#------------------------------------------------------------------------------
#$Date: 2019-11-24 12:11:58 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237880 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/89/4088916.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4088916
loop_
_publ_author_name
'El Aziz, Youssef'
'Taylor, Peter G.'
'Bassindale, Alan R.'
'Coles, Simon J.'
'Pitak, Mateusz B.'
_publ_section_title
;
 Synthesis and Structures of Novel Molecular Ionic Compounds Based on
 Encapsulation of Anions and Cations
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4004
_journal_paper_doi               10.1021/acs.organomet.6b00565
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C52 H80 K O34 Si8, F'
_chemical_formula_sum            'C52 H80 F K O34 Si8'
_chemical_formula_weight         1531.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                73.882(13)
_cell_angle_beta                 79.293(13)
_cell_angle_gamma                88.688(14)
_cell_formula_units_Z            1
_cell_length_a                   8.445(3)
_cell_length_b                   14.704(5)
_cell_length_c                   16.727(5)
_cell_measurement_reflns_used    5493
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      2.5
_cell_volume                     1959.8(11)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29209
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.980
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.903
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     1165
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1032P)²+2.5805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7413
_reflns_number_total             8934
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00565_si_002.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088916
_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.
;
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2A-O8A
 1.2 with sigma of 0.01
 C1-O7A
 1.455 with sigma of 0.01
 O7A-C2A
 1.34 with sigma of 0.01
 C2A-C3A
 1.49 with sigma of 0.01
 C3A-C5A
 1.318 with sigma of 0.01
 C3A-C4A
 1.506 with sigma of 0.01
 C2B-O8B
 1.2 with sigma of 0.01
 C1-O7B
 1.455 with sigma of 0.01
 O7B-C2B
 1.34 with sigma of 0.01
 C2B-C3B
 1.49 with sigma of 0.01
 C3B-C5B
 1.318 with sigma of 0.01
 C3B-C4B
 1.506 with sigma of 0.01
 C16-O13
 1.455 with sigma of 0.01
 C16-O13
 1.455 with sigma of 0.01
 C18A-C19A
 1.5 with sigma of 0.01
 C18-C19
 1.5 with sigma of 0.01
 C18A-C20A
 1.32 with sigma of 0.01
 C18-C20
 1.32 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H1BC)=Sof(H1BD)=Sof(O7B)=Sof(O8B)=Sof(C2B)=Sof(C3B)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(H4BC)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(O7A)=Sof(O8A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=FVAR(1)
 Sof(H16C)=Sof(H16D)=Sof(O13A)=Sof(O14A)=Sof(C17A)=Sof(C18A)=Sof(C19A)=
 Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(H16A)=Sof(H16B)=Sof(O13)=Sof(O14)=Sof(C17)=Sof(C18)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C6(H6A,H6B), C11(H11A,H11B), C16(H16A,H16B),
 C16(H16C,H16D), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B)
7.b Me refined with riding coordinates:
 C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC)
7.c X=CH2 refined with riding coordinates:
 C9(H9A,H9B), C14(H14A,H14B), C5A(H5AA,H5AB), C20(H20A,H20B), C5B(H5BA,H5BB),
 C20A(H20C,H20D)
7.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C19A(H19D,H19E,
 H19F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Si1 Si 0.83077(9) 0.41849(6) 0.91955(6) 0.0291(2) Uani 1 1 d . U . . .
Si2 Si 0.71769(9) 0.43863(6) 1.09676(6) 0.0282(2) Uani 1 1 d . U . . .
Si3 Si 1.15770(9) 0.35547(6) 0.96450(5) 0.0268(2) Uani 1 1 d . U . . .
Si4 Si 0.95643(9) 0.62533(6) 0.85711(5) 0.0286(2) Uani 1 1 d . U . . .
O1 O 0.7156(2) 0.40783(15) 1.01103(14) 0.0317(5) Uani 1 1 d . U . . .
O2 O 0.7241(2) 0.55255(15) 1.08133(14) 0.0301(5) Uani 1 1 d . U . . .
O3 O 0.8740(2) 0.67135(15) 0.93241(14) 0.0305(4) Uani 1 1 d . U . . .
O4 O 0.8643(2) 0.52781(15) 0.86304(14) 0.0311(5) Uani 1 1 d . U . . .
O5 O 0.9930(2) 0.35827(15) 0.92706(14) 0.0307(5) Uani 1 1 d . U . . .
O6 O 0.8503(2) 0.38362(15) 1.14954(14) 0.0306(5) Uani 1 1 d . U . . .
O9 O 1.2753(3) 0.25769(16) 0.85209(14) 0.0351(5) Uani 1 1 d . U . . .
