#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:01:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180165 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/61/7106190.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_7106190
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 Na O6 Si4'
_chemical_formula_weight         412.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6614(18)
_cell_length_b                   9.8943(12)
_cell_length_c                   17.206(2)
_cell_measurement_temperature    150(2)
_cell_volume                     2666.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.782
_diffrn_measured_fraction_theta_max 0.782
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18024
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.8855
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.00000(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.815
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.815
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.810
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0082P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0666
_reflns_number_gt                2398
_reflns_number_total             3658
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10148j.txt
_cod_data_source_block           krempner1a
_cod_database_code               7106190
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Na1 Na 0.75015(6) 0.49825(9) 0.30163(5) 0.0287(2) Uani 1 1 d . . .
Si1 Si 0.74558(4) 0.61453(7) 0.07902(4) 0.03410(19) Uani 1 1 d . . .
Si2 Si 0.72917(4) 0.77796(7) 0.17466(4) 0.03152(18) Uani 1 1 d . . .
Si3 Si 0.86781(5) 0.51364(8) 0.12809(4) 0.03474(19) Uani 1 1 d . . .
Si4 Si 0.64364(4) 0.46235(7) 0.12245(4) 0.03070(17) Uani 1 1 d . . .
O1 O 0.70840(11) 0.71221(15) 0.26233(9) 0.0362(4) Uani 1 1 d . . .
O2 O 0.87293(10) 0.51844(18) 0.22612(9) 0.0405(5) Uani 1 1 d . . .
O3 O 0.66931(10) 0.38909(15) 0.20764(9) 0.0329(4) Uani 1 1 d . . .
O4 O 0.65439(10) 0.58914(16) 0.39533(9) 0.0358(4) Uani 1 1 d . . .
O5 O 0.86950(12) 0.5101(2) 0.38601(9) 0.0493(5) Uani 1 1 d . . .
O6 O 0.72454(11) 0.27229(16) 0.34466(10) 0.0406(4) Uani 1 1 d . . .
C1 C 0.82586(17) 0.8885(3) 0.18790(16) 0.0474(7) Uani 1 1 d . . .
H1A H 0.8148 0.9548 0.2290 0.071 Uiso 1 1 calc R . .
H1B H 0.8382 0.9359 0.1392 0.071 Uiso 1 1 calc R . .
H1C H 0.8749 0.8325 0.2024 0.071 Uiso 1 1 calc R . .
C2 C 0.63787(18) 0.8956(3) 0.15360(17) 0.0504(8) Uani 1 1 d . . .
H2A H 0.5882 0.8431 0.1365 0.076 Uiso 1 1 calc R . .
H2B H 0.6545 0.9590 0.1126 0.076 Uiso 1 1 calc R . .
H2C H 0.6232 0.9460 0.2008 0.076 Uiso 1 1 calc R . .
C3 C 0.96704(17) 0.6026(3) 0.09306(16) 0.0540(8) Uani 1 1 d . . .
H3A H 0.9698 0.6931 0.1161 0.081 Uiso 1 1 calc R . .
H3B H 0.9654 0.6102 0.0363 0.081 Uiso 1 1 calc R . .
H3C H 1.0175 0.5507 0.1086 0.081 Uiso 1 1 calc R . .
C4 C 0.88045(18) 0.3307(3) 0.10092(17) 0.0533(8) Uani 1 1 d . . .
H4A H 0.9325 0.2947 0.1247 0.080 Uiso 1 1 calc R . .
H4B H 0.8844 0.3225 0.0443 0.080 Uiso 1 1 calc R . .
H4C H 0.8310 0.2795 0.1196 0.080 Uiso 1 1 calc R . .
C5 C 0.53539(16) 0.5385(3) 0.13688(18) 0.0498(8) Uani 1 1 d . . .
H5A H 0.4947 0.4673 0.1510 0.075 Uiso 1 1 calc R . .
H5B H 0.5169 0.5821 0.0886 0.075 Uiso 1 1 calc R . .
H5C H 0.5380 0.6058 0.1786 0.075 Uiso 1 1 calc R . .
