#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:05:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178933 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/62/4116233.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_4116233
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 Li4 O8 Rb4'
_chemical_formula_weight         954.54
_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                90.000(2)
_cell_angle_beta                 110.347(19)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            2
_cell_length_a                   11.705(3)
_cell_length_b                   17.070(5)
_cell_length_c                   12.957(5)
_cell_measurement_reflns_used    4907
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.39
_cell_volume                     2427.3(14)
_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 0.986
_diffrn_measured_fraction_theta_max 0.903
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11978
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.044
_exptl_absorpt_correction_T_max  0.1358
_exptl_absorpt_correction_T_min  0.0500
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.80
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0517P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                3022
_reflns_number_total             5679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002217z_3.cif
_cod_data_source_block           rem250
_cod_original_cell_volume        2427.4(14)
_cod_database_code               4116233
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
Rb1 Rb 0.67773(4) 0.36776(3) 0.09898(3) 0.03854(14) Uani 1 1 d .
Rb2 Rb 0.80997(3) 0.36834(3) 0.43628(3) 0.03528(14) Uani 1 1 d .
Li1 Li 0.9129(9) 0.2500 0.1737(8) 0.035(2) Uani 1 2 d S
Li2 Li 0.9876(9) 0.2500 0.3743(8) 0.033(2) Uani 1 2 d S
Li3 Li 0.5419(6) 0.3218(5) 0.2665(5) 0.0340(17) Uani 1 1 d .
O1 O 0.5096(3) 0.2500 0.1477(3) 0.0286(9) Uani 1 2 d S
C1 C 0.3960(5) 0.2500 0.0614(5) 0.0350(15) Uani 1 2 d S
C2 C 0.3263(5) 0.3214(4) 0.0658(5) 0.118(3) Uani 1 1 d .
H2A H 0.3154 0.3243 0.1374 0.177 Uiso 1 1 calc R
H2B H 0.2464 0.3194 0.0071 0.177 Uiso 1 1 calc R
H2C H 0.3709 0.3677 0.0559 0.177 Uiso 1 1 calc R
C3 C 0.4151(7) 0.2500 -0.0480(6) 0.079(3) Uani 1 2 d S
H3A H 0.3370 0.2409 -0.1072 0.118 Uiso 0.50 1 calc PR
H3B H 0.4725 0.2083 -0.0486 0.118 Uiso 0.50 1 calc PR
H3C H 0.4481 0.3008 -0.0591 0.118 Uiso 0.50 1 calc PR
O2 O 0.8029(3) 0.2500 0.0347(3) 0.0358(10) Uani 1 2 d S
C4 C 0.8204(5) 0.2500 -0.0662(5) 0.0395(16) Uani 1 2 d S
C5 C 0.7682(7) 0.3241(4) -0.1303(4) 0.099(3) Uani 1 1 d .
H5A H 0.6795 0.3245 -0.1496 0.149 Uiso 1 1 calc R
H5B H 0.7882 0.3255 -0.1978 0.149 Uiso 1 1 calc R
H5C H 0.8034 0.3701 -0.0851 0.149 Uiso 1 1 calc R
C6 C 0.9556(7) 0.2500 -0.0480(6) 0.081(3) Uani 1 2 d S
H6A H 0.9958 0.2918 0.0037 0.121 Uiso 0.50 1 calc PR
H6B H 0.9675 0.2588 -0.1183 0.121 Uiso 0.50 1 calc PR
H6C H 0.9909 0.1993 -0.0175 0.121 Uiso 0.50 1 calc PR
O3 O 0.6087(3) 0.2500 0.3879(3) 0.0275(9) Uani 1 2 d S
C7 C 0.5584(5) 0.2500 0.4720(5) 0.0314(14) Uani 1 2 d S
C8 C 0.4208(6) 0.2500 0.4207(6) 0.073(3) Uani 1 2 d S
H8A H 0.3945 0.2937 0.3688 0.109 Uiso 0.50 1 calc PR
H8B H 0.3853 0.2558 0.4786 0.109 Uiso 0.50 1 calc PR
H8C H 0.3934 0.2005 0.3816 0.109 Uiso 0.50 1 calc PR
C9 C 0.5999(5) 0.3216(3) 0.5457(4) 0.0556(14) Uani 1 1 d .
