#------------------------------------------------------------------------------
#$Date: 2016-09-20 14:11:36 +0300 (Tue, 20 Sep 2016) $
#$Revision: 186650 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/31/1543105.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_1543105
loop_
_publ_author_name
'Tsoureas, Nikolaos'
'Kilpatrick, Alexander F. R.'
'Inman, Christopher J.'
'Cloke, F. Geoffrey N.'
_publ_section_title
;
 Steric control of redox events in organo-uranium chemistry: synthesis and
 characterisation of U(v) oxo and nitrido complexes
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4624
_journal_paper_doi               10.1039/C6SC00632A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C55 H95 K O7 Si2 U'
_chemical_formula_weight         1201.62
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.901(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1168(4)
_cell_length_b                   19.7384(6)
_cell_length_c                   13.0100(5)
_cell_measurement_reflns_used    6484
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9870
_cell_measurement_theta_min      3.6430
_cell_volume                     2854.40(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1033
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17568
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.470
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.58240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,Version 1.171.37.34i
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1240
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.454
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0371
_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)+(0.0246P)²+0.0683P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5357
_reflns_number_total             6004
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc00632a2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 1543100--1543105.cif.'
_cod_original_formula_sum        'C27.50 H47.50 K0.50 O3.50 Si U0.50'
_cod_database_code               1543105
_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_min   0.466
_shelx_estimated_absorpt_t_max   0.864
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
C1 C -0.0175(3) 0.21466(17) 0.4186(3) 0.0259(8) Uani 1 1 d . . .
H1 H -0.0858 0.1967 0.4521 0.031 Uiso 1 1 calc R U .
C2 C 0.0580(3) 0.16316(18) 0.3815(3) 0.0252(8) Uani 1 1 d . . .
H2 H 0.0236 0.1194 0.3891 0.030 Uiso 1 1 calc R U .
C3 C 0.1732(3) 0.16057(17) 0.3356(3) 0.0254(8) Uani 1 1 d . . .
C4 C 0.2490(3) 0.21440(16) 0.3060(3) 0.0249(8) Uani 1 1 d . . .
H4 H 0.3213 0.1974 0.2778 0.030 Uiso 1 1 calc R U .
C5 C -0.2989(5) 0.2500 0.3329(5) 0.0487(17) Uani 1 2 d S T P
H5A H -0.3067 0.2965 0.3584 0.073 Uiso 0.5 1 calc R U P
H5B H -0.2585 0.2221 0.3853 0.073 Uiso 0.5 1 calc R U P
H5C H -0.3790 0.2314 0.3179 0.073 Uiso 0.5 1 calc R U P
C6 C -0.2241(4) 0.11997(19) 0.2089(4) 0.0481(13) Uani 1 1 d . . .
H6A H -0.1941 0.0893 0.1558 0.072 Uiso 1 1 calc R U .
H6B H -0.3112 0.1141 0.2152 0.072 Uiso 1 1 calc R U .
H6C H -0.1844 0.1095 0.2748 0.072 Uiso 1 1 calc R U .
C7 C -0.1145(4) 0.1700(2) -0.0037(4) 0.0458(12) Uani 1 1 d . . .
H7A H -0.0866 0.1984 -0.0603 0.069 Uiso 1 1 calc R U .
H7B H -0.1837 0.1430 -0.0272 0.069 Uiso 1 1 calc R U .
H7C H -0.0494 0.1397 0.0188 0.069 Uiso 1 1 calc R U .
C8 C -0.1512(4) 0.21429(18) 0.0847(3) 0.0315(9) Uani 1 1 d . . .
C9 C -0.1972(3) 0.19206(18) 0.1794(3) 0.0309(10) Uani 1 1 d . . .
C10 C -0.2267(5) 0.2500 0.2374(5) 0.0293(13) Uani 1 2 d S T P
C11 C 0.1850(4) 0.0254(2) 0.5120(4) 0.0476(12) Uani 1 1 d . . .
H11A H 0.1672 0.0732 0.5253 0.071 Uiso 1 1 calc R U .