C6 C 0.62788(18) 0.3180(3) 0.05275(16) 0.0508(8) Uani 1 1 d . . .
H6A H 0.6814 0.2675 0.0475 0.076 Uiso 1 1 calc R . .
H6B H 0.6108 0.3534 0.0019 0.076 Uiso 1 1 calc R . .
H6C H 0.5832 0.2578 0.0726 0.076 Uiso 1 1 calc R . .
C7 C 0.69613(18) 0.7887(2) 0.33143(14) 0.0416(7) Uani 1 1 d . . .
H7A H 0.6791 0.8822 0.3180 0.050 Uiso 1 1 calc R . .
H7B H 0.7501 0.7928 0.3612 0.050 Uiso 1 1 calc R . .
C8 C 0.62849(16) 0.7240(2) 0.37932(14) 0.0397(6) Uani 1 1 d . . .
H8A H 0.6207 0.7745 0.4285 0.048 Uiso 1 1 calc R . .
H8B H 0.5736 0.7239 0.3508 0.048 Uiso 1 1 calc R . .
C9 C 0.94520(18) 0.4763(4) 0.26922(16) 0.0677(10) Uani 1 1 d . . .
H9A H 0.9981 0.4999 0.2407 0.081 Uiso 1 1 calc R . .
H9B H 0.9438 0.3771 0.2765 0.081 Uiso 1 1 calc R . .
C10 C 0.94440(18) 0.5455(3) 0.34684(17) 0.0604(9) Uani 1 1 d . . .
H10A H 0.9948 0.5174 0.3776 0.072 Uiso 1 1 calc R . .
H10B H 0.9468 0.6447 0.3397 0.072 Uiso 1 1 calc R . .
C11 C 0.61920(16) 0.2897(2) 0.24597(15) 0.0393(7) Uani 1 1 d . . .
H11A H 0.5854 0.2383 0.2074 0.047 Uiso 1 1 calc R . .
H11B H 0.5791 0.3339 0.2824 0.047 Uiso 1 1 calc R . .
C12 C 0.67684(18) 0.1958(2) 0.28957(16) 0.0428(7) Uani 1 1 d . . .
H12A H 0.6426 0.1261 0.3166 0.051 Uiso 1 1 calc R . .
H12B H 0.7161 0.1498 0.2530 0.051 Uiso 1 1 calc R . .
C13 C 0.5902(2) 0.5166(3) 0.43607(16) 0.0598(9) Uani 1 1 d . . .
H13A H 0.5779 0.5623 0.4854 0.090 Uiso 1 1 calc R . .
H13B H 0.6102 0.4245 0.4464 0.090 Uiso 1 1 calc R . .
H13C H 0.5382 0.5131 0.4045 0.090 Uiso 1 1 calc R . .
C14 C 0.8645(2) 0.5644(4) 0.46323(17) 0.0903(14) Uani 1 1 d . . .
H14A H 0.9103 0.5261 0.4951 0.135 Uiso 1 1 calc R . .
H14B H 0.8091 0.5414 0.4861 0.135 Uiso 1 1 calc R . .
H14C H 0.8707 0.6629 0.4612 0.135 Uiso 1 1 calc R . .
C15 C 0.7865(2) 0.1911(3) 0.38312(17) 0.0603(9) Uani 1 1 d . . .
H15A H 0.7579 0.1164 0.4100 0.090 Uiso 1 1 calc R . .
H15B H 0.8177 0.2463 0.4210 0.090 Uiso 1 1 calc R . .
H15C H 0.8267 0.1545 0.3448 0.090 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
O1 Na1 O3 93.89(6) . . ?
O1 Na1 O2 89.53(7) . . ?
O3 Na1 O2 95.83(7) . . ?
O1 Na1 O5 110.87(7) . . ?
O3 Na1 O5 151.69(7) . . ?
O2 Na1 O5 71.72(6) . . ?
O1 Na1 O4 71.00(6) . . ?
O3 Na1 O4 107.72(7) . . ?
O2 Na1 O4 150.02(7) . . ?
O5 Na1 O4 93.63(7) . . ?
