#------------------------------------------------------------------------------
#$Date: 2015-08-05 22:32:45 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152883 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/59/4085950.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_4085950
loop_
_publ_author_name
'Araneda, Juan F.'
'Piers, Warren E.'
'Sgro, Michael J.'
'Parvez, Masood'
_publ_section_title
;
 Ring Expansion Reactions of Electron-Rich Boron-Containing Heterocycles
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3408
_journal_paper_doi               10.1021/acs.organomet.5b00390
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C138 H162 B6 K6 O12, 2(C4 H8 O)'
_chemical_formula_sum            'C146 H178 B6 K6 O14'
_chemical_formula_weight         2456.33
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.599(11)
_cell_length_b                   24.599(11)
_cell_length_c                   40.161(10)
_cell_measurement_reflns_used    11938
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.00
_cell_volume                     21046(14)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al., 1991)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius APEX2 CCD'
_diffrn_measurement_method       ' ω and φ scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            27816
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       Block
_exptl_crystal_F_000             7860
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.1158
_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)+(0.0518P)²+151.5189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3003
_reflns_number_total             4279
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00390_si_001.cif
_cod_data_source_block           Compound_I
_cod_depositor_comments
'Adding full bibliography for 4085950--4085951.cif.'
_cod_original_cell_volume        21046(23)
_cod_database_code               4085950
_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   0.939
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2014-1
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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
K1 K 0.0000 0.0000 0.16142(5) 0.0515(5) Uani 1 3 d S T P
K2 K 0.0000 0.0000 0.2500 0.0494(7) Uani 1 6 d S T P
K3 K -0.14410(7) 0.0000 0.2500 0.0644(5) Uani 1 2 d S T P
O1 O 0.03207(17) 0.12330(15) 0.17859(8) 0.0520(9) Uani 1 1 d . . .
O2 O -0.04613(16) 0.04990(16) 0.20819(8) 0.0507(8) Uani 1 1 d . . .
C1 C -0.0011(3) 0.1053(2) 0.20843(12) 0.0478(12) Uani 1 1 d . . .
C2 C 0.0189(3) 0.1476(2) 0.23440(12) 0.0507(13) Uani 1 1 d . . .
C3 C 0.0715(3) 0.2084(2) 0.23095(13) 0.0605(15) Uani 1 1 d . . .
C4 C 0.0918(4) 0.2516(3) 0.25749(16) 0.084(2) Uani 1 1 d . . .
H4 H 0.0694 0.2403 0.2779 0.101 Uiso 1 1 calc R U .
C5 C 0.1427(4) 0.3089(3) 0.25403(19) 0.111(3) Uani 1 1 d . . .
H5 H 0.1558 0.3371 0.2723 0.133 Uiso 1 1 calc R U .
C6 C 0.1769(4) 0.3281(3) 0.2244(2) 0.122(3) Uani 1 1 d . . .
H6 H 0.2125 0.3689 0.2223 0.146 Uiso 1 1 calc R U .
C7 C 0.1580(4) 0.2871(3) 0.19887(17) 0.096(3) Uani 1 1 d . . .
H7 H 0.1809 0.2995 0.1786 0.115 Uiso 1 1 calc R U .
C8 C 0.1058(3) 0.2268(3) 0.20121(14) 0.0668(16) Uani 1 1 d . . .
C9 C 0.1140(3) 0.1951(3) 0.13739(15) 0.0692(17) Uani 1 1 d . . .
C10 C 0.1667(3) 0.1903(3) 0.13059(16) 0.0782(19) Uani 1 1 d . . .
C11 C 0.1944(4) 0.2066(4) 0.09947(19) 0.104(3) Uani 1 1 d . . .
H11 H 0.2311 0.2041 0.0954 0.125 Uiso 1 1 calc R U .
C12 C 0.1709(5) 0.2262(5) 0.0746(2) 0.119(3) Uani 1 1 d . . .
C13 C 0.1200(5) 0.2322(4) 0.08161(18) 0.120(3) Uani 1 1 d . . .
H13 H 0.1037 0.2468 0.0645 0.143 Uiso 1 1 calc R U .
C14 C 0.0905(4) 0.2179(4) 0.11257(16) 0.089(2) Uani 1 1 d . . .
C15 C 0.1948(4) 0.1682(3) 0.15717(19) 0.089(2) Uani 1 1 d . . .
H15 H 0.1658 0.1547 0.1768 0.107 Uiso 1 1 calc R U .
C16 C 0.1994(4) 0.1121(4) 0.1460(2) 0.104(3) Uani 1 1 d . . .
H16A H 0.2152 0.0977 0.1644 0.124 Uiso 1 1 calc R U .
H16B H 0.2283 0.1240 0.1271 0.124 Uiso 1 1 calc R U .