O10 O 1.3996(5) 0.1211(2) 0.86992(19) 0.0750(11) Uani 1 1 d . U . . .
O11 O 0.8052(3) 0.3863(2) 0.77382(17) 0.0486(6) Uani 1 1 d . U . . .
O12 O 0.6729(6) 0.2759(4) 0.7462(3) 0.127(2) Uani 1 1 d . U . . .
C1 C 0.9226(4) 0.7070(3) 0.7542(2) 0.0439(8) Uani 1 1 d D U . . .
H1AA H 0.9224 0.6700 0.7130 0.053 Uiso 0.579(6) 1 calc R . . A 1
H1AB H 0.8153 0.7351 0.7631 0.053 Uiso 0.579(6) 1 calc R . . A 1
H1BC H 0.8488 0.6743 0.7309 0.053 Uiso 0.421(6) 1 calc R . . A 2
H1BD H 0.8667 0.7631 0.7661 0.053 Uiso 0.421(6) 1 calc R . . A 2
C6 C 1.2713(3) 0.2522(2) 0.9405(2) 0.0303(6) Uani 1 1 d . U . . .
H6A H 1.3824 0.2542 0.9512 0.036 Uiso 1 1 calc R . . . .
H6B H 1.2173 0.1921 0.9773 0.036 Uiso 1 1 calc R . . . .
C7 C 1.3421(4) 0.1860(2) 0.8252(2) 0.0404(7) Uani 1 1 d . U . . .
C8 C 1.3287(5) 0.1926(3) 0.7369(2) 0.0506(9) Uani 1 1 d . U . . .
C9 C 1.2156(8) 0.2441(5) 0.7027(3) 0.095(2) Uani 1 1 d . U . . .
H9A H 1.1431 0.2768 0.7349 0.114 Uiso 1 1 calc R . . . .
H9B H 1.2066 0.2485 0.6460 0.114 Uiso 1 1 calc R . . . .
C10 C 1.4432(8) 0.1342(4) 0.6939(3) 0.0813(16) Uani 1 1 d . U . . .
H10A H 1.4265 0.0673 0.7259 0.122 Uiso 1 1 calc GR . . . .
H10B H 1.5542 0.1545 0.6913 0.122 Uiso 1 1 calc GR . . . .
H10C H 1.4239 0.1427 0.6363 0.122 Uiso 1 1 calc GR . . . .
C11 C 0.7114(4) 0.3647(2) 0.8601(2) 0.0378(7) Uani 1 1 d . U . . .
H11A H 0.6976 0.2954 0.8857 0.045 Uiso 1 1 calc R . . . .
H11B H 0.6036 0.3926 0.8602 0.045 Uiso 1 1 calc R . . . .
C12 C 0.7698(6) 0.3396(4) 0.7235(3) 0.0724(13) Uani 1 1 d . U . . .
C13 C 0.8729(8) 0.3741(5) 0.6359(4) 0.0864(16) Uani 1 1 d . U . . .
C14 C 0.8502(12) 0.3340(7) 0.5768(5) 0.130(3) Uani 1 1 d . U . . .
H14A H 0.9120 0.3553 0.5212 0.156 Uiso 1 1 calc R . . . .
H14B H 0.7723 0.2838 0.5902 0.156 Uiso 1 1 calc R . . . .
C15 C 0.9901(9) 0.4516(6) 0.6210(4) 0.105(2) Uani 1 1 d . U . . .
H15A H 1.0448 0.4691 0.5616 0.158 Uiso 1 1 calc GR . . . .
H15B H 1.0697 0.4312 0.6577 0.158 Uiso 1 1 calc GR . . . .
H15C H 0.9342 0.5065 0.6338 0.158 Uiso 1 1 calc GR . . . .
C16 C 0.5199(4) 0.3954(2) 1.1665(2) 0.0399(7) Uani 1 1 d D U . . .