O1 Na1 O6 153.93(7) . . ?
O3 Na1 O6 71.87(6) . . ?
O2 Na1 O6 113.06(7) . . ?
O5 Na1 O6 89.37(7) . . ?
O4 Na1 O6 92.17(6) . . ?
Si3 Si1 Si4 99.88(4) . . ?
Si3 Si1 Si2 97.65(4) . . ?
Si4 Si1 Si2 98.49(4) . . ?
O1 Si2 C2 105.45(11) . . ?
O1 Si2 C1 105.85(11) . . ?
C2 Si2 C1 106.01(12) . . ?
O1 Si2 Si1 112.92(6) . . ?
C2 Si2 Si1 112.27(10) . . ?
C1 Si2 Si1 113.68(9) . . ?
O2 Si3 C4 105.69(12) . . ?
O2 Si3 C3 105.49(11) . . ?
C4 Si3 C3 106.45(13) . . ?
O2 Si3 Si1 113.00(7) . . ?
C4 Si3 Si1 114.27(9) . . ?
C3 Si3 Si1 111.30(10) . . ?
O3 Si4 C5 105.90(11) . . ?
O3 Si4 C6 105.04(11) . . ?
C5 Si4 C6 105.73(13) . . ?
O3 Si4 Si1 113.32(6) . . ?
C5 Si4 Si1 113.91(9) . . ?
C6 Si4 Si1 112.20(10) . . ?
C7 O1 Si2 124.92(13) . . ?
C7 O1 Na1 106.29(13) . . ?
Si2 O1 Na1 124.27(8) . . ?
C9 O2 Si3 123.55(16) . . ?
C9 O2 Na1 110.03(15) . . ?
Si3 O2 Na1 121.02(9) . . ?
C11 O3 Si4 124.77(14) . . ?
C11 O3 Na1 107.46(13) . . ?
Si4 O3 Na1 122.45(8) . . ?
C13 O4 C8 111.57(19) . . ?
C13 O4 Na1 126.16(16) . . ?
C8 O4 Na1 113.80(13) . . ?
C10 O5 C14 113.5(2) . . ?
C10 O5 Na1 112.27(14) . . ?
C14 O5 Na1 122.86(19) . . ?
C15 O6 C12 111.52(19) . . ?
C15 O6 Na1 123.91(16) . . ?
C12 O6 Na1 112.29(13) . . ?
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 109.3(2) . . ?
O1 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
O1 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
O4 C8 C7 107.97(19) . . ?
O4 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
O4 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
O2 C9 C10 109.0(2) . . ?
O2 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O2 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O5 C10 C9 108.8(2) . . ?
O5 C10 H10A 109.9 . . ?
C9 C10 H10A 109.9 . . ?
O5 C10 H10B 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O3 C11 C12 109.2(2) . . ?
O3 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
O3 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
O6 C12 C11 108.63(19) . . ?
O6 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
O6 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
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 . . ?
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
Na1 O1 2.3166(17) . ?
Na1 O3 2.3205(17) . ?
Na1 O2 2.3292(19) . ?
Na1 O5 2.3698(19) . ?
Na1 O4 2.3785(17) . ?
Na1 O6 2.3891(18) . ?
Si1 Si3 2.3181(10) . ?
Si1 Si4 2.3183(10) . ?
Si1 Si2 2.3214(10) . ?
Si2 O1 1.6747(16) . ?
Si2 C2 1.879(3) . ?
Si2 C1 1.882(3) . ?
Si3 O2 1.6893(17) . ?
Si3 C4 1.880(3) . ?
Si3 C3 1.885(3) . ?
Si4 O3 1.6838(17) . ?
Si4 C5 1.872(3) . ?
Si4 C6 1.881(3) . ?
O1 C7 1.423(3) . ?
O2 C9 1.416(3) . ?
O3 C11 1.421(3) . ?
O4 C13 1.420(3) . ?
O4 C8 1.421(3) . ?
O5 C10 1.397(3) . ?
O5 C14 1.435(3) . ?
O6 C15 1.424(3) . ?
O6 C12 1.425(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.487(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.501(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.497(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
