# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2beta


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H31 Li O4 Si, 0.5 (C4 H8 O)'
_chemical_formula_sum            'C28 H35 Li O4.50 Si'
_chemical_formula_weight         478.59

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'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'

_cell_length_a                   11.9898(9)
_cell_length_b                   11.9898(9)
_cell_length_c                   21.5449(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2682.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_F_000             1023.8
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.120
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30183
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.961
_diffrn_reflns_theta_max         26.402
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1837
_reflns_number_gt                1216
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1500P)²+3.0000P]
 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         1837
_refine_ls_number_parameters     114
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0961
_refine_ls_wR_factor_ref         0.3126
_refine_ls_wR_factor_gt          0.2733
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002

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 0.6667 0.3333 0.13890(6) 0.0602(6) Uani 1 3 d S T P A .
C9 C 0.5056(4) 0.2868(4) 0.09917(14) 0.0605(10) Uani 1 1 d . . . . .
C10 C 0.4878(5) 0.3427(5) 0.04606(18) 0.0851(13) Uani 1 1 d . . . . .
H10 H 0.5605 0.4076 0.0255 0.102 Uiso 1 1 calc R U . . .
C11 C 0.3662(5) 0.3056(5) 0.0226(2) 0.0923(15) Uani 1 1 d . . . . .
H11 H 0.3581 0.3468 -0.0128 0.111 Uiso 1 1 calc R U . . .
C12 C 0.2592(5) 0.2108(5) 0.0502(2) 0.0833(13) Uani 1 1 d . . . . .
H12 H 0.1772 0.1860 0.0341 0.100 Uiso 1 1 calc R U . . .
C13 C 0.2719(4) 0.1511(4) 0.1019(2) 0.0797(12) Uani 1 1 d . . . . .
H13 H 0.1985 0.0837 0.1208 0.096 Uiso 1 1 calc R U . . .
C14 C 0.3928(4) 0.1904(4) 0.12601(18) 0.0665(10) Uani 1 1 d . . . . .
H14 H 0.3991 0.1502 0.1622 0.080 Uiso 1 1 calc R U . . .
Li1 Li 0.6667 0.3333 0.2619(4) 0.055(2) Uani 1 3 d S T P . .
O1 O 0.8318(11) 0.4978(11) 0.3126(5) 0.0953(13) Uiso 0.3333 1 d D U P A -1
O2 O 0.7533(11) 0.2373(10) 0.3007(5) 0.0953(13) Uiso 0.3333 1 d D U P A -1
O3 O 0.5094(10) 0.1736(10) 0.2983(5) 0.0953(13) Uiso 0.3333 1 d D U P A -1
O4 O 0.5678(11) 0.4160(11) 0.3028(4) 0.0953(13) Uiso 0.3333 1 d D U P A -1
C1 C 0.8836(15) 0.4364(12) 0.3497(7) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H1A H 0.8821 0.4632 0.3925 0.114 Uiso 0.3333 1 calc R U P A -1
H1B H 0.9746 0.4761 0.3380 0.114 Uiso 0.3333 1 calc R U P A -1
C2 C 0.8341(15) 0.2946(12) 0.3524(6) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H2A H 0.9061 0.2778 0.3514 0.114 Uiso 0.3333 1 calc R U P A -1
H2B H 0.7858 0.2587 0.3909 0.114 Uiso 0.3333 1 calc R U P A -1
C3 C 0.6652(11) 0.1045(11) 0.3098(8) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H3A H 0.6981 0.0702 0.3417 0.114 Uiso 0.3333 1 calc R U P A -1
H3B H 0.6551 0.0572 0.2712 0.114 Uiso 0.3333 1 calc R U P A -1
C4 C 0.5375(13) 0.0867(14) 0.3296(7) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H4A H 0.4698 -0.0019 0.3208 0.114 Uiso 0.3333 1 calc R U P A -1
H4B H 0.5384 0.1005 0.3745 0.114 Uiso 0.3333 1 calc R U P A -1
C5 C 0.4187(12) 0.2029(13) 0.3244(8) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H5A H 0.3685 0.1398 0.3566 0.114 Uiso 0.3333 1 calc R U P A -1
H5B H 0.3592 0.1993 0.2923 0.114 Uiso 0.3333 1 calc R U P A -1
C6 C 0.4896(14) 0.3352(11) 0.3519(6) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H6A H 0.4293 0.3623 0.3663 0.114 Uiso 0.3333 1 calc R U P A -1
H6B H 0.5430 0.3378 0.3870 0.114 Uiso 0.3333 1 calc R U P A -1
C7 C 0.6473(14) 0.5211(14) 0.3416(7) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H7A H 0.5996 0.5133 0.3798 0.114 Uiso 0.3333 1 calc R U P A -1
H7B H 0.6630 0.6003 0.3208 0.114 Uiso 0.3333 1 calc R U P A -1
C8 C 0.7749(13) 0.5360(16) 0.3593(6) 0.0953(13) Uiso 0.3333 1 d D U P A -1
H8A H 0.8341 0.6265 0.3696 0.114 Uiso 0.3333 1 calc R U P A -1
H8B H 0.7637 0.4849 0.3967 0.114 Uiso 0.3333 1 calc R U P A -1
O5 O 0.138(4) 0.036(3) 0.253(2) 0.140(7) Uiso 0.1667 1 d D U P B -1
C15 C 0.054(4) -0.094(4) 0.235(4) 0.140(7) Uiso 0.1667 1 d D U P B -1
H15A H 0.0781 -0.1534 0.2534 0.168 Uiso 0.1667 1 calc R U P B -1
H15B H 0.0470 -0.1051 0.1896 0.168 Uiso 0.1667 1 calc R U P B -1
C16 C -0.066(6) -0.106(6) 0.263(3) 0.140(7) Uiso 0.1667 1 d D U P B -1
H16A H -0.0815 -0.1484 0.3037 0.168 Uiso 0.1667 1 calc R U P B -1
H16B H -0.1403 -0.1594 0.2365 0.168 Uiso 0.1667 1 calc R U P B -1
C17 C -0.052(4) 0.025(5) 0.271(3) 0.140(7) Uiso 0.1667 1 d D U P B -1
H17A H -0.1182 0.0317 0.2474 0.168 Uiso 0.1667 1 calc R U P B -1
H17B H -0.0563 0.0441 0.3145 0.168 Uiso 0.1667 1 calc R U P B -1
C18 C 0.080(5) 0.113(5) 0.244(5) 0.140(7) Uiso 0.1667 1 d D U P B -1
H18A H 0.0756 0.1324 0.2005 0.168 Uiso 0.1667 1 calc R U P B -1
H18B H 0.1250 0.1939 0.2679 0.168 Uiso 0.1667 1 calc R U P B -1