H16A H 0.4319 0.4123 1.1338 0.048 Uiso 0.632(17) 1 calc R . . B 1
H16B H 0.5188 0.3256 1.1894 0.048 Uiso 0.632(17) 1 calc R . . B 1
H16C H 0.4298 0.4268 1.1402 0.048 Uiso 0.368(17) 1 calc R . . B 2
H16D H 0.5061 0.3260 1.1778 0.048 Uiso 0.368(17) 1 calc R . . B 2
O7A O 1.0440(5) 0.7825(3) 0.7190(3) 0.0393(11) Uani 0.579(6) 1 d D U . A 1
O8A O 1.1643(10) 0.7124(6) 0.6219(5) 0.104(3) Uani 0.579(6) 1 d D U . A 1
O13 O 0.4972(14) 0.4391(7) 1.2345(5) 0.0406(17) Uani 0.632(17) 1 d D U . B 1
O14 O 0.3812(14) 0.3075(9) 1.3321(6) 0.073(3) Uani 0.632(17) 1 d . U . B 1
C2A C 1.1542(9) 0.7775(6) 0.6525(4) 0.0602(18) Uani 0.579(6) 1 d D U . A 1
C3A C 1.2931(18) 0.8441(11) 0.6218(10) 0.100(4) Uani 0.579(6) 1 d D U . A 1
C4A C 1.2562(15) 0.9262(8) 0.6581(7) 0.097(3) Uani 0.579(6) 1 d D U . A 1
H4AA H 1.1883 0.9043 0.7144 0.145 Uiso 0.579(6) 1 calc R . . A 1
H4AB H 1.3570 0.9545 0.6626 0.145 Uiso 0.579(6) 1 calc R . . A 1
H4AC H 1.1992 0.9737 0.6210 0.145 Uiso 0.579(6) 1 calc R . . A 1
C5A C 1.3849(16) 0.8597(12) 0.5448(7) 0.129(5) Uani 0.579(6) 1 d D U . A 1
H5AA H 1.3614 0.8267 0.5067 0.155 Uiso 0.579(6) 1 calc R . . A 1
H5AB H 1.4737 0.9036 0.5281 0.155 Uiso 0.579(6) 1 calc R . . A 1
C17 C 0.4416(16) 0.3868(9) 1.3129(8) 0.057(2) Uani 0.632(17) 1 d . U . B 1
C18 C 0.4357(10) 0.4452(9) 1.3735(5) 0.070(2) Uani 0.632(17) 1 d D U . B 1
C19 C 0.3454(16) 0.3980(13) 1.4603(6) 0.111(4) Uani 0.632(17) 1 d D U . B 1
H19A H 0.2609 0.3555 1.4566 0.167 Uiso 0.632(17) 1 calc GR . . B 1
H19B H 0.2962 0.4461 1.4867 0.167 Uiso 0.632(17) 1 calc GR . . B 1
H19C H 0.4198 0.3613 1.4946 0.167 Uiso 0.632(17) 1 calc GR . . B 1
C20 C 0.5105(12) 0.5288(9) 1.3507(6) 0.083(3) Uani 0.632(17) 1 d D U . B 1
H20A H 0.5092 0.5636 1.3909 0.099 Uiso 0.632(17) 1 calc R . . B 1
H20B H 0.5656 0.5543 1.2940 0.099 Uiso 0.632(17) 1 calc R . . B 1
O7B O 1.0603(7) 0.7390(5) 0.6913(4) 0.0409(15) Uani 0.421(6) 1 d D U . A 2
O8B O 1.1201(11) 0.8477(6) 0.7525(5) 0.072(2) Uani 0.421(6) 1 d D U . A 2
O13A O 0.527(2) 0.4213(13) 1.2468(11) 0.045(3) Uani 0.368(17) 1 d . U . B 2
O14A O 0.420(3) 0.2829(12) 1.3164(14) 0.078(5) Uani 0.368(17) 1 d . U . B 2
C2B C 1.1505(11) 0.8091(6) 0.6970(6) 0.0489(19) Uani 0.421(6) 1 d D U . A 2
C3B C 1.266(2) 0.8534(14) 0.6191(11) 0.082(4) Uani 0.421(6) 1 d D U . A 2
C4B C 1.3135(18) 0.7819(13) 0.5691(10) 0.101(4) Uani 0.421(6) 1 d D U . A 2
H4BA H 1.2173 0.7458 0.5692 0.151 Uiso 0.421(6) 1 calc R . . A 2
H4BB H 1.3624 0.8154 0.5106 0.151 Uiso 0.421(6) 1 calc R . . A 2
H4BC H 1.3912 0.7386 0.5951 0.151 Uiso 0.421(6) 1 calc R . . A 2
C5B C 1.395(2) 0.9028(14) 0.6195(14) 0.124(6) Uani 0.421(6) 1 d D U . A 2
H5BA H 1.4154 0.9105 0.6712 0.148 Uiso 0.421(6) 1 calc R . . A 2
H5BB H 1.4676 0.9305 0.5679 0.148 Uiso 0.421(6) 1 calc R . . A 2
C17A C 0.455(4) 0.3590(17) 1.3179(18) 0.066(4) Uani 0.368(17) 1 d . U . B 2
C18A C 0.473(2) 0.4014(13) 1.3929(11) 0.074(4) Uani 0.368(17) 1 d D U . B 2
C19A C 0.385(4) 0.3379(19) 1.4738(12) 0.114(8) Uani 0.368(17) 1 d D U . B 2
H19D H 0.2872 0.3119 1.4642 0.171 Uiso 0.368(17) 1 calc GR . . B 2
H19E H 0.3568 0.3739 1.5155 0.171 Uiso 0.368(17) 1 calc GR . . B 2
H19F H 0.4549 0.2860 1.4953 0.171 Uiso 0.368(17) 1 calc GR . . B 2
C20A C 0.578(2) 0.4717(15) 1.3857(13) 0.094(7) Uani 0.368(17) 1 d D U . B 2
H20C H 0.6016 0.4840 1.4351 0.113 Uiso 0.368(17) 1 calc R . . B 2
H20D H 0.6285 0.5090 1.3312 0.113 Uiso 0.368(17) 1 calc R . . B 2
K1 K 1.5000 0.0000 1.0000 0.0318(2) Uani 1 2 d S TU P . .