H11B H 0.2689 0.0159 0.5310 0.071 Uiso 1 1 calc R U .
H11C H 0.1318 -0.0032 0.5529 0.071 Uiso 1 1 calc R U .
C12 C 0.1645(4) 0.01015(18) 0.3976(4) 0.0356(10) Uani 1 1 d . . .
H12 H 0.0761 0.0157 0.3847 0.043 Uiso 1 1 calc R U .
C13 C 0.1918(4) -0.06481(18) 0.3771(4) 0.0455(12) Uani 1 1 d . . .
H13A H 0.1780 -0.0748 0.3041 0.068 Uiso 1 1 calc R U .
H13B H 0.1389 -0.0932 0.4186 0.068 Uiso 1 1 calc R U .
H13C H 0.2759 -0.0744 0.3956 0.068 Uiso 1 1 calc R U .
C14 C 0.4502(4) 0.1209(2) 0.4276(4) 0.0454(12) Uani 1 1 d . . .
H14A H 0.4131 0.1658 0.4226 0.068 Uiso 1 1 calc R U .
H14B H 0.5379 0.1255 0.4286 0.068 Uiso 1 1 calc R U .
H14C H 0.4246 0.0986 0.4909 0.068 Uiso 1 1 calc R U .
C15 C 0.4109(3) 0.07804(19) 0.3347(4) 0.0346(10) Uani 1 1 d . . .
H15 H 0.4457 0.1004 0.2729 0.042 Uiso 1 1 calc R U .
C16 C 0.4711(4) 0.0084(2) 0.3434(4) 0.0492(13) Uani 1 1 d . . .
H16A H 0.4468 -0.0196 0.2844 0.074 Uiso 1 1 calc R U .
H16B H 0.4462 -0.0137 0.4070 0.074 Uiso 1 1 calc R U .
H16C H 0.5587 0.0140 0.3442 0.074 Uiso 1 1 calc R U .
C17 C 0.0800(4) 0.0400(2) 0.1475(4) 0.0491(13) Uani 1 1 d . . .
H17A H 0.0322 0.0766 0.1771 0.074 Uiso 1 1 calc R U .
H17B H 0.0560 -0.0033 0.1779 0.074 Uiso 1 1 calc R U .
H17C H 0.0661 0.0385 0.0730 0.074 Uiso 1 1 calc R U .
C18 C 0.2129(4) 0.05254(19) 0.1702(3) 0.0341(10) Uani 1 1 d . . .
H18 H 0.2338 0.0944 0.1310 0.041 Uiso 1 1 calc R U .
C19 C 0.2891(4) -0.0043(2) 0.1236(4) 0.0503(13) Uani 1 1 d . . .
H19A H 0.3744 0.0043 0.1384 0.075 Uiso 1 1 calc R U .
H19B H 0.2755 -0.0057 0.0490 0.075 Uiso 1 1 calc R U .
H19C H 0.2659 -0.0479 0.1536 0.075 Uiso 1 1 calc R U .
C20 C 0.3786(7) 0.2500 0.6342(7) 0.071(2) Uani 1 2 d S T P
H20A H 0.3268 0.2500 0.6944 0.107 Uiso 1 2 calc R U P
H20B H 0.3623 0.2095 0.5928 0.107 Uiso 0.5 1 calc R U P
H20C H 0.3623 0.2905 0.5928 0.107 Uiso 0.5 1 calc R U P
C21 C 0.5074(7) 0.2500 0.6685(6) 0.0569(19) Uani 1 2 d S T P
C22 C 0.6008(7) 0.2500 0.6016(6) 0.062(2) Uani 1 2 d S T P
H22 H 0.5835 0.2500 0.5299 0.075 Uiso 1 2 calc R U P
C23 C 0.7213(7) 0.2500 0.6351(7) 0.059(2) Uani 1 2 d S T P
H23 H 0.7839 0.2500 0.5862 0.071 Uiso 1 2 calc R U P
C24 C 0.7492(7) 0.2500 0.7376(7) 0.060(2) Uani 1 2 d S T P
H24 H 0.8306 0.2500 0.7609 0.072 Uiso 1 2 calc R U P
C25 C 0.6590(8) 0.2500 0.8046(7) 0.085(3) Uani 1 2 d S T P
H25 H 0.6770 0.2500 0.8763 0.102 Uiso 1 2 calc R U P
C26 C 0.5378(8) 0.2500 0.7710(8) 0.091(3) Uani 1 2 d S T P
H26 H 0.4758 0.2500 0.8204 0.109 Uiso 1 2 calc R U P
C27 C 0.4981(4) 0.1905(2) 0.0670(4) 0.0506(13) Uani 1 1 d . . .