_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
Si1 C9 1.923(4) 2_655 ?
Si1 C9 1.923(4) 3_665 ?
Si1 C9 1.923(4) . ?
Si1 Li1 2.650(8) . ?
C9 C14 1.391(5) . ?
C9 C10 1.395(5) . ?
C10 C11 1.390(6) . ?
C10 H10 0.9400 . ?
C11 C12 1.354(7) . ?
C11 H11 0.9400 . ?
C12 C13 1.373(6) . ?
C12 H12 0.9400 . ?
C13 C14 1.382(6) . ?
C13 H13 0.9400 . ?
C14 H14 0.9400 . ?
Li1 O3 2.056(11) . ?
Li1 O2 2.074(12) . ?
Li1 O4 2.084(12) . ?
Li1 O1 2.258(13) . ?
O1 C8 1.413(5) . ?
O1 C1 1.421(5) . ?
O2 C2 1.409(5) . ?
O2 C3 1.417(5) . ?
O3 C4 1.415(5) . ?
O3 C5 1.416(5) . ?
O4 C7 1.412(5) . ?
O4 C6 1.423(5) . ?
C1 C2 1.496(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.499(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.498(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.499(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
O5 C15 1.420(5) . ?
O5 C18 1.421(5) . ?
C15 C16 1.501(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 C17 1.501(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.501(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?

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
C9 Si1 C9 101.70(13) 2_655 3_665 ?
C9 Si1 C9 101.70(13) 2_655 . ?
C9 Si1 C9 101.70(13) 3_665 . ?
C9 Si1 Li1 116.43(11) 2_655 . ?
C9 Si1 Li1 116.43(11) 3_665 . ?
C9 Si1 Li1 116.43(11) . . ?
C14 C9 C10 114.9(4) . . ?
C14 C9 Si1 118.3(3) . . ?
C10 C9 Si1 126.7(3) . . ?
C11 C10 C9 122.2(4) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 119.2(4) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C9 123.0(4) . . ?
C13 C14 H14 118.5 . . ?
C9 C14 H14 118.5 . . ?
O3 Li1 O2 79.0(4) . . ?
O3 Li1 O4 78.8(4) . . ?
O2 Li1 O4 131.0(6) . . ?
O3 Li1 O1 128.6(5) . . ?
O2 Li1 O1 80.0(4) . . ?
O4 Li1 O1 80.7(4) . . ?
O3 Li1 Si1 112.4(3) . . ?
O2 Li1 Si1 113.8(3) . . ?
O4 Li1 Si1 115.0(3) . . ?
O1 Li1 Si1 119.0(3) . . ?
C8 O1 C1 100.1(10) . . ?
C8 O1 Li1 105.8(9) . . ?
C1 O1 Li1 103.8(8) . . ?
C2 O2 C3 112.5(11) . . ?
C2 O2 Li1 117.4(9) . . ?
C3 O2 Li1 112.4(9) . . ?
C4 O3 C5 119.2(12) . . ?
C4 O3 Li1 115.0(9) . . ?
C5 O3 Li1 112.4(9) . . ?
C7 O4 C6 95.1(11) . . ?
C7 O4 Li1 112.6(8) . . ?
C6 O4 Li1 109.2(9) . . ?
O1 C1 C2 125.6(12) . . ?
O1 C1 H1A 105.9 . . ?
C2 C1 H1A 105.9 . . ?
O1 C1 H1B 105.9 . . ?
C2 C1 H1B 105.9 . . ?
H1A C1 H1B 106.2 . . ?
O2 C2 C1 108.0(11) . . ?
O2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
O2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
O2 C3 C4 109.5(13) . . ?
O2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 C3 111.2(12) . . ?
O3 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
O3 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O3 C5 C6 108.7(12) . . ?
O3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.3 . . ?
O4 C6 C5 105.0(12) . . ?
O4 C6 H6A 110.7 . . ?
C5 C6 H6A 110.7 . . ?
O4 C6 H6B 110.7 . . ?
C5 C6 H6B 110.7 . . ?
H6A C6 H6B 108.8 . . ?
O4 C7 C8 116.8(12) . . ?
O4 C7 H7A 108.1 . . ?
C8 C7 H7A 108.1 . . ?
O4 C7 H7B 108.1 . . ?
C8 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
O1 C8 C7 114.2(12) . . ?
O1 C8 H8A 108.7 . . ?
C7 C8 H8A 108.7 . . ?
O1 C8 H8B 108.7 . . ?
C7 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C15 O5 C18 112(4) . . ?
O5 C15 C16 97(5) . . ?
O5 C15 H15A 112.4 . . ?
C16 C15 H15A 112.4 . . ?
O5 C15 H15B 112.4 . . ?
C16 C15 H15B 112.4 . . ?
H15A C15 H15B 110.0 . . ?
C15 C16 C17 110(6) . . ?
C15 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
C15 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C18 C17 C16 103(5) . . ?
C18 C17 H17A 111.1 . . ?
C16 C17 H17A 111.1 . . ?
C18 C17 H17B 111.1 . . ?
C16 C17 H17B 111.1 . . ?
H17A C17 H17B 109.1 . . ?
O5 C18 C17 100(4) . . ?
C17 C18 H18A 111.7 . . ?
O5 C18 H18B 111.7 . . ?
C17 C18 H18B 111.7 . . ?
H18A C18 H18B 109.5 . . ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.060

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 993779'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3beta

