#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:05:15 +0100 (mar 22 de mar de 2016) $
#$Revision: 178933 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/62/4116234.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_4116234
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 Cs4 Li4 O8'
_chemical_formula_weight         1144.30
_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                 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       '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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21840
_diffrn_reflns_theta_full        26.00
_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
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_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/[σ²(Fo²)+(0.0287P)²+0.6298P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                4750
_reflns_number_total             6176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002217z_4.cif
_cod_data_source_block           rem282
_cod_original_cell_volume        2516.3(9)
_cod_database_code               4116234
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
Cs1 Cs 0.689263(15) 0.625024(10) 0.090048(14) 0.04375(6) Uani 1 1 d .
Cs2 Cs 0.821931(13) 0.626256(9) 0.442488(13) 0.03908(5) Uani 1 1 d .
Li1 Li 0.9250(5) 0.7500 0.1681(5) 0.0357(13) Uani 1 2 d S
Li2 Li 1.0024(5) 0.7500 0.3703(5) 0.0344(12) Uani 1 2 d S
Li3 Li 0.5513(3) 0.6777(2) 0.2677(3) 0.0324(8) Uani 1 1 d .
O1 O 0.5169(2) 0.7500 0.14731(18) 0.0331(5) Uani 1 2 d S
C1 C 0.4076(3) 0.7500 0.0617(3) 0.0387(8) Uani 1 2 d S
C2 C 0.4246(4) 0.7500 -0.0508(3) 0.0623(12) Uani 1 2 d S
H2A H 0.4864 0.7872 -0.0499 0.093 Uiso 0.50 1 calc PR
H2B H 0.3512 0.7654 -0.1076 0.093 Uiso 0.50 1 calc PR
H2C H 0.4470 0.6974 -0.0668 0.093 Uiso 0.50 1 calc PR
C3 C 0.3386(3) 0.6776(3) 0.0671(3) 0.1025(17) Uani 1 1 d .
H3A H 0.3851 0.6310 0.0652 0.154 Uiso 1 1 calc R
H3B H 0.2657 0.6768 0.0042 0.154 Uiso 1 1 calc R
H3C H 0.3202 0.6780 0.1355 0.154 Uiso 1 1 calc R
O2 O 0.8228(2) 0.7500 0.02752(19) 0.0403(6) Uani 1 2 d S
C4 C 0.8427(4) 0.7500 -0.0731(3) 0.0493(10) Uani 1 2 d S
C5 C 0.7924(4) 0.6775(3) -0.1386(3) 0.0949(14) Uani 1 1 d .
H5A H 0.8256 0.6309 -0.0949 0.142 Uiso 1 1 calc R
H5B H 0.8118 0.6771 -0.2064 0.142 Uiso 1 1 calc R
H5C H 0.7070 0.6773 -0.1569 0.142 Uiso 1 1 calc R
C6 C 0.9753(5) 0.7500 -0.0533(4) 0.094(2) Uani 1 2 d S
H6A H 1.0119 0.7942 -0.0059 0.142 Uiso 0.50 1 calc PR
H6B H 0.9888 0.7548 -0.1237 0.142 Uiso 0.50 1 calc PR
H6C H 1.0097 0.7009 -0.0175 0.142 Uiso 0.50 1 calc PR
O3 O 0.6132(2) 0.7500 0.38833(17) 0.0293(5) Uani 1 2 d S
C7 C 0.5594(3) 0.7500 0.4698(3) 0.0362(7) Uani 1 2 d S
C8 C 0.4272(4) 0.7500 0.4164(4) 0.0784(17) Uani 1 2 d S
H8A H 0.4040 0.7912 0.3604 0.118 Uiso 0.50 1 calc PR
H8B H 0.3906 0.7598 0.4723 0.118 Uiso 0.50 1 calc PR
H8C H 0.4015 0.6990 0.3819 0.118 Uiso 0.50 1 calc PR
C9 C 0.5970(3) 0.67831(18) 0.5446(3) 0.0613(9) Uani 1 1 d .
H9A H 0.5847 0.6308 0.4995 0.092 Uiso 1 1 calc R
H9B H 0.5502 0.6753 0.5934 0.092 Uiso 1 1 calc R
H9C H 0.6802 0.6829 0.5886 0.092 Uiso 1 1 calc R
O4 O 1.0009(2) 0.7500 0.51152(18) 0.0341(5) Uani 1 2 d S
C10 C 1.0890(3) 0.7500 0.6138(3) 0.0351(7) Uani 1 2 d S
C11 C 1.2106(3) 0.7500 0.6007(3) 0.0450(9) Uani 1 2 d S
H11A H 1.2218 0.7009 0.5663 0.068 Uiso 0.50 1 calc PR
H11B H 1.2711 0.7549 0.6732 0.068 Uiso 0.50 1 calc PR
H11C H 1.2163 0.7942 0.5544 0.068 Uiso 0.50 1 calc PR
C12 C 1.0783(3) 0.67714(17) 0.6799(2) 0.0500(7) Uani 1 1 d .