H27A H 0.4363 0.1856 0.1204 0.061 Uiso 1 1 calc R U .
H27B H 0.5780 0.1925 0.1014 0.061 Uiso 1 1 calc R U .
C28 C 0.4930(4) 0.1319(2) -0.0034(4) 0.0537(14) Uani 1 1 d . . .
H28A H 0.5523 0.1378 -0.0586 0.064 Uiso 1 1 calc R U .
H28B H 0.5132 0.0899 0.0347 0.064 Uiso 1 1 calc R U .
C29 C 0.3668(4) 0.0775(2) -0.1252(4) 0.0500(13) Uani 1 1 d . . .
H29A H 0.3959 0.0333 -0.0986 0.060 Uiso 1 1 calc R U .
H29B H 0.4178 0.0908 -0.1835 0.060 Uiso 1 1 calc R U .
C30 C 0.2390(4) 0.07128(18) -0.1605(4) 0.0485(13) Uani 1 1 d . . .
H30A H 0.2304 0.0331 -0.2094 0.058 Uiso 1 1 calc R U .
H30B H 0.1867 0.0624 -0.1011 0.058 Uiso 1 1 calc R U .
C31 C 0.0855(4) 0.13012(18) -0.2489(3) 0.0354(10) Uani 1 1 d . . .
H31A H 0.0276 0.1302 -0.1918 0.043 Uiso 1 1 calc R U .
H31B H 0.0734 0.0881 -0.2892 0.043 Uiso 1 1 calc R U .
C32 C 0.0652(4) 0.19066(18) -0.3160(3) 0.0344(10) Uani 1 1 d . . .
H32A H 0.1253 0.1916 -0.3713 0.041 Uiso 1 1 calc R U .
H32B H -0.0161 0.1886 -0.3481 0.041 Uiso 1 1 calc R U .
O1 O 0.1176(3) 0.2500 0.0914(3) 0.0414(10) Uani 1 2 d S T P
O2 O 0.0763(3) 0.2500 -0.2539(3) 0.0305(9) Uani 1 2 d S T P
O3 O 0.2048(2) 0.13264(12) -0.2091(2) 0.0354(7) Uani 1 1 d . . .
O4 O 0.3747(2) 0.12675(13) -0.0471(2) 0.0408(8) Uani 1 1 d . . .
O5 O 0.4775(4) 0.2500 0.0110(3) 0.0386(10) Uani 1 2 d S T P
Si1 Si 0.24048(9) 0.07430(5) 0.31093(9) 0.0262(2) Uani 1 1 d . . .
U1 U 0.03616(2) 0.2500 0.21794(2) 0.02272(7) Uani 1 2 d S T P
K1 K 0.23835(10) 0.2500 -0.07655(10) 0.0280(3) Uani 1 2 d S T 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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
C1 C1 C2 136.2(2) 4_565 .
C1 C1 U1 75.44(7) 4_565 .
C2 C1 U1 73.8(2) . .
C1 C1 H1 111.9 4_565 .
C2 C1 H1 111.9 . .
U1 C1 H1 135.3 . .
C1 C2 C3 135.6(3) . .
C1 C2 U1 76.6(2) . .
C3 C2 U1 76.4(2) . .
C1 C2 H2 112.2 . .
C3 C2 H2 112.2 . .
U1 C2 H2 128.1 . .
C4 C3 C2 129.2(3) . .
C4 C3 Si1 113.1(3) . .
C2 C3 Si1 117.7(3) . .
C4 C3 U1 72.3(2) . .