_vrf_PLAT019_3beta               
;
PROBLEM: _diffrn_measured_fraction_theta_full/_max < 1.0      0.977 Why ?
RESPONSE:
	The overall data quality is quite low due to large disordered parts and
	high temperature data collection (necessary because of an phase transition)
;
_vrf_PLAT242_3beta               
;
PROBLEM: Low Ueq as Compared to Neighbors for .....        Na1 Check 
RESPONSE:
	Neighbors of Na1 are strongly disordered atoms.
;
_vrf_PLAT340_3beta               
;
PROBLEM:  Low Bond Precision on  C-C Bonds ...............     0.0115 Ang.
RESPONSE:
	The overall data quality is quite low due to large disordered parts and
	high temperature data collection (necessary because of an phase transition)
;
_vrf_PLAT411_3beta               
;
PROBLEM: Short Inter H...H Contact  H13    ..  H19A    ..       1.97 Ang.  
RESPONSE:
	H19A is part of the disordered THF molecule. The discrete orientation
	of the THF molecule however is not significant and the model is rather
	to adress the diffuse electron density in the void.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H35 Na O5 Si, 0.5 (C4 H8 O)'
_chemical_formula_sum            'C30 H39 Na O5.50 Si'
_chemical_formula_weight         538.69

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'
Na Na 0.0362 0.0249 '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      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   12.858(5)
_cell_length_b                   12.858(5)
_cell_length_c                   10.756(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1540.1(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    0.126
_shelx_estimated_absorpt_T_min   0.951
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4593
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.829
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             1817
_reflns_number_gt                1052
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0100P)²+4.0000P]
 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         1817
_refine_ls_number_parameters     123
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1155
_refine_ls_wR_factor_ref         0.2141
_refine_ls_wR_factor_gt          0.1900
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.004

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 0.3333 0.6667 0.2608(2) 0.0855(9) Uani 1 3 d S T P A .
C11 C 0.4824(6) 0.7744(5) 0.1814(5) 0.0825(16) Uani 1 1 d . . . . .
C12 C 0.5855(6) 0.7864(5) 0.2308(6) 0.0918(18) Uani 1 1 d . . . . .
H12 H 0.5795 0.7403 0.3012 0.110 Uiso 1 1 calc R U . . .
C13 C 0.6985(6) 0.8628(6) 0.1829(7) 0.105(2) Uani 1 1 d . . . . .
H13 H 0.7663 0.8650 0.2184 0.126 Uiso 1 1 calc R U . . .
C14 C 0.5000(7) 0.8495(7) 0.0811(6) 0.129(3) Uani 1 1 d . . . . .
H14 H 0.4326 0.8471 0.0440 0.155 Uiso 1 1 calc R U . . .
C15 C 0.7116(8) 0.9345(6) 0.0848(7) 0.119(2) Uani 1 1 d . . . . .
H15 H 0.7882 0.9881 0.0531 0.142 Uiso 1 1 calc R U . . .
C16 C 0.6125(8) 0.9276(8) 0.0336(7) 0.149(4) Uani 1 1 d . . . . .
H16 H 0.6201 0.9764 -0.0349 0.178 Uiso 1 1 calc R U . . .
Na1 Na 0.3333 0.6667 0.5381(3) 0.0742(10) Uani 1 3 d DS T P . .
O1 O 0.2913(11) 0.8310(8) 0.6026(15) 0.175(3) Uiso 0.3333 1 d D U P A -1
O2 O 0.5111(8) 0.8366(11) 0.6472(14) 0.175(3) Uiso 0.3333 1 d D U P A -1
O3 O 0.5061(8) 0.6303(10) 0.5785(14) 0.175(3) Uiso 0.3333 1 d D U P A -1
O4 O 0.2437(9) 0.4804(9) 0.6721(13) 0.175(3) Uiso 0.3333 1 d D U P A -1
O5 O 0.1302(8) 0.6080(11) 0.6293(15) 0.175(3) Uiso 0.3333 1 d D U P A -1
C1 C 0.4056(15) 0.9320(8) 0.6405(19) 0.175(3) Uiso 0.3333 1 d D U P A -1
H1A H 0.3932 0.9944 0.6780 0.210 Uiso 0.3333 1 calc R U P A -1
H1B H 0.4581 0.9664 0.5680 0.210 Uiso 0.3333 1 calc R U P A -1
C3 C 0.6096(7) 0.8129(13) 0.635(2) 0.175(3) Uiso 0.3333 1 d D U P A -1
H3A H 0.6812 0.8735 0.6787 0.210 Uiso 0.3333 1 calc R U P A -1
H3B H 0.6297 0.8112 0.5473 0.210 Uiso 0.3333 1 calc R U P A -1
C5 C 0.4533(12) 0.5068(14) 0.6200(19) 0.175(3) Uiso 0.3333 1 d D U P A -1
H5A H 0.5130 0.5011 0.6715 0.210 Uiso 0.3333 1 calc R U P A -1
H5B H 0.4403 0.4570 0.5462 0.210 Uiso 0.3333 1 calc R U P A -1
C7 C 0.1179(9) 0.4108(8) 0.6380(17) 0.175(3) Uiso 0.3333 1 d D U P A -1
H7A H 0.0760 0.3307 0.6757 0.210 Uiso 0.3333 1 calc R U P A -1
H7B H 0.1040 0.4062 0.5481 0.210 Uiso 0.3333 1 calc R U P A -1
C9 C 0.1105(10) 0.7079(14) 0.6058(18) 0.175(3) Uiso 0.3333 1 d D U P A -1
H9A H 0.0294 0.6909 0.6271 0.210 Uiso 0.3333 1 calc R U P A -1
H9B H 0.1323 0.7403 0.5214 0.210 Uiso 0.3333 1 calc R U P A -1
C2 C 0.4626(14) 0.8885(12) 0.7330(14) 0.175(3) Uiso 0.3333 1 d D U P A -1
H2A H 0.5258 0.9546 0.7812 0.210 Uiso 0.3333 1 calc R U P A -1
H2B H 0.4034 0.8283 0.7896 0.210 Uiso 0.3333 1 calc R U P A -1
C4 C 0.5610(12) 0.6916(16) 0.6939(15) 0.175(3) Uiso 0.3333 1 d D U P A -1
H4A H 0.6239 0.6759 0.7236 0.210 Uiso 0.3333 1 calc R U P A -1
H4B H 0.5026 0.6763 0.7599 0.210 Uiso 0.3333 1 calc R U P A -1
C6 C 0.3378(13) 0.4513(15) 0.692(2) 0.175(3) Uiso 0.3333 1 d D U P A -1
H6A H 0.3004 0.3643 0.6801 0.210 Uiso 0.3333 1 calc R U P A -1
H6B H 0.3599 0.4669 0.7796 0.210 Uiso 0.3333 1 calc R U P A -1
C8 C 0.0946(12) 0.5006(13) 0.7024(18) 0.175(3) Uiso 0.3333 1 d D U P A -1
H8A H 0.0087 0.4629 0.7213 0.210 Uiso 0.3333 1 calc R U P A -1
H8B H 0.1384 0.5234 0.7814 0.210 Uiso 0.3333 1 calc R U P A -1
C10 C 0.2031(15) 0.7817(16) 0.7017(15) 0.175(3) Uiso 0.3333 1 d D U P A -1
H10A H 0.1886 0.8411 0.7431 0.210 Uiso 0.3333 1 calc R U P A -1
H10B H 0.2184 0.7341 0.7623 0.210 Uiso 0.3333 1 calc R U P A -1
O6 O 0.1002(12) 0.0055(15) 0.484(2) 0.184(9) Uiso 0.1667 1 d D U P B -1
C17 C -0.0085(10) -0.083(2) 0.4278(18) 0.184(9) Uiso 0.1667 1 d D U P B -1
H17A H -0.0094 -0.1596 0.4234 0.220 Uiso 0.1667 1 calc R U P B -1
H17B H -0.0143 -0.0586 0.3430 0.220 Uiso 0.1667 1 calc R U P B -1
C18 C -0.1130(11) -0.098(2) 0.5035(16) 0.184(9) Uiso 0.1667 1 d D U P B -1
H18A H -0.1619 -0.0730 0.4558 0.220 Uiso 0.1667 1 calc R U P B -1
H18B H -0.1638 -0.1817 0.5290 0.220 Uiso 0.1667 1 calc R U P B -1
C19 C -0.0583(15) -0.018(2) 0.6146(14) 0.184(9) Uiso 0.1667 1 d D U P B -1
H19A H -0.1042 0.0200 0.6407 0.220 Uiso 0.1667 1 calc R U P B -1
H19B H -0.0492 -0.0616 0.6849 0.220 Uiso 0.1667 1 calc R U P B -1
C20 C 0.0603(13) 0.0698(15) 0.558(2) 0.184(9) Uiso 0.1667 1 d D U P B -1
H20A H 0.0516 0.1281 0.5072 0.220 Uiso 0.1667 1 calc R U P B -1
H20B H 0.1190 0.1134 0.6239 0.220 Uiso 0.1667 1 calc R U P B -1