H9A H 0.6884 0.3195 0.5832 0.083 Uiso 1 1 calc R
H9B H 0.5595 0.3223 0.6004 0.083 Uiso 1 1 calc R
H9C H 0.5786 0.3692 0.5007 0.083 Uiso 1 1 calc R
O4 O 0.9810(3) 0.2500 0.5123(3) 0.0325(10) Uani 1 2 d S
C10 C 1.0689(5) 0.2500 0.6178(5) 0.0329(15) Uani 1 2 d S
C11 C 1.0553(4) 0.3231(3) 0.6803(4) 0.0467(12) Uani 1 1 d .
H11A H 1.0644 0.3699 0.6400 0.070 Uiso 1 1 calc R
H11B H 1.1181 0.3231 0.7537 0.070 Uiso 1 1 calc R
H11C H 0.9745 0.3233 0.6872 0.070 Uiso 1 1 calc R
C12 C 1.1962(5) 0.2500 0.6085(5) 0.0423(17) Uani 1 2 d S
H12A H 1.1948 0.2185 0.5448 0.063 Uiso 0.50 1 calc PR
H12B H 1.2551 0.2276 0.6756 0.063 Uiso 0.50 1 calc PR
H12C H 1.2199 0.3039 0.5992 0.063 Uiso 0.50 1 calc PR
O5 O 0.6020(2) 0.42019(16) 0.2685(2) 0.0304(7) Uani 1 1 d .
C13 C 0.5594(4) 0.4948(3) 0.2738(4) 0.0359(11) Uani 1 1 d .
C14 C 0.5458(6) 0.5400(3) 0.1701(5) 0.085(2) Uani 1 1 d .
H14A H 0.6252 0.5440 0.1608 0.127 Uiso 1 1 calc R
H14B H 0.5150 0.5926 0.1754 0.127 Uiso 1 1 calc R
H14C H 0.4883 0.5127 0.1067 0.127 Uiso 1 1 calc R
C15 C 0.4347(4) 0.4920(3) 0.2877(4) 0.0454(12) Uani 1 1 d .
H15A H 0.3781 0.4611 0.2279 0.068 Uiso 1 1 calc R
H15B H 0.4031 0.5453 0.2856 0.068 Uiso 1 1 calc R
H15C H 0.4432 0.4677 0.3585 0.068 Uiso 1 1 calc R
C16 C 0.6452(4) 0.5395(3) 0.3710(5) 0.0683(17) Uani 1 1 d .
H16A H 0.6541 0.5112 0.4392 0.103 Uiso 1 1 calc R
H16B H 0.6119 0.5918 0.3739 0.103 Uiso 1 1 calc R
H16C H 0.7250 0.5444 0.3627 0.103 Uiso 1 1 calc R
O6 O 0.9339(2) 0.33669(16) 0.2742(2) 0.0287(6) Uani 1 1 d .
C17 C 1.0131(4) 0.3986(3) 0.2734(3) 0.0339(10) Uani 1 1 d .
C18 C 0.9535(5) 0.4538(3) 0.1767(4) 0.0710(18) Uani 1 1 d .
H18A H 0.9334 0.4246 0.1075 0.106 Uiso 1 1 calc R
H18B H 1.0101 0.4963 0.1776 0.106 Uiso 1 1 calc R
H18C H 0.8789 0.4758 0.1830 0.106 Uiso 1 1 calc R
C19 C 1.0444(5) 0.4467(3) 0.3775(4) 0.0572(15) Uani 1 1 d .
