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#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/67/4326757.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_4326757
loop_
_publ_author_name
'David J. Wolstenholme'
'Paul D. Prince'
'G. Sean McGrady'
'Michael J. Landry'
'Jonathan W. Steed'
_publ_section_title
;
 Structure and Bonding of KSiH3 and Its 18-Crown-6 Derivatives: Unusual
 Ambidentate Behavior of the SiH3- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11222
_journal_page_last               11227
_journal_paper_doi               10.1021/ic201774x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H43 K O6 Si2'
_chemical_formula_weight         594.92
_space_group_IT_number           160
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'P 3* -2'
_symmetry_space_group_name_H-M   'R 3 m :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.201(10)
_cell_angle_beta                 98.201(10)
_cell_angle_gamma                98.201(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4687(10)
_cell_length_b                   9.4687(10)
_cell_length_c                   9.4687(10)
_cell_measurement_temperature    115(2)
_cell_volume                     820.06(16)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi scans 7.5s/o'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4204
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_correction_T_min  0.8757
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prism
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1303
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0378
_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)+(0.0455P)²+0.2873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                1232
_reflns_number_total             1303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201774x_si_003.cif
_cod_data_source_block           22.CIF
_cod_original_cell_volume        820.06(15)
_cod_original_sg_symbol_H-M      'R 3 m:R'
_cod_database_code               4326757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'y, x, z'
'x, z, y'
'z, y, x'
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
K1 K 0.64113(8) 0.64113(8) 0.64113(8) 0.0214(2) Uani 1 6 d S
Si1 Si 0.38758(12) 0.38758(12) 0.38758(12) 0.0319(4) Uani 1 6 d S
O1 O 0.8992(2) 0.56030(19) 0.56030(19) 0.0238(4) Uani 1 2 d S
C1 C 0.9856(3) 0.4920(3) 0.6557(3) 0.0348(5) Uani 1 1 d .
H1A H 1.049(3) 0.565(3) 0.727(3) 0.031(6) Uiso 1 1 d .
H1B H 1.044(3) 0.439(3) 0.604(3) 0.043(8) Uiso 1 1 d .
Si2 Si 0.96904(11) 0.96904(11) 0.96904(11) 0.0260(3) Uani 1 6 d S
O2 O 0.80798(17) 0.4752(2) 0.80798(17) 0.0260(5) Uani 1 2 d S
C2 C 0.8871(3) 0.3916(3) 0.7217(3) 0.0389(6) Uani 1 1 d .
H2A H 0.821(3) 0.326(4) 0.646(4) 0.052(9) Uiso 1 1 d .
H2B H 0.939(3) 0.339(3) 0.780(3) 0.042(8) Uiso 1 1 d .
C3 C 1.0833(3) 0.8670(3) 1.0833(3) 0.0279(6) Uani 1 2 d S
C4 C 1.0579(4) 0.7167(4) 1.0579(4) 0.0387(9) Uani 1 2 d S
H4 H 0.9830 0.6651 0.9830 0.046 Uiso 1 2 calc SR
C5 C 1.1454(6) 0.6404(5) 1.1454(6) 0.0542(12) Uani 1 2 d S
H5 H 1.1291 0.5376 1.1291 0.065 Uiso 1 2 calc SR
C6 C 1.2531(4) 0.7162(6) 1.2531(4) 0.0541(12) Uani 1 2 d S
H6 H 1.3115 0.6658 1.3115 0.065 Uiso 1 2 calc SR
C7 C 1.2760(4) 0.8599(6) 1.2760(4) 0.0560(11) Uani 1 2 d S
H7 H 1.3509 0.9110 1.3509 0.067 Uiso 1 2 calc SR
C8 C 1.1933(3) 0.9369(4) 1.1933(3) 0.0417(8) Uani 1 2 d S
H8 H 1.2124 1.0397 1.2124 0.050 Uiso 1 2 calc SR
H1S H 0.496(5) 0.344(6) 0.496(5) 0.072(16) Uiso 1 2 d S
H2S H 0.869(5) 0.869(5) 0.869(5) 0.025(15) Uiso 1 6 d S
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'
Si Si 0.0817 0.0704 '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'
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
O1 K1 O1 117.58(3) . 3
O1 K1 O1 117.58(3) . 2
O1 K1 O1 117.58(3) 3 2
O1 K1 O2 155.22(8) . 3
O1 K1 O2 58.809(12) 3 3
O1 K1 O2 58.809(12) 2 3
O1 K1 O2 58.809(12) . 2
O1 K1 O2 155.22(8) 3 2
O1 K1 O2 58.809(12) 2 2
O2 K1 O2 112.93(4) 3 2
O1 K1 O2 58.809(12) . .