_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
Si1 C11 1.915(6) 2_665 ?
Si1 C11 1.915(6) . ?
Si1 C11 1.915(6) 3_565 ?
Si1 Na1 2.982(4) . ?
C11 C12 1.363(8) . ?
C11 C14 1.390(8) . ?
C12 C13 1.384(8) . ?
C13 C15 1.355(9) . ?
C14 C16 1.382(10) . ?
C15 C16 1.349(10) . ?
Na1 O5 2.526(6) . ?
Na1 O3 2.526(6) . ?
Na1 O2 2.527(6) . ?
Na1 O4 2.527(6) . ?
Na1 O1 2.527(6) . ?
O1 C1 1.4501(12) . ?
O1 C10 1.4502(11) . ?
O2 C3 1.4499(12) . ?
O2 C2 1.4499(11) . ?
O3 C5 1.4499(11) . ?
O3 C4 1.4502(12) . ?
O4 C6 1.4496(12) . ?
O4 C7 1.4500(12) . ?
O5 C9 1.4499(12) . ?
O5 C8 1.4499(11) . ?
C1 C2 1.4999(11) . ?
C3 C4 1.4999(11) . ?
C5 C6 1.4998(11) . ?
C7 C8 1.5002(11) . ?
C9 C10 1.5001(11) . ?
O6 C17 1.4200(7) . ?
O6 C20 1.4200(7) . ?
C17 C18 1.5000(7) . ?
C18 C19 1.5000(7) . ?
C19 C20 1.5000(7) . ?

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
C11 Si1 C11 101.7(2) 2_665 . ?
C11 Si1 C11 101.7(2) 2_665 3_565 ?
C11 Si1 C11 101.7(2) . 3_565 ?
C11 Si1 Na1 116.47(17) 2_665 . ?
C11 Si1 Na1 116.47(17) . . ?
C11 Si1 Na1 116.47(17) 3_565 . ?
C12 C11 C14 114.4(6) . . ?
C12 C11 Si1 118.3(4) . . ?
C14 C11 Si1 127.2(5) . . ?
C11 C12 C13 123.5(6) . . ?
C15 C13 C12 120.2(7) . . ?
C16 C14 C11 122.6(7) . . ?
C16 C15 C13 118.8(7) . . ?
C15 C16 C14 120.6(7) . . ?
O5 Na1 O3 138.7(5) . . ?
O5 Na1 O2 115.5(5) . . ?
O3 Na1 O2 65.2(4) . . ?
O5 Na1 O4 65.3(4) . . ?
O3 Na1 O4 75.7(3) . . ?
O2 Na1 O4 110.0(5) . . ?
O5 Na1 O1 61.4(4) . . ?
O3 Na1 O1 133.1(4) . . ?
O2 Na1 O1 68.2(4) . . ?
O4 Na1 O1 116.7(5) . . ?
O5 Na1 Si1 112.9(4) . . ?
O3 Na1 Si1 99.9(3) . . ?
O2 Na1 Si1 117.7(4) . . ?
O4 Na1 Si1 124.8(4) . . ?
O1 Na1 Si1 106.0(4) . . ?
C1 O1 C10 113.9(16) . . ?
C1 O1 Na1 106.3(4) . . ?
C10 O1 Na1 106.5(4) . . ?
C3 O2 C2 141.0(12) . . ?
C3 O2 Na1 106.4(4) . . ?
C2 O2 Na1 106.4(4) . . ?
C5 O3 C4 99.6(15) . . ?
C5 O3 Na1 106.4(4) . . ?
C4 O3 Na1 106.3(4) . . ?
C6 O4 C7 133.9(14) . . ?
C6 O4 Na1 106.5(4) . . ?
C7 O4 Na1 106.3(4) . . ?
C9 O5 C8 145.7(10) . . ?
C9 O5 Na1 106.3(4) . . ?
C8 O5 Na1 106.4(4) . . ?
O1 C1 C2 108.6(11) . . ?
O2 C3 C4 103.1(12) . . ?
O3 C5 C6 119.3(9) . . ?
O4 C7 C8 89.9(10) . . ?
O5 C9 C10 90.4(12) . . ?
O2 C2 C1 98.7(10) . . ?
O3 C4 C3 92.3(10) . . ?
O4 C6 C5 123.9(5) . . ?
O5 C8 C7 113.2(10) . . ?
O1 C10 C9 88.4(10) . . ?
C17 O6 C20 102.0(16) . . ?
O6 C17 C18 109.5(12) . . ?
C19 C18 C17 105.1(10) . . ?
C20 C19 C18 98.4(12) . . ?
O6 C20 C19 108.4(16) . . ?