O15 O 1.6849(3) 0.13498(19) 1.0373(2) 0.0552(7) Uani 1 1 d . U . . .
O16 O 1.8299(3) 0.0281(2) 0.9238(2) 0.0541(7) Uani 1 1 d . U . . .
O17 O 1.6201(3) -0.0700(2) 0.8620(2) 0.0544(7) Uani 1 1 d . U . . .
C21 C 1.8496(5) 0.1183(3) 1.0208(3) 0.0593(11) Uani 1 1 d . U . . .
H21A H 1.8733 0.0582 1.0606 0.071 Uiso 1 1 calc R . . . .
H21B H 1.9116 0.1701 1.0293 0.071 Uiso 1 1 calc R . . . .
C22 C 1.8994(4) 0.1129(3) 0.9314(3) 0.0482(9) Uani 1 1 d . U . . .
H22A H 1.8620 0.1690 0.8919 0.058 Uiso 1 1 calc R . . . .
H22B H 2.0184 0.1121 0.9166 0.058 Uiso 1 1 calc R . . . .
C23 C 1.8548(5) 0.0229(3) 0.8408(3) 0.0589(10) Uani 1 1 d . U . . .
H23A H 1.9719 0.0284 0.8174 0.071 Uiso 1 1 calc R . . . .
H23B H 1.8027 0.0768 0.8063 0.071 Uiso 1 1 calc R . . . .
C24 C 1.7897(5) -0.0662(3) 0.8345(3) 0.0585(11) Uani 1 1 d . U . . .
H24A H 1.8160 -0.0694 0.7752 0.070 Uiso 1 1 calc R . . . .
H24B H 1.8383 -0.1208 0.8703 0.070 Uiso 1 1 calc R . . . .
C25 C 1.5441(5) -0.1508(3) 0.8569(3) 0.0539(9) Uani 1 1 d . U . . .
H25A H 1.5790 -0.2076 0.8967 0.065 Uiso 1 1 calc R . . . .
H25B H 1.5745 -0.1576 0.7988 0.065 Uiso 1 1 calc R . . . .
C26 C 1.3674(5) -0.1428(3) 0.8784(3) 0.0530(10) Uani 1 1 d . U . . .
H26A H 1.3337 -0.0865 0.8377 0.064 Uiso 1 1 calc R . . . .
H26B H 1.3140 -0.1993 0.8726 0.064 Uiso 1 1 calc R . . . .
F1 F 1.0000 0.5000 1.0000 0.0292(5) Uani 1 2 d S TU P . .
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'
F F 0.0171 0.0103 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Si1 O4 113.15(12) . .
O1 Si1 C11 105.25(14) . .
O4 Si1 C11 104.75(14) . .
O5 Si1 O1 112.39(12) . .
O5 Si1 O4 113.66(11) . .
O5 Si1 C11 106.74(13) . .
O1 Si2 O2 113.23(12) . .
O1 Si2 C16 105.15(14) . .
O2 Si2 C16 106.17(13) . .
O6 Si2 O1 112.89(12) . .
O6 Si2 O2 113.73(12) . .
O6 Si2 C16 104.64(15) . .
O2 Si3 O3 113.49(12) 2_767 2_767
O2 Si3 O5 113.74(12) 2_767 .
O2 Si3 C6 105.93(12) 2_767 .
O3 Si3 C6 103.34(13) 2_767 .
O5 Si3 O3 113.08(11) . 2_767
O5 Si3 C6 106.11(13) . .
O3 Si4 C1 107.70(15) . .
O4 Si4 O3 111.62(12) . .
O4 Si4 O6 113.79(12) . 2_767
O4 Si4 C1 103.77(15) . .
O6 Si4 O3 112.45(12) 2_767 .
O6 Si4 C1 106.82(14) 2_767 .
