# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dq0217_2
_database_code_depnum_ccdc_archive 'CCDC 1436078'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H43 K O6 Si'
_chemical_formula_weight         542.81

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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.6776(9)
_cell_length_b                   16.8062(15)
_cell_length_c                   18.2542(17)
_cell_angle_alpha                90
_cell_angle_beta                 92.9686(17)
_cell_angle_gamma                90
_cell_volume                     2964.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    9958
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      35.18

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.257
_shelx_estimated_absorpt_T_min   0.922
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69399
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.721
_diffrn_reflns_theta_max         35.326
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             12708
_reflns_number_gt                10908
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12708
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.604
_refine_ls_restrained_S_all      1.604
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.40093(2) 0.52301(2) 0.23905(2) 0.01677(4) Uani 1 1 d . . . . .
Si1 Si 0.28022(2) 0.34454(2) 0.30179(2) 0.01472(5) Uani 1 1 d . . . . .
O1 O 0.50959(6) 0.45497(3) 0.10730(3) 0.02102(10) Uani 1 1 d . . . . .
O2 O 0.66267(5) 0.45868(3) 0.24400(3) 0.02091(10) Uani 1 1 d . . . . .
O3 O 0.59410(5) 0.56580(3) 0.35396(3) 0.01735(9) Uani 1 1 d . . . . .
O4 O 0.31683(5) 0.61784(3) 0.35353(3) 0.02170(11) Uani 1 1 d . . . . .
O5 O 0.16148(5) 0.62317(3) 0.21916(3) 0.02199(11) Uani 1 1 d . . . . .
O6 O 0.23997(6) 0.51914(3) 0.10884(3) 0.02272(11) Uani 1 1 d . . . . .
C1 C 0.60217(9) 0.39395(5) 0.13159(4) 0.02464(15) Uani 1 1 d . . . . .
H1A H 0.6400 0.3669 0.0888 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5526 0.3540 0.1602 0.030 Uiso 1 1 calc R U . . .
C2 C 0.71792(8) 0.43009(5) 0.17854(4) 0.02454(15) Uani 1 1 d . . . . .
H2A H 0.7900 0.3896 0.1903 0.029 Uiso 1 1 calc R U . . .
H2B H 0.7606 0.4744 0.1520 0.029 Uiso 1 1 calc R U . . .
C3 C 0.76455(7) 0.49127(4) 0.29427(4) 0.02063(13) Uani 1 1 d . . . . .
H3A H 0.8008 0.5417 0.2748 0.025 Uiso 1 1 calc R U . . .
H3B H 0.8426 0.4536 0.3020 0.025 Uiso 1 1 calc R U . . .
C4 C 0.69735(8) 0.50621(5) 0.36537(4) 0.02150(13) Uani 1 1 d . . . . .
H4A H 0.6549 0.4565 0.3827 0.026 Uiso 1 1 calc R U . . .
H4B H 0.7676 0.5241 0.4032 0.026 Uiso 1 1 calc R U . . .
C5 C 0.52348(8) 0.58062(5) 0.41893(4) 0.02230(14) Uani 1 1 d . . . . .
H5A H 0.5905 0.5959 0.4593 0.027 Uiso 1 1 calc R U . . .
H5B H 0.4745 0.5320 0.4338 0.027 Uiso 1 1 calc R U . . .
C6 C 0.42146(8) 0.64675(5) 0.40411(4) 0.02218(14) Uani 1 1 d . . . . .
H6A H 0.3803 0.6634 0.4502 0.027 Uiso 1 1 calc R U . . .
H6B H 0.4682 0.6933 0.3832 0.027 Uiso 1 1 calc R U . . .
C7 C 0.20758(8) 0.67307(5) 0.33922(4) 0.02467(15) Uani 1 1 d . . . . .
H7A H 0.2434 0.7218 0.3164 0.030 Uiso 1 1 calc R U . . .
H7B H 0.1656 0.6881 0.3855 0.030 Uiso 1 1 calc R U . . .
C8 C 0.10190(8) 0.63409(5) 0.28831(5) 0.02604(16) Uani 1 1 d . . . . .
H8A H 0.0745 0.5821 0.3085 0.031 Uiso 1 1 calc R U . . .
H8B H 0.0184 0.6680 0.2824 0.031 Uiso 1 1 calc R U . . .
C9 C 0.06493(8) 0.59157(5) 0.16529(5) 0.02898(17) Uani 1 1 d . . . . .
H9A H -0.0126 0.6293 0.1563 0.035 Uiso 1 1 calc R U . . .
H9B H 0.0267 0.5408 0.1829 0.035 Uiso 1 1 calc R U . . .
C10 C 0.13676(9) 0.57779(5) 0.09566(5) 0.02985(17) Uani 1 1 d . . . . .
H10A H 0.0693 0.5597 0.0565 0.036 Uiso 1 1 calc R U . . .
H10B H 0.1794 0.6279 0.0794 0.036 Uiso 1 1 calc R U . . .
C11 C 0.29788(9) 0.49050(6) 0.04398(4) 0.02774(16) Uani 1 1 d . . . . .
H11A H 0.3483 0.5339 0.0202 0.033 Uiso 1 1 calc R U . . .
H11B H 0.2234 0.4715 0.0091 0.033 Uiso 1 1 calc R U . . .
C12 C 0.39503(8) 0.42369(5) 0.06382(4) 0.02550(15) Uani 1 1 d . . . . .
H12A H 0.3469 0.3826 0.0918 0.031 Uiso 1 1 calc R U . . .
H12B H 0.4281 0.3988 0.0188 0.031 Uiso 1 1 calc R U . . .
C13 C 0.11867(7) 0.34625(4) 0.36011(4) 0.01590(12) Uani 1 1 d . . . . .
C14 C -0.00360(7) 0.30373(4) 0.34339(4) 0.01999(13) Uani 1 1 d . . . . .
H14 H -0.0082 0.2705 0.3012 0.024 Uiso 1 1 calc R U . . .
C15 C -0.11857(8) 0.30818(5) 0.38599(5) 0.02727(16) Uani 1 1 d . . . . .
H15 H -0.1998 0.2788 0.3725 0.033 Uiso 1 1 calc R U . . .
C16 C -0.11419(9) 0.35560(5) 0.44815(5) 0.03057(19) Uani 1 1 d . . . . .
H16 H -0.1921 0.3587 0.4776 0.037 Uiso 1 1 calc R U . . .
C17 C 0.00436(9) 0.39826(5) 0.46701(4) 0.02906(17) Uani 1 1 d . . . . .
H17 H 0.0085 0.4303 0.5100 0.035 Uiso 1 1 calc R U . . .
C18 C 0.11802(8) 0.39448(4) 0.42321(4) 0.02219(14) Uani 1 1 d . . . . .
H18 H 0.1976 0.4254 0.4363 0.027 Uiso 1 1 calc R U . . .
C19 C 0.19539(7) 0.30730(4) 0.21012(4) 0.01539(11) Uani 1 1 d . . . . .
C20 C 0.09320(7) 0.35695(4) 0.17662(4) 0.01959(13) Uani 1 1 d . . . . .
H20 H 0.0610 0.4009 0.2037 0.024 Uiso 1 1 calc R U . . .
C21 C 0.03718(8) 0.34470(5) 0.10582(4) 0.02252(14) Uani 1 1 d . . . . .
H21 H -0.0318 0.3798 0.0858 0.027 Uiso 1 1 calc R U . . .
C22 C 0.08199(8) 0.28103(5) 0.06419(4) 0.02246(14) Uani 1 1 d . . . . .
H22 H 0.0458 0.2728 0.0154 0.027 Uiso 1 1 calc R U . . .
C23 C 0.18086(7) 0.22991(5) 0.09575(4) 0.02113(13) Uani 1 1 d . . . . .
H23 H 0.2116 0.1857 0.0685 0.025 Uiso 1 1 calc R U . . .
C24 C 0.23557(7) 0.24265(4) 0.16702(4) 0.01754(12) Uani 1 1 d . . . . .
H24 H 0.3024 0.2063 0.1872 0.021 Uiso 1 1 calc R U . . .
C25 C 0.38615(7) 0.25464(4) 0.34513(4) 0.01588(11) Uani 1 1 d . . . . .
C26 C 0.30583(8) 0.17666(4) 0.35222(4) 0.02145(13) Uani 1 1 d . . . . .
H26A H 0.3676 0.1357 0.3736 0.032 Uiso 1 1 calc R U . . .
H26B H 0.2699 0.1595 0.3036 0.032 Uiso 1 1 calc R U . . .
H26C H 0.2286 0.1850 0.3840 0.032 Uiso 1 1 calc R U . . .
C27 C 0.51508(7) 0.23977(5) 0.30128(4) 0.02255(14) Uani 1 1 d . . . . .
H27A H 0.5649 0.2900 0.2955 0.034 Uiso 1 1 calc R U . . .
H27B H 0.4868 0.2185 0.2528 0.034 Uiso 1 1 calc R U . . .
H27C H 0.5757 0.2014 0.3276 0.034 Uiso 1 1 calc R U . . .
C28 C 0.43815(8) 0.28004(5) 0.42245(4) 0.02201(14) Uani 1 1 d . . . . .
H28A H 0.3591 0.2872 0.4532 0.033 Uiso 1 1 calc R U . . .
H28B H 0.4890 0.3303 0.4196 0.033 Uiso 1 1 calc R U . . .
H28C H 0.4995 0.2389 0.4438 0.033 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
K1 O2 2.7514(6) . ?
K1 O6 2.7743(6) . ?
K1 O4 2.7830(6) . ?
K1 O3 2.8293(5) . ?
K1 O5 2.8718(6) . ?
K1 O1 2.9086(6) . ?
K1 Si1 3.4367(3) . ?
Si1 C19 1.9296(7) . ?
Si1 C13 1.9367(7) . ?
Si1 C25 1.9687(7) . ?
O1 C1 1.4177(9) . ?
O1 C12 1.4298(9) . ?
O2 C2 1.4181(9) . ?
O2 C3 1.4214(9) . ?
O3 C4 1.4224(9) . ?
O3 C5 1.4212(9) . ?
O4 C6 1.4202(9) . ?
O4 C7 1.4208(9) . ?
O5 C9 1.4238(9) . ?
O5 C8 1.4265(10) . ?
O6 C10 1.4150(10) . ?
O6 C11 1.4199(10) . ?
C1 C2 1.5029(11) . ?
C3 C4 1.5025(11) . ?
C5 C6 1.5018(11) . ?
C7 C8 1.4967(12) . ?
C9 C10 1.4979(13) . ?
C11 C12 1.4969(12) . ?
C13 C14 1.4023(10) . ?
C13 C18 1.4088(10) . ?
C14 C15 1.3921(10) . ?
C15 C16 1.3854(13) . ?
C16 C17 1.3813(14) . ?
C17 C18 1.3944(11) . ?
C19 C24 1.4080(9) . ?
C19 C20 1.4092(10) . ?
C20 C21 1.3908(10) . ?
C21 C22 1.3945(11) . ?
C22 C23 1.3887(11) . ?
C23 C24 1.3955(10) . ?
C25 C26 1.5325(10) . ?
C25 C28 1.5341(10) . ?
C25 C27 1.5374(10) . ?

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
O2 K1 O6 119.607(17) . . ?
O2 K1 O4 120.326(16) . . ?
O6 K1 O4 118.925(17) . . ?
O2 K1 O3 60.244(16) . . ?
O6 K1 O3 163.989(17) . . ?
O4 K1 O3 60.364(16) . . ?
O2 K1 O5 165.918(17) . . ?
O6 K1 O5 59.460(17) . . ?
O4 K1 O5 59.593(16) . . ?
O3 K1 O5 116.269(17) . . ?
O2 K1 O1 60.065(15) . . ?
O6 K1 O1 59.558(17) . . ?
O4 K1 O1 168.050(17) . . ?
O3 K1 O1 117.362(17) . . ?
O5 K1 O1 116.731(17) . . ?
O2 K1 Si1 88.529(14) . . ?
O6 K1 Si1 94.564(13) . . ?
O4 K1 Si1 97.582(14) . . ?
O3 K1 Si1 101.404(12) . . ?
O5 K1 Si1 105.527(13) . . ?
O1 K1 Si1 94.366(13) . . ?
C19 Si1 C13 99.33(3) . . ?
C19 Si1 C25 106.79(3) . . ?
C13 Si1 C25 102.05(3) . . ?
C19 Si1 K1 97.52(2) . . ?
C13 Si1 K1 117.92(2) . . ?
C25 Si1 K1 128.67(2) . . ?
C1 O1 C12 111.52(6) . . ?
C1 O1 K1 105.99(4) . . ?
C12 O1 K1 107.48(4) . . ?
C2 O2 C3 113.30(6) . . ?
C2 O2 K1 119.48(4) . . ?
C3 O2 K1 118.45(4) . . ?
C4 O3 C5 111.45(5) . . ?
C4 O3 K1 111.21(4) . . ?
C5 O3 K1 109.60(4) . . ?
C6 O4 C7 113.25(6) . . ?
C6 O4 K1 117.24(4) . . ?
C7 O4 K1 118.67(4) . . ?
C9 O5 C8 112.23(6) . . ?
C9 O5 K1 111.41(4) . . ?
C8 O5 K1 108.91(4) . . ?
C10 O6 C11 113.57(6) . . ?
C10 O6 K1 119.30(5) . . ?
C11 O6 K1 119.60(4) . . ?
O1 C1 C2 109.04(6) . . ?
O2 C2 C1 108.37(6) . . ?
O2 C3 C4 107.77(6) . . ?
O3 C4 C3 108.86(6) . . ?
O3 C5 C6 108.63(6) . . ?
O4 C6 C5 107.69(6) . . ?
O4 C7 C8 107.84(6) . . ?
O5 C8 C7 108.13(6) . . ?
O5 C9 C10 109.08(6) . . ?
O6 C10 C9 108.53(7) . . ?
O6 C11 C12 108.82(6) . . ?
O1 C12 C11 108.52(6) . . ?
C14 C13 C18 115.57(6) . . ?
C14 C13 Si1 124.68(5) . . ?
C18 C13 Si1 119.73(5) . . ?
C15 C14 C13 122.75(7) . . ?
C16 C15 C14 119.80(8) . . ?
C17 C16 C15 119.51(7) . . ?
C16 C17 C18 120.21(8) . . ?
C17 C18 C13 122.15(7) . . ?
C24 C19 C20 114.98(6) . . ?
C24 C19 Si1 128.14(5) . . ?
C20 C19 Si1 116.21(5) . . ?
C21 C20 C19 123.14(7) . . ?
C20 C21 C22 120.18(7) . . ?
C23 C22 C21 118.41(7) . . ?
C22 C23 C24 120.79(7) . . ?
C23 C24 C19 122.47(7) . . ?
C26 C25 C28 107.69(6) . . ?
C26 C25 C27 109.50(6) . . ?
C28 C25 C27 106.73(6) . . ?
C26 C25 Si1 115.75(5) . . ?
C28 C25 Si1 107.18(5) . . ?
C27 C25 Si1 109.59(5) . . ?

_refine_diff_density_max         0.542
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.073

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_apx1891s
_database_code_depnum_ccdc_archive 'CCDC 1436079'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_apx1891s            
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: Molecular formula correct- PLATON/SQUEEZE use to treat
disordered thf solvent.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H43 K O6.50 S Si'
_chemical_formula_weight         630.91

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'
S S 0.1246 0.1234 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.188(8)
_cell_length_b                   10.473(9)
_cell_length_c                   17.685(14)
_cell_angle_alpha                95.930(9)
_cell_angle_beta                 93.438(9)
_cell_angle_gamma                94.815(9)
_cell_volume                     1683(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9162
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16688
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_sigmaI/netI    0.1150
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.78
_reflns_number_total             6366
_reflns_number_gt                3605
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 182 48 thf