_refine_diff_density_max         0.450
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.056

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 993780'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H47 K O7 Si'
_chemical_formula_sum            'C34 H47 K O7 Si'
_chemical_formula_weight         634.90

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.801(6)
_cell_length_b                   14.731(4)
_cell_length_c                   12.752(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.535(5)
_cell_angle_gamma                90
_cell_volume                     3435.6(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.420
_exptl_absorpt_coefficient_mu    0.234
_shelx_estimated_absorpt_T_min   0.892
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   TWINABS

_exptl_special_details           
;
Absorption correction was done with TWINABS.
Friedel pairs were treated as equal for refinement.
A HKLF5 format file containing only reflections of domain 1 was generated by averaging equivalent reflections.
Friedel pairs were not merged.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12783
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.775
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 0.900
_reflns_number_total             7033
_reflns_number_gt                6143
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_max     0.776
_reflns_Friedel_fraction_full    0.800

_reflns_special_details          
;
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1000P)²+4.0000P]
 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_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7033
_refine_ls_number_parameters     389
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1862
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003

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 0.13614(9) 0.25764(10) -0.04277(13) 0.0237(4) Uani 1 1 d . . . . .
Si1 Si 0.01081(11) 0.22851(14) 0.08264(17) 0.0250(5) Uani 1 1 d . . . . .
O1 O 0.1054(3) 0.0852(4) -0.1413(5) 0.0312(12) Uani 1 1 d . . . . .
O7 O 0.2484(3) 0.2922(4) -0.1194(5) 0.0313(13) Uani 1 1 d . . . . .
O2 O 0.0528(3) 0.2400(4) -0.2772(5) 0.0310(14) Uani 1 1 d . . . . .
O3 O 0.0668(3) 0.4099(4) -0.1700(5) 0.0303(13) Uani 1 1 d . . . . .
O6 O 0.2233(3) 0.1055(4) 0.0724(5) 0.0296(13) Uani 1 1 d . . . . .
O5 O 0.2390(3) 0.2772(4) 0.1730(5) 0.0294(13) Uani 1 1 d . . . . .
O4 O 0.1847(3) 0.4331(4) 0.0443(5) 0.0301(13) Uani 1 1 d . . . . .
C1 C 0.0471(4) 0.2071(5) 0.2455(7) 0.0254(16) Uani 1 1 d . . . . .
C7 C -0.0435(4) 0.3386(5) 0.0783(7) 0.0270(17) Uani 1 1 d . . . . .
C13 C -0.0686(4) 0.1425(5) 0.0311(6) 0.0249(16) Uani 1 1 d . . . . .
C8 C -0.0646(4) 0.3694(5) 0.1660(8) 0.0320(18) Uani 1 1 d . . . . .
H10 H -0.0502 0.3361 0.2349 0.038 Uiso 1 1 calc R U . . .
C9 C -0.1061(5) 0.4476(6) 0.1531(9) 0.041(2) Uani 1 1 d . . . . .
H9 H -0.1193 0.4667 0.2138 0.049 Uiso 1 1 calc R U . . .
C15 C -0.1872(4) 0.0816(5) 0.0160(7) 0.0308(17) Uani 1 1 d . . . . .
H14 H -0.2303 0.0885 0.0311 0.037 Uiso 1 1 calc R U . . .
C2 C 0.0126(4) 0.1563(5) 0.3028(7) 0.0268(16) Uani 1 1 d . . . . .
H5 H -0.0316 0.1255 0.2602 0.032 Uiso 1 1 calc R U . . .
C10 C -0.1288(4) 0.4982(6) 0.0548(8) 0.037(2) Uani 1 1 d . . . . .
H8 H -0.1576 0.5513 0.0472 0.044 Uiso 1 1 calc R U . . .
C11 C -0.1086(5) 0.4697(6) -0.0328(8) 0.039(2) Uani 1 1 d . . . . .
H7 H -0.1236 0.5033 -0.1016 0.047 Uiso 1 1 calc R U . . .
C4 C 0.1055(5) 0.1924(5) 0.4846(7) 0.0329(18) Uani 1 1 d . . . . .
H3 H 0.1244 0.1881 0.5651 0.039 Uiso 1 1 calc R U . . .
C16 C -0.1772(4) 0.0037(5) -0.0373(7) 0.0317(18) Uani 1 1 d . . . . .
H13 H -0.2130 -0.0430 -0.0586 0.038 Uiso 1 1 calc R U . . .
C5 C 0.1423(5) 0.2418(6) 0.4307(8) 0.034(2) Uani 1 1 d . . . . .
H2 H 0.1871 0.2713 0.4737 0.041 Uiso 1 1 calc R U . . .
C33 C 0.2850(5) 0.2025(6) -0.2400(8) 0.0365(19) Uani 1 1 d . . . . .
H42 H 0.2615 0.1438 -0.2370 0.044 Uiso 1 1 calc R U . . .
H43 H 0.2971 0.2041 -0.3084 0.044 Uiso 1 1 calc R U . . .
C31 C 0.3188(5) 0.2551(6) -0.0520(7) 0.0336(19) Uani 1 1 d . . . . .
H46 H 0.3136 0.2055 -0.0033 0.040 Uiso 1 1 calc R U . . .
H47 H 0.3506 0.3027 -0.0027 0.040 Uiso 1 1 calc R U . . .
C27 C 0.2836(5) 0.2025(6) 0.2313(7) 0.0315(18) Uani 1 1 d . . . . .
H22 H 0.2985 0.2097 0.3144 0.038 Uiso 1 1 calc R U . . .
H23 H 0.3282 0.1994 0.2140 0.038 Uiso 1 1 calc R U . . .
C25 C 0.2171(5) 0.4344(5) 0.1643(7) 0.0342(19) Uani 1 1 d . . . . .
H26 H 0.1792 0.4238 0.1958 0.041 Uiso 1 1 calc R U . . .
H27 H 0.2394 0.4946 0.1906 0.041 Uiso 1 1 calc R U . . .
C21 C 0.0069(4) 0.3145(6) -0.3274(7) 0.0341(19) Uani 1 1 d . . . . .
H34 H -0.0360 0.3142 -0.3055 0.041 Uiso 1 1 calc R U . . .
H35 H -0.0109 0.3101 -0.4112 0.041 Uiso 1 1 calc R U . . .