Si1 O1 Si2 138.52(13) . .
Si3 O2 Si2 141.30(13) 2_767 .
Si4 O3 Si3 138.67(14) . 2_767
Si4 O4 Si1 142.94(15) . .
Si1 O5 Si3 140.46(14) . .
Si2 O6 Si4 141.10(14) . 2_767
C7 O9 C6 116.6(3) . .
C7 O10 K1 165.0(3) . .
C12 O11 C11 118.3(4) . .
Si4 C1 H1AA 109.0 . .
Si4 C1 H1AB 109.0 . .
Si4 C1 H1BC 108.1 . .
Si4 C1 H1BD 108.1 . .
H1AA C1 H1AB 107.8 . .
H1BC C1 H1BD 107.3 . .
O7A C1 Si4 112.8(3) . .
O7A C1 H1AA 109.0 . .
O7A C1 H1AB 109.0 . .
O7B C1 Si4 116.6(3) . .
O7B C1 H1BC 108.1 . .
O7B C1 H1BD 108.1 . .
Si3 C6 H6A 110.0 . .
Si3 C6 H6B 110.0 . .
O9 C6 Si3 108.3(2) . .
O9 C6 H6A 110.0 . .
O9 C6 H6B 110.0 . .
H6A C6 H6B 108.4 . .
O9 C7 C8 113.3(3) . .
O10 C7 O9 122.6(3) . .
O10 C7 C8 124.0(3) . .
C7 C8 C10 115.6(4) . .
C9 C8 C7 119.8(4) . .
C9 C8 C10 124.5(4) . .
C8 C9 H9A 120.0 . .
C8 C9 H9B 120.0 . .
H9A C9 H9B 120.0 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Si1 C11 H11A 110.7 . .
Si1 C11 H11B 110.7 . .
O11 C11 Si1 105.2(2) . .
O11 C11 H11A 110.7 . .
O11 C11 H11B 110.7 . .
H11A C11 H11B 108.8 . .
O11 C12 C13 111.2(5) . .
O12 C12 O11 122.8(5) . .
O12 C12 C13 125.9(5) . .
C14 C13 C12 118.5(7) . .
C14 C13 C15 123.8(7) . .
C15 C13 C12 117.7(5) . .
C13 C14 H14A 120.0 . .
C13 C14 H14B 120.0 . .
H14A C14 H14B 120.0 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15B 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
Si2 C16 H16A 110.1 . .
Si2 C16 H16B 110.1 . .
Si2 C16 H16C 110.9 . .
Si2 C16 H16D 110.9 . .
H16A C16 H16B 108.4 . .
H16C C16 H16D 108.9 . .
O13 C16 Si2 108.0(5) . .
O13 C16 H16A 110.1 . .
O13 C16 H16B 110.1 . .
O13A C16 Si2 104.4(9) . .
O13A C16 H16C 110.9 . .
O13A C16 H16D 110.9 . .
C2A O7A C1 118.1(5) . .
C17 O13 C16 119.2(9) . .
O7A C2A C3A 120.4(8) . .
O8A C2A O7A 124.2(7) . .
O8A C2A C3A 114.2(8) . .
C2A C3A C4A 108.2(9) . .
C5A C3A C2A 123.5(12) . .
C5A C3A C4A 118.6(13) . .
C3A C4A H4AA 109.5 . .
C3A C4A H4AB 109.5 . .
C3A C4A H4AC 109.5 . .
H4AA C4A H4AB 109.5 . .
H4AA C4A H4AC 109.5 . .
H4AB C4A H4AC 109.5 . .
C3A C5A H5AA 120.0 . .
C3A C5A H5AB 120.0 . .
H5AA C5A H5AB 120.0 . .
O13 C17 C18 110.0(9) . .
O14 C17 O13 125.3(12) . .
O14 C17 C18 123.8(10) . .
C19 C18 C17 113.6(10) . .
C20 C18 C17 121.4(8) . .
C20 C18 C19 124.9(10) . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C18 C20 H20A 120.0 . .
C18 C20 H20B 120.0 . .
H20A C20 H20B 120.0 . .
C2B O7B C1 118.4(7) . .
C17A O13A C16 115.1(18) . .
O7B C2B C3B 114.2(8) . .
O8B C2B O7B 123.8(9) . .
O8B C2B C3B 120.2(10) . .
C2B C3B C4B 109.9(12) . .
C5B C3B C2B 122.2(16) . .
C5B C3B C4B 110.1(17) . .
C3B C4B H4BA 109.5 . .
C3B C4B H4BB 109.5 . .
C3B C4B H4BC 109.5 . .
H4BA C4B H4BB 109.5 . .