H16C H 0.1578 0.0783 0.1393 0.124 Uiso 1 1 calc R U .
C17 C 0.2581(4) 0.2200(4) 0.1690(2) 0.123(3) Uani 1 1 d . . .
H17A H 0.2749 0.2033 0.1857 0.148 Uiso 1 1 calc R U .
H17B H 0.2534 0.2539 0.1788 0.148 Uiso 1 1 calc R U .
H17C H 0.2870 0.2364 0.1500 0.148 Uiso 1 1 calc R U .
C18 C 0.1995(7) 0.2410(8) 0.0399(3) 0.191(6) Uani 1 1 d . . .
H18 H 0.1799 0.2646 0.0303 0.229 Uiso 1 1 calc R U .
C19 C 0.1767(9) 0.1905(10) 0.0191(3) 0.358(16) Uani 1 1 d . . .
H19A H 0.2010 0.2027 -0.0017 0.429 Uiso 1 1 calc R U .
H19B H 0.1325 0.1760 0.0141 0.429 Uiso 1 1 calc R U .
H19C H 0.1802 0.1566 0.0298 0.429 Uiso 1 1 calc R U .
C20 C 0.2594(9) 0.2840(6) 0.0389(3) 0.251(10) Uani 1 1 d . . .
H20A H 0.2659 0.3218 0.0506 0.301 Uiso 1 1 calc R U .
H20B H 0.2727 0.2945 0.0156 0.301 Uiso 1 1 calc R U .
H20C H 0.2842 0.2679 0.0497 0.301 Uiso 1 1 calc R U .
C21 C 0.0361(4) 0.2279(5) 0.1196(2) 0.106(3) Uani 1 1 d . . .
H21 H 0.0124 0.1997 0.1386 0.127 Uiso 1 1 calc R U .
C22 C 0.0577(5) 0.2939(5) 0.1306(2) 0.137(4) Uani 1 1 d . . .
H22A H 0.0211 0.2986 0.1350 0.164 Uiso 1 1 calc R U .
H22B H 0.0833 0.3233 0.1131 0.164 Uiso 1 1 calc R U .
H22C H 0.0827 0.3029 0.1510 0.164 Uiso 1 1 calc R U .
C23 C -0.0091(5) 0.2100(5) 0.0910(2) 0.151(4) Uani 1 1 d . . .
H23A H -0.0468 0.2105 0.0984 0.182 Uiso 1 1 calc R U .
H23B H -0.0207 0.1678 0.0833 0.182 Uiso 1 1 calc R U .
H23C H 0.0107 0.2401 0.0728 0.182 Uiso 1 1 calc R U .
B1 B 0.0829(3) 0.1806(3) 0.17294(16) 0.0595(17) Uani 1 1 d . . .
O3 O 0.0000 0.0000 0.0952 0.320 Uani 1 3 d S T P
C2A C 0.0190 0.0482 0.0792 0.361 Uani 0.6667 1 d . . P
H2A H 0.0645 0.0716 0.0800 0.433 Uiso 0.6667 1 d . U P
H2B H 0.0037 0.0739 0.0893 0.433 Uiso 0.6667 1 d . U P
C3A C 0.0003 0.0369 0.0473 0.298 Uani 0.6667 1 d . . P
H3A H 0.0357 0.0535 0.0321 0.358 Uiso 0.3334 1 d . U P
H3B H -0.0265 0.0540 0.0417 0.358 Uiso 0.3334 1 d . U P
H3C H 0.0183 0.0737 0.0331 0.358 Uiso 0.3334 1 d . U P
H3D H -0.0447 0.0112 0.0442 0.358 Uiso 0.3334 1 d . U 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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
O3 K1 O2 132.54(7) . 3
O3 K1 O2 132.54(7) . 2
O2 K1 O2 79.29(11) 3 2
O3 K1 O2 132.54(7) . .
O2 K1 O2 79.29(11) 3 .
O2 K1 O2 79.29(11) 2 .
O3 K1 O1 104.20(7) . 2
O2 K1 O1 121.20(11) 3 2
O2 K1 O1 46.66(10) 2 2
O2 K1 O1 70.79(11) . 2
O3 K1 O1 104.20(7) . .
O2 K1 O1 70.78(11) 3 .
O2 K1 O1 121.20(11) 2 .
O2 K1 O1 46.66(10) . .
O1 K1 O1 114.19(6) 2 .
O3 K1 O1 104.20(7) . 3
O2 K1 O1 46.66(10) 3 3
O2 K1 O1 70.78(11) 2 3
O2 K1 O1 121.20(11) . 3
O1 K1 O1 114.19(6) 2 3
O1 K1 O1 114.19(6) . 3
O3 K1 C1 125.94(9) . .
O2 K1 C1 67.81(12) 3 .