_platon_squeeze_details          
;
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1017P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0102(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6366
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1594
_refine_ls_wR_factor_gt          0.1339
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_restrained_S_all      0.781
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
K1 K 0.70314(8) 0.77714(7) 0.66762(5) 0.0301(2) Uani 1 1 d . . .
S1 S 0.43572(10) 0.58279(9) 0.69348(5) 0.0292(3) Uani 1 1 d . . .
Si1 Si 0.46258(10) 0.53833(9) 0.80273(6) 0.0221(3) Uani 1 1 d . . .
O1 O 0.4943(3) 0.9399(2) 0.61382(14) 0.0307(6) Uani 1 1 d . . .
O2 O 0.6393(2) 0.9992(2) 0.75776(14) 0.0297(6) Uani 1 1 d . . .
O3 O 0.9126(3) 0.9082(2) 0.78932(14) 0.0308(6) Uani 1 1 d . . .
O4 O 0.9633(3) 0.6823(2) 0.69919(15) 0.0329(6) Uani 1 1 d . . .
O5 O 0.8350(3) 0.6184(2) 0.55065(15) 0.0341(6) Uani 1 1 d . . .
O6 O 0.5665(3) 0.7211(2) 0.52450(14) 0.0321(6) Uani 1 1 d . . .
C1 C 0.4256(4) 0.9994(4) 0.6774(2) 0.0362(10) Uani 1 1 d . . .
H1A H 0.3788 0.9339 0.7051 0.043 Uiso 1 1 calc R . .
H1B H 0.3515 1.0522 0.6597 0.043 Uiso 1 1 calc R . .
C2 C 0.5403(4) 1.0804(4) 0.7277(2) 0.0363(10) Uani 1 1 d . . .
H2A H 0.5918 1.1417 0.6989 0.044 Uiso 1 1 calc R . .
H2B H 0.4958 1.1281 0.7689 0.044 Uiso 1 1 calc R . .
C3 C 0.7462(4) 1.0682(4) 0.8114(2) 0.0348(9) Uani 1 1 d . . .
H3A H 0.6991 1.1186 0.8504 0.042 Uiso 1 1 calc R . .
H3B H 0.8100 1.1264 0.7862 0.042 Uiso 1 1 calc R . .
C4 C 0.8335(4) 0.9716(4) 0.8466(2) 0.0365(10) Uani 1 1 d . . .
H4A H 0.9010 1.0149 0.8874 0.044 Uiso 1 1 calc R . .
H4B H 0.7685 0.9090 0.8680 0.044 Uiso 1 1 calc R . .
C5 C 0.9914(4) 0.8089(4) 0.8176(2) 0.0335(9) Uani 1 1 d . . .
H5A H 0.9238 0.7461 0.8371 0.040 Uiso 1 1 calc R . .
H5B H 1.0611 0.8458 0.8590 0.040 Uiso 1 1 calc R . .
C6 C 1.0696(4) 0.7449(4) 0.7555(2) 0.0348(10) Uani 1 1 d . . .
H6A H 1.1326 0.8082 0.7336 0.042 Uiso 1 1 calc R . .
H6B H 1.1298 0.6824 0.7753 0.042 Uiso 1 1 calc R . .
C7 C 1.0256(4) 0.6003(4) 0.6436(2) 0.0405(10) Uani 1 1 d . . .
H7A H 1.0816 0.5397 0.6682 0.049 Uiso 1 1 calc R . .
H7B H 1.0912 0.6508 0.6149 0.049 Uiso 1 1 calc R . .
C8 C 0.9052(4) 0.5294(4) 0.5917(2) 0.0418(10) Uani 1 1 d . . .
H8A H 0.9447 0.4659 0.5566 0.050 Uiso 1 1 calc R . .
H8B H 0.8353 0.4848 0.6211 0.050 Uiso 1 1 calc R . .
C9 C 0.7216(4) 0.5592(4) 0.4977(2) 0.0447(11) Uani 1 1 d . . .
H9A H 0.6554 0.5032 0.5230 0.054 Uiso 1 1 calc R . .
H9B H 0.7630 0.5069 0.4574 0.054 Uiso 1 1 calc R . .
C10 C 0.6408(4) 0.6572(4) 0.4652(2) 0.0426(11) Uani 1 1 d . . .
H10A H 0.7078 0.7187 0.4442 0.051 Uiso 1 1 calc R . .
H10B H 0.5709 0.6173 0.4246 0.051 Uiso 1 1 calc R . .
C11 C 0.4680(5) 0.8045(4) 0.4970(2) 0.0395(10) Uani 1 1 d . . .
H11A H 0.3982 0.7575 0.4586 0.047 Uiso 1 1 calc R . .
H11B H 0.5208 0.8732 0.4741 0.047 Uiso 1 1 calc R . .
C12 C 0.3899(4) 0.8596(4) 0.5630(2) 0.0370(10) Uani 1 1 d . . .
H12A H 0.3132 0.9098 0.5451 0.044 Uiso 1 1 calc R . .
H12B H 0.3454 0.7908 0.5890 0.044 Uiso 1 1 calc R . .
C13 C 0.4056(3) 0.6678(3) 0.8746(2) 0.0211(8) Uani 1 1 d . . .
C14 C 0.3242(4) 0.6457(3) 0.9363(2) 0.0255(8) Uani 1 1 d . . .
H14 H 0.2958 0.5613 0.9448 0.031 Uiso 1 1 calc R . .
C15 C 0.2841(4) 0.7468(3) 0.9857(2) 0.0285(9) Uani 1 1 d . . .
H15 H 0.2283 0.7297 1.0263 0.034 Uiso 1 1 calc R . .
C16 C 0.3267(4) 0.8715(3) 0.9745(2) 0.0322(9) Uani 1 1 d . . .
H16 H 0.3009 0.9392 1.0079 0.039 Uiso 1 1 calc R . .
C17 C 0.4082(4) 0.8970(3) 0.9136(2) 0.0298(9) Uani 1 1 d . . .
H17 H 0.4378 0.9815 0.9058 0.036 Uiso 1 1 calc R . .
C18 C 0.4449(4) 0.7956(3) 0.8645(2) 0.0263(8) Uani 1 1 d . . .
H18 H 0.4981 0.8134 0.8231 0.032 Uiso 1 1 calc R . .
C19 C 0.6587(4) 0.5153(3) 0.8319(2) 0.0232(8) Uani 1 1 d . . .
C20 C 0.7287(4) 0.5639(3) 0.9026(2) 0.0267(8) Uani 1 1 d . . .
H20 H 0.6783 0.6129 0.9373 0.032 Uiso 1 1 calc R . .
C21 C 0.8716(4) 0.5406(3) 0.9221(2) 0.0315(9) Uani 1 1 d . . .
H21 H 0.9157 0.5736 0.9696 0.038 Uiso 1 1 calc R . .
C22 C 0.9486(4) 0.4686(4) 0.8715(2) 0.0356(10) Uani 1 1 d . . .
H22 H 1.0444 0.4529 0.8847 0.043 Uiso 1 1 calc R . .
C23 C 0.8830(4) 0.4201(4) 0.8011(2) 0.0361(10) Uani 1 1 d . . .
H23 H 0.9347 0.3721 0.7665 0.043 Uiso 1 1 calc R . .
C24 C 0.7399(4) 0.4430(3) 0.7820(2) 0.0307(9) Uani 1 1 d . . .
H24 H 0.6966 0.4091 0.7345 0.037 Uiso 1 1 calc R . .
C25 C 0.3587(4) 0.3825(3) 0.8203(2) 0.0241(8) Uani 1 1 d . . .
C26 C 0.3832(4) 0.3302(3) 0.8885(2) 0.0292(9) Uani 1 1 d . . .
H26 H 0.4525 0.3728 0.9250 0.035 Uiso 1 1 calc R . .
C27 C 0.3077(4) 0.2166(3) 0.9039(2) 0.0375(10) Uani 1 1 d . . .
H27 H 0.3258 0.1840 0.9502 0.045 Uiso 1 1 calc R . .
C28 C 0.2062(4) 0.1529(4) 0.8501(3) 0.0442(12) Uani 1 1 d . . .
H28 H 0.1550 0.0767 0.8599 0.053 Uiso 1 1 calc R . .
C29 C 0.1796(4) 0.2010(4) 0.7818(3) 0.0408(11) Uani 1 1 d . . .
H29 H 0.1110 0.1570 0.7454 0.049 Uiso 1 1 calc R . .
C30 C 0.2548(4) 0.3149(3) 0.7670(2) 0.0302(9) Uani 1 1 d . . .
H30 H 0.2356 0.3469 0.7206 0.036 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
K1 O4 2.713(3) . ?
K1 O6 2.741(3) . ?
K1 O2 2.805(3) . ?
K1 O1 2.856(3) . ?
K1 O5 2.905(3) . ?
K1 O3 2.945(3) . ?
K1 S1 3.143(2) . ?
K1 C8 3.517(4) . ?
S1 Si1 2.039(2) . ?
Si1 C25 1.884(4) . ?
Si1 C19 1.886(4) . ?
Si1 C13 1.890(4) . ?
O1 C12 1.429(4) . ?
O1 C1 1.434(4) . ?
O2 C2 1.413(4) . ?
O2 C3 1.419(4) . ?
O3 C4 1.424(4) . ?
O3 C5 1.430(4) . ?
O4 C7 1.417(4) . ?
O4 C6 1.420(4) . ?
O5 C8 1.413(4) . ?
O5 C9 1.415(4) . ?
O6 C11 1.409(4) . ?
O6 C10 1.426(4) . ?
C1 C2 1.485(5) . ?
C3 C4 1.504(5) . ?
C5 C6 1.482(5) . ?
C7 C8 1.489(5) . ?
C9 C10 1.461(6) . ?
C11 C12 1.497(5) . ?
C13 C14 1.388(5) . ?
C13 C18 1.389(5) . ?
C14 C15 1.391(5) . ?
C15 C16 1.370(5) . ?
C16 C17 1.384(5) . ?
C17 C18 1.378(5) . ?
C19 C24 1.394(5) . ?
C19 C20 1.398(5) . ?
C20 C21 1.385(5) . ?
C21 C22 1.377(5) . ?
C22 C23 1.378(6) . ?
C23 C24 1.384(5) . ?
C25 C26 1.390(5) . ?
C25 C30 1.394(5) . ?
C26 C27 1.386(5) . ?
C27 C28 1.371(6) . ?
C28 C29 1.373(6) . ?
C29 C30 1.384(5) . ?

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
O4 K1 O6 119.29(8) . . ?
O4 K1 O2 117.51(8) . . ?
O6 K1 O2 118.85(8) . . ?
O4 K1 O1 160.52(8) . . ?
O6 K1 O1 59.89(8) . . ?
O2 K1 O1 58.97(8) . . ?
O4 K1 O5 59.79(8) . . ?
O6 K1 O5 59.50(8) . . ?
O2 K1 O5 159.04(8) . . ?
O1 K1 O5 115.71(9) . . ?
O4 K1 O3 59.19(8) . . ?
O6 K1 O3 158.04(8) . . ?
O2 K1 O3 58.35(8) . . ?
O1 K1 O3 113.41(9) . . ?
O5 K1 O3 114.35(9) . . ?
O4 K1 S1 112.12(8) . . ?
O6 K1 S1 76.96(7) . . ?
O2 K1 S1 101.18(7) . . ?
O1 K1 S1 87.04(8) . . ?
O5 K1 S1 98.63(7) . . ?
O3 K1 S1 124.75(7) . . ?
O4 K1 C8 42.09(9) . . ?
O6 K1 C8 79.07(9) . . ?
O2 K1 C8 159.29(9) . . ?
O1 K1 C8 137.94(10) . . ?
O5 K1 C8 22.99(8) . . ?
O3 K1 C8 101.08(10) . . ?
S1 K1 C8 92.70(9) . . ?
Si1 S1 K1 107.03(5) . . ?
C25 Si1 C19 103.81(15) . . ?
C25 Si1 C13 106.81(15) . . ?
C19 Si1 C13 106.17(15) . . ?
C25 Si1 S1 114.07(12) . . ?
C19 Si1 S1 112.71(12) . . ?
C13 Si1 S1 112.55(12) . . ?
C12 O1 C1 111.1(3) . . ?
C12 O1 K1 106.84(19) . . ?
C1 O1 K1 109.2(2) . . ?
C2 O2 C3 112.2(3) . . ?
C2 O2 K1 119.3(2) . . ?
C3 O2 K1 121.0(2) . . ?
C4 O3 C5 111.9(3) . . ?
C4 O3 K1 108.9(2) . . ?
C5 O3 K1 105.6(2) . . ?
C7 O4 C6 112.3(3) . . ?
C7 O4 K1 120.7(2) . . ?
C6 O4 K1 122.7(2) . . ?
C8 O5 C9 113.1(3) . . ?
C8 O5 K1 103.6(2) . . ?
C9 O5 K1 108.0(2) . . ?
C11 O6 C10 112.5(3) . . ?
C11 O6 K1 119.9(2) . . ?
C10 O6 K1 119.7(2) . . ?
O1 C1 C2 108.1(3) . . ?
O2 C2 C1 108.6(3) . . ?
O2 C3 C4 107.8(3) . . ?
O3 C4 C3 108.7(3) . . ?
O3 C5 C6 109.7(3) . . ?
O4 C6 C5 108.0(3) . . ?
O4 C7 C8 108.6(3) . . ?
O5 C8 C7 109.0(3) . . ?
O5 C8 K1 53.39(17) . . ?
C7 C8 K1 82.9(2) . . ?
O5 C9 C10 110.1(3) . . ?
O6 C10 C9 108.0(3) . . ?
O6 C11 C12 107.9(3) . . ?
O1 C12 C11 108.2(3) . . ?
C14 C13 C18 116.9(3) . . ?
C14 C13 Si1 125.1(3) . . ?
C18 C13 Si1 118.0(3) . . ?
C13 C14 C15 121.5(3) . . ?
C16 C15 C14 119.9(3) . . ?
C15 C16 C17 120.0(3) . . ?
C18 C17 C16 119.2(3) . . ?
C17 C18 C13 122.5(3) . . ?
C24 C19 C20 116.8(3) . . ?
C24 C19 Si1 119.4(3) . . ?
C20 C19 Si1 123.8(3) . . ?
C21 C20 C19 121.5(3) . . ?
C22 C21 C20 120.2(4) . . ?
C21 C22 C23 119.7(3) . . ?
C22 C23 C24 119.8(4) . . ?
C23 C24 C19 122.0(4) . . ?
C26 C25 C30 117.0(3) . . ?
C26 C25 Si1 120.4(3) . . ?
C30 C25 Si1 122.6(3) . . ?
C27 C26 C25 122.2(4) . . ?
C28 C27 C26 119.2(4) . . ?
C27 C28 C29 120.4(4) . . ?
C28 C29 C30 120.1(4) . . ?
C29 C30 C25 121.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.081
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dq0089
_database_code_depnum_ccdc_archive 'CCDC 1436080'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H47 K O7 Se Si'
_chemical_formula_weight         713.87

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2695(5)
_cell_length_b                   10.3732(6)
_cell_length_c                   18.6978(11)
_cell_angle_alpha                98.7616(12)
_cell_angle_beta                 93.9586(12)
_cell_angle_gamma                95.8326(12)
_cell_volume                     1761.15(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       slab
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7349
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37364
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         32.63
_reflns_number_total             12746
_reflns_number_gt                10638
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0281P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12746
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_restrained_S_all      1.247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Se1 Se -0.075500(12) 0.051901(11) 0.196478(6) 0.01453(3) Uani 1 1 d . . .
K1 K 0.20018(2) 0.27303(2) 0.173786(12) 0.01313(5) Uani 1 1 d . . .
Si1 Si -0.04008(3) 0.01978(3) 0.309092(15) 0.00977(6) Uani 1 1 d . . .
O1 O 0.05707(9) 0.21610(8) 0.03584(4) 0.01499(15) Uani 1 1 d . . .
O2 O -0.01374(9) 0.43787(8) 0.13176(4) 0.01679(16) Uani 1 1 d . . .
O3 O 0.13586(9) 0.48678(7) 0.27076(4) 0.01520(15) Uani 1 1 d . . .
O4 O 0.40588(9) 0.39648(8) 0.29980(4) 0.01618(16) Uani 1 1 d . . .
O5 O 0.45593(9) 0.17132(8) 0.20336(4) 0.01800(16) Uani 1 1 d . . .
O6 O 0.33277(9) 0.12036(7) 0.05939(4) 0.01659(16) Uani 1 1 d . . .
O7 O 0.34396(9) 0.46030(8) 0.10243(5) 0.02238(18) Uani 1 1 d . . .
C1 C -0.09493(11) 0.15792(10) 0.37631(5) 0.01059(18) Uani 1 1 d . . .
C2 C -0.05491(12) 0.28721(11) 0.36624(6) 0.0148(2) Uani 1 1 d . . .
H2 H -0.0006 0.3024 0.3265 0.018 Uiso 1 1 calc R . .
C3 C -0.09215(13) 0.39368(11) 0.41261(6) 0.0176(2) Uani 1 1 d . . .
H3 H -0.0620 0.4805 0.4049 0.021 Uiso 1 1 calc R . .
C4 C -0.17375(13) 0.37343(11) 0.47046(6) 0.0175(2) Uani 1 1 d . . .
H4 H -0.2003 0.4461 0.5022 0.021 Uiso 1 1 calc R . .
C5 C -0.21579(13) 0.24707(11) 0.48139(6) 0.0167(2) Uani 1 1 d . . .
H5 H -0.2722 0.2326 0.5206 0.020 Uiso 1 1 calc R . .
C6 C -0.17592(12) 0.14059(10) 0.43529(6) 0.0135(2) Uani 1 1 d . . .
H6 H -0.2043 0.0542 0.4440 0.016 Uiso 1 1 calc R . .
C7 C -0.14387(11) -0.13449(10) 0.33017(6) 0.01176(19) Uani 1 1 d . . .
C8 C -0.25702(12) -0.20701(11) 0.28320(6) 0.0156(2) Uani 1 1 d . . .
H8 H -0.2809 -0.1809 0.2377 0.019 Uiso 1 1 calc R . .
C9 C -0.33568(13) -0.31709(11) 0.30182(7) 0.0201(2) Uani 1 1 d . . .
H9 H -0.4123 -0.3652 0.2691 0.024 Uiso 1 1 calc R . .
C10 C -0.30218(13) -0.35646(11) 0.36800(7) 0.0216(2) Uani 1 1 d . . .
H10 H -0.3559 -0.4314 0.3807 0.026 Uiso 1 1 calc R . .
C11 C -0.19003(14) -0.28615(11) 0.41563(7) 0.0194(2) Uani 1 1 d . . .
H11 H -0.1672 -0.3124 0.4612 0.023 Uiso 1 1 calc R . .
C12 C -0.11139(13) -0.17730(11) 0.39647(6) 0.0152(2) Uani 1 1 d . . .
H12 H -0.0337 -0.1307 0.4290 0.018 Uiso 1 1 calc R . .
C13 C 0.15679(11) 0.00368(10) 0.33604(6) 0.01166(19) Uani 1 1 d . . .
C14 C 0.22306(12) 0.04949(11) 0.40608(6) 0.0146(2) Uani 1 1 d . . .
H14 H 0.1692 0.0949 0.4412 0.017 Uiso 1 1 calc R . .
C15 C 0.36583(13) 0.03008(12) 0.42548(6) 0.0185(2) Uani 1 1 d . . .
H15 H 0.4086 0.0628 0.4733 0.022 Uiso 1 1 calc R . .
C16 C 0.44571(13) -0.03707(12) 0.37510(7) 0.0208(2) Uani 1 1 d . . .
H16 H 0.5427 -0.0518 0.3884 0.025 Uiso 1 1 calc R . .
C17 C 0.38296(13) -0.08259(12) 0.30518(7) 0.0193(2) Uani 1 1 d . . .
H17 H 0.4375 -0.1279 0.2703 0.023 Uiso 1 1 calc R . .
C18 C 0.24075(12) -0.06213(11) 0.28600(6) 0.0155(2) Uani 1 1 d . . .
H18 H 0.1994 -0.0935 0.2378 0.019 Uiso 1 1 calc R . .
C19 C -0.03211(14) 0.30859(12) 0.01452(6) 0.0203(2) Uani 1 1 d . . .
H19A H -0.1014 0.2667 -0.0272 0.024 Uiso 1 1 calc R . .
H19B H 0.0286 0.3822 -0.0006 0.024 Uiso 1 1 calc R . .
C20 C -0.11386(13) 0.35893(12) 0.07754(7) 0.0218(2) Uani 1 1 d . . .
H20A H -0.1895 0.4116 0.0614 0.026 Uiso 1 1 calc R . .
H20B H -0.1624 0.2844 0.0975 0.026 Uiso 1 1 calc R . .
C21 C -0.08146(13) 0.48091(13) 0.19575(7) 0.0211(2) Uani 1 1 d . . .
H21A H -0.1213 0.4042 0.2168 0.025 Uiso 1 1 calc R . .
H21B H -0.1627 0.5311 0.1839 0.025 Uiso 1 1 calc R . .
C22 C 0.02956(13) 0.56633(12) 0.24959(6) 0.0192(2) Uani 1 1 d . . .
H22A H 0.0759 0.6389 0.2273 0.023 Uiso 1 1 calc R . .
H22B H -0.0176 0.6047 0.2925 0.023 Uiso 1 1 calc R . .
C23 C 0.23959(13) 0.55440(11) 0.32714(6) 0.0182(2) Uani 1 1 d . . .
H23A H 0.1893 0.6009 0.3666 0.022 Uiso 1 1 calc R . .
H23B H 0.3051 0.6200 0.3080 0.022 Uiso 1 1 calc R . .
C24 C 0.32575(13) 0.45546(12) 0.35560(6) 0.0193(2) Uani 1 1 d . . .
H24A H 0.3933 0.4991 0.3976 0.023 Uiso 1 1 calc R . .
H24B H 0.2592 0.3873 0.3721 0.023 Uiso 1 1 calc R . .
C25 C 0.47910(13) 0.29235(12) 0.32244(6) 0.0194(2) Uani 1 1 d . . .
H25A H 0.4073 0.2251 0.3362 0.023 Uiso 1 1 calc R . .
H25B H 0.5482 0.3273 0.3654 0.023 Uiso 1 1 calc R . .
C26 C 0.55928(12) 0.23189(12) 0.26180(7) 0.0196(2) Uani 1 1 d . . .
H26A H 0.6261 0.3001 0.2455 0.024 Uiso 1 1 calc R . .
H26B H 0.6177 0.1656 0.2784 0.024 Uiso 1 1 calc R . .
C27 C 0.52027(13) 0.09417(12) 0.14735(7) 0.0208(2) Uani 1 1 d . . .
H27A H 0.5750 0.0292 0.1679 0.025 Uiso 1 1 calc R . .
H27B H 0.5889 0.1511 0.1242 0.025 Uiso 1 1 calc R . .
C28 C 0.40126(13) 0.02503(11) 0.09223(7) 0.0198(2) Uani 1 1 d . . .
H28A H 0.4424 -0.0354 0.0548 0.024 Uiso 1 1 calc R . .
H28B H 0.3292 -0.0272 0.1161 0.024 Uiso 1 1 calc R . .
C29 C 0.22230(13) 0.06182(12) 0.00388(7) 0.0214(2) Uani 1 1 d . . .
H29A H 0.1541 -0.0019 0.0229 0.026 Uiso 1 1 calc R . .
H29B H 0.2667 0.0143 -0.0375 0.026 Uiso 1 1 calc R . .
C30 C 0.14197(13) 0.16745(12) -0.02077(6) 0.0196(2) Uani 1 1 d . . .
H30A H 0.2117 0.2393 -0.0316 0.024 Uiso 1 1 calc R . .
H30B H 0.0781 0.1316 -0.0655 0.024 Uiso 1 1 calc R . .
C31 C 0.32466(14) 0.59413(12) 0.12754(7) 0.0231(3) Uani 1 1 d . . .
H31A H 0.3341 0.6130 0.1813 0.028 Uiso 1 1 calc R . .
H31B H 0.2277 0.6141 0.1096 0.028 Uiso 1 1 calc R . .
C32 C 0.44494(14) 0.67395(12) 0.09664(7) 0.0223(2) Uani 1 1 d . . .
H32A H 0.4768 0.7580 0.1292 0.027 Uiso 1 1 calc R . .
H32B H 0.4124 0.6925 0.0481 0.027 Uiso 1 1 calc R . .
C33 C 0.56776(13) 0.58452(12) 0.09191(7) 0.0191(2) Uani 1 1 d . . .
H33A H 0.6009 0.5712 0.0424 0.023 Uiso 1 1 calc R . .
H33B H 0.6518 0.6222 0.1270 0.023 Uiso 1 1 calc R . .
C34 C 0.49721(13) 0.45541(12) 0.11095(7) 0.0205(2) Uani 1 1 d . . .
H34A H 0.5250 0.3796 0.0780 0.025 Uiso 1 1 calc R . .
H34B H 0.5285 0.4470 0.1616 0.025 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Se1 Si1 2.1893(3) . ?
Se1 K1 3.3506(3) . ?
K1 O5 2.7467(8) . ?
K1 O1 2.7687(8) . ?
K1 O3 2.7843(8) . ?
K1 O7 2.7998(9) . ?
K1 O6 2.8845(8) . ?
K1 O2 2.8908(8) . ?
K1 O4 2.9651(8) . ?
Si1 C13 1.8902(11) . ?
Si1 C7 1.8904(11) . ?
Si1 C1 1.8918(11) . ?
O1 C19 1.4124(13) . ?
O1 C30 1.4238(13) . ?
O2 C20 1.4221(14) . ?
O2 C21 1.4223(13) . ?
O3 C22 1.4211(14) . ?
O3 C23 1.4233(14) . ?
O4 C24 1.4210(14) . ?
O4 C25 1.4336(14) . ?
O5 C27 1.4216(14) . ?
O5 C26 1.4249(14) . ?
O6 C28 1.4201(13) . ?
O6 C29 1.4245(14) . ?
O7 C34 1.4255(14) . ?
O7 C31 1.4294(15) . ?
C1 C2 1.3990(14) . ?
C1 C6 1.3997(14) . ?
C2 C3 1.3849(15) . ?
C3 C4 1.3914(16) . ?
C4 C5 1.3786(16) . ?
C5 C6 1.3916(15) . ?
C7 C8 1.3959(15) . ?
C7 C12 1.4028(15) . ?
C8 C9 1.3941(16) . ?
C9 C10 1.3860(18) . ?
C10 C11 1.3878(18) . ?
C11 C12 1.3880(15) . ?
C13 C14 1.3994(15) . ?
C13 C18 1.4003(15) . ?
C14 C15 1.3906(16) . ?
C15 C16 1.3864(17) . ?
C16 C17 1.3861(17) . ?
C17 C18 1.3879(16) . ?
C19 C20 1.5005(17) . ?
C21 C22 1.5024(17) . ?
C23 C24 1.4996(17) . ?
C25 C26 1.4918(17) . ?
C27 C28 1.5002(17) . ?
C29 C30 1.4966(17) . ?
C31 C32 1.5197(17) . ?
C32 C33 1.5389(17) . ?
C33 C34 1.5321(16) . ?