H4BA C4B H4BC 109.5 . .
H4BB C4B H4BC 109.5 . .
C3B C5B H5BA 120.0 . .
C3B C5B H5BB 120.0 . .
H5BA C5B H5BB 120.0 . .
O13A C17A C18A 106.4(18) . .
O14A C17A O13A 120(2) . .
O14A C17A C18A 132(2) . .
C19A C18A C17A 109.0(16) . .
C20A C18A C17A 124.1(16) . .
C20A C18A C19A 125.5(18) . .
C18A C19A H19D 109.5 . .
C18A C19A H19E 109.5 . .
C18A C19A H19F 109.5 . .
H19D C19A H19E 109.5 . .
H19D C19A H19F 109.5 . .
H19E C19A H19F 109.5 . .
C18A C20A H20C 120.0 . .
C18A C20A H20D 120.0 . .
H20C C20A H20D 120.0 . .
O10 K1 O10 180.0 2_857 .
O10 K1 O15 95.68(11) . .
O10 K1 O15 84.32(11) 2_857 .
O10 K1 O15 84.32(11) . 2_857
O10 K1 O15 95.68(11) 2_857 2_857
O10 K1 O16 85.79(11) . 2_857
O10 K1 O16 94.21(11) 2_857 2_857
O10 K1 O16 85.79(11) 2_857 .
O10 K1 O16 94.21(11) . .
O10 K1 O17 104.20(9) 2_857 .
O10 K1 O17 75.80(9) . .
O10 K1 O17 104.20(9) . 2_857
O10 K1 O17 75.80(9) 2_857 2_857
O15 K1 O15 180.0 2_857 .
O15 K1 O16 118.77(9) 2_857 .
O15 K1 O16 118.77(9) . 2_857
O15 K1 O16 61.23(9) 2_857 2_857
O15 K1 O16 61.23(9) . .
O16 K1 O16 180.00(13) . 2_857
O17 K1 O15 119.56(9) 2_857 2_857
O17 K1 O15 119.56(9) . .
O17 K1 O15 60.44(9) 2_857 .
O17 K1 O15 60.44(9) . 2_857
O17 K1 O16 60.02(9) 2_857 2_857
O17 K1 O16 119.98(9) . 2_857
O17 K1 O16 60.02(9) . .
O17 K1 O16 119.98(9) 2_857 .
O17 K1 O17 180.00(7) . 2_857
C21 O15 K1 111.6(2) . .
C21 O15 C26 111.9(3) . 2_857
C26 O15 K1 112.7(2) 2_857 .
C22 O16 K1 112.8(2) . .
C23 O16 K1 111.2(2) . .
C23 O16 C22 112.8(3) . .
C24 O17 K1 117.3(2) . .
C25 O17 K1 117.5(2) . .
C25 O17 C24 114.0(3) . .
O15 C21 H21A 109.7 . .
O15 C21 H21B 109.7 . .
O15 C21 C22 109.9(4) . .
H21A C21 H21B 108.2 . .
C22 C21 H21A 109.7 . .
C22 C21 H21B 109.7 . .
O16 C22 C21 109.1(3) . .
O16 C22 H22A 109.9 . .
O16 C22 H22B 109.9 . .
C21 C22 H22A 109.9 . .
C21 C22 H22B 109.9 . .
H22A C22 H22B 108.3 . .
O16 C23 H23A 109.2 . .
O16 C23 H23B 109.2 . .
O16 C23 C24 112.2(4) . .
H23A C23 H23B 107.9 . .
C24 C23 H23A 109.2 . .
C24 C23 H23B 109.2 . .
O17 C24 C23 108.8(4) . .
O17 C24 H24A 109.9 . .
O17 C24 H24B 109.9 . .
C23 C24 H24A 109.9 . .
C23 C24 H24B 109.9 . .
H24A C24 H24B 108.3 . .
O17 C25 H25A 109.8 . .
O17 C25 H25B 109.8 . .
O17 C25 C26 109.5(3) . .
H25A C25 H25B 108.2 . .
C26 C25 H25A 109.8 . .
C26 C25 H25B 109.8 . .
O15 C26 C25 112.6(3) 2_857 .
O15 C26 H26A 109.1 2_857 .
O15 C26 H26B 109.1 2_857 .
C25 C26 H26A 109.1 . .
C25 C26 H26B 109.1 . .
H26A C26 H26B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.622(2) .
Si1 O4 1.623(2) .
Si1 O5 1.620(2) .
Si1 C11 1.865(3) .
Si2 O1 1.622(2) .
Si2 O2 1.623(2) .
Si2 O6 1.618(2) .
Si2 C16 1.862(3) .
