#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:58:54 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178927 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/56/4115646.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_4115646
loop_
_publ_author_name
'Michael J. Bearpark'
'G. Sean McGrady'
'Paul D. Prince'
'Jonathan W. Steed'
_publ_section_title
;
 The First Structurally Characterized Hypervalent Silicon Hydride:
 Unexpected Molecular Geometry and Si-H...K Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7736
_journal_page_last               7737
_journal_paper_doi               10.1021/ja0162616
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C30 H41 K O6 Si'
_chemical_formula_weight         564.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'P 3*'
_symmetry_space_group_name_H-M   'R 3 :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.930(10)
_cell_angle_beta                 97.930(10)
_cell_angle_gamma                97.930(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4424(15)
_cell_length_b                   9.4424(15)
_cell_length_c                   9.4424(15)
_cell_measurement_temperature    393(2)
_cell_volume                     815.2(2)
_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      393(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi scans 6s/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  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1117
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4386
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.9543
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(7)
_refine_ls_extinction_coef       0.041(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0462
_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)+(0.0291P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                1650
_reflns_number_total             2257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0162616_s1.cif
_cod_data_source_block           ppbypa(trigonal_K[Ph3SiH2]18C6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4115646
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, 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 0.61310(7) 0.61310(7) 0.61310(7) 0.0251(3) Uani 1 3 d S
Si1 Si 0.92404(11) 0.92404(11) 0.92404(11) 0.0342(4) Uani 1 3 d S
O1 O 0.3687(2) 0.7064(2) 0.7066(3) 0.0343(5) Uani 1 1 d .
C1 C 0.2821(4) 0.6140(5) 0.7799(5) 0.0489(10) Uani 1 1 d .
H1 H 1.042(3) 1.042(3) 1.042(3) 0.038(14) Uiso 1 3 d S
H2 H 0.8073 0.8063 0.8063 0.046 Uiso 1 3 d SR
O2 O 0.7927(2) 0.4605(2) 0.4602(2) 0.0347(6) Uani 1 1 d .
C2 C 0.2824(4) 0.7806(5) 0.6140(5) 0.0488(10) Uani 1 1 d .
C3 C 0.8780(4) 0.5481(5) 0.3814(4) 0.0478(10) Uani 1 1 d .
C4 C 0.8777(4) 0.3812(4) 0.5478(5) 0.0483(10) Uani 1 1 d .
C5 C 1.0006(3) 0.7659(3) 1.0001(3) 0.0334(8) Uani 1 1 d .
C6 C 0.9439(3) 0.6202(3) 0.9435(3) 0.0335(7) Uani 1 1 d .
H6 H 0.855(3) 0.595(3) 0.859(3) 0.040(8) Uiso 1 1 d .
C7 C 0.9981(4) 0.5055(4) 0.9989(4) 0.0401(9) Uani 1 1 d .
H7 H 0.956(4) 0.408(4) 0.960(4) 0.048(10) Uiso 1 1 d .
C8 C 1.1121(4) 0.5314(4) 1.1115(4) 0.0419(9) Uani 1 1 d .
H8 H 1.155(3) 0.442(3) 1.153(3) 0.031(8) Uiso 1 1 d .
C9 C 1.1696(4) 0.6730(5) 1.1713(4) 0.0497(10) Uani 1 1 d .
H9 H 1.240(4) 0.685(4) 1.239(4) 0.042(10) Uiso 1 1 d .
C10 C 1.1157(4) 0.7887(5) 1.1162(4) 0.0409(9) Uani 1 1 d .
H10 H 1.154(4) 0.891(5) 1.153(4) 0.077(14) Uiso 1 1 d .
H1A H 0.215(4) 0.532(4) 0.708(4) 0.051(10) Uiso 1 1 d .
H2A H 0.221(4) 0.841(4) 0.673(4) 0.052(10) Uiso 1 1 d .
H3A H 0.943(4) 0.482(4) 0.335(4) 0.070(11) Uiso 1 1 d .
H4A H 0.945(4) 0.444(4) 0.622(4) 0.047(11) Uiso 1 1 d .
H1B H 0.225(4) 0.667(4) 0.843(4) 0.054(10) Uiso 1 1 d .
H2B H 0.217(4) 0.714(4) 0.539(4) 0.053(11) Uiso 1 1 d .
H3B H 0.945(4) 0.620(4) 0.450(4) 0.043(10) Uiso 1 1 d .
H4B H 0.942(4) 0.330(4) 0.480(4) 0.054(10) Uiso 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'
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 119.096(19) 3 2
O1 K1 O1 119.096(19) 3 .
O1 K1 O1 119.10(2) 2 .
O1 K1 O2 59.53(7) 3 .