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
Si1 Se1 K1 105.236(9) . . ?
O5 K1 O1 120.33(2) . . ?
O5 K1 O3 117.38(2) . . ?
O1 K1 O3 119.86(2) . . ?
O5 K1 O7 91.22(3) . . ?
O1 K1 O7 77.89(3) . . ?
O3 K1 O7 85.56(3) . . ?
O5 K1 O6 59.61(2) . . ?
O1 K1 O6 60.85(2) . . ?
O3 K1 O6 160.64(2) . . ?
O7 K1 O6 75.60(2) . . ?
O5 K1 O2 163.93(3) . . ?
O1 K1 O2 60.55(2) . . ?
O3 K1 O2 59.31(2) . . ?
O7 K1 O2 73.07(2) . . ?
O6 K1 O2 117.54(2) . . ?
O5 K1 O4 59.12(2) . . ?
O1 K1 O4 161.96(2) . . ?
O3 K1 O4 58.35(2) . . ?
O7 K1 O4 84.07(2) . . ?
O6 K1 O4 114.23(2) . . ?
O2 K1 O4 114.47(2) . . ?
O5 K1 Se1 107.945(19) . . ?
O1 K1 Se1 78.128(18) . . ?
O3 K1 Se1 99.431(18) . . ?
O7 K1 Se1 154.66(2) . . ?
O6 K1 Se1 99.522(17) . . ?
O2 K1 Se1 88.062(18) . . ?
O4 K1 Se1 119.771(17) . . ?
C13 Si1 C7 104.47(5) . . ?
C13 Si1 C1 106.69(5) . . ?
C7 Si1 C1 105.13(5) . . ?
C13 Si1 Se1 112.53(3) . . ?
C7 Si1 Se1 114.75(4) . . ?
C1 Si1 Se1 112.53(3) . . ?
C19 O1 C30 111.79(9) . . ?
C19 O1 K1 117.33(6) . . ?
C30 O1 K1 115.75(6) . . ?
C20 O2 C21 111.93(9) . . ?
C20 O2 K1 107.12(6) . . ?
C21 O2 K1 106.07(6) . . ?
C22 O3 C23 112.95(9) . . ?
C22 O3 K1 120.10(6) . . ?
C23 O3 K1 121.88(6) . . ?
C24 O4 C25 111.36(9) . . ?
C24 O4 K1 108.89(6) . . ?
C25 O4 K1 105.95(6) . . ?
C27 O5 C26 112.60(9) . . ?
C27 O5 K1 120.53(7) . . ?
C26 O5 K1 121.95(7) . . ?
C28 O6 C29 112.11(9) . . ?
C28 O6 K1 105.96(6) . . ?
C29 O6 K1 108.78(6) . . ?
C34 O7 C31 104.93(9) . . ?
C34 O7 K1 110.04(6) . . ?
C31 O7 K1 116.13(7) . . ?
C2 C1 C6 116.92(9) . . ?
C2 C1 Si1 118.36(8) . . ?
C6 C1 Si1 124.70(8) . . ?
C3 C2 C1 121.88(10) . . ?
C2 C3 C4 119.93(10) . . ?
C5 C4 C3 119.49(10) . . ?
C4 C5 C6 120.27(10) . . ?
C5 C6 C1 121.50(10) . . ?
C8 C7 C12 117.50(10) . . ?
C8 C7 Si1 122.66(8) . . ?
C12 C7 Si1 119.81(8) . . ?
C9 C8 C7 121.22(11) . . ?
C10 C9 C8 120.06(11) . . ?
C9 C10 C11 119.84(11) . . ?
C10 C11 C12 119.77(11) . . ?
C11 C12 C7 121.59(11) . . ?
C14 C13 C18 117.12(10) . . ?
C14 C13 Si1 122.83(8) . . ?
C18 C13 Si1 119.97(8) . . ?
C15 C14 C13 121.61(10) . . ?
C16 C15 C14 120.01(11) . . ?
C17 C16 C15 119.51(11) . . ?
C16 C17 C18 120.20(11) . . ?
C17 C18 C13 121.54(11) . . ?
O1 C19 C20 108.75(9) . . ?
O2 C20 C19 108.66(10) . . ?
O2 C21 C22 108.91(10) . . ?
O3 C22 C21 107.88(9) . . ?
O3 C23 C24 108.20(9) . . ?
O4 C24 C23 109.46(9) . . ?
O4 C25 C26 109.45(9) . . ?
O5 C26 C25 108.53(9) . . ?
O5 C27 C28 108.36(9) . . ?
O6 C28 C27 108.75(9) . . ?
O6 C29 C30 108.84(9) . . ?
O1 C30 C29 108.19(10) . . ?
O7 C31 C32 104.84(10) . . ?
C31 C32 C33 103.43(9) . . ?
C34 C33 C32 103.74(9) . . ?
O7 C34 C33 106.14(9) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.062
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_apx2159
_database_code_depnum_ccdc_archive 'CCDC 1436081'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H47 K O7 Si Te'
_chemical_formula_weight         762.50

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2562(19)
_cell_length_b                   10.431(2)
_cell_length_c                   19.332(4)
_cell_angle_alpha                99.814(2)
_cell_angle_beta                 93.297(2)
_cell_angle_gamma                96.939(2)
_cell_volume                     1820.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    9869
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.007
_shelx_estimated_absorpt_T_min   0.677
_shelx_estimated_absorpt_T_max   0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21415
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.999
_diffrn_reflns_theta_max         28.688
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8616
_reflns_number_gt                7965
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0281P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8616
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0585
_refine_ls_wR_factor_gt          0.0571
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te -0.08209(2) 0.02412(2) 0.19338(2) 0.01931(4) Uani 1 1 d . . . . .
K1 K 0.19865(4) 0.28413(3) 0.17853(2) 0.01731(7) Uani 1 1 d . . . . .
Si1 Si -0.04068(4) 0.00480(4) 0.31575(2) 0.01207(8) Uani 1 1 d . . . . .
O1 O 0.05356(12) 0.22585(11) 0.04469(5) 0.0204(2) Uani 1 1 d . . . . .
O2 O -0.01541(12) 0.44314(11) 0.14163(6) 0.0223(2) Uani 1 1 d . . . . .
O3 O 0.12699(12) 0.48783(10) 0.27750(6) 0.0195(2) Uani 1 1 d . . . . .
O4 O 0.39569(12) 0.39645(11) 0.30391(6) 0.0209(2) Uani 1 1 d . . . . .
O5 O 0.44434(12) 0.17395(11) 0.20735(6) 0.0240(2) Uani 1 1 d . . . . .
O6 O 0.32663(13) 0.13002(11) 0.06759(6) 0.0235(2) Uani 1 1 d . . . . .
O7 O 0.34424(14) 0.47386(12) 0.11226(7) 0.0345(3) Uani 1 1 d . . . . .
C1 C -0.09559(15) 0.14777(14) 0.37824(7) 0.0131(3) Uani 1 1 d . . . . .
C2 C -0.05836(17) 0.27583(15) 0.36553(8) 0.0178(3) Uani 1 1 d . . . . .
H2 H -0.0072 0.2885 0.3255 0.021 Uiso 1 1 calc R U . . .
C3 C -0.09443(18) 0.38408(15) 0.40996(8) 0.0213(3) Uani 1 1 d . . . . .
H3 H -0.0657 0.4698 0.4009 0.026 Uiso 1 1 calc R U . . .
C4 C -0.17253(18) 0.36752(15) 0.46768(8) 0.0213(3) Uani 1 1 d . . . . .
H4 H -0.1986 0.4417 0.4978 0.026 Uiso 1 1 calc R U . . .
C5 C -0.21210(17) 0.24294(15) 0.48119(8) 0.0193(3) Uani 1 1 d . . . . .
H5 H -0.2659 0.2311 0.5205 0.023 Uiso 1 1 calc R U . . .
C6 C -0.17291(16) 0.13410(14) 0.43692(8) 0.0156(3) Uani 1 1 d . . . . .
H6 H -0.1996 0.0489 0.4471 0.019 Uiso 1 1 calc R U . . .
C7 C -0.14487(15) -0.14668(14) 0.33969(8) 0.0144(3) Uani 1 1 d . . . . .
C8 C -0.26254(16) -0.22150(15) 0.29728(9) 0.0190(3) Uani 1 1 d . . . . .
H8 H -0.2901 -0.1982 0.2534 0.023 Uiso 1 1 calc R U . . .
C9 C -0.34054(18) -0.32951(16) 0.31772(10) 0.0264(4) Uani 1 1 d . . . . .
H9 H -0.4200 -0.3796 0.2879 0.032 Uiso 1 1 calc R U . . .
C10 C -0.30199(18) -0.36387(16) 0.38178(10) 0.0276(4) Uani 1 1 d . . . . .
H10 H -0.3558 -0.4370 0.3961 0.033 Uiso 1 1 calc R U . . .
C11 C -0.18519(19) -0.29174(15) 0.42490(9) 0.0236(3) Uani 1 1 d . . . . .
H11 H -0.1586 -0.3153 0.4688 0.028 Uiso 1 1 calc R U . . .
C12 C -0.10699(17) -0.18486(14) 0.40378(8) 0.0181(3) Uani 1 1 d . . . . .
H12 H -0.0261 -0.1366 0.4334 0.022 Uiso 1 1 calc R U . . .
C13 C 0.15814(15) -0.00407(14) 0.34092(8) 0.0137(3) Uani 1 1 d . . . . .
C14 C 0.22284(17) 0.04617(15) 0.40892(8) 0.0177(3) Uani 1 1 d . . . . .
H14 H 0.1670 0.0900 0.4430 0.021 Uiso 1 1 calc R U . . .
C15 C 0.36699(18) 0.03337(16) 0.42776(9) 0.0230(3) Uani 1 1 d . . . . .
H15 H 0.4087 0.0688 0.4741 0.028 Uiso 1 1 calc R U . . .
C16 C 0.44960(17) -0.03085(17) 0.37901(9) 0.0250(4) Uani 1 1 d . . . . .
H16 H 0.5478 -0.0405 0.3919 0.030 Uiso 1 1 calc R U . . .
C17 C 0.38848(17) -0.08094(16) 0.31136(9) 0.0232(3) Uani 1 1 d . . . . .
H17 H 0.4447 -0.1254 0.2778 0.028 Uiso 1 1 calc R U . . .
C18 C 0.24499(16) -0.06643(15) 0.29243(8) 0.0185(3) Uani 1 1 d . . . . .
H18 H 0.2051 -0.0996 0.2455 0.022 Uiso 1 1 calc R U . . .
C19 C -0.0312(2) 0.32069(18) 0.02614(9) 0.0301(4) Uani 1 1 d . . . . .
H19A H -0.0993 0.2815 -0.0155 0.036 Uiso 1 1 calc R U . . .
H19B H 0.0332 0.3953 0.0141 0.036 Uiso 1 1 calc R U . . .
C20 C -0.11528(19) 0.36800(19) 0.08707(9) 0.0309(4) Uani 1 1 d . . . . .
H20A H -0.1878 0.4226 0.0725 0.037 Uiso 1 1 calc R U . . .
H20B H -0.1680 0.2923 0.1039 0.037 Uiso 1 1 calc R U . . .
C21 C -0.08549(18) 0.48782(18) 0.20327(9) 0.0270(4) Uani 1 1 d . . . . .
H21A H -0.1318 0.4118 0.2221 0.032 Uiso 1 1 calc R U . . .
H21B H -0.1625 0.5406 0.1916 0.032 Uiso 1 1 calc R U . . .
C22 C 0.02632(19) 0.56979(16) 0.25725(9) 0.0251(4) Uani 1 1 d . . . . .
H22A H 0.0780 0.6420 0.2372 0.030 Uiso 1 1 calc R U . . .
H22B H -0.0217 0.6087 0.2988 0.030 Uiso 1 1 calc R U . . .
C23 C 0.23299(18) 0.55527(16) 0.33181(9) 0.0243(4) Uani 1 1 d . . . . .
H23A H 0.1843 0.6030 0.3706 0.029 Uiso 1 1 calc R U . . .
H23B H 0.3005 0.6198 0.3132 0.029 Uiso 1 1 calc R U . . .
C24 C 0.31652(18) 0.45640(18) 0.35858(8) 0.0260(4) Uani 1 1 d . . . . .
H24A H 0.3849 0.5004 0.3993 0.031 Uiso 1 1 calc R U . . .
H24B H 0.2481 0.3887 0.3743 0.031 Uiso 1 1 calc R U . . .
C25 C 0.46618(19) 0.29249(16) 0.32428(9) 0.0254(4) Uani 1 1 d . . . . .
H25A H 0.3925 0.2245 0.3363 0.030 Uiso 1 1 calc R U . . .
H25B H 0.5347 0.3270 0.3664 0.030 Uiso 1 1 calc R U . . .
C26 C 0.54777(18) 0.23356(17) 0.26474(9) 0.0262(4) Uani 1 1 d . . . . .
H26A H 0.6166 0.3025 0.2503 0.031 Uiso 1 1 calc R U . . .
H26B H 0.6045 0.1670 0.2797 0.031 Uiso 1 1 calc R U . . .
C27 C 0.50963(19) 0.09922(17) 0.15181(10) 0.0282(4) Uani 1 1 d . . . . .
H27A H 0.5618 0.0330 0.1702 0.034 Uiso 1 1 calc R U . . .
H27B H 0.5810 0.1575 0.1312 0.034 Uiso 1 1 calc R U . . .
C28 C 0.39143(19) 0.03252(16) 0.09672(10) 0.0280(4) Uani 1 1 d . . . . .
H28A H 0.4330 -0.0259 0.0593 0.034 Uiso 1 1 calc R U . . .
H28B H 0.3169 -0.0215 0.1180 0.034 Uiso 1 1 calc R U . . .
C29 C 0.2185(2) 0.07447(18) 0.01145(9) 0.0308(4) Uani 1 1 d . . . . .
H29A H 0.1471 0.0088 0.0270 0.037 Uiso 1 1 calc R U . . .
H29B H 0.2651 0.0298 -0.0291 0.037 Uiso 1 1 calc R U . . .
C30 C 0.1429(2) 0.18164(18) -0.00972(9) 0.0281(4) Uani 1 1 d . . . . .
H30A H 0.2156 0.2550 -0.0168 0.034 Uiso 1 1 calc R U . . .
H30B H 0.0820 0.1487 -0.0545 0.034 Uiso 1 1 calc R U . . .
C31 C 0.3307(2) 0.60840(19) 0.13309(11) 0.0361(4) Uani 1 1 d . . . . .
H31A H 0.3456 0.6346 0.1849 0.043 Uiso 1 1 calc R U . . .
H31B H 0.2330 0.6269 0.1172 0.043 Uiso 1 1 calc R U . . .
C32 C 0.4490(2) 0.68102(19) 0.09774(11) 0.0361(4) Uani 1 1 d . . . . .
H32A H 0.4855 0.7681 0.1264 0.043 Uiso 1 1 calc R U . . .
H32B H 0.4125 0.6928 0.0504 0.043 Uiso 1 1 calc R U . . .
C33 C 0.56862(19) 0.59108(17) 0.09285(10) 0.0282(4) Uani 1 1 d . . . . .
H33A H 0.5984 0.5724 0.0442 0.034 Uiso 1 1 calc R U . . .
H33B H 0.6554 0.6313 0.1250 0.034 Uiso 1 1 calc R U . . .
C34 C 0.49697(19) 0.46600(17) 0.11505(10) 0.0297(4) Uani 1 1 d . . . . .
H34A H 0.5175 0.3873 0.0826 0.036 Uiso 1 1 calc R U . . .
H34B H 0.5344 0.4608 0.1634 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Te1 Si1 2.4210(6) . ?
Te1 K1 3.5832(6) . ?
K1 O5 2.7398(12) . ?
K1 O3 2.7778(12) . ?
K1 O1 2.7812(12) . ?
K1 O7 2.7917(13) . ?
K1 O6 2.8573(12) . ?
K1 O2 2.8672(12) . ?
K1 O4 2.9293(12) . ?
Si1 C7 1.8903(15) . ?
Si1 C1 1.8925(15) . ?
Si1 C13 1.8935(15) . ?
O1 C19 1.414(2) . ?
O1 C30 1.4248(19) . ?
O2 C20 1.419(2) . ?
O2 C21 1.4250(19) . ?
O3 C22 1.4202(19) . ?
O3 C23 1.4222(19) . ?
O4 C24 1.421(2) . ?
O4 C25 1.430(2) . ?
O5 C27 1.424(2) . ?
O5 C26 1.4258(19) . ?
O6 C28 1.419(2) . ?
O6 C29 1.427(2) . ?
O7 C31 1.415(2) . ?
O7 C34 1.424(2) . ?
C1 C6 1.394(2) . ?
C1 C2 1.405(2) . ?
C2 C3 1.385(2) . ?
C3 C4 1.388(2) . ?
C4 C5 1.379(2) . ?
C5 C6 1.399(2) . ?
C7 C8 1.393(2) . ?
C7 C12 1.403(2) . ?
C8 C9 1.391(2) . ?
C9 C10 1.386(3) . ?
C10 C11 1.384(2) . ?
C11 C12 1.388(2) . ?
C13 C18 1.398(2) . ?
C13 C14 1.400(2) . ?
C14 C15 1.391(2) . ?
C15 C16 1.383(2) . ?
C16 C17 1.383(2) . ?
C17 C18 1.390(2) . ?
C19 C20 1.495(2) . ?
C21 C22 1.500(2) . ?
C23 C24 1.503(2) . ?
C25 C26 1.498(2) . ?
C27 C28 1.498(2) . ?
C29 C30 1.490(2) . ?
C31 C32 1.517(3) . ?
C32 C33 1.532(3) . ?
C33 C34 1.530(2) . ?