H19A H 0.9712 0.4736 0.3794 0.086 Uiso 1 1 calc R
H19B H 1.1067 0.4855 0.3790 0.086 Uiso 1 1 calc R
H19C H 1.0757 0.4122 0.4417 0.086 Uiso 1 1 calc R
C20 C 1.1282(5) 0.3653(3) 0.2645(6) 0.081(2) Uani 1 1 d .
H20A H 1.1705 0.3343 0.3304 0.122 Uiso 1 1 calc R
H20B H 1.1811 0.4082 0.2582 0.122 Uiso 1 1 calc R
H20C H 1.1080 0.3318 0.1992 0.122 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'
Rb Rb -0.9393 2.9676 '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 Rb1 O5 144.44(9) . .
O2 Rb1 O1 91.78(7) . .
O5 Rb1 O1 68.96(8) . .
O2 Rb1 O6 67.72(9) . .
O5 Rb1 O6 88.25(8) . .
O1 Rb1 O6 105.42(8) . .
O4 Rb2 O5 146.72(9) . .
O4 Rb2 O6 69.55(9) . .
O5 Rb2 O6 90.86(8) . .
O4 Rb2 O3 90.07(8) . .
O5 Rb2 O3 68.96(8) . .
O6 Rb2 O3 105.62(8) . .
O2 Li1 O6 123.4(3) . .
O2 Li1 O6 123.4(3) . 4_565
O6 Li1 O6 100.2(5) . 4_565
O4 Li2 O6 123.2(3) . 4_565
O4 Li2 O6 123.2(3) . .
O6 Li2 O6 100.6(5) 4_565 .
O5 Li3 O1 125.1(4) . .
O5 Li3 O3 122.0(4) . .
O1 Li3 O3 99.2(4) . .
C1 O1 Li3 120.7(3) . .
C1 O1 Li3 120.7(3) . 4_565
Li3 O1 Li3 80.4(4) . 4_565
C1 O1 Rb1 109.7(2) . .
Li3 O1 Rb1 77.3(2) . .
Li3 O1 Rb1 129.5(3) 4_565 .
C1 O1 Rb1 109.7(2) . 4_565
Li3 O1 Rb1 129.5(3) . 4_565
Li3 O1 Rb1 77.3(2) 4_565 4_565
Rb1 O1 Rb1 83.13(9) . 4_565
O1 C1 C2 110.5(3) . 4_565
O1 C1 C2 110.5(3) . .
C2 C1 C2 111.0(8) 4_565 .
O1 C1 C3 109.8(5) . .
C2 C1 C3 107.5(4) 4_565 .
C2 C1 C3 107.5(4) . .
C4 O2 Li1 130.3(5) . .
C4 O2 Rb1 123.11(17) . 4_565
Li1 O2 Rb1 88.2(2) . 4_565
C4 O2 Rb1 123.11(17) . .
Li1 O2 Rb1 88.2(2) . .
Rb1 O2 Rb1 92.61(11) 4_565 .
O2 C4 C6 109.9(5) . .
O2 C4 C5 110.6(3) . 4_565
C6 C4 C5 106.5(4) . 4_565
O2 C4 C5 110.6(3) . .
C6 C4 C5 106.5(4) . .
C5 C4 C5 112.6(7) 4_565 .
C7 O3 Li3 118.1(3) . 4_565
C7 O3 Li3 118.1(3) . .
Li3 O3 Li3 78.8(5) 4_565 .
C7 O3 Rb2 110.3(2) . .
Li3 O3 Rb2 131.6(2) 4_565 .
Li3 O3 Rb2 79.0(2) . .
C7 O3 Rb2 110.3(2) . 4_565
Li3 O3 Rb2 79.0(2) 4_565 4_565
Li3 O3 Rb2 131.6(2) . 4_565
Rb2 O3 Rb2 84.66(10) . 4_565
O3 C7 C8 109.1(5) . .
O3 C7 C9 110.9(3) . .
C8 C7 C9 109.5(3) . .
