#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:01:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180165 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/61/7106189.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_7106189
loop_
_publ_author_name
'Hui Li'
'Louisa J. Hope-Weeks'
'Clemens Krempner'
_publ_section_title
;
 A supramolecular approach to zwitterionic alkaline metal silanides and
 formation of heterobimetallic silanides
;
_journal_name_full               Chem.Commun.
_journal_page_first              4117
_journal_paper_doi               10.1039/c1cc10148j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C15 H Li O6 Si4'
_chemical_formula_weight         396.46
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 117.9710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.560(2)
_cell_length_b                   9.6993(7)
_cell_length_c                   17.1971(12)
_cell_measurement_temperature    150(2)
_cell_volume                     5091.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21754
_diffrn_reflns_theta_full        23.73
_diffrn_reflns_theta_max         23.73
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.9563
_exptl_absorpt_correction_T_min  0.9115
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.00000(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          3.483
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0329P)²+4.8777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                3238
_reflns_number_total             3859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10148j.txt
_cod_data_source_block           ljhw_krempner_2_0m
_cod_original_cell_volume        5091.3(6)
_cod_database_code               7106189
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
C1 C 0.91974(7) 0.6287(2) 0.97566(15) 0.0416(6) Uani 1 1 d . . .
H1A H 0.9449 0.5722 0.9842 0.062 Uiso 1 1 calc R . .
H1B H 0.9263 0.6766 1.0307 0.062 Uiso 1 1 calc R . .
H1C H 0.9137 0.6967 0.9292 0.062 Uiso 1 1 calc R . .
C2 C 0.82335(7) 0.6362(2) 0.91687(16) 0.0423(6) Uani 1 1 d . . .
H2A H 0.8167 0.6872 0.8628 0.063 Uiso 1 1 calc R . .
H2B H 0.8312 0.7012 0.9656 0.063 Uiso 1 1 calc R . .
H2C H 0.7976 0.5829 0.9085 0.063 Uiso 1 1 calc R . .
C3 C 0.76691(7) 0.2888(2) 0.88228(17) 0.0477(6) Uani 1 1 d . . .
H3A H 0.7681 0.3592 0.8426 0.071 Uiso 1 1 calc R . .
H3B H 0.7580 0.3315 0.9231 0.071 Uiso 1 1 calc R . .
H3C H 0.7456 0.2176 0.8478 0.071 Uiso 1 1 calc R . .
C4 C 0.81370(8) 0.0538(2) 1.00211(16) 0.0449(6) Uani 1 1 d . . .
H4A H 0.7894 -0.0013 0.9588 0.067 Uiso 1 1 calc R . .
H4B H 0.8067 0.0845 1.0484 0.067 Uiso 1 1 calc R . .
H4C H 0.8404 -0.0022 1.0282 0.067 Uiso 1 1 calc R . .
C5 C 0.94261(9) 0.0533(3) 1.08539(19) 0.0623(8) Uani 1 1 d . . .
H5A H 0.9164 0.0002 1.0472 0.093 Uiso 1 1 calc R . .
H5B H 0.9472 0.0501 1.1461 0.093 Uiso 1 1 calc R . .
H5C H 0.9681 0.0138 1.0830 0.093 Uiso 1 1 calc R . .
C6 C 0.98869(7) 0.3253(3) 1.12024(16) 0.0578(7) Uani 1 1 d . . .
H6A H 1.0131 0.2657 1.1277 0.087 Uiso 1 1 calc R . .
H6B H 0.9904 0.3435 1.1778 0.087 Uiso 1 1 calc R . .
H6C H 0.9903 0.4126 1.0933 0.087 Uiso 1 1 calc R . .
C7 C 0.85453(7) 0.5236(2) 0.77129(13) 0.0349(5) Uani 1 1 d . . .
H7A H 0.8815 0.5244 0.7646 0.042 Uiso 1 1 calc R . .
H7B H 0.8472 0.6199 0.7783 0.042 Uiso 1 1 calc R . .
C8 C 0.81768(7) 0.4600(2) 0.69211(14) 0.0351(5) Uani 1 1 d . . .
H8A H 0.7899 0.4691 0.6954 0.042 Uiso 1 1 calc R . .
H8B H 0.8141 0.5066 0.6379 0.042 Uiso 1 1 calc R . .
C9 C 0.80988(7) 0.0407(2) 0.80841(14) 0.0360(5) Uani 1 1 d . . .
H9A H 0.7891 0.0827 0.7515 0.043 Uiso 1 1 calc R . .