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
Si1 Te1 K1 101.588(12) . . ?
O5 K1 O3 118.37(4) . . ?
O5 K1 O1 120.65(4) . . ?
O3 K1 O1 120.07(3) . . ?
O5 K1 O7 94.46(4) . . ?
O3 K1 O7 87.83(4) . . ?
O1 K1 O7 78.38(4) . . ?
O5 K1 O6 59.89(4) . . ?
O3 K1 O6 164.52(3) . . ?
O1 K1 O6 61.09(3) . . ?
O7 K1 O6 77.20(4) . . ?
O5 K1 O2 167.89(4) . . ?
O3 K1 O2 59.65(3) . . ?
O1 K1 O2 60.47(3) . . ?
O7 K1 O2 73.73(4) . . ?
O6 K1 O2 118.35(3) . . ?
O5 K1 O4 59.52(3) . . ?
O3 K1 O4 59.13(3) . . ?
O1 K1 O4 165.36(3) . . ?
O7 K1 O4 86.99(4) . . ?
O6 K1 O4 115.34(4) . . ?
O2 K1 O4 115.96(3) . . ?
O5 K1 Te1 101.09(3) . . ?
O3 K1 Te1 101.37(3) . . ?
O1 K1 Te1 77.05(3) . . ?
O7 K1 Te1 155.16(3) . . ?
O6 K1 Te1 93.94(3) . . ?
O2 K1 Te1 90.94(3) . . ?
O4 K1 Te1 117.59(2) . . ?
C7 Si1 C1 105.27(6) . . ?
C7 Si1 C13 105.33(6) . . ?
C1 Si1 C13 106.89(6) . . ?
C7 Si1 Te1 114.08(5) . . ?
C1 Si1 Te1 112.64(5) . . ?
C13 Si1 Te1 112.00(5) . . ?
C19 O1 C30 111.92(12) . . ?
C19 O1 K1 116.23(9) . . ?
C30 O1 K1 113.92(9) . . ?
C20 O2 C21 112.24(13) . . ?
C20 O2 K1 109.03(9) . . ?
C21 O2 K1 108.24(9) . . ?
C22 O3 C23 112.52(12) . . ?
C22 O3 K1 119.52(9) . . ?
C23 O3 K1 120.07(9) . . ?
C24 O4 C25 111.82(13) . . ?
C24 O4 K1 110.32(9) . . ?
C25 O4 K1 107.48(9) . . ?
C27 O5 C26 112.31(13) . . ?
C27 O5 K1 120.06(9) . . ?
C26 O5 K1 121.23(9) . . ?
C28 O6 C29 112.21(13) . . ?
C28 O6 K1 107.48(9) . . ?
C29 O6 K1 110.15(9) . . ?
C31 O7 C34 105.86(14) . . ?
C31 O7 K1 120.82(10) . . ?
C34 O7 K1 110.81(9) . . ?
C6 C1 C2 117.07(13) . . ?
C6 C1 Si1 123.75(11) . . ?
C2 C1 Si1 119.18(11) . . ?
C3 C2 C1 121.59(14) . . ?
C2 C3 C4 120.10(14) . . ?
C5 C4 C3 119.71(14) . . ?
C4 C5 C6 119.94(14) . . ?
C1 C6 C5 121.56(14) . . ?
C8 C7 C12 117.51(14) . . ?
C8 C7 Si1 122.87(12) . . ?
C12 C7 Si1 119.59(11) . . ?
C9 C8 C7 121.45(15) . . ?
C10 C9 C8 119.80(15) . . ?
C11 C10 C9 120.06(15) . . ?
C10 C11 C12 119.78(16) . . ?
C11 C12 C7 121.39(15) . . ?
C18 C13 C14 117.20(14) . . ?
C18 C13 Si1 120.75(11) . . ?
C14 C13 Si1 122.00(11) . . ?
C15 C14 C13 121.49(15) . . ?
C16 C15 C14 120.04(15) . . ?
C15 C16 C17 119.63(15) . . ?
C16 C17 C18 120.18(16) . . ?
C17 C18 C13 121.44(15) . . ?
O1 C19 C20 108.90(14) . . ?
O2 C20 C19 108.33(14) . . ?
O2 C21 C22 108.86(13) . . ?
O3 C22 C21 108.29(13) . . ?
O3 C23 C24 108.55(13) . . ?
O4 C24 C23 109.39(13) . . ?
O4 C25 C26 109.30(13) . . ?
O5 C26 C25 108.24(13) . . ?
O5 C27 C28 108.39(13) . . ?
O6 C28 C27 108.59(14) . . ?
O6 C29 C30 108.72(14) . . ?
O1 C30 C29 108.38(14) . . ?
O7 C31 C32 105.05(15) . . ?
C31 C32 C33 103.46(15) . . ?
C34 C33 C32 103.96(15) . . ?
O7 C34 C33 106.14(14) . . ?

_refine_diff_density_max         0.465
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.059

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_apx2133s
_database_code_depnum_ccdc_archive 'CCDC 1436082'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_apx2133s            
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: Molecular weight is correct- PLATON/SQUEEZE used to treat
disordered thf solvent
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H47 K O6.50 S Si'
_chemical_formula_weight         610.93

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   25.991(6)
_cell_length_b                   9.800(2)
_cell_length_c                   26.079(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.188(3)
_cell_angle_gamma                90.00
_cell_volume                     6493(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8980
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62353
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.35
_reflns_number_total             11888
_reflns_number_gt                9437
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.213 0.250 115 35 tetrahydrofuran
2 0.750 0.516 0.250 119 34 tetrahydrofuran
3 0.250 0.484 0.750 119 35 tetrahydrofuran
4 0.750 0.786 0.750 115 35 tetrahydrofuran
_platon_squeeze_details          
;
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0430P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11888
_refine_ls_number_parameters     673
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0936
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
S1 S 0.53911(2) 0.32090(5) 0.779502(19) 0.02287(12) Uani 1 1 d . . .
S2 S 0.281638(19) 0.96170(5) 0.539464(19) 0.02095(12) Uani 1 1 d . . .
K1 K 0.615349(19) 0.56596(4) 0.769679(17) 0.02567(12) Uani 1 1 d . . .
K2 K 0.275445(17) 0.70426(4) 0.615962(18) 0.02573(12) Uani 1 1 d . . .
Si1 Si 0.51521(2) 0.32228(5) 0.84967(2) 0.01503(12) Uani 1 1 d . . .
Si2 Si 0.35202(2) 0.96189(5) 0.51539(2) 0.01529(12) Uani 1 1 d . . .
O1 O 0.59113(5) 0.47912(13) 0.66466(5) 0.0215(3) Uani 1 1 d . . .
O2 O 0.66989(5) 0.33528(13) 0.73595(5) 0.0200(3) Uani 1 1 d . . .
O3 O 0.69345(5) 0.42898(13) 0.84011(5) 0.0224(3) Uani 1 1 d . . .
O4 O 0.67356(6) 0.70081(14) 0.86203(5) 0.0285(3) Uani 1 1 d . . .
O5 O 0.59426(6) 0.84078(14) 0.79249(6) 0.0337(4) Uani 1 1 d . . .
O6 O 0.57285(5) 0.75351(14) 0.68887(6) 0.0274(3) Uani 1 1 d . . .
O7 O 0.19696(5) 0.49528(14) 0.57534(5) 0.0259(3) Uani 1 1 d . . .
O8 O 0.30443(6) 0.43476(14) 0.59941(6) 0.0306(4) Uani 1 1 d . . .
O9 O 0.37078(5) 0.58289(14) 0.67760(5) 0.0265(3) Uani 1 1 d . . .
O10 O 0.34245(5) 0.84995(13) 0.69573(5) 0.0205(3) Uani 1 1 d . . .
O11 O 0.23601(5) 0.92468(13) 0.66865(5) 0.0206(3) Uani 1 1 d . . .
O12 O 0.16891(5) 0.76490(13) 0.59229(5) 0.0224(3) Uani 1 1 d . . .
C1 C 0.62283(8) 0.3754(2) 0.64922(8) 0.0264(5) Uani 1 1 d . . .
H1A H 0.6549 0.4149 0.6423 0.032 Uiso 1 1 calc R . .
H1B H 0.6040 0.3318 0.6174 0.032 Uiso 1 1 calc R . .
C2 C 0.63583(8) 0.2732(2) 0.69204(8) 0.0262(5) Uani 1 1 d . . .
H2A H 0.6039 0.2420 0.7020 0.031 Uiso 1 1 calc R . .
H2B H 0.6531 0.1950 0.6802 0.031 Uiso 1 1 calc R . .
C3 C 0.68170(8) 0.2453(2) 0.77978(8) 0.0250(5) Uani 1 1 d . . .
H3A H 0.6974 0.1622 0.7700 0.030 Uiso 1 1 calc R . .
H3B H 0.6496 0.2214 0.7911 0.030 Uiso 1 1 calc R . .
C4 C 0.71898(8) 0.3145(2) 0.82335(8) 0.0276(5) Uani 1 1 d . . .
H4A H 0.7299 0.2516 0.8523 0.033 Uiso 1 1 calc R . .
H4B H 0.7501 0.3439 0.8114 0.033 Uiso 1 1 calc R . .
C5 C 0.72601(9) 0.5009(2) 0.88217(8) 0.0338(6) Uani 1 1 d . . .
H5A H 0.7546 0.5453 0.8700 0.041 Uiso 1 1 calc R . .
H5B H 0.7410 0.4380 0.9100 0.041 Uiso 1 1 calc R . .
C6 C 0.69302(9) 0.6052(2) 0.90218(8) 0.0356(6) Uani 1 1 d . . .
H6A H 0.6639 0.5606 0.9132 0.043 Uiso 1 1 calc R . .
H6B H 0.7140 0.6518 0.9323 0.043 Uiso 1 1 calc R . .
C7 C 0.64088(10) 0.8007(3) 0.87965(9) 0.0425(6) Uani 1 1 d . . .
H7A H 0.6601 0.8443 0.9113 0.051 Uiso 1 1 calc R . .
H7B H 0.6100 0.7570 0.8876 0.051 Uiso 1 1 calc R . .
C8 C 0.62466(10) 0.9046(2) 0.83774(10) 0.0454(7) Uani 1 1 d . . .
H8A H 0.6041 0.9754 0.8499 0.054 Uiso 1 1 calc R . .
H8B H 0.6556 0.9466 0.8292 0.054 Uiso 1 1 calc R . .
C9 C 0.57894(10) 0.9343(2) 0.75015(10) 0.0423(6) Uani 1 1 d . . .
H9A H 0.6098 0.9689 0.7391 0.051 Uiso 1 1 calc R . .
H9B H 0.5603 1.0109 0.7613 0.051 Uiso 1 1 calc R . .
C10 C 0.54408(9) 0.8616(2) 0.70580(10) 0.0410(6) Uani 1 1 d . . .
H10A H 0.5135 0.8255 0.7171 0.049 Uiso 1 1 calc R . .
H10B H 0.5320 0.9246 0.6771 0.049 Uiso 1 1 calc R . .
C11 C 0.54310(8) 0.6842(2) 0.64424(9) 0.0336(5) Uani 1 1 d . . .
H11A H 0.5302 0.7490 0.6164 0.040 Uiso 1 1 calc R . .
H11B H 0.5131 0.6390 0.6534 0.040 Uiso 1 1 calc R . .
C12 C 0.57779(9) 0.5815(2) 0.62620(8) 0.0316(5) Uani 1 1 d . . .
H12A H 0.5596 0.5412 0.5934 0.038 Uiso 1 1 calc R . .
H12B H 0.6095 0.6256 0.6204 0.038 Uiso 1 1 calc R . .
C13 C 0.44443(7) 0.25445(19) 0.84110(7) 0.0184(4) Uani 1 1 d . . .
C14 C 0.41031(8) 0.3284(2) 0.79424(9) 0.0314(5) Uani 1 1 d . . .
H14A H 0.3753 0.2915 0.7876 0.047 Uiso 1 1 calc R . .
H14B H 0.4251 0.3160 0.7638 0.047 Uiso 1 1 calc R . .
H14C H 0.4091 0.4240 0.8020 0.047 Uiso 1 1 calc R . .
C15 C 0.42018(8) 0.2786(2) 0.88894(8) 0.0256(5) Uani 1 1 d . . .
H15A H 0.3839 0.2513 0.8809 0.038 Uiso 1 1 calc R . .
H15B H 0.4226 0.3737 0.8980 0.038 Uiso 1 1 calc R . .
H15C H 0.4389 0.2259 0.9180 0.038 Uiso 1 1 calc R . .
C16 C 0.44392(8) 0.10171(19) 0.82827(8) 0.0232(5) Uani 1 1 d . . .
H16A H 0.4631 0.0526 0.8581 0.035 Uiso 1 1 calc R . .
H16B H 0.4601 0.0873 0.7988 0.035 Uiso 1 1 calc R . .
H16C H 0.4082 0.0696 0.8198 0.035 Uiso 1 1 calc R . .
C17 C 0.51394(7) 0.50108(19) 0.87744(7) 0.0167(4) Uani 1 1 d . . .
C18 C 0.50042(8) 0.6127(2) 0.84418(8) 0.0249(5) Uani 1 1 d . . .
H18 H 0.4941 0.5987 0.8081 0.030 Uiso 1 1 calc R . .
C19 C 0.49605(8) 0.7436(2) 0.86281(9) 0.0306(5) Uani 1 1 d . . .
H19 H 0.4867 0.8159 0.8396 0.037 Uiso 1 1 calc R . .
C20 C 0.50576(8) 0.7657(2) 0.91628(9) 0.0296(5) Uani 1 1 d . . .
H20 H 0.5026 0.8530 0.9292 0.036 Uiso 1 1 calc R . .
C21 C 0.52008(8) 0.6592(2) 0.95044(9) 0.0275(5) Uani 1 1 d . . .
H21 H 0.5271 0.6747 0.9864 0.033 Uiso 1 1 calc R . .
C22 C 0.52404(7) 0.5278(2) 0.93121(8) 0.0217(4) Uani 1 1 d . . .
H22 H 0.5336 0.4563 0.9547 0.026 Uiso 1 1 calc R . .
C23 C 0.56207(7) 0.22308(18) 0.90255(7) 0.0170(4) Uani 1 1 d . . .
C24 C 0.61611(7) 0.2381(2) 0.90492(8) 0.0207(4) Uani 1 1 d . . .
H24 H 0.6271 0.2959 0.8811 0.025 Uiso 1 1 calc R . .
C25 C 0.65357(8) 0.1702(2) 0.94146(8) 0.0254(5) Uani 1 1 d . . .
H25 H 0.6891 0.1840 0.9422 0.030 Uiso 1 1 calc R . .
C26 C 0.63871(8) 0.0820(2) 0.97692(8) 0.0283(5) Uani 1 1 d . . .
H26 H 0.6639 0.0349 1.0011 0.034 Uiso 1 1 calc R . .
C27 C 0.58594(8) 0.0651(2) 0.97584(8) 0.0284(5) Uani 1 1 d . . .
H27 H 0.5753 0.0061 0.9996 0.034 Uiso 1 1 calc R . .
C28 C 0.54842(8) 0.1352(2) 0.93964(8) 0.0229(5) Uani 1 1 d . . .
H28 H 0.5130 0.1232 0.9401 0.027 Uiso 1 1 calc R . .
C29 C 0.21977(10) 0.3978(2) 0.54693(9) 0.0385(6) Uani 1 1 d . . .
H29A H 0.2313 0.4418 0.5180 0.046 Uiso 1 1 calc R . .
H29B H 0.1940 0.3288 0.5327 0.046 Uiso 1 1 calc R . .
C30 C 0.26566(10) 0.3330(2) 0.58276(10) 0.0427(6) Uani 1 1 d . . .
H30A H 0.2547 0.2937 0.6129 0.051 Uiso 1 1 calc R . .
H30B H 0.2800 0.2606 0.5645 0.051 Uiso 1 1 calc R . .
C31 C 0.35152(9) 0.3768(2) 0.62955(10) 0.0395(6) Uani 1 1 d . . .
H31A H 0.3653 0.3091 0.6089 0.047 Uiso 1 1 calc R . .
H31B H 0.3441 0.3322 0.6604 0.047 Uiso 1 1 calc R . .
C32 C 0.39108(9) 0.4870(2) 0.64562(9) 0.0350(6) Uani 1 1 d . . .
H32A H 0.4238 0.4484 0.6651 0.042 Uiso 1 1 calc R . .
H32B H 0.3982 0.5324 0.6148 0.042 Uiso 1 1 calc R . .
C33 C 0.40860(8) 0.6852(2) 0.69677(9) 0.0313(5) Uani 1 1 d . . .
H33A H 0.4186 0.7321 0.6676 0.038 Uiso 1 1 calc R . .
H33B H 0.4399 0.6438 0.7180 0.038 Uiso 1 1 calc R . .
C34 C 0.38551(8) 0.7844(2) 0.72896(8) 0.0322(5) Uani 1 1 d . . .
H34A H 0.3737 0.7372 0.7571 0.039 Uiso 1 1 calc R . .
H34B H 0.4117 0.8513 0.7444 0.039 Uiso 1 1 calc R . .
C35 C 0.32177(8) 0.9608(2) 0.72030(8) 0.0258(5) Uani 1 1 d . . .
H35A H 0.3490 1.0284 0.7319 0.031 Uiso 1 1 calc R . .
H35B H 0.3093 0.9285 0.7507 0.031 Uiso 1 1 calc R . .
C36 C 0.27732(8) 1.0228(2) 0.68150(8) 0.0248(5) Uani 1 1 d . . .
H36A H 0.2646 1.1036 0.6964 0.030 Uiso 1 1 calc R . .
H36B H 0.2892 1.0493 0.6501 0.030 Uiso 1 1 calc R . .
C37 C 0.19185(7) 0.9792(2) 0.63268(8) 0.0230(5) Uani 1 1 d . . .
H37A H 0.2024 1.0083 0.6009 0.028 Uiso 1 1 calc R . .
H37B H 0.1782 1.0578 0.6481 0.028 Uiso 1 1 calc R . .
C38 C 0.15031(8) 0.8718(2) 0.62003(8) 0.0270(5) Uani 1 1 d . . .
H38A H 0.1421 0.8367 0.6521 0.032 Uiso 1 1 calc R . .
H38B H 0.1185 0.9105 0.5988 0.032 Uiso 1 1 calc R . .
C39 C 0.13060(8) 0.6603(2) 0.57680(9) 0.0323(5) Uani 1 1 d . . .
H39A H 0.0983 0.6996 0.5568 0.039 Uiso 1 1 calc R . .
H39B H 0.1229 0.6160 0.6076 0.039 Uiso 1 1 calc R . .
C40 C 0.15174(8) 0.5590(2) 0.54414(8) 0.0309(5) Uani 1 1 d . . .
H40A H 0.1252 0.4908 0.5310 0.037 Uiso 1 1 calc R . .
H40B H 0.1612 0.6042 0.5143 0.037 Uiso 1 1 calc R . .
C41 C 0.34406(7) 1.03423(19) 0.44554(7) 0.0186(4) Uani 1 1 d . . .
C42 C 0.29817(8) 0.9582(2) 0.41053(8) 0.0266(5) Uani 1 1 d . . .
H42A H 0.2928 0.9931 0.3754 0.040 Uiso 1 1 calc R . .
H42B H 0.2668 0.9714 0.4238 0.040 Uiso 1 1 calc R . .
H42C H 0.3062 0.8626 0.4105 0.040 Uiso 1 1 calc R . .
C43 C 0.32954(8) 1.1862(2) 0.44579(8) 0.0266(5) Uani 1 1 d . . .
H43A H 0.3214 1.2198 0.4104 0.040 Uiso 1 1 calc R . .
H43B H 0.3587 1.2364 0.4658 0.040 Uiso 1 1 calc R . .
H43C H 0.2994 1.1971 0.4613 0.040 Uiso 1 1 calc R . .
C44 C 0.39245(8) 1.0154(2) 0.42145(8) 0.0241(5) Uani 1 1 d . . .
H44A H 0.4009 0.9201 0.4209 0.036 Uiso 1 1 calc R . .
H44B H 0.4217 1.0639 0.4421 0.036 Uiso 1 1 calc R . .
H44C H 0.3851 1.0504 0.3863 0.036 Uiso 1 1 calc R . .
C45 C 0.37785(7) 0.78185(19) 0.51240(7) 0.0168(4) Uani 1 1 d . . .
C46 C 0.34309(8) 0.6720(2) 0.50164(8) 0.0240(5) Uani 1 1 d . . .
H46 H 0.3071 0.6884 0.4960 0.029 Uiso 1 1 calc R . .
C47 C 0.36057(9) 0.5391(2) 0.49904(8) 0.0282(5) Uani 1 1 d . . .
H47 H 0.3365 0.4679 0.4919 0.034 Uiso 1 1 calc R . .
C48 C 0.41351(9) 0.5129(2) 0.50700(8) 0.0272(5) Uani 1 1 d . . .
H48 H 0.4254 0.4238 0.5055 0.033 Uiso 1 1 calc R . .
C49 C 0.44903(9) 0.6190(2) 0.51721(8) 0.0285(5) Uani 1 1 d . . .
H49 H 0.4849 0.6015 0.5226 0.034 Uiso 1 1 calc R . .
C50 C 0.43119(8) 0.7523(2) 0.51941(8) 0.0239(5) Uani 1 1 d . . .
H50 H 0.4555 0.8232 0.5257 0.029 Uiso 1 1 calc R . .
C51 C 0.40545(7) 1.05585(18) 0.56374(7) 0.0158(4) Uani 1 1 d . . .
C52 C 0.40627(8) 1.0401(2) 0.61715(7) 0.0204(4) Uani 1 1 d . . .
H52 H 0.3817 0.9829 0.6273 0.024 Uiso 1 1 calc R . .
C53 C 0.44253(8) 1.1070(2) 0.65552(8) 0.0251(5) Uani 1 1 d . . .
H53 H 0.4418 1.0940 0.6907 0.030 Uiso 1 1 calc R . .
C54 C 0.47965(8) 1.1925(2) 0.64208(8) 0.0266(5) Uani 1 1 d . . .
H54 H 0.5035 1.2388 0.6678 0.032 Uiso 1 1 calc R . .
C55 C 0.48081(8) 1.2082(2) 0.58983(8) 0.0290(5) Uani 1 1 d . . .
H55 H 0.5060 1.2643 0.5802 0.035 Uiso 1 1 calc R . .
C56 C 0.44445(8) 1.1406(2) 0.55146(8) 0.0237(5) Uani 1 1 d . . .
H56 H 0.4461 1.1520 0.5164 0.028 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
S1 Si1 2.0529(8) . ?
S1 K1 3.1582(8) . ?
S2 Si2 2.0556(8) . ?
S2 K2 3.2413(9) . ?
K1 O3 2.7788(14) . ?
K1 O1 2.8094(14) . ?
K1 O5 2.8364(16) . ?
K1 O6 2.8384(14) . ?
K1 O4 2.8805(15) . ?
K1 O2 2.9017(14) . ?
K2 O12 2.7713(15) . ?
K2 O8 2.8046(15) . ?
K2 O10 2.8053(14) . ?
K2 O11 2.8634(14) . ?
K2 O9 2.9081(15) . ?
K2 O7 2.9266(15) . ?
Si1 C17 1.899(2) . ?
Si1 C23 1.9030(19) . ?
Si1 C13 1.9241(19) . ?
Si2 C45 1.895(2) . ?
Si2 C51 1.9044(19) . ?
Si2 C41 1.925(2) . ?
O1 C12 1.410(2) . ?
O1 C1 1.419(2) . ?
O2 C3 1.425(2) . ?
O2 C2 1.427(2) . ?
O3 C4 1.418(2) . ?
O3 C5 1.423(2) . ?
O4 C6 1.417(3) . ?
O4 C7 1.434(3) . ?
O5 C8 1.419(3) . ?
O5 C9 1.425(3) . ?
O6 C10 1.420(3) . ?
O6 C11 1.426(2) . ?
O7 C29 1.414(3) . ?
O7 C40 1.425(2) . ?
O8 C30 1.419(3) . ?
O8 C31 1.426(3) . ?
O9 C33 1.419(2) . ?
O9 C32 1.429(2) . ?
O10 C34 1.416(2) . ?
O10 C35 1.423(2) . ?
O11 C37 1.424(2) . ?
O11 C36 1.427(2) . ?
O12 C38 1.415(2) . ?
O12 C39 1.427(2) . ?
C1 C2 1.485(3) . ?
C3 C4 1.492(3) . ?
C5 C6 1.497(3) . ?
C7 C8 1.488(3) . ?
C9 C10 1.491(3) . ?
C11 C12 1.492(3) . ?
C13 C15 1.530(3) . ?
C13 C14 1.532(3) . ?
C13 C16 1.533(3) . ?
C17 C18 1.394(3) . ?
C17 C22 1.396(3) . ?
C18 C19 1.385(3) . ?
C19 C20 1.381(3) . ?
C20 C21 1.371(3) . ?
C21 C22 1.394(3) . ?
C23 C28 1.396(3) . ?
C23 C24 1.401(3) . ?
C24 C25 1.381(3) . ?
C25 C26 1.379(3) . ?
C26 C27 1.376(3) . ?
C27 C28 1.387(3) . ?
C29 C30 1.493(3) . ?
C31 C32 1.489(3) . ?
C33 C34 1.491(3) . ?
C35 C36 1.495(3) . ?
C37 C38 1.493(3) . ?
C39 C40 1.487(3) . ?
C41 C44 1.531(3) . ?
C41 C42 1.534(3) . ?
C41 C43 1.536(3) . ?
C45 C50 1.390(3) . ?
C45 C46 1.396(3) . ?
C46 C47 1.385(3) . ?
C47 C48 1.372(3) . ?
C48 C49 1.379(3) . ?
C49 C50 1.391(3) . ?
C51 C52 1.397(3) . ?
C51 C56 1.399(3) . ?
C52 C53 1.386(3) . ?
C53 C54 1.378(3) . ?
C54 C55 1.378(3) . ?
C55 C56 1.391(3) . ?