C2 C3 U1 73.7(2) . .
Si1 C3 U1 134.03(19) . .
C4 C4 C3 138.8(2) 4_565 .
C4 C4 U1 74.94(7) 4_565 .
C3 C4 U1 77.8(2) . .
C4 C4 H4 110.6 4_565 .
C3 C4 H4 110.6 . .
U1 C4 H4 131.9 . .
C10 C5 H5A 109.5 . .
C10 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C10 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C9 C6 H6A 109.5 . .
C9 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C9 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C8 C7 H7A 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C8 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C8 C8 C9 108.1(2) 4_565 .
C8 C8 C7 125.5(2) 4_565 .
C9 C8 C7 126.3(4) . .
C8 C8 U1 75.31(7) 4_565 .
C9 C8 U1 79.2(2) . .
C7 C8 U1 114.5(3) . .
C10 C9 C8 107.8(3) . .
C10 C9 C6 125.5(4) . .
C8 C9 C6 126.3(4) . .
C10 C9 U1 78.5(3) . .
C8 C9 U1 72.0(2) . .
C6 C9 U1 121.0(2) . .
C9 C10 C9 108.2(5) 4_565 .
C9 C10 C5 125.3(3) 4_565 .
C9 C10 C5 125.3(3) . .
C9 C10 U1 73.4(3) 4_565 .
C9 C10 U1 73.4(3) . .
C5 C10 U1 128.4(4) . .
C12 C11 H11A 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C12 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C11 C12 C13 109.3(4) . .
C11 C12 Si1 112.6(3) . .
C13 C12 Si1 116.6(3) . .
C11 C12 H12 105.8 . .
C13 C12 H12 105.8 . .
Si1 C12 H12 105.8 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 H14A 109.5 . .
C15 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C15 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 C15 C14 108.5(3) . .
C16 C15 Si1 114.0(3) . .
C14 C15 Si1 114.6(3) . .
C16 C15 H15 106.3 . .
C14 C15 H15 106.3 . .
Si1 C15 H15 106.3 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C18 C17 H17A 109.5 . .
C18 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C18 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C17 C18 C19 110.1(3) . .
C17 C18 Si1 111.4(3) . .
C19 C18 Si1 117.6(3) . .
C17 C18 H18 105.6 . .
C19 C18 H18 105.6 . .
Si1 C18 H18 105.6 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C21 C20 H20A 109.5 . .
C21 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C21 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C22 C21 C26 116.2(8) . .
C22 C21 C20 123.0(8) . .
C26 C21 C20 120.8(8) . .
C21 C22 C23 122.3(8) . .
C21 C22 H22 118.9 . .
C23 C22 H22 118.9 . .
C24 C23 C22 120.3(8) . .
C24 C23 H23 119.8 . .
C22 C23 H23 119.8 . .
C25 C24 C23 118.4(8) . .
C25 C24 H24 120.8 . .
C23 C24 H24 120.8 . .
C24 C25 C26 121.3(9) . .
C24 C25 H25 119.4 . .
C26 C25 H25 119.3 . .
C21 C26 C25 121.5(9) . .
C21 C26 H26 119.3 . .
C25 C26 H26 119.3 . .
O5 C27 C28 109.3(4) . .
O5 C27 H27A 109.8 . .
C28 C27 H27A 109.8 . .
O5 C27 H27B 109.8 . .
C28 C27 H27B 109.8 . .
H27A C27 H27B 108.3 . .
O4 C28 C27 109.2(4) . .
O4 C28 H28A 109.8 . .
C27 C28 H28A 109.8 . .
O4 C28 H28B 109.8 . .
C27 C28 H28B 109.8 . .
H28A C28 H28B 108.3 . .
O4 C29 C30 109.1(4) . .
O4 C29 H29A 109.9 . .
C30 C29 H29A 109.9 . .
O4 C29 H29B 109.9 . .
C30 C29 H29B 109.9 . .
H29A C29 H29B 108.3 . .
O3 C30 C29 108.4(3) . .
O3 C30 H30A 110.0 . .
C29 C30 H30A 110.0 . .
O3 C30 H30B 110.0 . .