H9B H 0.7929 -0.0113 0.8316 0.043 Uiso 1 1 calc R . .
C10 C 0.84042(7) -0.0539(2) 0.79557(15) 0.0386(5) Uani 1 1 d . . .
H10B H 0.8598 -0.1013 0.8515 0.046 Uiso 1 1 calc R . .
H10A H 0.8236 -0.1247 0.7509 0.046 Uiso 1 1 calc R . .
C13 C 0.79588(8) 0.2498(3) 0.61550(14) 0.0478(6) Uani 1 1 d . . .
H13A H 0.7675 0.2558 0.6152 0.072 Uiso 1 1 calc R . .
H13B H 0.8041 0.1527 0.6170 0.072 Uiso 1 1 calc R . .
H13C H 0.7938 0.2934 0.5623 0.072 Uiso 1 1 calc R . .
C14 C 0.89520(8) -0.0580(3) 0.75166(17) 0.0519(7) Uani 1 1 d . . .
H14A H 0.9147 -0.1073 0.8058 0.078 Uiso 1 1 calc R . .
H14B H 0.9127 0.0003 0.7334 0.078 Uiso 1 1 calc R . .
H14C H 0.8785 -0.1248 0.7051 0.078 Uiso 1 1 calc R . .
C15 C 0.92554(8) 0.3142(3) 0.70908(15) 0.0545(7) Uani 1 1 d . . .
H15A H 0.9356 0.4102 0.7204 0.082 Uiso 1 1 calc R . .
H15B H 0.8957 0.3109 0.6602 0.082 Uiso 1 1 calc R . .
H15C H 0.9451 0.2606 0.6938 0.082 Uiso 1 1 calc R . .
C16 C 0.96677(6) 0.1792(2) 0.93146(13) 0.0339(5) Uani 1 1 d . . .
H11A H 0.9616 0.0808 0.9145 0.041 Uiso 1 1 calc R . .
H11B H 0.9950 0.1872 0.9860 0.041 Uiso 1 1 calc R . .
C17 C 0.96821(7) 0.2614(2) 0.85944(14) 0.0383(5) Uani 1 1 d . . .
H12A H 0.9767 0.3578 0.8789 0.046 Uiso 1 1 calc R . .
H12B H 0.9901 0.2217 0.8439 0.046 Uiso 1 1 calc R . .
Li1 Li 0.87488(10) 0.2428(3) 0.8255(2) 0.0280(7) Uani 1 1 d . . .
O1 O 0.86147(4) 0.44382(13) 0.84668(8) 0.0308(3) Uani 1 1 d . . .
O2 O 0.83514(4) 0.14552(13) 0.86921(9) 0.0307(3) Uani 1 1 d . . .
O3 O 0.93209(4) 0.23143(14) 0.94599(8) 0.0299(3) Uani 1 1 d . . .
O4 O 0.82819(4) 0.31845(14) 0.69094(8) 0.0317(3) Uani 1 1 d . . .
O5 O 0.86572(5) 0.02574(14) 0.76726(9) 0.0354(4) Uani 1 1 d . . .
O6 O 0.92604(4) 0.25770(14) 0.78562(9) 0.0328(3) Uani 1 1 d . . .
Si1 Si 0.876363(18) 0.35208(6) 1.04649(4) 0.02855(15) Uani 1 1 d . . .
Si2 Si 0.870598(18) 0.51540(5) 0.94313(4) 0.02636(15) Uani 1 1 d . . .
Si3 Si 0.822482(18) 0.20841(6) 0.94623(4) 0.02762(15) Uani 1 1 d . . .
Si4 Si 0.935238(18) 0.23682(6) 1.04696(4) 0.02958(16) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 '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
_geom_angle_publ_flag
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si3 C3 H3A 109.5 . . ?
Si3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si4 C5 H5A 109.5 . . ?
Si4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si4 C6 H6A 109.5 . . ?
Si4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C7 C8 108.18(17) . . ?
O1 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
O1 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
O4 C8 C7 107.29(16) . . ?
O4 C8 H8A 110.3 . . ?
C7 C8 H8A 110.3 . . ?
O4 C8 H8B 110.3 . . ?
C7 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
O2 C9 C10 108.37(17) . . ?
O2 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
O2 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O5 C10 C9 108.03(17) . . ?
O5 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
O5 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
H10B C10 H10A 108.4 . . ?
O4 C13 H13A 109.5 . . ?
O4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O3 C16 C17 108.28(17) . . ?
O3 C16 H11A 110.0 . . ?
C17 C16 H11A 110.0 . . ?
O3 C16 H11B 110.0 . . ?