C34 C 0.2376(5) 0.2820(7) -0.2366(8) 0.038(2) Uani 1 1 d . . . . .
H40 H 0.2527 0.3377 -0.2653 0.046 Uiso 1 1 calc R U . . .
H41 H 0.1856 0.2696 -0.2835 0.046 Uiso 1 1 calc R U . . .
C23 C 0.1003(5) 0.4950(5) -0.1272(7) 0.0318(19) Uani 1 1 d . . . . .
H30 H 0.0649 0.5448 -0.1599 0.038 Uiso 1 1 calc R U . . .
H31 H 0.1426 0.5047 -0.1492 0.038 Uiso 1 1 calc R U . . .
C3 C 0.0407(4) 0.1493(6) 0.4197(7) 0.0317(18) Uani 1 1 d . . . . .
H4 H 0.0155 0.1146 0.4560 0.038 Uiso 1 1 calc R U . . .
C17 C -0.1143(5) -0.0049(6) -0.0588(8) 0.0328(18) Uani 1 1 d . . . . .
H12 H -0.1069 -0.0574 -0.0964 0.039 Uiso 1 1 calc R U . . .
C22 C 0.0493(5) 0.4006(6) -0.2880(7) 0.0313(18) Uani 1 1 d . . . . .
H32 H 0.0946 0.3985 -0.3033 0.038 Uiso 1 1 calc R U . . .
H33 H 0.0198 0.4531 -0.3292 0.038 Uiso 1 1 calc R U . . .
C14 C -0.1342(4) 0.1504(5) 0.0479(7) 0.0307(17) Uani 1 1 d . . . . .
H15 H -0.1431 0.2041 0.0819 0.037 Uiso 1 1 calc R U . . .
C32 C 0.3517(5) 0.2193(6) -0.1330(8) 0.0350(19) Uani 1 1 d . . . . .
H44 H 0.3846 0.2646 -0.1460 0.042 Uiso 1 1 calc R U . . .
H45 H 0.3792 0.1624 -0.1042 0.042 Uiso 1 1 calc R U . . .
C26 C 0.2745(5) 0.3621(6) 0.2056(7) 0.0314(18) Uani 1 1 d . . . . .
H24 H 0.3113 0.3704 0.1713 0.038 Uiso 1 1 calc R U . . .
H25 H 0.2997 0.3653 0.2892 0.038 Uiso 1 1 calc R U . . .
C24 C 0.1251(5) 0.4954(6) -0.0016(8) 0.0329(19) Uani 1 1 d . . . . .
H28 H 0.1409 0.5572 0.0280 0.039 Uiso 1 1 calc R U . . .
H29 H 0.0844 0.4771 0.0208 0.039 Uiso 1 1 calc R U . . .
C28 C 0.2390(5) 0.1178(6) 0.1915(7) 0.0321(19) Uani 1 1 d . . . . .
H20 H 0.2664 0.0648 0.2350 0.039 Uiso 1 1 calc R U . . .
H21 H 0.1928 0.1231 0.2040 0.039 Uiso 1 1 calc R U . . .
C19 C 0.0694(5) 0.0783(6) -0.2601(7) 0.036(2) Uani 1 1 d . . . . .
H38 H 0.0441 0.0191 -0.2808 0.044 Uiso 1 1 calc R U . . .
H39 H 0.1052 0.0830 -0.2969 0.044 Uiso 1 1 calc R U . . .
C30 C 0.1619(5) 0.0188(6) -0.0947(7) 0.0308(18) Uani 1 1 d . . . . .
H16 H 0.2033 0.0322 -0.1175 0.037 Uiso 1 1 calc R U . . .
H17 H 0.1429 -0.0424 -0.1228 0.037 Uiso 1 1 calc R U . . .
C20 C 0.0142(5) 0.1556(6) -0.2994(7) 0.035(2) Uani 1 1 d . . . . .
H36 H -0.0153 0.1497 -0.3817 0.042 Uiso 1 1 calc R U . . .
H37 H -0.0192 0.1532 -0.2583 0.042 Uiso 1 1 calc R U . . .
C29 C 0.1864(5) 0.0223(6) 0.0309(7) 0.035(2) Uani 1 1 d . . . . .
H18 H 0.1436 0.0171 0.0525 0.042 Uiso 1 1 calc R U . . .
H19 H 0.2196 -0.0292 0.0652 0.042 Uiso 1 1 calc R U . . .
C12 C -0.0666(5) 0.3923(6) -0.0199(7) 0.0328(18) Uani 1 1 d . . . . .
H6 H -0.0528 0.3746 -0.0805 0.039 Uiso 1 1 calc R U . . .
C6 C 0.1130(5) 0.2477(6) 0.3129(7) 0.0300(18) Uani 1 1 d . . . . .
H1 H 0.1391 0.2810 0.2768 0.036 Uiso 1 1 calc R U . . .
C18 C -0.0611(4) 0.0641(5) -0.0253(7) 0.0271(17) Uani 1 1 d . . . . .
H11 H -0.0184 0.0571 -0.0415 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 O5 2.740(6) . ?
K1 O1 2.796(6) . ?
K1 O7 2.797(5) . ?
K1 O3 2.801(6) . ?
K1 O2 2.819(6) . ?
K1 O4 2.833(6) . ?
K1 O6 2.867(6) . ?
K1 Si1 3.456(3) . ?
Si1 C13 1.929(8) . ?
Si1 C7 1.935(8) . ?
Si1 C1 1.945(8) . ?
O1 C19 1.410(10) . ?
O1 C30 1.431(10) . ?
O7 C31 1.435(10) . ?
O7 C34 1.435(10) . ?
O2 C21 1.413(10) . ?
O2 C20 1.429(10) . ?
O3 C23 1.425(10) . ?
O3 C22 1.416(10) . ?
O6 C29 1.420(10) . ?
O6 C28 1.441(10) . ?
O5 C26 1.417(10) . ?
O5 C27 1.428(10) . ?
O4 C25 1.414(9) . ?
O4 C24 1.432(10) . ?
C1 C6 1.394(11) . ?
C1 C2 1.393(11) . ?
C7 C8 1.410(12) . ?
C7 C12 1.401(11) . ?
C13 C18 1.399(11) . ?
C13 C14 1.399(11) . ?
C8 C9 1.388(12) . ?
C8 H10 0.9500 . ?
C9 C10 1.377(13) . ?
C9 H9 0.9500 . ?
C15 C16 1.387(11) . ?
C15 C14 1.402(11) . ?
C15 H14 0.9500 . ?
C2 C3 1.381(11) . ?
C2 H5 0.9500 . ?
C10 C11 1.389(14) . ?
C10 H8 0.9500 . ?
C11 C12 1.383(12) . ?
C11 H7 0.9500 . ?
C4 C5 1.385(12) . ?
C4 C3 1.385(12) . ?
C4 H3 0.9500 . ?
C16 C17 1.380(12) . ?
C16 H13 0.9500 . ?
C5 C6 1.390(13) . ?
C5 H2 0.9500 . ?
C33 C32 1.512(12) . ?
C33 C34 1.512(12) . ?
C33 H42 0.9900 . ?
C33 H43 0.9900 . ?
C31 C32 1.512(12) . ?
C31 H46 0.9900 . ?
C31 H47 0.9900 . ?
C27 C28 1.501(12) . ?
C27 H22 0.9900 . ?
C27 H23 0.9900 . ?
C25 C26 1.498(12) . ?
C25 H26 0.9900 . ?
C25 H27 0.9900 . ?
C21 C22 1.497(12) . ?
C21 H34 0.9900 . ?
C21 H35 0.9900 . ?
C34 H40 0.9900 . ?
C34 H41 0.9900 . ?
C23 C24 1.484(12) . ?
C23 H30 0.9900 . ?
C23 H31 0.9900 . ?
C3 H4 0.9500 . ?
C17 C18 1.407(12) . ?
C17 H12 0.9500 . ?
C22 H32 0.9900 . ?
C22 H33 0.9900 . ?
C14 H15 0.9500 . ?
C32 H44 0.9900 . ?
C32 H45 0.9900 . ?
C26 H24 0.9900 . ?
C26 H25 0.9900 . ?
C24 H28 0.9900 . ?
C24 H29 0.9900 . ?
C28 H20 0.9900 . ?
C28 H21 0.9900 . ?
C19 C20 1.524(13) . ?
C19 H38 0.9900 . ?
C19 H39 0.9900 . ?
C30 C29 1.485(11) . ?
C30 H16 0.9900 . ?
C30 H17 0.9900 . ?
C20 H36 0.9900 . ?
C20 H37 0.9900 . ?
C29 H18 0.9900 . ?
C29 H19 0.9900 . ?
C12 H6 0.9500 . ?
C6 H1 0.9500 . ?
C18 H11 0.9500 . ?

