1 1 calc R . .
H21B H 1.0919 0.4878 0.3834 0.082 Uiso 1 1 calc R . .
H21C H 1.0623 0.4142 0.4459 0.082 Uiso 1 1 calc R . .
C22 C 1.1269(2) 0.36730(14) 0.2737(3) 0.0791(8) Uani 1 1 d . . .
H22A H 1.1667 0.3347 0.3381 0.119 Uiso 1 1 calc R . .
H22B H 1.1813 0.4111 0.2731 0.119 Uiso 1 1 calc R . .
H22C H 1.1114 0.3361 0.2071 0.119 Uiso 1 1 calc R . .
C23 C 0.9445(2) 0.45149(13) 0.17924(18) 0.0636(6) Uani 1 1 d . . .
H23A H 0.9222 0.4206 0.1118 0.095 Uiso 1 1 calc R . .
H23B H 1.0029 0.4925 0.1772 0.095 Uiso 1 1 calc R . .
H23C H 0.8699 0.4753 0.1855 0.095 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 K1 O5 150.73(4) . .
O2 K1 O6 73.11(4) . .
O5 K1 O6 90.07(3) . .
O2 K1 O1 89.80(3) . .
O5 K1 O1 72.56(3) . .
O6 K1 O1 108.21(4) . .
O4 K2 O5 148.75(4) . .
O4 K2 O3 90.85(3) . .
O5 K2 O3 72.55(3) . .
O4 K2 O6 71.72(4) . .
O5 K2 O6 88.14(3) . .
O3 K2 O6 108.07(4) . .
O2 Li1 O6 121.71(13) . 4_565
O2 Li1 O6 121.71(13) . .
O6 Li1 O6 99.42(18) 4_565 .
O4 Li2 O6 122.23(12) . .
O4 Li2 O6 122.23(12) . 4_565
O6 Li2 O6 99.93(18) . 4_565
O5 Li3 O3 122.95(15) . .
O5 Li3 O1 121.30(15) . .
O3 Li3 O1 99.29(13) . .
C1 O1 Li3 119.34(12) . 4_565
C1 O1 Li3 119.34(12) . .
Li3 O1 Li3 79.06(17) 4_565 .
C1 O1 K1 110.38(8) . .
Li3 O1 K1 130.28(10) 4_565 .
Li3 O1 K1 78.02(8) . .
C1 O1 K1 110.38(8) . 4_565
Li3 O1 K1 78.02(8) 4_565 4_565
Li3 O1 K1 130.28(10) . 4_565
K1 O1 K1 84.28(4) . 4_565
O1 C1 C2 110.83(12) . .
O1 C1 C2 110.84(12) . 4_565
C2 C1 C2 108.2(2) . 4_565
O1 C1 C3 109.26(19) . .
C2 C1 C3 108.81(14) . .
C2 C1 C3 108.81(14) 4_565 .
C4 O2 Li1 132.48(18) . .
C4 O2 K1 124.61(7) . 4_565
Li1 O2 K1 84.62(9) . 4_565
C4 O2 K1 124.61(7) . .
Li1 O2 K1 84.62(9) . .
K1 O2 K1 92.63(5) 4_565 .
O2 C4 C6 110.13(19) . .
O2 C4 C5 110.11(13) . .
C6 C4 C5 108.87(14) . .
O2 C4 C5 110.11(13) . 4_565
C6 C4 C5 108.87(14) . 4_565
C5 C4 C5 108.7(2) . 4_565
C7 O3 Li3 120.89(12) . .
C7 O3 Li3 120.89(12) . 4_565
Li3 O3 Li3 79.47(17) . 4_565
C7 O3 K2 110.68(9) . .
Li3 O3 K2 76.83(8) . .
Li3 O3 K2 128.35(10) 4_565 .
C7 O3 K2 110.68(9) . 4_565
Li3 O3 K2 128.35(10) . 4_565
Li3 O3 K2 76.83(8) 4_565 4_565
K2 O3 K2 83.13(4) . 4_565
O3 C7 C10 115.3(7) . 4_565
O3 C7 C10 115.3(7) . .
O3 C7 C12 109.2(3) . .
O3 C7 C12 109.2(3) . 4_565
C12 C7 C12 112.4(9) . 4_565
O3 C7 C8 110.6(3) . 4_565
C10 C7 C8 114.0(11) 4_565 4_565
O3 C7 C8 110.6(3) . .