O2 K1 C1 96.32(12) 2 .
O2 K1 C1 22.67(11) . .
O1 K1 C1 93.36(13) 2 .
O1 K1 C1 25.58(11) . .
O1 K1 C1 114.31(12) 3 .
O3 K1 C1 125.94(9) . 2
O2 K1 C1 96.31(12) 3 2
O2 K1 C1 22.67(11) 2 2
O2 K1 C1 67.81(12) . 2
O1 K1 C1 25.58(11) 2 2
O1 K1 C1 114.31(12) . 2
O1 K1 C1 93.35(13) 3 2
C1 K1 C1 89.05(13) . 2
O3 K1 C1 125.94(9) . 3
O2 K1 C1 22.68(11) 3 3
O2 K1 C1 67.81(11) 2 3
O2 K1 C1 96.32(12) . 3
O1 K1 C1 114.30(12) 2 3
O1 K1 C1 93.36(13) . 3
O1 K1 C1 25.58(11) 3 3
C1 K1 C1 89.05(13) . 3
C1 K1 C1 89.04(13) 2 3
O3 K1 C2A 17.394(12) . 2
O2 K1 C2A 149.68(8) 3 2
O2 K1 C2A 120.59(7) 2 2
O2 K1 C2A 124.30(7) . 2
O1 K1 C2A 86.99(7) 2 2
O1 K1 C2A 109.88(8) . 2
O1 K1 C2A 114.50(8) 3 2
C1 K1 C2A 125.94(9) . 2
C1 K1 C2A 109.77(9) 2 2
C1 K1 C2A 139.01(9) 3 2
O3 K1 C2A 17.394(12) . 3
O2 K1 C2A 120.59(7) 3 3
O2 K1 C2A 124.30(7) 2 3
O2 K1 C2A 149.68(8) . 3
O1 K1 C2A 109.88(8) 2 3
O1 K1 C2A 114.50(8) . 3
O1 K1 C2A 86.99(7) 3 3
C1 K1 C2A 139.01(9) . 3
C1 K1 C2A 125.94(9) 2 3
C1 K1 C2A 109.77(9) 3 3
C2A K1 C2A 30.01(2) 2 3
O2 K2 O2 177.99(15) 5 2
O2 K2 O2 84.05(11) 5 6
O2 K2 O2 97.32(15) 2 6
O2 K2 O2 84.05(11) 5 4
O2 K2 O2 94.62(15) 2 4
O2 K2 O2 84.05(11) 6 4
O2 K2 O2 97.32(15) 5 3
O2 K2 O2 84.05(11) 2 3
O2 K2 O2 94.62(15) 6 3
O2 K2 O2 177.99(15) 4 3
O2 K2 O2 94.62(15) 5 .
O2 K2 O2 84.05(11) 2 .
O2 K2 O2 177.99(16) 6 .
O2 K2 O2 97.32(15) 4 .
O2 K2 O2 84.05(11) 3 .
O2 K2 C1 71.25(12) 5 6
O2 K2 C1 110.55(13) 2 6
O2 K2 C1 23.64(12) 6 6
O2 K2 C1 102.16(12) 4 6
O2 K2 C1 76.96(13) 3 6
O2 K2 C1 154.36(14) . 6
O2 K2 C1 154.36(14) 5 2
O2 K2 C1 23.64(12) 2 2
O2 K2 C1 110.55(13) 6 2
O2 K2 C1 76.96(13) 4 2
O2 K2 C1 102.16(12) 3 2
O2 K2 C1 71.25(12) . 2
C1 K2 C1 129.35(19) 6 2
O2 K2 C1 102.16(12) 5 4
O2 K2 C1 76.96(13) 2 4
O2 K2 C1 71.25(12) 6 4
O2 K2 C1 23.64(12) 4 4
O2 K2 C1 154.36(14) 3 4
O2 K2 C1 110.55(13) . 4
C1 K2 C1 93.63(13) 6 4
C1 K2 C1 65.32(19) 2 4
O2 K2 C1 76.96(13) 5 .
O2 K2 C1 102.16(12) 2 .
O2 K2 C1 154.36(14) 6 .
O2 K2 C1 110.55(13) 4 .
O2 K2 C1 71.25(12) 3 .
O2 K2 C1 23.64(12) . .
C1 K2 C1 131.1(2) 6 .
C1 K2 C1 93.63(13) 2 .
C1 K2 C1 129.35(19) 4 .