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
O5 K1 O1 119.80(17) . . ?
O5 K1 O7 86.95(17) . . ?
O1 K1 O7 94.21(17) . . ?
O5 K1 O3 120.54(17) . . ?
O1 K1 O3 119.58(18) . . ?
O7 K1 O3 86.06(17) . . ?
O5 K1 O2 169.26(18) . . ?
O1 K1 O2 60.10(17) . . ?
O7 K1 O2 82.38(18) . . ?
O3 K1 O2 60.12(17) . . ?
O5 K1 O4 60.00(17) . . ?
O1 K1 O4 171.20(19) . . ?
O7 K1 O4 77.00(16) . . ?
O3 K1 O4 60.89(17) . . ?
O2 K1 O4 118.22(17) . . ?
O5 K1 O6 59.87(17) . . ?
O1 K1 O6 60.28(16) . . ?
O7 K1 O6 85.29(17) . . ?
O3 K1 O6 171.31(18) . . ?
O2 K1 O6 117.65(17) . . ?
O4 K1 O6 117.74(17) . . ?
O5 K1 Si1 86.44(14) . . ?
O1 K1 Si1 91.37(14) . . ?
O7 K1 Si1 172.88(13) . . ?
O3 K1 Si1 95.03(13) . . ?
O2 K1 Si1 104.28(13) . . ?
O4 K1 Si1 97.36(13) . . ?
O6 K1 Si1 93.67(13) . . ?
C13 Si1 C7 99.7(3) . . ?
C13 Si1 C1 100.1(3) . . ?
C7 Si1 C1 98.1(3) . . ?
C13 Si1 K1 124.1(2) . . ?
C7 Si1 K1 111.9(2) . . ?
C1 Si1 K1 118.5(2) . . ?
C19 O1 C30 113.0(6) . . ?
C19 O1 K1 118.8(5) . . ?
C30 O1 K1 115.7(4) . . ?
C31 O7 C34 107.9(6) . . ?
C31 O7 K1 116.2(5) . . ?
C34 O7 K1 121.6(5) . . ?
C21 O2 C20 112.6(6) . . ?
C21 O2 K1 115.0(5) . . ?
C20 O2 K1 110.0(5) . . ?
C23 O3 C22 112.4(6) . . ?
C23 O3 K1 115.4(4) . . ?
C22 O3 K1 113.8(4) . . ?
C29 O6 C28 111.9(6) . . ?
C29 O6 K1 111.1(4) . . ?
C28 O6 K1 106.6(4) . . ?
C26 O5 C27 112.9(6) . . ?
C26 O5 K1 118.8(5) . . ?
C27 O5 K1 121.0(5) . . ?
C25 O4 C24 113.3(6) . . ?
C25 O4 K1 112.4(4) . . ?
C24 O4 K1 108.7(4) . . ?
C6 C1 C2 116.0(8) . . ?
C6 C1 Si1 117.7(6) . . ?
C2 C1 Si1 126.4(6) . . ?
C8 C7 C12 115.6(7) . . ?
C8 C7 Si1 125.3(6) . . ?
C12 C7 Si1 119.1(6) . . ?
C18 C13 C14 115.9(7) . . ?
C18 C13 Si1 118.9(6) . . ?
C14 C13 Si1 125.2(6) . . ?
C7 C8 C9 121.0(8) . . ?
C7 C8 H10 119.5 . . ?
C9 C8 H10 119.5 . . ?
C10 C9 C8 122.0(9) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C16 C15 C14 120.6(7) . . ?
C16 C15 H14 119.7 . . ?
C14 C15 H14 119.7 . . ?
C3 C2 C1 122.0(7) . . ?
C3 C2 H5 119.0 . . ?
C1 C2 H5 119.0 . . ?
C11 C10 C9 118.3(8) . . ?
C11 C10 H8 120.9 . . ?
C9 C10 H8 120.8 . . ?
C10 C11 C12 119.9(8) . . ?
C10 C11 H7 120.0 . . ?
C12 C11 H7 120.0 . . ?
C5 C4 C3 119.2(8) . . ?
C5 C4 H3 120.4 . . ?
C3 C4 H3 120.4 . . ?
C17 C16 C15 118.9(7) . . ?
C17 C16 H13 120.6 . . ?
C15 C16 H13 120.6 . . ?
C4 C5 C6 119.2(8) . . ?
C4 C5 H2 120.4 . . ?
C6 C5 H2 120.4 . . ?
C32 C33 C34 100.6(7) . . ?
C32 C33 H42 111.6 . . ?
C34 C33 H42 111.6 . . ?
C32 C33 H43 111.6 . . ?
C34 C33 H43 111.6 . . ?
H42 C33 H43 109.4 . . ?
O7 C31 C32 107.3(7) . . ?
O7 C31 H46 110.2 . . ?
C32 C31 H46 110.2 . . ?
O7 C31 H47 110.3 . . ?
C32 C31 H47 110.3 . . ?
H46 C31 H47 108.5 . . ?