C29 C30 H30B 110.0 . .
H30A C30 H30B 108.4 . .
O3 C31 C32 108.5(3) . .
O3 C31 H31A 110.0 . .
C32 C31 H31A 110.0 . .
O3 C31 H31B 110.0 . .
C32 C31 H31B 110.0 . .
H31A C31 H31B 108.4 . .
O2 C32 C31 108.3(3) . .
O2 C32 H32A 110.0 . .
C31 C32 H32A 110.0 . .
O2 C32 H32B 110.0 . .
C31 C32 H32B 110.0 . .
H32A C32 H32B 108.4 . .
U1 O1 K1 177.3(2) . .
C32 O2 C32 110.3(4) 4_565 .
C32 O2 K1 119.8(2) 4_565 .
C32 O2 K1 119.8(2) . .
C30 O3 C31 112.1(3) . .
C30 O3 K1 112.7(2) . .
C31 O3 K1 110.8(2) . .
C29 O4 C28 112.5(3) . .
C29 O4 K1 117.3(2) . .
C28 O4 K1 118.1(2) . .
C27 O5 C27 114.2(5) 4_565 .
C27 O5 K1 110.4(2) 4_565 .
C27 O5 K1 110.4(2) . .
C3 Si1 C18 107.98(17) . .
C3 Si1 C12 108.60(18) . .
C18 Si1 C12 110.72(18) . .
C3 Si1 C15 109.32(16) . .
C18 Si1 C15 108.0(2) . .
C12 Si1 C15 112.18(18) . .
O1 U1 C4 86.63(14) . 4_565
O1 U1 C4 86.63(14) . .
C4 U1 C4 30.11(14) 4_565 .
O1 U1 C2 129.66(10) . 4_565
C4 U1 C2 56.11(11) 4_565 4_565
C4 U1 C2 76.55(11) . 4_565
O1 U1 C2 129.66(10) . .
C4 U1 C2 76.55(11) 4_565 .
C4 U1 C2 56.11(11) . .
C2 U1 C2 77.44(15) 4_565 .
O1 U1 C1 158.66(11) . .
C4 U1 C1 82.33(11) 4_565 .
C4 U1 C1 74.69(11) . .
C2 U1 C1 56.27(11) 4_565 .
C2 U1 C1 29.57(10) . .
O1 U1 C1 158.67(11) . 4_565
C4 U1 C1 74.69(11) 4_565 4_565
C4 U1 C1 82.33(11) . 4_565
C2 U1 C1 29.57(10) 4_565 4_565
C2 U1 C1 56.26(11) . 4_565
C1 U1 C1 29.11(14) . 4_565
O1 U1 C3 102.34(12) . .
C4 U1 C3 57.52(10) 4_565 .
C4 U1 C3 29.84(10) . .
C2 U1 C3 85.90(10) 4_565 .
C2 U1 C3 29.89(11) . .
C1 U1 C3 56.36(11) . .
C1 U1 C3 76.45(11) 4_565 .
O1 U1 C3 102.34(12) . 4_565
C4 U1 C3 29.84(10) 4_565 4_565
C4 U1 C3 57.52(10) . 4_565
C2 U1 C3 29.89(11) 4_565 4_565
C2 U1 C3 85.90(10) . 4_565
C1 U1 C3 76.45(11) . 4_565
C1 U1 C3 56.36(11) 4_565 4_565
C3 U1 C3 78.97(14) . 4_565
O1 U1 C8 79.71(14) . 4_565
C4 U1 C8 147.14(11) 4_565 4_565
C4 U1 C8 166.33(12) . 4_565
C2 U1 C8 112.47(11) 4_565 4_565
C2 U1 C8 134.37(11) . 4_565
C1 U1 C8 118.70(12) . 4_565
C1 U1 C8 110.66(12) 4_565 4_565
C3 U1 C8 154.75(10) . 4_565
C3 U1 C8 125.59(10) 4_565 4_565
O1 U1 C8 79.70(14) . .
C4 U1 C8 166.33(12) 4_565 .
C4 U1 C8 147.14(11) . .