H12A H 1.0015 0.6769 0.6896 0.075 Uiso 1 1 calc R
H12B H 1.1401 0.6782 0.7520 0.075 Uiso 1 1 calc R
H12C H 1.0867 0.6299 0.6401 0.075 Uiso 1 1 calc R
O5 O 0.60340(14) 0.57737(9) 0.26944(14) 0.0352(4) Uani 1 1 d .
C13 C 0.5577(2) 0.50336(14) 0.2765(2) 0.0421(6) Uani 1 1 d .
C14 C 0.5439(4) 0.4566(2) 0.1734(4) 0.1014(17) Uani 1 1 d .
H14A H 0.4927 0.4850 0.1094 0.152 Uiso 1 1 calc R
H14B H 0.5091 0.4055 0.1786 0.152 Uiso 1 1 calc R
H14C H 0.6209 0.4489 0.1655 0.152 Uiso 1 1 calc R
C15 C 0.4374(3) 0.50973(18) 0.2916(3) 0.0602(8) Uani 1 1 d .
H15A H 0.4458 0.5372 0.3605 0.090 Uiso 1 1 calc R
H15B H 0.4060 0.4571 0.2940 0.090 Uiso 1 1 calc R
H15C H 0.3836 0.5390 0.2299 0.090 Uiso 1 1 calc R
C16 C 0.6374(3) 0.45799(18) 0.3747(3) 0.0719(11) Uani 1 1 d .
H16A H 0.7150 0.4522 0.3676 0.108 Uiso 1 1 calc R
H16B H 0.6038 0.4061 0.3772 0.108 Uiso 1 1 calc R
H16C H 0.6446 0.4865 0.4425 0.108 Uiso 1 1 calc R
O6 O 0.95143(14) 0.66331(9) 0.26907(13) 0.0330(3) Uani 1 1 d .
C17 C 1.0306(2) 0.60291(15) 0.2669(2) 0.0389(6) Uani 1 1 d .
C18 C 0.9783(4) 0.5488(2) 0.1698(3) 0.0912(14) Uani 1 1 d .
H18A H 0.9099 0.5220 0.1776 0.137 Uiso 1 1 calc R
H18B H 1.0369 0.5100 0.1673 0.137 Uiso 1 1 calc R
H18C H 0.9542 0.5794 0.1017 0.137 Uiso 1 1 calc R
C19 C 1.1417(3) 0.6382(2) 0.2596(4) 0.0916(15) Uani 1 1 d .
H19A H 1.1236 0.6696 0.1924 0.137 Uiso 1 1 calc R
H19B H 1.1964 0.5963 0.2579 0.137 Uiso 1 1 calc R
H19C H 1.1776 0.6716 0.3237 0.137 Uiso 1 1 calc R
C20 C 1.0620(3) 0.5533(2) 0.3707(3) 0.0697(10) Uani 1 1 d .
H20A H 1.0907 0.5872 0.4354 0.105 Uiso 1 1 calc R
H20B H 1.1233 0.5157 0.3709 0.105 Uiso 1 1 calc R
H20C H 0.9923 0.5250 0.3727 0.105 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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 Cs1 O5 141.58(5) . .
O2 Cs1 O1 92.27(5) . .
O5 Cs1 O1 65.16(5) . .
O2 Cs1 O6 64.05(5) . .
O5 Cs1 O6 90.77(4) . .
O1 Cs1 O6 104.54(5) . .
O4 Cs2 O5 144.48(5) . .
O4 Cs2 O3 92.26(5) . .
O5 Cs2 O3 65.04(5) . .
O4 Cs2 O6 65.56(5) . .
O5 Cs2 O6 92.92(5) . .
O3 Cs2 O6 104.68(5) . .
O2 Li1 O6 125.26(18) . 4_575
O2 Li1 O6 125.26(18) . .
O6 Li1 O6 100.4(3) 4_575 .
O4 Li2 O6 124.48(19) . .
O4 Li2 O6 124.48(19) . 4_575
O6 Li2 O6 99.9(3) . 4_575
O5 Li3 O1 126.6(2) . .
O5 Li3 O3 123.4(2) . .
O1 Li3 O3 99.31(18) . .
C1 O1 Li3 121.77(18) . 4_575
C1 O1 Li3 121.77(18) . .
Li3 O1 Li3 80.2(2) 4_575 .
C1 O1 Cs1 109.14(13) . 4_575
Li3 O1 Cs1 77.21(13) 4_575 4_575
Li3 O1 Cs1 128.87(15) . 4_575
C1 O1 Cs1 109.14(13) . .
Li3 O1 Cs1 128.87(15) 4_575 .
Li3 O1 Cs1 77.21(13) . .
Cs1 O1 Cs1 82.46(6) 4_575 .
O1 C1 C3 110.6(2) . 4_575
O1 C1 C3 110.6(2) . .
C3 C1 C3 110.3(5) 4_575 .
O1 C1 C2 110.7(3) . .
C3 C1 C2 107.2(3) 4_575 .
C3 C1 C2 107.2(3) . .
C4 O2 Li1 130.9(3) . .
C4 O2 Cs1 122.34(12) . .
Li1 O2 Cs1 88.78(14) . .