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
Si1 S1 K1 112.36(3) . . ?
Si2 S2 K2 110.59(3) . . ?
O3 K1 O1 118.69(4) . . ?
O3 K1 O5 117.81(4) . . ?
O1 K1 O5 118.59(4) . . ?
O3 K1 O6 156.78(4) . . ?
O1 K1 O6 60.02(4) . . ?
O5 K1 O6 58.59(5) . . ?
O3 K1 O4 59.17(4) . . ?
O1 K1 O4 157.53(4) . . ?
O5 K1 O4 58.65(4) . . ?
O6 K1 O4 112.16(5) . . ?
O3 K1 O2 59.24(4) . . ?
O1 K1 O2 59.46(4) . . ?
O5 K1 O2 158.70(4) . . ?
O6 K1 O2 114.70(4) . . ?
O4 K1 O2 114.01(4) . . ?
O3 K1 S1 87.84(3) . . ?
O1 K1 S1 80.41(3) . . ?
O5 K1 S1 123.55(4) . . ?
O6 K1 S1 113.59(4) . . ?
O4 K1 S1 120.59(3) . . ?
O2 K1 S1 77.71(3) . . ?
O12 K2 O8 117.12(4) . . ?
O12 K2 O10 119.39(4) . . ?
O8 K2 O10 116.65(4) . . ?
O12 K2 O11 60.20(4) . . ?
O8 K2 O11 156.81(4) . . ?
O10 K2 O11 59.29(4) . . ?
O12 K2 O9 154.90(4) . . ?
O8 K2 O9 58.31(4) . . ?
O10 K2 O9 58.34(4) . . ?
O11 K2 O9 113.13(4) . . ?
O12 K2 O7 58.81(4) . . ?
O8 K2 O7 58.31(4) . . ?
O10 K2 O7 154.25(4) . . ?
O11 K2 O7 114.13(4) . . ?
O9 K2 O7 111.18(4) . . ?
O12 K2 S2 82.71(3) . . ?
O8 K2 S2 126.04(4) . . ?
O10 K2 S2 87.51(3) . . ?
O11 K2 S2 77.14(3) . . ?
O9 K2 S2 120.75(3) . . ?
O7 K2 S2 116.31(3) . . ?
C17 Si1 C23 104.77(8) . . ?
C17 Si1 C13 105.66(8) . . ?
C23 Si1 C13 110.95(9) . . ?
C17 Si1 S1 112.27(6) . . ?
C23 Si1 S1 112.02(6) . . ?
C13 Si1 S1 110.86(6) . . ?
C45 Si2 C51 105.20(8) . . ?
C45 Si2 C41 105.78(8) . . ?
C51 Si2 C41 111.48(8) . . ?
C45 Si2 S2 110.95(6) . . ?
C51 Si2 S2 111.70(6) . . ?
C41 Si2 S2 111.38(6) . . ?
C12 O1 C1 112.22(15) . . ?
C12 O1 K1 116.68(12) . . ?
C1 O1 K1 118.01(11) . . ?
C3 O2 C2 111.84(15) . . ?
C3 O2 K1 105.97(10) . . ?
C2 O2 K1 108.38(10) . . ?
C4 O3 C5 112.87(15) . . ?
C4 O3 K1 120.16(11) . . ?
C5 O3 K1 120.19(12) . . ?
C6 O4 C7 110.99(17) . . ?
C6 O4 K1 110.91(11) . . ?
C7 O4 K1 109.82(12) . . ?
C8 O5 C9 112.10(17) . . ?
C8 O5 K1 119.63(13) . . ?
C9 O5 K1 118.86(13) . . ?
C10 O6 C11 112.25(15) . . ?
C10 O6 K1 113.59(13) . . ?
C11 O6 K1 110.89(11) . . ?
C29 O7 C40 112.54(16) . . ?
C29 O7 K2 108.97(12) . . ?
C40 O7 K2 109.16(11) . . ?
C30 O8 C31 111.10(16) . . ?
C30 O8 K2 120.84(12) . . ?
C31 O8 K2 121.17(12) . . ?
C33 O9 C32 110.89(16) . . ?
C33 O9 K2 110.58(11) . . ?
C32 O9 K2 108.82(12) . . ?
C34 O10 C35 113.29(15) . . ?
C34 O10 K2 120.64(12) . . ?
C35 O10 K2 119.21(11) . . ?
C37 O11 C36 111.35(14) . . ?
C37 O11 K2 106.69(10) . . ?
C36 O11 K2 107.04(10) . . ?
C38 O12 C39 112.54(15) . . ?
C38 O12 K2 118.55(11) . . ?
C39 O12 K2 120.93(11) . . ?
O1 C1 C2 108.85(16) . . ?
O2 C2 C1 108.67(16) . . ?
O2 C3 C4 108.97(16) . . ?
O3 C4 C3 108.87(15) . . ?
O3 C5 C6 108.41(17) . . ?
O4 C6 C5 109.59(17) . . ?
O4 C7 C8 109.07(19) . . ?
O5 C8 C7 109.33(19) . . ?
O5 C9 C10 108.58(18) . . ?
O6 C10 C9 108.89(18) . . ?
O6 C11 C12 108.59(17) . . ?
O1 C12 C11 109.26(17) . . ?
C15 C13 C14 107.97(16) . . ?
C15 C13 C16 110.04(16) . . ?
C14 C13 C16 108.09(16) . . ?
C15 C13 Si1 113.60(13) . . ?
C14 C13 Si1 107.91(13) . . ?
C16 C13 Si1 109.06(13) . . ?
C18 C17 C22 116.55(18) . . ?
C18 C17 Si1 120.60(15) . . ?
C22 C17 Si1 122.79(15) . . ?
C19 C18 C17 122.49(19) . . ?
C20 C19 C18 119.2(2) . . ?
C21 C20 C19 120.26(19) . . ?
C20 C21 C22 120.0(2) . . ?
C21 C22 C17 121.50(19) . . ?
C28 C23 C24 115.70(17) . . ?
C28 C23 Si1 126.88(15) . . ?
C24 C23 Si1 117.42(15) . . ?
C25 C24 C23 122.27(19) . . ?
C26 C25 C24 120.55(19) . . ?
C27 C26 C25 118.74(19) . . ?
C26 C27 C28 120.6(2) . . ?
C27 C28 C23 122.13(19) . . ?
O7 C29 C30 109.13(18) . . ?
O8 C30 C29 108.30(18) . . ?
O8 C31 C32 109.12(18) . . ?
O9 C32 C31 108.85(19) . . ?
O9 C33 C34 109.14(17) . . ?
O10 C34 C33 108.12(16) . . ?
O10 C35 C36 108.49(16) . . ?
O11 C36 C35 108.72(16) . . ?
O11 C37 C38 109.03(16) . . ?
O12 C38 C37 108.99(16) . . ?
O12 C39 C40 108.77(17) . . ?
O7 C40 C39 108.99(17) . . ?
C44 C41 C42 107.47(16) . . ?
C44 C41 C43 110.02(16) . . ?
C42 C41 C43 108.20(16) . . ?
C44 C41 Si2 114.24(13) . . ?
C42 C41 Si2 107.41(13) . . ?
C43 C41 Si2 109.29(13) . . ?
C50 C45 C46 116.81(18) . . ?
C50 C45 Si2 122.73(14) . . ?
C46 C45 Si2 120.45(14) . . ?
C47 C46 C45 122.00(19) . . ?
C48 C47 C46 119.8(2) . . ?
C47 C48 C49 119.82(19) . . ?
C48 C49 C50 120.0(2) . . ?
C45 C50 C49 121.46(19) . . ?
C52 C51 C56 115.75(17) . . ?
C52 C51 Si2 117.54(14) . . ?
C56 C51 Si2 126.70(15) . . ?
C53 C52 C51 122.20(19) . . ?
C54 C53 C52 120.65(19) . . ?
C53 C54 C55 118.82(19) . . ?
C54 C55 C56 120.3(2) . . ?
C55 C56 C51 122.22(19) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.049
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dq0189s
_database_code_depnum_ccdc_archive 'CCDC 1436083'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_CHEMW03_dq0189s             
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: Molecular weight is correct- PLATON/SQUEEZE was used to
treat disordered thf solvent molecule
;
# end Validation Reply Form

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H47 K O6.50 Se Si'
_chemical_formula_weight         657.83