C2 U1 C8 134.37(11) 4_565 .
C2 U1 C8 112.47(11) . .
C1 U1 C8 110.66(12) . .
C1 U1 C8 118.70(12) 4_565 .
C3 U1 C8 125.59(10) . .
C3 U1 C8 154.75(10) 4_565 .
C8 U1 C8 29.38(15) 4_565 .
O1 U1 C9 106.96(14) . 4_565
C4 U1 C9 138.76(10) 4_565 4_565
C4 U1 C9 163.51(12) . 4_565
C2 U1 C9 87.43(11) 4_565 4_565
C2 U1 C9 116.95(12) . 4_565
C1 U1 C9 93.28(12) . 4_565
C1 U1 C9 81.78(12) 4_565 4_565
C3 U1 C9 146.71(12) . 4_565
C3 U1 C9 109.23(10) 4_565 4_565
C8 U1 C9 28.88(12) 4_565 4_565
C8 U1 C9 47.65(11) . 4_565
O1 K1 O5 98.90(13) . .
O1 K1 O4 99.58(8) . 4_565
O5 K1 O4 57.82(6) . 4_565
O1 K1 O4 99.58(8) . .
O5 K1 O4 57.82(6) . .
O4 K1 O4 114.73(11) 4_565 .
O1 K1 O2 110.36(12) . .
O5 K1 O2 150.74(13) . .
O4 K1 O2 115.03(7) 4_565 .
O4 K1 O2 115.03(7) . .
O1 K1 O3 115.99(8) . .
O5 K1 O3 110.10(8) . .
O4 K1 O3 144.24(10) 4_565 .
O4 K1 O3 57.99(8) . .
O2 K1 O3 57.11(6) . .
O1 K1 O3 115.99(8) . 4_565
O5 K1 O3 110.10(8) . 4_565
O4 K1 O3 57.99(8) 4_565 4_565
O4 K1 O3 144.24(10) . 4_565
O2 K1 O3 57.12(6) . 4_565
O3 K1 O3 105.60(12) . 4_565
O1 K1 U1 1.15(8) . .
O5 K1 U1 97.75(10) . .
O4 K1 U1 98.98(7) 4_565 .
O4 K1 U1 98.98(7) . .
O2 K1 U1 111.51(9) . .
O3 K1 U1 116.52(6) . .
O3 K1 U1 116.52(6) 4_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C1 1.395(7) 4_565
C1 C2 1.408(5) .
C1 U1 2.776(4) .
C1 H1 0.9500 .
C2 C3 1.423(5) .
C2 U1 2.740(4) .
C2 H2 0.9500 .
C3 C4 1.413(5) .
C3 Si1 1.889(4) .
C3 U1 2.776(3) .
C4 C4 1.405(7) 4_565
C4 U1 2.705(3) .
C4 H4 0.9500 .
C5 C10 1.490(9) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C9 1.505(5) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.506(6) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C8 1.410(7) 4_565
C8 C9 1.412(6) .
C8 U1 2.780(4) .
C9 C10 1.411(5) .
C9 U1 2.872(4) .
C10 C9 1.411(5) 4_565
C10 U1 2.937(5) .
C11 C12 1.532(6) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C13 1.534(5) .
C12 Si1 1.902(4) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.533(6) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.532(5) .
C15 Si1 1.916(4) .
C15 H15 1.0000 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 C18 1.522(6) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 C19 1.537(6) .
C18 Si1 1.901(4) .
C18 H18 1.0000 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.493(10) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 C22 1.365(10) .
C21 C26 1.370(12) .
C22 C23 1.403(10) .
C22 H22 0.9500 .
C23 C24 1.364(11) .
C23 H23 0.9500 .
C24 C25 1.340(11) .
C24 H24 0.9500 .
C25 C26 1.410(12) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C27 O5 1.399(5) .
C27 C28 1.475(6) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C28 O4 1.428(5) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 O4 1.408(5) .
C29 C30 1.492(6) .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C30 O3 1.415(5) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C31 O3 1.417(5) .
C31 C32 1.495(5) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C32 O2 1.427(4) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
O1 U1 1.892(4) .