Si3 O2 1.617(2) 2_767
Si3 O3 1.630(2) 2_767
Si3 O5 1.623(2) .
Si3 C6 1.874(3) .
Si4 O3 1.629(2) .
Si4 O4 1.617(2) .
Si4 O6 1.620(2) 2_767
Si4 C1 1.873(4) .
O2 Si3 1.617(2) 2_767
O3 Si3 1.630(2) 2_767
O6 Si4 1.620(2) 2_767
O9 C6 1.453(4) .
O9 C7 1.331(4) .
O10 C7 1.194(4) .
O10 K1 2.663(3) .
O11 C11 1.464(4) .
O11 C12 1.301(5) .
O12 C12 1.189(7) .
C1 H1AA 0.9900 .
C1 H1AB 0.9900 .
C1 H1BC 0.9900 .
C1 H1BD 0.9900 .
C1 O7A 1.447(5) .
C1 O7B 1.406(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.478(5) .
C8 C9 1.320(7) .
C8 C10 1.495(6) .
C9 H9A 0.9500 .
C9 H9B 0.9500 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.515(8) .
C13 C14 1.327(9) .
C13 C15 1.464(9) .
C14 H14A 0.9500 .
C14 H14B 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C16 H16C 0.9900 .
C16 H16D 0.9900 .
C16 O13 1.437(6) .
C16 O13A 1.506(16) .
O7A C2A 1.329(7) .
O8A C2A 1.198(7) .
O13 C17 1.327(13) .
O14 C17 1.217(14) .
C2A C3A 1.465(9) .
C3A C4A 1.498(9) .
C3A C5A 1.337(9) .
C4A H4AA 0.9800 .
C4A H4AB 0.9800 .
C4A H4AC 0.9800 .
C5A H5AA 0.9500 .
C5A H5AB 0.9500 .
C17 C18 1.493(16) .
C18 C19 1.492(8) .
C18 C20 1.319(8) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9500 .
C20 H20B 0.9500 .
O7B C2B 1.330(8) .
O8B C2B 1.204(8) .
O13A C17A 1.33(3) .
O14A C17A 1.17(3) .
C2B C3B 1.469(9) .
C3B C4B 1.519(10) .
C3B C5B 1.327(10) .
C4B H4BA 0.9800 .
C4B H4BB 0.9800 .
C4B H4BC 0.9800 .
C5B H5BA 0.9500 .
C5B H5BB 0.9500 .
C17A C18A 1.58(3) .
C18A C19A 1.486(10) .
C18A C20A 1.343(9) .
C19A H19D 0.9800 .
C19A H19E 0.9800 .
C19A H19F 0.9800 .
C20A H20C 0.9500 .
C20A H20D 0.9500 .
K1 O10 2.663(3) 2_857
K1 O15 2.821(3) 2_857
K1 O15 2.821(3) .
K1 O16 2.828(3) .
K1 O16 2.828(3) 2_857
K1 O17 2.796(3) .
K1 O17 2.796(3) 2_857
O15 C21 1.396(5) .
O15 C26 1.432(5) 2_857
O16 C22 1.436(4) .
O16 C23 1.388(6) .
O17 C24 1.417(5) .
O17 C25 1.394(5) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C21 C22 1.500(6) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C23 C24 1.471(6) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C25 C26 1.478(6) .
C26 O15 1.432(5) 2_857
C26 H26A 0.9900 .
C26 H26B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Si2 C16 O13 C17 -136.1(9) . .
Si2 C16 O13A C17A -144.0(16) . .
Si4 C1 O7A C2A 106.0(5) . .
Si4 C1 O7B C2B -79.1(7) . .
O1 Si1 O4 Si4 69.6(3) . .
O1 Si1 O5 Si3 -66.5(3) . .
O1 Si1 C11 O11 172.2(2) . .
O1 Si2 O2 Si3 -68.2(3) . 2_767
O1 Si2 O6 Si4 66.7(3) . 2_767
O1 Si2 C16 O13 -166.6(4) . .
O1 Si2 C16 O13A 177.9(7) . .
O2 Si2 O1 Si1 62.5(2) . .
O2 Si2 O6 Si4 -64.1(3) . 2_767
O2 Si2 C16 O13 -46.3(4) . .
O2 Si2 C16 O13A -61.8(7) . .
O2 Si3 O5 Si1 -64.6(3) 2_767 .
O2 Si3 C6 O9 -72.9(2) 2_767 .
O3 Si3 O5 Si1 66.7(3) 2_767 .
O3 Si3 C6 O9 167.48(18) 2_767 .
O3 Si4 O4 Si1 -69.2(3) . .