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'
Se Se -0.0929 2.2259 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   26.2187(15)
_cell_length_b                   9.7757(6)
_cell_length_c                   26.2094(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.8380(10)
_cell_angle_gamma                90.00
_cell_volume                     6549.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2768
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4076
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81128
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.73
_reflns_number_total             12444
_reflns_number_gt                10686
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.208 0.250 114 30 thf
2 0.250 0.491 0.750 118 28 thf
3 0.750 0.509 0.250 118 28 thf
4 0.750 0.792 0.750 114 30 thf
_platon_squeeze_details          
;
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12444
_refine_ls_number_parameters     673
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_restrained_S_all      0.868
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Se1 Se 0.533283(9) 0.33448(2) 0.773669(9) 0.01962(8) Uani 1 1 d . . .
Se2 Se 0.277239(8) 0.96438(2) 0.534568(9) 0.01697(8) Uani 1 1 d . . .
K1 K 0.61694(2) 0.57746(5) 0.769472(19) 0.02157(12) Uani 1 1 d . . .
K2 K 0.27545(2) 0.70545(5) 0.61657(2) 0.02216(13) Uani 1 1 d . . .
Si1 Si 0.51041(2) 0.33430(6) 0.84928(2) 0.01189(13) Uani 1 1 d . . .
Si2 Si 0.35236(2) 0.96041(6) 0.51071(2) 0.01141(13) Uani 1 1 d . . .
O1 O 0.59194(6) 0.48767(17) 0.66538(6) 0.0211(4) Uani 1 1 d . . .
O2 O 0.67034(6) 0.34506(16) 0.73668(6) 0.0189(4) Uani 1 1 d . . .
O3 O 0.69313(6) 0.43826(17) 0.84075(6) 0.0202(4) Uani 1 1 d . . .
O4 O 0.67301(7) 0.70953(18) 0.86289(7) 0.0268(4) Uani 1 1 d . . .
O5 O 0.59356(7) 0.84688(17) 0.79278(8) 0.0324(4) Uani 1 1 d . . .
O6 O 0.57216(6) 0.76140(18) 0.68891(7) 0.0270(4) Uani 1 1 d . . .
O8 O 0.19786(7) 0.49867(17) 0.57531(6) 0.0236(4) Uani 1 1 d . . .
O9 O 0.30527(7) 0.44203(17) 0.59712(7) 0.0292(4) Uani 1 1 d . . .
O10 O 0.37164(7) 0.58815(18) 0.67547(7) 0.0253(4) Uani 1 1 d . . .
O11 O 0.34315(6) 0.85385(16) 0.69455(6) 0.0192(4) Uani 1 1 d . . .
O12 O 0.23666(6) 0.92694(16) 0.66928(6) 0.0176(3) Uani 1 1 d . . .
O13 O 0.16934(6) 0.76667(17) 0.59354(6) 0.0202(4) Uani 1 1 d . . .
C1 C 0.62368(9) 0.3849(3) 0.64983(10) 0.0253(6) Uani 1 1 d . . .
H1A H 0.6553 0.4254 0.6431 0.030 Uiso 1 1 calc R . .
H1B H 0.6049 0.3410 0.6180 0.030 Uiso 1 1 calc R . .
C2 C 0.63719(10) 0.2822(3) 0.69269(10) 0.0255(6) Uani 1 1 d . . .
H2A H 0.6056 0.2494 0.7021 0.031 Uiso 1 1 calc R . .
H2B H 0.6549 0.2048 0.6812 0.031 Uiso 1 1 calc R . .
C3 C 0.68170(10) 0.2554(2) 0.78013(10) 0.0242(5) Uani 1 1 d . . .
H3A H 0.6973 0.1719 0.7706 0.029 Uiso 1 1 calc R . .
H3B H 0.6497 0.2315 0.7908 0.029 Uiso 1 1 calc R . .
C4 C 0.71861(10) 0.3240(3) 0.82426(11) 0.0265(6) Uani 1 1 d . . .
H4A H 0.7293 0.2605 0.8531 0.032 Uiso 1 1 calc R . .
H4B H 0.7496 0.3538 0.8129 0.032 Uiso 1 1 calc R . .
C5 C 0.72549(11) 0.5106(3) 0.88301(10) 0.0325(6) Uani 1 1 d . . .
H5A H 0.7537 0.5560 0.8711 0.039 Uiso 1 1 calc R . .
H5B H 0.7407 0.4475 0.9108 0.039 Uiso 1 1 calc R . .
C6 C 0.69252(12) 0.6141(3) 0.90288(10) 0.0348(7) Uani 1 1 d . . .
H6A H 0.6637 0.5687 0.9135 0.042 Uiso 1 1 calc R . .
H6B H 0.7133 0.6609 0.9331 0.042 Uiso 1 1 calc R . .
C7 C 0.64010(13) 0.8081(3) 0.87991(12) 0.0409(7) Uani 1 1 d . . .
H7A H 0.6590 0.8521 0.9117 0.049 Uiso 1 1 calc R . .
H7B H 0.6097 0.7629 0.8875 0.049 Uiso 1 1 calc R . .
C8 C 0.62322(13) 0.9123(3) 0.83829(13) 0.0433(8) Uani 1 1 d . . .
H8A H 0.6021 0.9817 0.8502 0.052 Uiso 1 1 calc R . .
H8B H 0.6536 0.9566 0.8302 0.052 Uiso 1 1 calc R . .
C9 C 0.57724(12) 0.9403(3) 0.75053(14) 0.0463(9) Uani 1 1 d . . .
H9A H 0.6075 0.9768 0.7395 0.056 Uiso 1 1 calc R . .
H9B H 0.5582 1.0159 0.7615 0.056 Uiso 1 1 calc R . .
C10 C 0.54292(11) 0.8658(3) 0.70638(14) 0.0439(8) Uani 1 1 d . . .
H10A H 0.5134 0.8262 0.7179 0.053 Uiso 1 1 calc R . .
H10B H 0.5295 0.9288 0.6780 0.053 Uiso 1 1 calc R . .
C11 C 0.54232(10) 0.6902(3) 0.64512(11) 0.0318(6) Uani 1 1 d . . .
H11A H 0.5284 0.7542 0.6172 0.038 Uiso 1 1 calc R . .
H11B H 0.5132 0.6437 0.6549 0.038 Uiso 1 1 calc R . .
C12 C 0.57672(11) 0.5889(3) 0.62684(10) 0.0331(6) Uani 1 1 d . . .
H12A H 0.5581 0.5470 0.5945 0.040 Uiso 1 1 calc R . .
H12B H 0.6074 0.6345 0.6202 0.040 Uiso 1 1 calc R . .
C13 C 0.44040(8) 0.2653(2) 0.84141(9) 0.0153(5) Uani 1 1 d . . .
C14 C 0.40508(10) 0.3411(3) 0.79546(11) 0.0303(6) Uani 1 1 d . . .
H14A H 0.4184 0.3286 0.7645 0.045 Uiso 1 1 calc R . .
H14B H 0.4046 0.4368 0.8035 0.045 Uiso 1 1 calc R . .
H14C H 0.3702 0.3051 0.7897 0.045 Uiso 1 1 calc R . .
C15 C 0.41747(9) 0.2868(3) 0.88983(10) 0.0226(5) Uani 1 1 d . . .
H15A H 0.3811 0.2623 0.8816 0.034 Uiso 1 1 calc R . .
H15B H 0.4211 0.3811 0.9002 0.034 Uiso 1 1 calc R . .
H15C H 0.4359 0.2304 0.9179 0.034 Uiso 1 1 calc R . .
C16 C 0.43973(9) 0.1132(2) 0.82741(9) 0.0207(5) Uani 1 1 d . . .
H16A H 0.4600 0.0629 0.8564 0.031 Uiso 1 1 calc R . .
H16B H 0.4544 0.1009 0.7973 0.031 Uiso 1 1 calc R . .
H16C H 0.4043 0.0804 0.8198 0.031 Uiso 1 1 calc R . .
C17 C 0.51026(8) 0.5128(2) 0.87772(9) 0.0148(5) Uani 1 1 d . . .
C18 C 0.49744(10) 0.6255(2) 0.84503(10) 0.0234(5) Uani 1 1 d . . .
H18 H 0.4907 0.6128 0.8090 0.028 Uiso 1 1 calc R . .
C19 C 0.49446(11) 0.7561(3) 0.86452(11) 0.0299(6) Uani 1 1 d . . .
H19 H 0.4852 0.8294 0.8417 0.036 Uiso 1 1 calc R . .
C20 C 0.50522(10) 0.7771(2) 0.91744(11) 0.0280(6) Uani 1 1 d . . .
H20 H 0.5034 0.8647 0.9307 0.034 Uiso 1 1 calc R . .
C21 C 0.51881(10) 0.6678(3) 0.95102(10) 0.0266(6) Uani 1 1 d . . .
H21 H 0.5263 0.6818 0.9870 0.032 Uiso 1 1 calc R . .
C22 C 0.52127(9) 0.5375(2) 0.93121(9) 0.0198(5) Uani 1 1 d . . .
H22 H 0.5305 0.4647 0.9543 0.024 Uiso 1 1 calc R . .
C23 C 0.55819(9) 0.2340(2) 0.90087(9) 0.0151(5) Uani 1 1 d . . .
C24 C 0.61161(9) 0.2477(2) 0.90214(9) 0.0183(5) Uani 1 1 d . . .
H24 H 0.6221 0.3043 0.8778 0.022 Uiso 1 1 calc R . .
C25 C 0.64931(9) 0.1790(3) 0.93877(10) 0.0239(6) Uani 1 1 d . . .
H25 H 0.6845 0.1912 0.9389 0.029 Uiso 1 1 calc R . .
C26 C 0.63524(10) 0.0933(3) 0.97488(10) 0.0255(6) Uani 1 1 d . . .
H26 H 0.6606 0.0466 0.9991 0.031 Uiso 1 1 calc R . .
C27 C 0.58286(10) 0.0775(3) 0.97469(10) 0.0267(6) Uani 1 1 d . . .
H27 H 0.5728 0.0199 0.9989 0.032 Uiso 1 1 calc R . .
C28 C 0.54522(9) 0.1475(2) 0.93848(9) 0.0210(5) Uani 1 1 d . . .
H28 H 0.5102 0.1365 0.9393 0.025 Uiso 1 1 calc R . .
C33 C 0.22056(12) 0.4053(3) 0.54522(12) 0.0379(7) Uani 1 1 d . . .
H33A H 0.2311 0.4533 0.5169 0.046 Uiso 1 1 calc R . .
H33B H 0.1952 0.3359 0.5302 0.046 Uiso 1 1 calc R . .
C34 C 0.26674(13) 0.3401(3) 0.57955(14) 0.0446(8) Uani 1 1 d . . .
H34A H 0.2567 0.2975 0.6093 0.053 Uiso 1 1 calc R . .
H34B H 0.2807 0.2699 0.5603 0.053 Uiso 1 1 calc R . .
C35 C 0.35263(12) 0.3836(3) 0.62630(12) 0.0390(7) Uani 1 1 d . . .
H35A H 0.3660 0.3176 0.6049 0.047 Uiso 1 1 calc R . .
H35B H 0.3461 0.3366 0.6568 0.047 Uiso 1 1 calc R . .
C36 C 0.39162(11) 0.4945(3) 0.64286(11) 0.0323(6) Uani 1 1 d . . .
H36A H 0.4244 0.4560 0.6620 0.039 Uiso 1 1 calc R . .
H36B H 0.3980 0.5418 0.6124 0.039 Uiso 1 1 calc R . .
C37 C 0.40923(10) 0.6893(3) 0.69532(11) 0.0299(6) Uani 1 1 d . . .
H37A H 0.4193 0.7372 0.6667 0.036 Uiso 1 1 calc R . .
H37B H 0.4402 0.6469 0.7166 0.036 Uiso 1 1 calc R . .
C38 C 0.38616(10) 0.7882(3) 0.72780(10) 0.0293(6) Uani 1 1 d . . .
H38A H 0.3746 0.7399 0.7556 0.035 Uiso 1 1 calc R . .
H38B H 0.4122 0.8553 0.7436 0.035 Uiso 1 1 calc R . .
C39 C 0.32276(10) 0.9634(3) 0.71972(10) 0.0240(5) Uani 1 1 d . . .
H39A H 0.3496 1.0318 0.7313 0.029 Uiso 1 1 calc R . .
H39B H 0.3112 0.9296 0.7501 0.029 Uiso 1 1 calc R . .
C40 C 0.27789(10) 1.0249(2) 0.68175(10) 0.0218(5) Uani 1 1 d . . .
H40A H 0.2657 1.1058 0.6969 0.026 Uiso 1 1 calc R . .
H40B H 0.2888 1.0518 0.6502 0.026 Uiso 1 1 calc R . .
C41 C 0.19221(9) 0.9815(3) 0.63381(10) 0.0223(5) Uani 1 1 d . . .
H41A H 0.2019 1.0109 0.6019 0.027 Uiso 1 1 calc R . .
H41B H 0.1789 1.0601 0.6494 0.027 Uiso 1 1 calc R . .
C42 C 0.15113(9) 0.8731(3) 0.62167(10) 0.0238(5) Uani 1 1 d . . .
H42A H 0.1439 0.8373 0.6539 0.029 Uiso 1 1 calc R . .
H42B H 0.1190 0.9113 0.6009 0.029 Uiso 1 1 calc R . .
C43 C 0.13175(10) 0.6610(3) 0.57919(11) 0.0299(6) Uani 1 1 d . . .
H43A H 0.0988 0.6992 0.5602 0.036 Uiso 1 1 calc R . .
H43B H 0.1258 0.6156 0.6102 0.036 Uiso 1 1 calc R . .
C44 C 0.15211(10) 0.5612(3) 0.54545(10) 0.0287(6) Uani 1 1 d . . .
H44A H 0.1258 0.4921 0.5326 0.034 Uiso 1 1 calc R . .
H44B H 0.1601 0.6080 0.5156 0.034 Uiso 1 1 calc R . .
C45 C 0.34488(9) 1.0293(2) 0.44072(8) 0.0144(5) Uani 1 1 d . . .
C46 C 0.29918(9) 0.9521(3) 0.40570(9) 0.0219(5) Uani 1 1 d . . .
H46A H 0.2678 0.9683 0.4179 0.033 Uiso 1 1 calc R . .
H46B H 0.3067 0.8558 0.4071 0.033 Uiso 1 1 calc R . .
H46C H 0.2945 0.9838 0.3703 0.033 Uiso 1 1 calc R . .
C47 C 0.33078(10) 1.1816(2) 0.43986(10) 0.0223(5) Uani 1 1 d . . .
H47A H 0.3600 1.2325 0.4593 0.033 Uiso 1 1 calc R . .
H47B H 0.3012 1.1943 0.4554 0.033 Uiso 1 1 calc R . .
H47C H 0.3222 1.2135 0.4043 0.033 Uiso 1 1 calc R . .
C48 C 0.39298(9) 1.0070(3) 0.41775(9) 0.0201(5) Uani 1 1 d . . .
H48A H 0.3856 1.0376 0.3821 0.030 Uiso 1 1 calc R . .
H48B H 0.4016 0.9114 0.4190 0.030 Uiso 1 1 calc R . .
H48C H 0.4220 1.0579 0.4377 0.030 Uiso 1 1 calc R . .
C49 C 0.37756(9) 0.7791(2) 0.50928(8) 0.0142(4) Uani 1 1 d . . .
C50 C 0.34276(9) 0.6693(2) 0.49862(9) 0.0185(5) Uani 1 1 d . . .
H50 H 0.3070 0.6860 0.4928 0.022 Uiso 1 1 calc R . .
C51 C 0.36031(10) 0.5356(2) 0.49655(10) 0.0228(5) Uani 1 1 d . . .
H51 H 0.3364 0.4641 0.4890 0.027 Uiso 1 1 calc R . .
C52 C 0.41343(10) 0.5095(2) 0.50575(9) 0.0219(5) Uani 1 1 d . . .
H52 H 0.4254 0.4201 0.5048 0.026 Uiso 1 1 calc R . .
C53 C 0.44857(10) 0.6160(2) 0.51635(9) 0.0225(5) Uani 1 1 d . . .
H53 H 0.4843 0.5984 0.5223 0.027 Uiso 1 1 calc R . .
C54 C 0.43097(9) 0.7497(2) 0.51814(9) 0.0186(5) Uani 1 1 d . . .
H54 H 0.4551 0.8206 0.5253 0.022 Uiso 1 1 calc R . .
C55 C 0.40539(8) 1.0548(2) 0.55915(9) 0.0134(4) Uani 1 1 d . . .
C56 C 0.40532(9) 1.0440(2) 0.61229(9) 0.0163(5) Uani 1 1 d . . .
H56 H 0.3799 0.9903 0.6223 0.020 Uiso 1 1 calc R . .
C57 C 0.44187(9) 1.1109(3) 0.65069(9) 0.0221(5) Uani 1 1 d . . .
H57 H 0.4411 1.1006 0.6858 0.026 Uiso 1 1 calc R . .
C58 C 0.47953(9) 1.1930(2) 0.63651(10) 0.0228(5) Uani 1 1 d . . .
H58 H 0.5036 1.2398 0.6619 0.027 Uiso 1 1 calc R . .
C59 C 0.48100(9) 1.2045(3) 0.58474(10) 0.0235(5) Uani 1 1 d . . .
H59 H 0.5065 1.2583 0.5751 0.028 Uiso 1 1 calc R . .
C60 C 0.44478(9) 1.1365(2) 0.54683(10) 0.0202(5) Uani 1 1 d . . .
H60 H 0.4467 1.1455 0.5120 0.024 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Se1 Si1 2.1943(6) . ?
Se1 K1 3.2515(6) . ?
Se2 Si2 2.1952(6) . ?
Se2 K2 3.3277(6) . ?
K1 O3 2.7700(16) . ?
K1 O1 2.8015(17) . ?
K1 O5 2.8022(17) . ?
K1 O6 2.8228(17) . ?
K1 O4 2.8677(18) . ?
K1 O2 2.8973(16) . ?
K2 O9 2.7712(17) . ?
K2 O13 2.7777(16) . ?
K2 O11 2.7964(16) . ?
K2 O12 2.8733(16) . ?
K2 O10 2.8858(17) . ?
K2 O8 2.9010(17) . ?
Si1 C17 1.897(2) . ?
Si1 C23 1.899(2) . ?
Si1 C13 1.923(2) . ?
Si2 C49 1.895(2) . ?
Si2 C55 1.900(2) . ?
Si2 C45 1.923(2) . ?
O1 C12 1.407(3) . ?
O1 C1 1.421(3) . ?
O2 C3 1.416(3) . ?
O2 C2 1.420(3) . ?
O3 C4 1.417(3) . ?
O3 C5 1.425(3) . ?
O4 C6 1.412(3) . ?
O4 C7 1.429(3) . ?
O5 C8 1.423(3) . ?
O5 C9 1.426(4) . ?
O6 C10 1.412(3) . ?
O6 C11 1.420(3) . ?
O8 C44 1.417(3) . ?
O8 C33 1.421(3) . ?
O9 C34 1.421(3) . ?
O9 C35 1.425(3) . ?
O10 C37 1.411(3) . ?
O10 C36 1.429(3) . ?
O11 C38 1.416(3) . ?
O11 C39 1.423(3) . ?
O12 C41 1.423(3) . ?
O12 C40 1.427(3) . ?
O13 C42 1.418(3) . ?
O13 C43 1.419(3) . ?
C1 C2 1.489(4) . ?
C3 C4 1.492(4) . ?
C5 C6 1.497(4) . ?
C7 C8 1.486(5) . ?
C9 C10 1.489(4) . ?
C11 C12 1.489(4) . ?
C13 C16 1.531(3) . ?
C13 C15 1.535(3) . ?
C13 C14 1.537(3) . ?
C17 C22 1.388(3) . ?
C17 C18 1.391(3) . ?
C18 C19 1.384(3) . ?
C19 C20 1.368(4) . ?
C20 C21 1.380(4) . ?
C21 C22 1.383(3) . ?
C23 C28 1.397(3) . ?
C23 C24 1.400(3) . ?
C24 C25 1.389(3) . ?
C25 C26 1.374(4) . ?
C26 C27 1.381(4) . ?
C27 C28 1.388(3) . ?
C33 C34 1.482(4) . ?
C35 C36 1.487(4) . ?
C37 C38 1.501(4) . ?
C39 C40 1.489(3) . ?
C41 C42 1.494(4) . ?
C43 C44 1.493(4) . ?
C45 C48 1.529(3) . ?
C45 C47 1.534(3) . ?
C45 C46 1.536(3) . ?
C49 C50 1.396(3) . ?
C49 C54 1.397(3) . ?
C50 C51 1.390(3) . ?
C51 C52 1.384(4) . ?
C52 C53 1.377(4) . ?
C53 C54 1.390(3) . ?
C55 C56 1.397(3) . ?
C55 C60 1.399(3) . ?
C56 C57 1.389(3) . ?
C57 C58 1.386(4) . ?
C58 C59 1.370(4) . ?
C59 C60 1.382(3) . ?