O1 K1 2.582(5) .
O2 C32 1.427(4) 4_565
O2 K1 2.905(4) .
O3 K1 2.908(3) .
O4 K1 2.889(3) .
O5 C27 1.399(5) 4_565
O5 K1 2.876(4) .
U1 C4 2.705(3) 4_565
U1 C2 2.740(4) 4_565
U1 C1 2.776(4) 4_565
U1 C3 2.776(3) 4_565
U1 C8 2.780(4) 4_565
U1 C9 2.872(4) 4_565
K1 O4 2.889(3) 4_565
K1 O3 2.908(3) 4_565
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
C1 C1 C2 C3 6.8(7) 4_565 .
U1 C1 C2 C3 53.9(5) . .
C1 C1 C2 U1 -47.1(2) 4_565 .
C1 C2 C3 C4 -4.3(8) . .
U1 C2 C3 C4 49.7(4) . .
C1 C2 C3 Si1 174.4(4) . .
U1 C2 C3 Si1 -131.6(2) . .
C1 C2 C3 U1 -54.0(5) . .
C2 C3 C4 C4 -0.6(6) . 4_565
Si1 C3 C4 C4 -179.37(11) . 4_565
U1 C3 C4 C4 49.6(2) . 4_565
C2 C3 C4 U1 -50.2(4) . .
Si1 C3 C4 U1 131.1(2) . .
C8 C8 C9 C10 0.6(3) 4_565 .
C7 C8 C9 C10 -176.4(4) . .
U1 C8 C9 C10 71.1(3) . .
C8 C8 C9 C6 173.9(3) 4_565 .
C7 C8 C9 C6 -3.1(6) . .
U1 C8 C9 C6 -115.6(4) . .
C8 C8 C9 U1 -70.48(8) 4_565 .
C7 C8 C9 U1 112.5(4) . .
C8 C9 C10 C9 -1.0(6) . 4_565
C6 C9 C10 C9 -174.3(3) . 4_565
U1 C9 C10 C9 65.6(3) . 4_565
C8 C9 C10 C5 167.7(5) . .
C6 C9 C10 C5 -5.7(7) . .
U1 C9 C10 C5 -125.7(5) . .
C8 C9 C10 U1 -66.6(3) . .
C6 C9 C10 U1 120.0(4) . .
C26 C21 C22 C23 0.000(2) . .
C20 C21 C22 C23 180.000(2) . .
C21 C22 C23 C24 0.000(2) . .
C22 C23 C24 C25 0.000(3) . .
C23 C24 C25 C26 0.000(3) . .
C22 C21 C26 C25 0.000(3) . .
C20 C21 C26 C25 180.000(2) . .
C24 C25 C26 C21 0.000(3) . .
O5 C27 C28 O4 -63.5(5) . .
O4 C29 C30 O3 66.4(5) . .
O3 C31 C32 O2 -63.1(4) . .
C31 C32 O2 C32 176.3(2) . 4_565
C31 C32 O2 K1 31.0(4) . .
C29 C30 O3 C31 177.6(4) . .
C29 C30 O3 K1 -56.6(4) . .
C32 C31 O3 C30 -169.0(4) . .
C32 C31 O3 K1 64.2(4) . .
C30 C29 O4 C28 175.4(4) . .
C30 C29 O4 K1 -42.6(5) . .
C27 C28 O4 C29 172.2(4) . .
C27 C28 O4 K1 30.6(5) . .
C28 C27 O5 C27 -170.9(3) . 4_565
C28 C27 O5 K1 64.1(4) . .
C4 C3 Si1 C18 -81.8(3) . .
C2 C3 Si1 C18 99.3(3) . .
U1 C3 Si1 C18 5.5(3) . .
C4 C3 Si1 C12 158.1(3) . .
C2 C3 Si1 C12 -20.8(4) . .
U1 C3 Si1 C12 -114.6(3) . .
C4 C3 Si1 C15 35.4(3) . .
C2 C3 Si1 C15 -143.5(3) . .
U1 C3 Si1 C15 122.8(2) . .