O5 C27 C28 107.4(6) . . ?
O5 C27 H22 110.2 . . ?
C28 C27 H22 110.2 . . ?
O5 C27 H23 110.2 . . ?
C28 C27 H23 110.2 . . ?
H22 C27 H23 108.5 . . ?
O4 C25 C26 109.8(7) . . ?
O4 C25 H26 109.7 . . ?
C26 C25 H26 109.7 . . ?
O4 C25 H27 109.7 . . ?
C26 C25 H27 109.7 . . ?
H26 C25 H27 108.2 . . ?
O2 C21 C22 109.0(6) . . ?
O2 C21 H34 109.9 . . ?
C22 C21 H34 109.9 . . ?
O2 C21 H35 109.9 . . ?
C22 C21 H35 109.9 . . ?
H34 C21 H35 108.3 . . ?
O7 C34 C33 105.3(7) . . ?
O7 C34 H40 110.7 . . ?
C33 C34 H40 110.7 . . ?
O7 C34 H41 110.7 . . ?
C33 C34 H41 110.7 . . ?
H40 C34 H41 108.8 . . ?
O3 C23 C24 109.3(6) . . ?
O3 C23 H30 109.8 . . ?
C24 C23 H30 109.8 . . ?
O3 C23 H31 109.8 . . ?
C24 C23 H31 109.8 . . ?
H30 C23 H31 108.3 . . ?
C2 C3 C4 120.6(8) . . ?
C2 C3 H4 119.7 . . ?
C4 C3 H4 119.7 . . ?
C16 C17 C18 120.1(8) . . ?
C16 C17 H12 120.0 . . ?
C18 C17 H12 120.0 . . ?
O3 C22 C21 108.4(7) . . ?
O3 C22 H32 110.0 . . ?
C21 C22 H32 110.0 . . ?
O3 C22 H33 110.0 . . ?
C21 C22 H33 110.0 . . ?
H32 C22 H33 108.4 . . ?
C15 C14 C13 122.0(7) . . ?
C15 C14 H15 119.0 . . ?
C13 C14 H15 119.0 . . ?
C33 C32 C31 102.6(7) . . ?
C33 C32 H44 111.2 . . ?
C31 C32 H44 111.2 . . ?
C33 C32 H45 111.3 . . ?
C31 C32 H45 111.3 . . ?
H44 C32 H45 109.2 . . ?
O5 C26 C25 107.4(7) . . ?
O5 C26 H24 110.2 . . ?
C25 C26 H24 110.2 . . ?
O5 C26 H25 110.2 . . ?
C25 C26 H25 110.2 . . ?
H24 C26 H25 108.5 . . ?
O4 C24 C23 108.6(7) . . ?
O4 C24 H28 110.0 . . ?
C23 C24 H28 110.0 . . ?
O4 C24 H29 110.0 . . ?
C23 C24 H29 110.0 . . ?
H28 C24 H29 108.4 . . ?
O6 C28 C27 108.8(7) . . ?
O6 C28 H20 109.9 . . ?
C27 C28 H20 109.9 . . ?
O6 C28 H21 109.9 . . ?
C27 C28 H21 109.9 . . ?
H20 C28 H21 108.3 . . ?
O1 C19 C20 107.6(7) . . ?
O1 C19 H38 110.2 . . ?
C20 C19 H38 110.2 . . ?
O1 C19 H39 110.2 . . ?
C20 C19 H39 110.2 . . ?
H38 C19 H39 108.5 . . ?
O1 C30 C29 107.7(7) . . ?
O1 C30 H16 110.2 . . ?
C29 C30 H16 110.2 . . ?
O1 C30 H17 110.2 . . ?
C29 C30 H17 110.2 . . ?
H16 C30 H17 108.5 . . ?
O2 C20 C19 108.9(7) . . ?
O2 C20 H36 109.9 . . ?
C19 C20 H36 109.9 . . ?
O2 C20 H37 109.9 . . ?
C19 C20 H37 109.9 . . ?
H36 C20 H37 108.3 . . ?
O6 C29 C30 109.9(7) . . ?
O6 C29 H18 109.7 . . ?
C30 C29 H18 109.7 . . ?
O6 C29 H19 109.7 . . ?
C30 C29 H19 109.7 . . ?
H18 C29 H19 108.2 . . ?
C11 C12 C7 123.2(9) . . ?
C11 C12 H6 118.4 . . ?
C7 C12 H6 118.4 . . ?
C1 C6 C5 123.0(8) . . ?
C1 C6 H1 118.5 . . ?
C5 C6 H1 118.5 . . ?
C13 C18 C17 122.5(8) . . ?
C13 C18 H11 118.8 . . ?
C17 C18 H11 118.8 . . ?

_refine_diff_density_max         0.751
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.080

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 993781'