O1 K1 O2 59.58(7) 2 .
O1 K1 O2 162.45(8) . .
O1 K1 O2 162.45(8) 3 3
O1 K1 O2 59.53(7) 2 3
O1 K1 O2 59.58(7) . 3
O2 K1 O2 115.75(3) . 3
O1 K1 O2 59.58(7) 3 2
O1 K1 O2 162.45(8) 2 2
O1 K1 O2 59.53(7) . 2
O2 K1 O2 115.75(3) . 2
O2 K1 O2 115.75(3) 3 2
C5 Si1 C5 119.983(5) 2 .
C5 Si1 C5 119.983(5) 2 3
C5 Si1 C5 119.983(5) . 3
C1 O1 C2 111.9(3) . .
C1 O1 K1 118.37(18) . .
C2 O1 K1 118.25(18) . .
O1 C1 C4 107.8(3) . 3
C3 O2 C4 112.4(3) . .
C3 O2 K1 113.13(19) . .
C4 O2 K1 113.02(19) . .
O1 C2 C3 108.0(3) . 2
O2 C3 C2 108.9(3) . 3
O2 C4 C1 109.1(3) . 2
C10 C5 C6 115.7(3) . .
C10 C5 Si1 122.2(3) . .
C6 C5 Si1 122.1(2) . .
C7 C6 C5 122.3(3) . .
C8 C7 C6 120.6(4) . .
C7 C8 C9 118.8(4) . .
C8 C9 C10 120.9(4) . .
C9 C10 C5 121.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.7907(18) 3
K1 O1 2.7907(18) 2
K1 O1 2.7907(18) .
K1 O2 2.795(2) .
K1 O2 2.795(2) 3
K1 O2 2.795(2) 2
Si1 C5 1.928(3) 2
Si1 C5 1.928(3) .
Si1 C5 1.928(3) 3
O1 C1 1.426(4) .
O1 C2 1.431(4) .
C1 C4 1.484(5) 3
O2 C3 1.428(4) .
O2 C4 1.429(4) .
C2 C3 1.479(5) 2
C3 C2 1.479(5) 3
C4 C1 1.484(5) 2
C5 C10 1.404(4) .
C5 C6 1.407(4) .
C6 C7 1.394(4) .
C7 C8 1.374(5) .
C8 C9 1.381(6) .
C9 C10 1.400(5) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C9 H9 O2 0.84(4) 2.72(4) 3.534(5) 166(3) 2_656
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 150.7(2) 3 .
O1 K1 O1 C1 -10.5(3) 2 .
O2 K1 O1 C1 70.2(4) . .
O2 K1 O1 C1 -9.1(2) 3 .
O2 K1 O1 C1 149.3(3) 2 .
O1 K1 O1 C2 10.2(3) 3 .
O1 K1 O1 C2 -151.0(2) 2 .
O2 K1 O1 C2 -70.3(4) . .
O2 K1 O1 C2 -149.6(3) 3 .
O2 K1 O1 C2 8.8(3) 2 .
C2 O1 C1 C4 -177.4(3) . 3
K1 O1 C1 C4 39.8(4) . 3
O1 K1 O2 C3 24.8(2) 3 .
O1 K1 O2 C3 -153.8(2) 2 .
O1 K1 O2 C3 115.5(3) . .
O2 K1 O2 C3 -174.3(2) 3 .
O2 K1 O2 C3 45.4(3) 2 .
O1 K1 O2 C4 154.0(2) 3 .
O1 K1 O2 C4 -24.6(2) 2 .
O1 K1 O2 C4 -115.4(3) . .
O2 K1 O2 C4 -45.2(3) 3 .
O2 K1 O2 C4 174.6(2) 2 .
C1 O1 C2 C3 177.6(3) . 2
K1 O1 C2 C3 -39.6(4) . 2
C4 O2 C3 C2 174.1(3) . 3
K1 O2 C3 C2 -56.4(3) . 3
C3 O2 C4 C1 -174.3(3) . 2
K1 O2 C4 C1 56.2(3) . 2
C5 Si1 C5 C10 91.8(3) 2 .
C5 Si1 C5 C10 -90.9(3) 3 .
C5 Si1 C5 C6 -88.8(3) 2 .
C5 Si1 C5 C6 88.6(3) 3 .
C10 C5 C6 C7 0.0(4) . .
Si1 C5 C6 C7 -179.4(2) . .
C5 C6 C7 C8 -0.9(5) . .
C6 C7 C8 C9 1.7(5) . .
C7 C8 C9 C10 -1.7(5) . .
C8 C9 C10 C5 0.8(5) . .
C6 C5 C10 C9 0.0(5) . .
Si1 C5 C10 C9 179.5(3) . .