O3 Si4 C1 O7A 85.4(3) . .
O3 Si4 C1 O7B 125.0(4) . .
O4 Si1 O1 Si2 -62.1(2) . .
O4 Si1 O5 Si3 63.7(3) . .
O4 Si1 C11 O11 52.6(2) . .
O4 Si4 O3 Si3 62.8(2) . 2_767
O4 Si4 C1 O7A -156.1(3) . .
O4 Si4 C1 O7B -116.6(4) . .
O5 Si1 O1 Si2 68.3(2) . .
O5 Si1 O4 Si4 -60.2(3) . .
O5 Si1 C11 O11 -68.2(2) . .
O5 Si3 C6 O9 48.3(2) . .
O6 Si2 O1 Si1 -68.6(2) . .
O6 Si2 O2 Si3 62.4(3) . 2_767
O6 Si2 C16 O13 74.3(4) . .
O6 Si2 C16 O13A 58.8(7) . .
O6 Si4 O3 Si3 -66.5(2) 2_767 2_767
O6 Si4 O4 Si1 59.4(3) 2_767 .
O6 Si4 C1 O7A -35.6(3) 2_767 .
O6 Si4 C1 O7B 4.0(4) 2_767 .
O9 C7 C8 C9 -22.0(6) . .
O9 C7 C8 C10 161.2(4) . .
O10 C7 C8 C9 154.5(6) . .
O10 C7 C8 C10 -22.3(6) . .
O11 C12 C13 C14 -179.4(6) . .
O11 C12 C13 C15 -0.6(8) . .
O12 C12 C13 C14 3.4(11) . .
O12 C12 C13 C15 -177.8(7) . .
C1 Si4 O3 Si3 176.1(2) . 2_767
C1 Si4 O4 Si1 175.1(2) . .
C1 O7A C2A O8A -3.6(12) . .
C1 O7A C2A C3A -171.1(11) . .
C1 O7B C2B O8B -0.8(12) . .
C1 O7B C2B C3B -165.5(12) . .
C6 Si3 O5 Si1 179.3(2) . .
C6 O9 C7 O10 -1.6(5) . .
C6 O9 C7 C8 174.9(3) . .
C7 O9 C6 Si3 -175.5(2) . .
C11 Si1 O1 Si2 -175.9(2) . .
C11 Si1 O4 Si4 -176.3(2) . .
C11 Si1 O5 Si3 178.7(2) . .
C11 O11 C12 O12 -5.5(8) . .
C11 O11 C12 C13 177.2(4) . .
C12 O11 C11 Si1 164.7(3) . .
C16 Si2 O1 Si1 177.9(2) . .
C16 Si2 O2 Si3 177.0(2) . 2_767
C16 Si2 O6 Si4 -179.5(2) . 2_767
C16 O13 C17 O14 -13.3(19) . .
C16 O13 C17 C18 177.0(8) . .
C16 O13A C17A O14A 15(3) . .
C16 O13A C17A C18A -178.7(14) . .
O7A C2A C3A C4A -17.2(19) . .
O7A C2A C3A C5A -162.4(15) . .
O8A C2A C3A C4A 174.1(11) . .
O8A C2A C3A C5A 29(2) . .
O13 C17 C18 C19 168.7(10) . .
O13 C17 C18 C20 -13.8(15) . .
O14 C17 C18 C19 -1.2(16) . .
O14 C17 C18 C20 176.3(12) . .
O7B C2B C3B C4B -28(2) . .
O7B C2B C3B C5B -159.4(19) . .
O8B C2B C3B C4B 166.6(12) . .
O8B C2B C3B C5B 35(3) . .
O13A C17A C18A C19A 176(2) . .
O13A C17A C18A C20A -16(3) . .
O14A C17A C18A C19A -19(4) . .
O14A C17A C18A C20A 148(3) . .
K1 O10 C7 O9 2.9(16) . .
K1 O10 C7 C8 -173.3(11) . .
K1 O15 C21 C22 54.0(4) . .
K1 O16 C22 C21 46.0(4) . .
K1 O16 C23 C24 -54.8(4) . .
K1 O17 C24 C23 -38.4(5) . .
K1 O17 C25 C26 42.9(4) . .
O15 C21 C22 O16 -69.1(4) . .
O16 C23 C24 O17 63.4(5) . .
O17 C25 C26 O15 -60.8(5) . 2_857
C22 O16 C23 C24 177.3(3) . .
C23 O16 C22 C21 173.1(3) . .
C24 O17 C25 C26 -174.2(4) . .
C25 O17 C24 C23 178.5(4) . .
C26 O15 C21 C22 -178.7(3) 2_857 .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.000 0.500 208.5 57.2