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
Si1 Se1 K1 110.669(19) . . ?
Si2 Se2 K2 108.228(19) . . ?
O3 K1 O1 118.72(5) . . ?
O3 K1 O5 118.33(6) . . ?
O1 K1 O5 119.44(6) . . ?
O3 K1 O6 159.25(5) . . ?
O1 K1 O6 60.18(5) . . ?
O5 K1 O6 59.31(6) . . ?
O3 K1 O4 59.29(5) . . ?
O1 K1 O4 159.59(5) . . ?
O5 K1 O4 59.08(6) . . ?
O6 K1 O4 113.64(5) . . ?
O3 K1 O2 59.42(5) . . ?
O1 K1 O2 59.30(5) . . ?
O5 K1 O2 160.94(6) . . ?
O6 K1 O2 115.20(5) . . ?
O4 K1 O2 114.62(5) . . ?
O3 K1 Se1 90.52(4) . . ?
O1 K1 Se1 77.90(4) . . ?
O5 K1 Se1 119.82(4) . . ?
O6 K1 Se1 108.61(4) . . ?
O4 K1 Se1 121.44(4) . . ?
O2 K1 Se1 79.12(3) . . ?
O9 K2 O13 118.05(5) . . ?
O9 K2 O11 117.21(5) . . ?
O13 K2 O11 119.31(5) . . ?
O9 K2 O12 158.94(5) . . ?
O13 K2 O12 59.85(5) . . ?
O11 K2 O12 59.51(5) . . ?
O9 K2 O10 58.69(5) . . ?
O13 K2 O10 156.33(5) . . ?
O11 K2 O10 58.52(5) . . ?
O12 K2 O10 113.75(5) . . ?
O9 K2 O8 59.15(5) . . ?
O13 K2 O8 58.91(5) . . ?
O11 K2 O8 155.86(5) . . ?
O12 K2 O8 114.24(5) . . ?
O10 K2 O8 112.31(5) . . ?
O9 K2 Se2 122.89(4) . . ?
O13 K2 Se2 81.54(4) . . ?
O11 K2 Se2 88.83(4) . . ?
O12 K2 Se2 78.15(3) . . ?
O10 K2 Se2 120.77(4) . . ?
O8 K2 Se2 113.49(4) . . ?
C17 Si1 C23 104.69(10) . . ?
C17 Si1 C13 106.23(10) . . ?
C23 Si1 C13 110.99(10) . . ?
C17 Si1 Se1 112.26(7) . . ?
C23 Si1 Se1 111.95(7) . . ?
C13 Si1 Se1 110.45(7) . . ?
C49 Si2 C55 105.11(9) . . ?
C49 Si2 C45 105.71(9) . . ?
C55 Si2 C45 111.82(10) . . ?
C49 Si2 Se2 111.16(7) . . ?
C55 Si2 Se2 111.76(7) . . ?
C45 Si2 Se2 110.96(7) . . ?
C12 O1 C1 112.48(19) . . ?
C12 O1 K1 116.52(15) . . ?
C1 O1 K1 118.40(13) . . ?
C3 O2 C2 111.52(18) . . ?
C3 O2 K1 106.03(13) . . ?
C2 O2 K1 109.33(13) . . ?
C4 O3 C5 112.87(19) . . ?
C4 O3 K1 119.97(14) . . ?
C5 O3 K1 119.74(15) . . ?
C6 O4 C7 111.0(2) . . ?
C6 O4 K1 111.63(14) . . ?
C7 O4 K1 109.84(16) . . ?
C8 O5 C9 112.1(2) . . ?
C8 O5 K1 120.01(16) . . ?
C9 O5 K1 118.36(17) . . ?
C10 O6 C11 112.0(2) . . ?
C10 O6 K1 112.55(17) . . ?
C11 O6 K1 110.82(14) . . ?
C44 O8 C33 112.2(2) . . ?
C44 O8 K2 110.05(13) . . ?
C33 O8 K2 108.01(15) . . ?
C34 O9 C35 111.4(2) . . ?
C34 O9 K2 120.12(16) . . ?
C35 O9 K2 121.45(15) . . ?
C37 O10 C36 110.5(2) . . ?
C37 O10 K2 112.01(14) . . ?
C36 O10 K2 109.13(14) . . ?
C38 O11 C39 112.68(18) . . ?
C38 O11 K2 120.26(14) . . ?
C39 O11 K2 119.11(13) . . ?
C41 O12 C40 111.52(18) . . ?
C41 O12 K2 107.11(13) . . ?
C40 O12 K2 106.56(12) . . ?
C42 O13 C43 112.17(18) . . ?
C42 O13 K2 118.81(13) . . ?
C43 O13 K2 120.26(14) . . ?
O1 C1 C2 108.44(19) . . ?
O2 C2 C1 108.7(2) . . ?
O2 C3 C4 109.22(19) . . ?
O3 C4 C3 108.80(19) . . ?
O3 C5 C6 108.4(2) . . ?
O4 C6 C5 109.3(2) . . ?
O4 C7 C8 109.6(2) . . ?
O5 C8 C7 109.0(2) . . ?
O5 C9 C10 108.4(2) . . ?
O6 C10 C9 109.1(2) . . ?
O6 C11 C12 108.8(2) . . ?
O1 C12 C11 109.4(2) . . ?
C16 C13 C15 110.21(19) . . ?
C16 C13 C14 107.92(19) . . ?
C15 C13 C14 107.67(19) . . ?
C16 C13 Si1 109.03(15) . . ?
C15 C13 Si1 113.78(15) . . ?
C14 C13 Si1 108.04(16) . . ?
C22 C17 C18 116.9(2) . . ?
C22 C17 Si1 122.58(17) . . ?
C18 C17 Si1 120.54(18) . . ?
C19 C18 C17 122.0(2) . . ?
C20 C19 C18 119.8(2) . . ?
C19 C20 C21 119.8(2) . . ?
C20 C21 C22 120.1(2) . . ?
C21 C22 C17 121.5(2) . . ?
C28 C23 C24 116.1(2) . . ?
C28 C23 Si1 126.11(18) . . ?
C24 C23 Si1 117.76(17) . . ?
C25 C24 C23 121.7(2) . . ?
C26 C25 C24 120.8(2) . . ?
C25 C26 C27 119.0(2) . . ?
C26 C27 C28 120.2(2) . . ?
C27 C28 C23 122.2(2) . . ?
O8 C33 C34 109.0(2) . . ?
O9 C34 C33 108.8(2) . . ?
O9 C35 C36 108.9(2) . . ?
O10 C36 C35 108.8(2) . . ?
O10 C37 C38 108.9(2) . . ?
O11 C38 C37 108.0(2) . . ?
O11 C39 C40 108.46(19) . . ?
O12 C40 C39 109.14(19) . . ?
O12 C41 C42 108.68(19) . . ?
O13 C42 C41 108.72(19) . . ?
O13 C43 C44 108.3(2) . . ?
O8 C44 C43 109.0(2) . . ?
C48 C45 C47 110.49(19) . . ?
C48 C45 C46 107.26(18) . . ?
C47 C45 C46 108.36(19) . . ?
C48 C45 Si2 114.05(16) . . ?
C47 C45 Si2 109.11(15) . . ?
C46 C45 Si2 107.37(15) . . ?
C50 C49 C54 117.5(2) . . ?
C50 C49 Si2 120.52(17) . . ?
C54 C49 Si2 122.01(17) . . ?
C51 C50 C49 121.5(2) . . ?
C52 C51 C50 119.7(2) . . ?
C53 C52 C51 119.8(2) . . ?
C52 C53 C54 120.4(2) . . ?
C53 C54 C49 121.0(2) . . ?
C56 C55 C60 116.0(2) . . ?
C56 C55 Si2 117.81(16) . . ?
C60 C55 Si2 126.23(17) . . ?
C57 C56 C55 122.2(2) . . ?
C58 C57 C56 119.7(2) . . ?
C59 C58 C57 119.5(2) . . ?
C58 C59 C60 120.4(2) . . ?
C59 C60 C55 122.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.061
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dq0244
_database_code_depnum_ccdc_archive 'CCDC 1436084'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H47 K O6.50 Si Te'
_chemical_formula_weight         706.47

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'
Te Te -0.5308 1.6751 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   16.0831(11)
_cell_length_b                   19.0939(14)
_cell_length_c                   21.8387(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6706.4(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2912
_exptl_absorpt_coefficient_mu    1.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_T_max  0.8628
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            124291
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         29.97
_reflns_number_total             19420
_reflns_number_gt                17298
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0327P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_number_reflns         19420
_refine_ls_number_parameters     718
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0614
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

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
Te1 Te -0.210185(7) 0.348011(6) 1.002844(6) 0.01827(3) Uani 1 1 d . . .
Te2 Te 0.200381(6) 0.353482(6) 0.497243(5) 0.01578(3) Uani 1 1 d . . .
K1 K -0.10264(3) 0.45867(2) 0.904684(19) 0.01638(8) Uani 1 1 d . . .
K2 K 0.10007(2) 0.470496(19) 0.593162(18) 0.01368(7) Uani 1 1 d . . .
Si1 Si -0.13197(3) 0.37242(2) 1.09602(2) 0.01213(9) Uani 1 1 d . . .
Si2 Si 0.13455(3) 0.36062(2) 0.39669(2) 0.01112(9) Uani 1 1 d . . .
O1 O 0.05195(8) 0.39039(7) 0.89871(6) 0.0193(3) Uani 1 1 d . . .
O2 O -0.07716(8) 0.33725(7) 0.82466(6) 0.0199(3) Uani 1 1 d . . .
O3 O -0.23088(9) 0.40612(7) 0.83105(6) 0.0184(3) Uani 1 1 d . . .
O4 O -0.23527(8) 0.54767(7) 0.86366(6) 0.0174(3) Uani 1 1 d . . .
O5 O -0.10343(8) 0.60053(7) 0.93170(6) 0.0184(3) Uani 1 1 d . . .
O6 O 0.04932(8) 0.53161(7) 0.92963(6) 0.0182(3) Uani 1 1 d . . .
O7 O -0.04101(9) 0.38640(7) 0.59412(7) 0.0245(3) Uani 1 1 d . . .
O8 O 0.08863(9) 0.35655(7) 0.67786(6) 0.0269(3) Uani 1 1 d . . .
O9 O 0.23768(9) 0.43766(9) 0.66906(7) 0.0312(4) Uani 1 1 d . . .
O10 O 0.22235(9) 0.57315(8) 0.61453(7) 0.0298(4) Uani 1 1 d . . .
O11 O 0.09490(9) 0.59505(7) 0.52940(7) 0.0242(3) Uani 1 1 d . . .
O12 O -0.05074(9) 0.52057(8) 0.54326(6) 0.0237(3) Uani 1 1 d . . .
O13 O 0.05202(12) 0.52533(8) 0.70334(8) 0.0403(5) Uani 1 1 d . . .
C1 C 0.06323(13) 0.33290(11) 0.85848(11) 0.0265(5) Uani 1 1 d . . .
H1A H 0.1066 0.3023 0.8739 0.032 Uiso 1 1 calc R . .
H1B H 0.0795 0.3494 0.8182 0.032 Uiso 1 1 calc R . .
C2 C -0.01776(13) 0.29395(11) 0.85457(11) 0.0254(5) Uani 1 1 d . . .
H2A H -0.0102 0.2508 0.8317 0.031 Uiso 1 1 calc R . .
H2B H -0.0371 0.2821 0.8953 0.031 Uiso 1 1 calc R . .
C3 C -0.15420(12) 0.30174(10) 0.81714(10) 0.0218(4) Uani 1 1 d . . .
H3A H -0.1745 0.2858 0.8566 0.026 Uiso 1 1 calc R . .
H3B H -0.1468 0.2612 0.7909 0.026 Uiso 1 1 calc R . .
C4 C -0.21558(12) 0.35120(10) 0.78891(9) 0.0211(4) Uani 1 1 d . . .
H4A H -0.1934 0.3701 0.7510 0.025 Uiso 1 1 calc R . .
H4B H -0.2669 0.3267 0.7797 0.025 Uiso 1 1 calc R . .
C5 C -0.29446(12) 0.45194(10) 0.81028(9) 0.0231(4) Uani 1 1 d . . .
H5A H -0.3453 0.4259 0.8031 0.028 Uiso 1 1 calc R . .
H5B H -0.2779 0.4739 0.7722 0.028 Uiso 1 1 calc R . .
C6 C -0.30847(12) 0.50648(10) 0.85841(10) 0.0229(4) Uani 1 1 d . . .
H6A H -0.3552 0.5359 0.8472 0.027 Uiso 1 1 calc R . .
H6B H -0.3209 0.4843 0.8973 0.027 Uiso 1 1 calc R . .
C7 C -0.24581(13) 0.60449(10) 0.90556(10) 0.0221(4) Uani 1 1 d . . .
H7A H -0.2595 0.5866 0.9459 0.026 Uiso 1 1 calc R . .
H7B H -0.2909 0.6345 0.8920 0.026 Uiso 1 1 calc R . .
C8 C -0.16665(12) 0.64512(9) 0.90813(9) 0.0214(4) Uani 1 1 d . . .
H8A H -0.1516 0.6612 0.8675 0.026 Uiso 1 1 calc R . .
H8B H -0.1733 0.6857 0.9344 0.026 Uiso 1 1 calc R . .
C9 C -0.02756(12) 0.63654(10) 0.94252(9) 0.0222(4) Uani 1 1 d . . .
H9A H -0.0373 0.6762 0.9693 0.027 Uiso 1 1 calc R . .
H9B H -0.0053 0.6539 0.9041 0.027 Uiso 1 1 calc R . .
C10 C 0.03328(13) 0.58730(10) 0.97163(9) 0.0218(4) Uani 1 1 d . . .
H10A H 0.0845 0.6118 0.9811 0.026 Uiso 1 1 calc R . .
H10B H 0.0105 0.5687 1.0094 0.026 Uiso 1 1 calc R . .
C11 C 0.11049(12) 0.48502(10) 0.95406(9) 0.0213(4) Uani 1 1 d . . .
H11A H 0.0905 0.4643 0.9919 0.026 Uiso 1 1 calc R . .
H11B H 0.1614 0.5104 0.9628 0.026 Uiso 1 1 calc R . .
C12 C 0.12650(12) 0.42921(10) 0.90767(10) 0.0223(4) Uani 1 1 d . . .
H12A H 0.1441 0.4502 0.8693 0.027 Uiso 1 1 calc R . .
H12B H 0.1704 0.3984 0.9219 0.027 Uiso 1 1 calc R . .
C13 C -0.09841(12) 0.46740(9) 1.10026(8) 0.0137(4) Uani 1 1 d . . .
C14 C -0.14909(12) 0.52017(9) 1.07569(9) 0.0184(4) Uani 1 1 d . . .
H14 H -0.1960 0.5077 1.0533 0.022 Uiso 1 1 calc R . .
C15 C -0.13082(13) 0.59095(10) 1.08413(9) 0.0210(4) Uani 1 1 d . . .
H15 H -0.1658 0.6251 1.0680 0.025 Uiso 1 1 calc R . .
C16 C -0.06042(13) 0.61027(10) 1.11656(9) 0.0229(4) Uani 1 1 d . . .
H16 H -0.0482 0.6574 1.1225 0.027 Uiso 1 1 calc R . .
C17 C -0.00842(13) 0.55922(10) 1.13999(9) 0.0224(4) Uani 1 1 d . . .
H17 H 0.0395 0.5721 1.1610 0.027 Uiso 1 1 calc R . .
C18 C -0.02737(12) 0.48860(10) 1.13222(9) 0.0192(4) Uani 1 1 d . . .
H18 H 0.0079 0.4549 1.1486 0.023 Uiso 1 1 calc R . .
C19 C -0.03355(11) 0.31736(8) 1.09929(8) 0.0134(3) Uani 1 1 d . . .
C20 C 0.01589(11) 0.31342(10) 1.04637(9) 0.0183(4) Uani 1 1 d . . .
H20 H 0.0005 0.3390 1.0120 0.022 Uiso 1 1 calc R . .
C21 C 0.08709(12) 0.27239(10) 1.04399(10) 0.0220(4) Uani 1 1 d . . .
H21 H 0.1188 0.2710 1.0084 0.026 Uiso 1 1 calc R . .
C22 C 0.11094(12) 0.23346(10) 1.09459(10) 0.0232(4) Uani 1 1 d . . .
H22 H 0.1584 0.2056 1.0929 0.028 Uiso 1 1 calc R . .
C23 C 0.06422(13) 0.23617(10) 1.14715(10) 0.0228(4) Uani 1 1 d . . .
H23 H 0.0801 0.2101 1.1812 0.027 Uiso 1 1 calc R . .
C24 C -0.00733(12) 0.27802(10) 1.14966(9) 0.0187(4) Uani 1 1 d . . .
H24 H -0.0381 0.2796 1.1857 0.022 Uiso 1 1 calc R . .
C25 C -0.19924(12) 0.35926(10) 1.16726(9) 0.0218(4) Uani 1 1 d . . .
C26 C -0.27782(14) 0.40472(13) 1.16111(11) 0.0377(6) Uani 1 1 d . . .
H26A H -0.3095 0.3894 1.1263 0.057 Uiso 1 1 calc R . .
H26B H -0.2620 0.4528 1.1557 0.057 Uiso 1 1 calc R . .
H26C H -0.3109 0.4003 1.1975 0.057 Uiso 1 1 calc R . .
C27 C -0.15525(14) 0.38270(11) 1.22614(9) 0.0280(5) Uani 1 1 d . . .
H27A H -0.1925 0.3778 1.2602 0.042 Uiso 1 1 calc R . .
H27B H -0.1388 0.4308 1.2223 0.042 Uiso 1 1 calc R . .
H27C H -0.1069 0.3542 1.2327 0.042 Uiso 1 1 calc R . .
C28 C -0.22687(14) 0.28257(12) 1.17350(11) 0.0337(5) Uani 1 1 d . . .
H28A H -0.1789 0.2533 1.1790 0.051 Uiso 1 1 calc R . .
H28B H -0.2560 0.2686 1.1371 0.051 Uiso 1 1 calc R . .
H28C H -0.2630 0.2779 1.2083 0.051 Uiso 1 1 calc R . .
C29 C -0.04689(15) 0.33343(12) 0.63893(12) 0.0359(6) Uani 1 1 d . . .
H29A H -0.0841 0.2967 0.6250 0.043 Uiso 1 1 calc R . .
H29B H -0.0689 0.3527 0.6767 0.043 Uiso 1 1 calc R . .
C30 C 0.03789(16) 0.30417(11) 0.64969(11) 0.0346(6) Uani 1 1 d . . .
H30A H 0.0343 0.2634 0.6761 0.042 Uiso 1 1 calc R . .
H30B H 0.0624 0.2898 0.6111 0.042 Uiso 1 1 calc R . .
C31 C 0.16928(16) 0.33149(13) 0.69110(11) 0.0379(6) Uani 1 1 d . . .
H31A H 0.1951 0.3139 0.6540 0.045 Uiso 1 1 calc R . .
H31B H 0.1661 0.2934 0.7204 0.045 Uiso 1 1 calc R . .
C32 C 0.21962(17) 0.38951(14) 0.71672(11) 0.0438(7) Uani 1 1 d . . .
H32A H 0.1890 0.4128 0.7491 0.053 Uiso 1 1 calc R . .
H32B H 0.2709 0.3713 0.7338 0.053 Uiso 1 1 calc R . .
C33 C 0.27953(14) 0.49888(14) 0.69025(11) 0.0405(6) Uani 1 1 d . . .
H33A H 0.3307 0.4859 0.7109 0.049 Uiso 1 1 calc R . .
H33B H 0.2446 0.5240 0.7191 0.049 Uiso 1 1 calc R . .
C34 C 0.29847(13) 0.54443(14) 0.63639(11) 0.0402(6) Uani 1 1 d . . .
H34A H 0.3360 0.5818 0.6483 0.048 Uiso 1 1 calc R . .
H34B H 0.3249 0.5171 0.6044 0.048 Uiso 1 1 calc R . .
C35 C 0.23393(15) 0.61330(13) 0.56040(12) 0.0402(6) Uani 1 1 d . . .
H35A H 0.2521 0.5831 0.5273 0.048 Uiso 1 1 calc R . .
H35B H 0.2764 0.6486 0.5672 0.048 Uiso 1 1 calc R . .
C36 C 0.15404(15) 0.64762(11) 0.54375(11) 0.0372(6) Uani 1 1 d . . .
H36A H 0.1342 0.6758 0.5777 0.045 Uiso 1 1 calc R . .
H36B H 0.1621 0.6781 0.5087 0.045 Uiso 1 1 calc R . .
C37 C 0.01782(14) 0.62440(11) 0.51111(10) 0.0331(5) Uani 1 1 d . . .
H37A H 0.0262 0.6561 0.4770 0.040 Uiso 1 1 calc R . .
H37B H -0.0063 0.6507 0.5447 0.040 Uiso 1 1 calc R . .
C38 C -0.03893(13) 0.56688(11) 0.49285(10) 0.0314(5) Uani 1 1 d . . .
H38A H -0.0920 0.5861 0.4802 0.038 Uiso 1 1 calc R . .
H38B H -0.0154 0.5414 0.4585 0.038 Uiso 1 1 calc R . .
C39 C -0.10797(13) 0.46698(12) 0.52814(10) 0.0306(5) Uani 1 1 d . . .
H39A H -0.0877 0.4409 0.4931 0.037 Uiso 1 1 calc R . .
H39B H -0.1611 0.4876 0.5173 0.037 Uiso 1 1 calc R . .
C40 C -0.11867(13) 0.41895(12) 0.58119(12) 0.0335(5) Uani 1 1 d . . .
H40A H -0.1375 0.4451 0.6167 0.040 Uiso 1 1 calc R . .
H40B H -0.1600 0.3836 0.5717 0.040 Uiso 1 1 calc R . .
C41 C 0.03239(11) 0.31007(9) 0.39410(8) 0.0141(3) Uani 1 1 d . . .
C42 C -0.00835(11) 0.29478(10) 0.44940(9) 0.0179(4) Uani 1 1 d . . .
H42 H 0.0151 0.3096 0.4861 0.022 Uiso 1 1 calc R . .
C43 C -0.08363(12) 0.25770(10) 0.45057(10) 0.0220(4) Uani 1 1 d . . .
H43 H -0.1097 0.2487 0.4878 0.026 Uiso 1 1 calc R . .
C44 C -0.11908(12) 0.23453(10) 0.39673(10) 0.0243(4) Uani 1 1 d . . .
H44 H -0.1682 0.2089 0.3976 0.029 Uiso 1 1 calc R . .
C45 C -0.08110(13) 0.24963(10) 0.34145(10) 0.0243(4) Uani 1 1 d . . .
H45 H -0.1050 0.2346 0.3050 0.029 Uiso 1 1 calc R . .
C46 C -0.00700(12) 0.28743(10) 0.34043(9) 0.0183(4) Uani 1 1 d . . .
H46 H 0.0171 0.2980 0.3028 0.022 Uiso 1 1 calc R . .
C47 C 0.10809(11) 0.45350(9) 0.37209(8) 0.0144(3) Uani 1 1 d . . .
C48 C 0.04775(11) 0.46687(10) 0.32767(9) 0.0186(4) Uani 1 1 d . . .
H48 H 0.0169 0.4297 0.3121 0.022 Uiso 1 1 calc R . .
C49 C 0.03249(13) 0.53404(11) 0.30600(10) 0.0238(5) Uani 1 1 d . . .
H49 H -0.0079 0.5414 0.2762 0.029 Uiso 1 1 calc R . .
C50 C 0.07739(13) 0.58982(10) 0.32866(10) 0.0260(5) Uani 1 1 d . . .
H50 H 0.0677 0.6348 0.3140 0.031 Uiso 1 1 calc R . .
C51 C 0.13668(14) 0.57879(10) 0.37314(10) 0.0261(5) Uani 1 1 d . . .
H51 H 0.1666 0.6164 0.3889 0.031 Uiso 1 1 calc R . .
C52 C 0.15180(12) 0.51104(9) 0.39458(9) 0.0197(4) Uani 1 1 d . . .
H52 H 0.1920 0.5042 0.4246 0.024 Uiso 1 1 calc R . .
C53 C 0.21200(11) 0.32763(9) 0.33570(8) 0.0148(3) Uani 1 1 d . . .
C54 C 0.23503(14) 0.25135(10) 0.34854(10) 0.0256(5) Uani 1 1 d . . .
H54A H 0.2787 0.2371 0.3213 0.038 Uiso 1 1 calc R . .
H54B H 0.1872 0.2221 0.3423 0.038 Uiso 1 1 calc R . .
H54C H 0.2537 0.2469 0.3901 0.038 Uiso 1 1 calc R . .
C55 C 0.17991(13) 0.33352(11) 0.26980(9) 0.0228(4) Uani 1 1 d . . .
H55A H 0.1577 0.3796 0.2632 0.034 Uiso 1 1 calc R . .
H55B H 0.1371 0.2993 0.2632 0.034 Uiso 1 1 calc R . .
H55C H 0.2249 0.3254 0.2418 0.034 Uiso 1 1 calc R . .
C56 C 0.29112(12) 0.37203(11) 0.34039(10) 0.0259(4) Uani 1 1 d . . .
H56A H 0.3311 0.3559 0.3109 0.039 Uiso 1 1 calc R . .
H56B H 0.3140 0.3678 0.3808 0.039 Uiso 1 1 calc R . .
H56C H 0.2779 0.4202 0.3323 0.039 Uiso 1 1 calc R . .
C57 C -0.01260(18) 0.50038(14) 0.73743(13) 0.0501(7) Uani 1 1 d . . .
H57A H 0.0039 0.4579 0.7586 0.060 Uiso 1 1 calc R . .
H57B H -0.0595 0.4895 0.7111 0.060 Uiso 1 1 calc R . .
C58 C -0.03646(13) 0.55548(11) 0.78276(9) 0.0242(4) Uani 1 1 d . . .
H58A H -0.0063 0.5498 0.8209 0.029 Uiso 1 1 calc R . .
H58B H -0.0957 0.5544 0.7911 0.029 Uiso 1 1 calc R . .
C59 C -0.01135(12) 0.62368(12) 0.75016(9) 0.0239(4) Uani 1 1 d . . .
H59A H -0.0600 0.6506 0.7384 0.029 Uiso 1 1 calc R . .
H59B H 0.0238 0.6523 0.7762 0.029 Uiso 1 1 calc R . .
C60 C 0.03599(18) 0.59830(12) 0.69404(11) 0.0421(7) Uani 1 1 d . . .
H60A H 0.0030 0.6052 0.6573 0.051 Uiso 1 1 calc R . .
H60B H 0.0878 0.6238 0.6897 0.051 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Te1 Si1 2.4373(5) . ?
Te1 K1 3.4715(5) . ?
Te2 Si2 2.4417(5) . ?
Te2 K2 3.4616(4) . ?
K1 O5 2.7723(13) . ?
K1 O3 2.8012(14) . ?
K1 O1 2.8104(14) . ?
K1 O6 2.8653(14) . ?
K1 O4 2.8707(13) . ?
K1 O2 2.9321(14) . ?
K2 O13 2.7355(16) . ?
K2 O11 2.7570(14) . ?
K2 O7 2.7798(14) . ?
K2 O10 2.8156(15) . ?
K2 O12 2.8256(14) . ?
K2 O9 2.8354(15) . ?
K2 O8 2.8617(14) . ?
Si1 C13 1.8944(18) . ?
Si1 C19 1.9015(18) . ?
Si1 C25 1.9115(19) . ?
Si2 C47 1.9013(18) . ?
Si2 C41 1.9064(18) . ?
Si2 C53 1.9293(18) . ?
O1 C1 1.417(2) . ?
O1 C12 1.423(2) . ?
O2 C3 1.422(2) . ?
O2 C2 1.422(2) . ?
O3 C4 1.417(2) . ?
O3 C5 1.420(2) . ?
O4 C6 1.420(2) . ?
O4 C7 1.429(2) . ?
O5 C9 1.420(2) . ?
O5 C8 1.423(2) . ?
O6 C10 1.428(2) . ?
O6 C11 1.430(2) . ?
O7 C29 1.411(3) . ?
O7 C40 1.423(3) . ?
O8 C31 1.412(3) . ?
O8 C30 1.430(3) . ?
O9 C32 1.419(3) . ?
O9 C33 1.426(3) . ?
O10 C35 1.421(3) . ?
O10 C34 1.424(3) . ?
O11 C36 1.418(2) . ?
O11 C37 1.418(2) . ?
O12 C39 1.415(2) . ?
O12 C38 1.425(3) . ?
O13 C57 1.364(3) . ?
O13 C60 1.431(3) . ?
C1 C2 1.502(3) . ?
C3 C4 1.499(3) . ?
C5 C6 1.497(3) . ?
C7 C8 1.492(3) . ?
C9 C10 1.499(3) . ?
C11 C12 1.493(3) . ?
C13 C18 1.399(3) . ?
C13 C14 1.403(2) . ?
C14 C15 1.395(3) . ?
C15 C16 1.386(3) . ?
C16 C17 1.383(3) . ?
C17 C18 1.393(3) . ?
C19 C24 1.397(3) . ?
C19 C20 1.405(3) . ?
C20 C21 1.388(3) . ?
C21 C22 1.386(3) . ?
C22 C23 1.373(3) . ?
C23 C24 1.402(3) . ?
C25 C27 1.534(3) . ?
C25 C28 1.536(3) . ?
C25 C26 1.539(3) . ?
C29 C30 1.492(3) . ?
C31 C32 1.482(4) . ?
C33 C34 1.494(4) . ?
C35 C36 1.487(4) . ?
C37 C38 1.483(3) . ?
C39 C40 1.488(3) . ?
C41 C46 1.401(3) . ?
C41 C42 1.405(3) . ?
C42 C43 1.403(3) . ?
C43 C44 1.380(3) . ?
C44 C45 1.383(3) . ?
C45 C46 1.393(3) . ?
C47 C52 1.394(2) . ?
C47 C48 1.396(3) . ?
C48 C49 1.389(3) . ?
C49 C50 1.379(3) . ?
C50 C51 1.377(3) . ?
C51 C52 1.397(3) . ?
C53 C54 1.529(2) . ?
C53 C56 1.533(3) . ?
C53 C55 1.533(3) . ?
C57 C58 1.495(3) . ?
C58 C59 1.538(3) . ?
C59 C60 1.522(3) . ?