O1 K1 O2 58.809(12) 3 .
O1 K1 O2 155.22(8) 2 .
O2 K1 O2 112.93(4) 3 .
O2 K1 O2 112.93(4) 2 .
O1 K1 Si1 99.04(5) . .
O1 K1 Si1 99.04(5) 3 .
O1 K1 Si1 99.04(5) 2 .
O2 K1 Si1 105.74(5) 3 .
O2 K1 Si1 105.74(5) 2 .
O2 K1 Si1 105.74(5) . .
C1 O1 C1 111.4(3) 5 .
C1 O1 K1 118.53(12) 5 .
C1 O1 K1 118.53(12) . .
O1 C1 C2 108.3(2) . .
C3 Si2 C3 110.80(10) 3 2
C3 Si2 C3 110.80(10) 3 .
C3 Si2 C3 110.80(10) 2 .
C2 O2 C2 113.1(3) . 6
C2 O2 K1 111.60(14) . .
C2 O2 K1 111.60(14) 6 .
O2 C2 C1 108.6(2) . .
C8 C3 C4 118.2(3) . .
C8 C3 Si2 122.0(2) . .
C4 C3 Si2 119.9(3) . .
C3 C4 C5 119.3(5) . .
C6 C5 C4 119.7(4) . .
C7 C6 C5 120.2(4) . .
C6 C7 C8 121.6(5) . .
C3 C8 C7 121.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.8360(19) .
K1 O1 2.8360(19) 3
K1 O1 2.8360(19) 2
K1 O2 2.858(2) 3
K1 O2 2.858(2) 2
K1 O2 2.858(2) .
K1 Si1 3.515(2) .
O1 C1 1.418(3) 5
O1 C1 1.418(3) .
C1 C2 1.499(3) .
Si2 C3 1.881(3) 3
Si2 C3 1.881(3) 2
Si2 C3 1.881(3) .
O2 C2 1.419(3) .
O2 C2 1.419(3) 6
C3 C8 1.380(5) .
C3 C4 1.389(5) .
C4 C5 1.428(6) .
C5 C6 1.371(8) .
C6 C7 1.328(7) .
C7 C8 1.381(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 K1 O1 C1 -144.90(15) 3 5
O1 K1 O1 C1 4.7(2) 2 5
O2 K1 O1 C1 -70.12(18) 3 5
O2 K1 O1 C1 6.89(18) 2 5
O2 K1 O1 C1 -147.1(2) . 5
Si1 K1 O1 C1 109.88(19) . 5
O1 K1 O1 C1 -4.7(2) 3 .
O1 K1 O1 C1 144.90(15) 2 .
O2 K1 O1 C1 70.12(19) 3 .
O2 K1 O1 C1 147.1(2) 2 .
O2 K1 O1 C1 -6.89(18) . .
Si1 K1 O1 C1 -109.88(19) . .
C1 O1 C1 C2 -179.14(16) 5 .
K1 O1 C1 C2 38.0(3) . .
O1 K1 O2 C2 -27.37(17) . .
O1 K1 O2 C2 154.95(18) 3 .
O1 K1 O2 C2 -116.21(17) 2 .
O2 K1 O2 C2 178.95(15) 3 .
O2 K1 O2 C2 -51.4(2) 2 .
Si1 K1 O2 C2 63.79(17) . .
O1 K1 O2 C2 -154.95(18) . 6
O1 K1 O2 C2 27.37(17) 3 6
O1 K1 O2 C2 116.21(17) 2 6
O2 K1 O2 C2 51.4(2) 3 6
O2 K1 O2 C2 -178.95(15) 2 6
Si1 K1 O2 C2 -63.79(17) . 6
C2 O2 C2 C1 -174.10(15) 6 .
K1 O2 C2 C1 59.1(2) . .
O1 C1 C2 O2 -64.7(3) . .
C3 Si2 C3 C8 -61.71(13) 3 .
C3 Si2 C3 C8 61.71(13) 2 .
C3 Si2 C3 C4 118.29(13) 3 .
C3 Si2 C3 C4 -118.29(13) 2 .
C8 C3 C4 C5 0.000(2) . .
Si2 C3 C4 C5 180.000(1) . .
C3 C4 C5 C6 0.000(2) . .
C4 C5 C6 C7 0.000(2) . .
C5 C6 C7 C8 0.000(3) . .
C4 C3 C8 C7 0.000(4) . .
Si2 C3 C8 C7 180.000(2) . .
C6 C7 C8 C3 0.000(4) . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139136342