C17 C16 H11B 110.0 . . ?
H11A C16 H11B 108.4 . . ?
O6 C17 C16 108.05(16) . . ?
O6 C17 H12A 110.1 . . ?
C16 C17 H12A 110.1 . . ?
O6 C17 H12B 110.1 . . ?
C16 C17 H12B 110.1 . . ?
H12A C17 H12B 108.4 . . ?
O2 Li1 O1 97.09(14) . . ?
O2 Li1 O3 95.52(14) . . ?
O1 Li1 O3 93.49(14) . . ?
O2 Li1 O6 156.32(18) . . ?
O1 Li1 O6 105.87(14) . . ?
O3 Li1 O6 77.63(12) . . ?
O2 Li1 O4 104.19(14) . . ?
O1 Li1 O4 76.17(12) . . ?
O3 Li1 O4 158.64(17) . . ?
O6 Li1 O4 87.16(12) . . ?
O2 Li1 O5 76.19(11) . . ?
O1 Li1 O5 160.82(18) . . ?
O3 Li1 O5 104.94(14) . . ?
O6 Li1 O5 83.65(12) . . ?
O4 Li1 O5 87.95(12) . . ?
C7 O1 Si2 122.93(12) . . ?
C7 O1 Li1 107.80(14) . . ?
Si2 O1 Li1 127.25(11) . . ?
C9 O2 Si3 122.49(12) . . ?
C9 O2 Li1 109.88(14) . . ?
Si3 O2 Li1 125.28(12) . . ?
C16 O3 Si4 122.45(12) . . ?
C16 O3 Li1 109.08(14) . . ?
Si4 O3 Li1 126.31(11) . . ?
C13 O4 C8 111.67(16) . . ?
C13 O4 Li1 131.97(16) . . ?
C8 O4 Li1 111.55(14) . . ?
C10 O5 C14 111.46(16) . . ?
C10 O5 Li1 109.46(14) . . ?
C14 O5 Li1 130.02(15) . . ?
C17 O6 C15 112.45(16) . . ?
C17 O6 Li1 111.44(14) . . ?
C15 O6 Li1 131.21(15) . . ?
Si3 Si1 Si4 96.33(3) . . ?
Si3 Si1 Si2 95.18(3) . . ?
Si4 Si1 Si2 95.27(3) . . ?
O1 Si2 C1 105.09(9) . . ?
O1 Si2 C2 106.20(9) . . ?
C1 Si2 C2 105.60(11) . . ?
O1 Si2 Si1 112.46(5) . . ?
C1 Si2 Si1 115.58(8) . . ?
C2 Si2 Si1 111.20(7) . . ?
O2 Si3 C3 105.09(10) . . ?
O2 Si3 C4 106.00(9) . . ?
C3 Si3 C4 105.33(11) . . ?
O2 Si3 Si1 112.75(5) . . ?
C3 Si3 Si1 115.49(8) . . ?
C4 Si3 Si1 111.42(8) . . ?
O3 Si4 C5 105.41(10) . . ?
O3 Si4 C6 105.78(9) . . ?
C5 Si4 C6 105.54(13) . . ?
O3 Si4 Si1 112.22(5) . . ?
C5 Si4 Si1 115.67(8) . . ?
C6 Si4 Si1 111.48(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Si2 1.875(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 Si2 1.884(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 Si3 1.877(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 Si3 1.881(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 Si4 1.874(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 Si4 1.885(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 O1 1.430(2) . ?
C7 C8 1.493(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O4 1.423(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 O2 1.426(2) . ?
C9 C10 1.491(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O5 1.413(2) . ?
C10 H10B 0.9900 . ?
C10 H10A 0.9900 . ?
C13 O4 1.419(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 O5 1.424(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O6 1.419(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 O3 1.427(2) . ?
C16 C17 1.493(3) . ?
C16 H11A 0.9900 . ?
C16 H11B 0.9900 . ?
C17 O6 1.415(2) . ?
C17 H12A 0.9900 . ?
C17 H12B 0.9900 . ?
Li1 O2 2.076(3) . ?
Li1 O1 2.076(3) . ?
Li1 O3 2.091(3) . ?
Li1 O6 2.181(3) . ?
Li1 O4 2.235(3) . ?
Li1 O5 2.289(3) . ?
O1 Si2 1.6858(14) . ?
O2 Si3 1.6916(14) . ?
O3 Si4 1.6888(14) . ?
Si1 Si3 2.3175(8) . ?
Si1 Si4 2.3184(8) . ?
Si1 Si2 2.3186(8) . ?