C4 O2 Cs1 122.34(12) . 4_575
Li1 O2 Cs1 88.78(14) . 4_575
Cs1 O2 Cs1 92.75(7) . 4_575
O2 C4 C5 111.0(2) . .
O2 C4 C5 111.0(2) . 4_575
C5 C4 C5 110.4(4) . 4_575
O2 C4 C6 109.8(3) . .
C5 C4 C6 107.3(3) . .
C5 C4 C6 107.3(3) 4_575 .
C7 O3 Li3 116.71(19) . .
C7 O3 Li3 116.71(19) . 4_575
Li3 O3 Li3 79.5(2) . 4_575
C7 O3 Cs2 111.51(13) . 4_575
Li3 O3 Cs2 131.79(15) . 4_575
Li3 O3 Cs2 79.54(13) 4_575 4_575
C7 O3 Cs2 111.51(13) . .
Li3 O3 Cs2 79.54(13) . .
Li3 O3 Cs2 131.79(15) 4_575 .
Cs2 O3 Cs2 83.09(6) 4_575 .
O3 C7 C8 110.0(3) . .
O3 C7 C9 110.9(2) . 4_575
C8 C7 C9 109.4(2) . 4_575
O3 C7 C9 110.9(2) . .
C8 C7 C9 109.4(2) . .
C9 C7 C9 106.2(3) 4_575 .
C10 O4 Li2 133.3(3) . .
C10 O4 Cs2 122.65(10) . .
Li2 O4 Cs2 87.12(15) . .
C10 O4 Cs2 122.65(10) . 4_575
Li2 O4 Cs2 87.12(15) . 4_575
Cs2 O4 Cs2 91.78(7) . 4_575
O4 C10 C11 110.7(3) . .
O4 C10 C12 110.28(19) . 4_575
C11 C10 C12 108.8(2) . 4_575
O4 C10 C12 110.28(19) . .
C11 C10 C12 108.8(2) . .
C12 C10 C12 108.0(3) 4_575 .
C13 O5 Li3 135.2(2) . .
C13 O5 Cs1 123.54(15) . .
Li3 O5 Cs1 86.69(14) . .
C13 O5 Cs2 118.72(15) . .
Li3 O5 Cs2 87.86(14) . .
Cs1 O5 Cs2 93.11(5) . .
O5 C13 C14 110.5(2) . .
O5 C13 C16 111.2(2) . .
C14 C13 C16 108.5(3) . .
O5 C13 C15 110.9(2) . .
C14 C13 C15 108.5(3) . .
C16 C13 C15 107.1(3) . .
C17 O6 Li1 120.5(2) . .
C17 O6 Li2 120.4(2) . .
Li1 O6 Li2 79.16(19) . .
C17 O6 Cs2 111.34(13) . .
Li1 O6 Cs2 128.05(18) . .
Li2 O6 Cs2 78.39(17) . .
C17 O6 Cs1 109.86(13) . .
Li1 O6 Cs1 77.04(17) . .
Li2 O6 Cs1 129.66(18) . .
Cs2 O6 Cs1 82.51(4) . .
O6 C17 C19 109.6(2) . .
O6 C17 C18 111.3(2) . .
C19 C17 C18 109.1(3) . .
O6 C17 C20 111.1(2) . .
C19 C17 C20 108.2(3) . .
C18 C17 C20 107.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cs1 O2 2.9490(17) .
Cs1 O5 2.9529(17) .
Cs1 O1 3.2389(18) .
Cs1 O6 3.3070(18) .
Cs2 O4 2.9437(17) .
Cs2 O5 2.9554(17) .
Cs2 O3 3.1870(18) .
Cs2 O6 3.1970(17) .
Li1 O2 1.823(6) .
Li1 O6 1.927(4) 4_575
Li1 O6 1.927(4) .
Li2 O4 1.830(6) .
Li2 O6 1.934(4) .
Li2 O6 1.934(4) 4_575
Li3 O5 1.823(4) .
Li3 O1 1.919(4) .
Li3 O3 1.933(4) .
O1 C1 1.412(4) .
O1 Li3 1.919(4) 4_575
O1 Cs1 3.2389(18) 4_575
C1 C3 1.506(4) 4_575
C1 C3 1.506(4) .
C1 C2 1.534(5) .
O2 C4 1.399(4) .
O2 Cs1 2.9490(17) 4_575
C4 C5 1.508(4) .
C4 C5 1.508(4) 4_575
C4 C6 1.539(6) .
O3 C7 1.410(4) .
O3 Li3 1.933(4) 4_575
O3 Cs2 3.1870(18) 4_575
C7 C8 1.516(5) .
C7 C9 1.532(4) 4_575
C7 C9 1.532(4) .
O4 C10 1.393(4) .
O4 Cs2 2.9437(17) 4_575
C10 C11 1.537(5) .
C10 C12 1.538(3) 4_575
C10 C12 1.538(3) .
O5 C13 1.395(3) .
C13 C14 1.514(4) .
C13 C16 1.523(4) .
C13 C15 1.537(4) .
O6 C17 1.415(3) .
C17 C19 1.506(4) .
C17 C18 1.515(4) .
C17 C20 1.523(4) .