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
Si1 Te1 K1 98.165(14) . . ?
Si2 Te2 K2 107.826(14) . . ?
O5 K1 O3 117.96(4) . . ?
O5 K1 O1 117.85(4) . . ?
O3 K1 O1 117.29(4) . . ?
O5 K1 O6 59.24(4) . . ?
O3 K1 O6 155.69(4) . . ?
O1 K1 O6 58.65(4) . . ?
O5 K1 O4 58.98(4) . . ?
O3 K1 O4 59.05(4) . . ?
O1 K1 O4 156.56(4) . . ?
O6 K1 O4 113.92(4) . . ?
O5 K1 O2 154.17(4) . . ?
O3 K1 O2 58.50(4) . . ?
O1 K1 O2 58.79(4) . . ?
O6 K1 O2 112.24(4) . . ?
O4 K1 O2 112.70(4) . . ?
O5 K1 Te1 117.45(3) . . ?
O3 K1 Te1 76.68(3) . . ?
O1 K1 Te1 100.79(3) . . ?
O6 K1 Te1 127.12(3) . . ?
O4 K1 Te1 100.53(3) . . ?
O2 K1 Te1 87.51(3) . . ?
O13 K2 O11 96.06(5) . . ?
O13 K2 O7 89.08(5) . . ?
O11 K2 O7 118.52(5) . . ?
O13 K2 O10 77.59(5) . . ?
O11 K2 O10 60.28(5) . . ?
O7 K2 O10 166.18(4) . . ?
O13 K2 O12 88.13(5) . . ?
O11 K2 O12 59.17(4) . . ?
O7 K2 O12 59.85(4) . . ?
O10 K2 O12 115.34(5) . . ?
O13 K2 O9 77.93(5) . . ?
O11 K2 O9 120.63(5) . . ?
O7 K2 O9 120.33(5) . . ?
O10 K2 O9 60.78(5) . . ?
O12 K2 O9 166.01(4) . . ?
O13 K2 O8 72.80(5) . . ?
O11 K2 O8 168.62(4) . . ?
O7 K2 O8 60.23(5) . . ?
O10 K2 O8 117.84(5) . . ?
O12 K2 O8 116.83(4) . . ?
O9 K2 O8 60.27(5) . . ?
O13 K2 Te2 155.64(4) . . ?
O11 K2 Te2 105.38(3) . . ?
O7 K2 Te2 90.70(3) . . ?
O10 K2 Te2 102.95(3) . . ?
O12 K2 Te2 112.65(3) . . ?
O9 K2 Te2 81.21(3) . . ?
O8 K2 Te2 86.01(3) . . ?
C13 Si1 C19 106.87(8) . . ?
C13 Si1 C25 104.32(9) . . ?
C19 Si1 C25 111.59(8) . . ?
C13 Si1 Te1 111.77(6) . . ?
C19 Si1 Te1 110.81(6) . . ?
C25 Si1 Te1 111.24(7) . . ?
C47 Si2 C41 105.72(8) . . ?
C47 Si2 C53 104.72(8) . . ?
C41 Si2 C53 111.76(8) . . ?
C47 Si2 Te2 113.78(6) . . ?
C41 Si2 Te2 111.85(6) . . ?
C53 Si2 Te2 108.83(6) . . ?
C1 O1 C12 112.38(15) . . ?
C1 O1 K1 120.08(11) . . ?
C12 O1 K1 119.82(10) . . ?
C3 O2 C2 111.17(15) . . ?
C3 O2 K1 108.91(11) . . ?
C2 O2 K1 106.25(11) . . ?
C4 O3 C5 111.93(14) . . ?
C4 O3 K1 120.67(11) . . ?
C5 O3 K1 119.53(10) . . ?
C6 O4 C7 111.94(14) . . ?
C6 O4 K1 108.26(10) . . ?
C7 O4 K1 109.73(11) . . ?
C9 O5 C8 112.61(14) . . ?
C9 O5 K1 120.30(11) . . ?
C8 O5 K1 120.73(11) . . ?
C10 O6 C11 110.37(14) . . ?
C10 O6 K1 109.27(11) . . ?
C11 O6 K1 110.81(10) . . ?
C29 O7 C40 113.08(17) . . ?
C29 O7 K2 118.30(13) . . ?
C40 O7 K2 117.55(12) . . ?
C31 O8 C30 112.03(17) . . ?
C31 O8 K2 109.32(13) . . ?
C30 O8 K2 106.87(12) . . ?
C32 O9 C33 112.95(18) . . ?
C32 O9 K2 114.35(13) . . ?
C33 O9 K2 112.13(13) . . ?
C35 O10 C34 111.96(17) . . ?
C35 O10 K2 109.22(12) . . ?
C34 O10 K2 112.83(14) . . ?
C36 O11 C37 111.65(16) . . ?
C36 O11 K2 118.61(13) . . ?
C37 O11 K2 120.63(12) . . ?
C39 O12 C38 110.79(16) . . ?
C39 O12 K2 113.80(12) . . ?
C38 O12 K2 113.18(11) . . ?
C57 O13 C60 106.26(19) . . ?
C57 O13 K2 124.16(16) . . ?
C60 O13 K2 107.37(13) . . ?
O1 C1 C2 107.92(17) . . ?
O2 C2 C1 108.70(17) . . ?
O2 C3 C4 108.72(15) . . ?
O3 C4 C3 108.28(15) . . ?
O3 C5 C6 108.22(16) . . ?
O4 C6 C5 108.48(16) . . ?
O4 C7 C8 108.52(16) . . ?
O5 C8 C7 108.19(15) . . ?
O5 C9 C10 109.13(15) . . ?
O6 C10 C9 108.23(16) . . ?
O6 C11 C12 108.04(16) . . ?
O1 C12 C11 108.66(16) . . ?
C18 C13 C14 117.24(17) . . ?
C18 C13 Si1 122.29(14) . . ?
C14 C13 Si1 120.22(14) . . ?
C15 C14 C13 121.52(18) . . ?
C16 C15 C14 119.85(18) . . ?
C17 C16 C15 119.71(17) . . ?
C16 C17 C18 120.34(19) . . ?
C17 C18 C13 121.31(18) . . ?
C24 C19 C20 116.62(17) . . ?
C24 C19 Si1 125.31(14) . . ?
C20 C19 Si1 118.03(14) . . ?
C21 C20 C19 121.86(19) . . ?
C22 C21 C20 120.07(19) . . ?
C23 C22 C21 119.67(18) . . ?
C22 C23 C24 120.2(2) . . ?
C19 C24 C23 121.56(19) . . ?
C27 C25 C28 109.70(17) . . ?
C27 C25 C26 106.69(18) . . ?
C28 C25 C26 107.94(18) . . ?
C27 C25 Si1 112.50(14) . . ?
C28 C25 Si1 111.17(14) . . ?
C26 C25 Si1 108.64(13) . . ?
O7 C29 C30 108.45(18) . . ?
O8 C30 C29 109.11(18) . . ?
O8 C31 C32 109.01(19) . . ?
O9 C32 C31 108.62(19) . . ?
O9 C33 C34 108.54(18) . . ?
O10 C34 C33 108.23(18) . . ?
O10 C35 C36 109.13(18) . . ?
O11 C36 C35 108.77(17) . . ?
O11 C37 C38 108.74(16) . . ?
O12 C38 C37 109.51(18) . . ?
O12 C39 C40 109.82(18) . . ?
O7 C40 C39 108.79(17) . . ?
C46 C41 C42 116.38(17) . . ?
C46 C41 Si2 124.81(14) . . ?
C42 C41 Si2 118.80(14) . . ?
C43 C42 C41 121.55(19) . . ?
C44 C43 C42 120.20(19) . . ?
C43 C44 C45 119.63(18) . . ?
C44 C45 C46 119.97(19) . . ?
C45 C46 C41 122.23(19) . . ?
C52 C47 C48 116.84(16) . . ?
C52 C47 Si2 121.52(14) . . ?
C48 C47 Si2 121.51(14) . . ?
C49 C48 C47 121.90(18) . . ?
C50 C49 C48 119.9(2) . . ?
C51 C50 C49 119.84(18) . . ?
C50 C51 C52 119.89(19) . . ?
C47 C52 C51 121.61(18) . . ?
C54 C53 C56 108.28(16) . . ?
C54 C53 C55 108.88(16) . . ?
C56 C53 C55 107.56(16) . . ?
C54 C53 Si2 109.93(13) . . ?
C56 C53 Si2 108.02(12) . . ?
C55 C53 Si2 114.00(13) . . ?
O13 C57 C58 108.1(2) . . ?
C57 C58 C59 102.82(16) . . ?
C60 C59 C58 103.56(16) . . ?
O13 C60 C59 106.60(18) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.062
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