C10 C7 C8 114.0(11) . .
O3 C7 C11 102.6(8) . .
C12 C7 C11 111.5(6) . .
C12 C7 C11 111.5(6) 4_565 .
O3 C7 C9 109.2(6) . .
C10 C7 C9 101.6(10) . .
C8 C7 C9 105.2(12) . .
O3 C7 C9 109.2(6) . 4_565
C10 C7 C9 101.6(10) 4_565 4_565
C8 C7 C9 105.2(12) 4_565 4_565
C13 O4 Li2 128.92(18) . .
C13 O4 K2 125.14(7) . 4_565
Li2 O4 K2 86.24(9) . 4_565
C13 O4 K2 125.14(7) . .
Li2 O4 K2 86.24(9) . .
K2 O4 K2 92.75(5) 4_565 .
O4 C13 C14 110.23(14) . 4_565
O4 C13 C14 110.23(14) . .
C14 C13 C14 111.1(3) 4_565 .
O4 C13 C15 109.9(2) . .
C14 C13 C15 107.65(16) 4_565 .
C14 C13 C15 107.65(16) . .
C16 O5 Li3 132.90(13) . .
C16 O5 K1 121.86(10) . .
Li3 O5 K1 85.47(9) . .
C16 O5 K2 125.32(10) . .
Li3 O5 K2 84.75(9) . .
K1 O5 K2 94.06(4) . .
O5 C16 C19 110.34(16) . .
O5 C16 C18 110.71(15) . .
C19 C16 C18 108.80(17) . .
O5 C16 C17 109.74(15) . .
C19 C16 C17 109.6(2) . .
C18 C16 C17 107.59(16) . .
C20 O6 Li2 120.84(13) . .
C20 O6 Li1 120.82(13) . .
Li2 O6 Li1 78.76(13) . .
C20 O6 K1 110.51(9) . .
Li2 O6 K1 128.58(11) . .
Li1 O6 K1 77.64(11) . .
C20 O6 K2 109.93(9) . .
Li2 O6 K2 76.62(11) . .
Li1 O6 K2 129.23(11) . .
K1 O6 K2 84.23(3) . .
O6 C20 C21 110.74(14) . .
O6 C20 C22 109.32(15) . .
C21 C20 C22 108.86(17) . .
O6 C20 C23 110.71(14) . .
C21 C20 C23 107.69(16) . .
C22 C20 C23 109.48(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O2 2.6435(11) .
K1 O5 2.6447(12) .
K1 O6 2.8425(11) .
K1 O1 2.8492(11) .
K2 O4 2.6366(11) .
K2 O5 2.6472(12) .
K2 O3 2.8768(11) .
K2 O6 2.9309(11) .
Li1 O2 1.828(4) .
Li1 O6 1.918(3) 4_565
Li1 O6 1.918(3) .
Li2 O4 1.824(4) .
Li2 O6 1.910(3) .
Li2 O6 1.910(3) 4_565
Li3 O5 1.815(3) .
Li3 O3 1.911(3) .
Li3 O1 1.919(3) .
O1 C1 1.413(3) .
O1 Li3 1.919(3) 4_565
O1 K1 2.8492(11) 4_565
C1 C2 1.521(2) .
C1 C2 1.521(2) 4_565
C1 C3 1.531(3) .
O2 C4 1.394(3) .
O2 K1 2.6435(11) 4_565
C4 C6 1.528(3) .
C4 C5 1.530(2) .
C4 C5 1.530(2) 4_565
O3 C7 1.413(3) .
O3 Li3 1.911(3) 4_565
O3 K2 2.8768(11) 4_565
C7 C10 1.437(19) 4_565
C7 C10 1.437(19) .
C7 C12 1.476(7) .
C7 C12 1.476(7) 4_565
C7 C8 1.521(8) 4_565
C7 C8 1.521(8) .
C7 C11 1.53(2) .
C7 C9 1.591(19) .
C7 C9 1.591(19) 4_565
O4 C13 1.398(3) .
O4 K2 2.6366(11) 4_565
C13 C14 1.513(3) 4_565
C13 C14 1.513(3) .
C13 C15 1.531(4) .
O5 C16 1.392(2) .
C16 C19 1.517(3) .
C16 C18 1.533(2) .
C16 C17 1.540(3) .
O6 C20 1.4108(19) .
C20 C21 1.526(3) .
C20 C22 1.526(3) .
C20 C23 1.531(3) .