O3 C7 C9 110.9(3) . 4_565
C8 C7 C9 109.5(3) . 4_565
C9 C7 C9 106.8(6) . 4_565
C10 O4 Li2 134.1(5) . .
C10 O4 Rb2 122.86(17) . 4_565
Li2 O4 Rb2 85.6(2) . 4_565
C10 O4 Rb2 122.86(17) . .
Li2 O4 Rb2 85.6(2) . .
Rb2 O4 Rb2 93.54(11) 4_565 .
O4 C10 C11 110.0(3) . .
O4 C10 C11 110.0(3) . 4_565
C11 C10 C11 109.8(5) . 4_565
O4 C10 C12 109.1(5) . .
C11 C10 C12 109.0(3) . .
C11 C10 C12 109.0(3) 4_565 .
C13 O5 Li3 135.2(3) . .
C13 O5 Rb2 119.2(2) . .
Li3 O5 Rb2 87.0(2) . .
C13 O5 Rb1 123.8(2) . .
Li3 O5 Rb1 85.4(2) . .
Rb2 O5 Rb1 94.71(8) . .
O5 C13 C14 110.8(4) . .
O5 C13 C16 111.1(4) . .
C14 C13 C16 108.5(5) . .
O5 C13 C15 110.7(3) . .
C14 C13 C15 108.1(4) . .
C16 C13 C15 107.5(4) . .
C17 O6 Li2 121.4(4) . .
C17 O6 Li1 120.1(4) . .
Li2 O6 Li1 78.5(3) . .
C17 O6 Rb2 110.5(2) . .
Li2 O6 Rb2 77.8(3) . .
Li1 O6 Rb2 129.3(3) . .
C17 O6 Rb1 109.7(2) . .
Li2 O6 Rb1 128.9(3) . .
Li1 O6 Rb1 77.0(3) . .
Rb2 O6 Rb1 84.36(7) . .
O6 C17 C20 109.1(4) . .
O6 C17 C19 111.0(3) . .
C20 C17 C19 109.2(4) . .
O6 C17 C18 110.8(3) . .
C20 C17 C18 109.6(4) . .
C19 C17 C18 107.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb1 O2 2.780(3) .
Rb1 O5 2.787(3) .
Rb1 O1 3.030(3) .
Rb1 O6 3.113(3) .
Rb2 O4 2.773(3) .
Rb2 O5 2.784(3) .
Rb2 O6 2.988(3) .
Rb2 O3 3.000(3) .
Li1 O2 1.814(11) .
Li1 O6 1.929(7) .
Li1 O6 1.929(7) 4_565
Li2 O4 1.816(11) .
Li2 O6 1.923(7) 4_565
Li2 O6 1.923(7) .
Li3 O5 1.817(8) .
Li3 O1 1.900(8) .
Li3 O3 1.932(7) .
O1 C1 1.408(6) .
O1 Li3 1.900(8) 4_565
O1 Rb1 3.030(3) 4_565
C1 C2 1.478(6) 4_565
C1 C2 1.478(6) .
C1 C3 1.510(9) .
O2 C4 1.392(7) .
O2 Rb1 2.780(3) 4_565
C4 C6 1.517(9) .
C4 C5 1.520(6) 4_565
C4 C5 1.520(6) .
O3 C7 1.408(6) .
O3 Li3 1.932(7) 4_565
O3 Rb2 3.000(3) 4_565
C7 C8 1.514(8) .
C7 C9 1.523(6) .
C7 C9 1.523(6) 4_565
O4 C10 1.397(6) .
O4 Rb2 2.773(3) 4_565
C10 C11 1.525(5) .
C10 C11 1.525(5) 4_565
C10 C12 1.537(8) .
O5 C13 1.378(5) .
C13 C14 1.509(6) .
C13 C16 1.515(6) .
C13 C15 1.532(5) .
O6 C17 1.408(5) .
C17 C20 1.503(6) .
C17 C19 1.511(6) .
C17 C18 1.528(6) .