O2 K2 C1 23.65(12) 5 5
O2 K2 C1 154.36(14) 2 5
O2 K2 C1 102.16(12) 6 5
O2 K2 C1 71.25(12) 4 5
O2 K2 C1 110.55(13) 3 5
O2 K2 C1 76.96(13) . 5
C1 K2 C1 93.63(13) 6 5
C1 K2 C1 131.1(2) 2 5
C1 K2 C1 93.63(13) 4 5
C1 K2 C1 65.32(19) . 5
O2 K2 C1 110.55(13) 5 3
O2 K2 C1 71.25(12) 2 3
O2 K2 C1 76.96(13) 6 3
O2 K2 C1 154.36(14) 4 3
O2 K2 C1 23.65(12) 3 3
O2 K2 C1 102.16(12) . 3
C1 K2 C1 65.32(19) 6 3
C1 K2 C1 93.63(13) 2 3
C1 K2 C1 131.1(2) 4 3
C1 K2 C1 93.63(13) . 3
C1 K2 C1 129.4(2) 5 3
O2 K3 O2 95.79(15) . 4
O2 K3 C3 75.68(13) . 5
O2 K3 C3 101.65(13) 4 5
O2 K3 C3 101.65(13) . 2
O2 K3 C3 75.68(13) 4 2
C3 K3 C3 176.1(2) 5 2
O2 K3 C2 57.78(12) . 5
O2 K3 C2 84.46(12) 4 5
C3 K3 C2 26.12(14) 5 5
C3 K3 C2 150.00(16) 2 5
O2 K3 C2 84.46(12) . 2
O2 K3 C2 57.78(12) 4 2
C3 K3 C2 150.00(16) 5 2
C3 K3 C2 26.12(14) 2 2
C2 K3 C2 123.99(19) 5 2
O2 K3 C8 92.81(13) . 2
O2 K3 C8 100.01(13) 4 2
C3 K3 C8 156.34(15) 5 2
C3 K3 C8 25.22(15) 2 2
C2 K3 C8 150.60(14) 5 2
C2 K3 C8 44.35(14) 2 2
O2 K3 C8 100.01(14) . 5
O2 K3 C8 92.81(13) 4 5
C3 K3 C8 25.22(15) 5 5
C3 K3 C8 156.34(15) 2 5
C2 K3 C8 44.35(14) 5 5
C2 K3 C8 150.60(14) 2 5
C8 K3 C8 160.9(2) 2 5
O2 K3 C4 124.93(14) . 2
O2 K3 C4 71.88(13) 4 2
C3 K3 C4 158.31(15) 5 2
C3 K3 C4 23.65(15) 2 2
C2 K3 C4 156.28(15) 5 2
C2 K3 C4 42.92(15) 2 2
C8 K3 C4 41.57(15) 2 2
C8 K3 C4 133.10(16) 5 2
O2 K3 C4 71.88(13) . 5
O2 K3 C4 124.93(14) 4 5
C3 K3 C4 23.65(15) 5 5
C3 K3 C4 158.31(15) 2 5
C2 K3 C4 42.92(15) 5 5
C2 K3 C4 156.28(15) 2 5
C8 K3 C4 133.10(16) 2 5
C8 K3 C4 41.57(15) 5 5
C4 K3 C4 157.5(2) 2 5
O2 K3 K2 47.90(8) . .
O2 K3 K2 47.90(8) 4 .
C3 K3 K2 88.06(11) 5 .
C3 K3 K2 88.06(11) 2 .
C2 K3 K2 61.99(9) 5 .
C2 K3 K2 61.99(9) 2 .
C8 K3 K2 99.57(11) 2 .
C8 K3 K2 99.57(11) 5 .
C4 K3 K2 101.25(12) 2 .
C4 K3 K2 101.25(12) 5 .
O2 K3 K1 23.47(7) . .
O2 K3 K1 88.33(9) 4 .
C3 K3 K1 98.96(11) 5 .
C3 K3 K1 78.26(11) 2 .
C2 K3 K1 78.92(9) 5 .
C2 K3 K1 61.92(9) 2 .
C8 K3 K1 72.23(10) 2 .
C8 K3 K1 122.67(11) 5 .
C4 K3 K1 101.47(12) 2 .
C4 K3 K1 94.39(11) 5 .
K2 K3 K1 45.10(3) . .
B1 O1 C1 124.3(4) . .
B1 O1 K1 134.1(4) . .
C1 O1 K1 93.7(3) . .
C1 O2 K2 98.6(3) . .
C1 O2 K3 126.6(3) . .
K2 O2 K3 83.44(10) . .
C1 O2 K1 98.7(3) . .
K2 O2 K1 81.92(10) . .
K3 O2 K1 133.95(14) . .
O2 C1 C2 127.9(5) . .
O2 C1 O1 113.4(4) . .
C2 C1 O1 118.6(5) . .
O2 C1 K2 57.8(2) . .
C2 C1 K2 94.3(3) . .
O1 C1 K2 118.8(3) . .
O2 C1 K1 58.6(3) . .
C2 C1 K1 155.2(4) . .
O1 C1 K1 60.7(2) . .
K2 C1 K1 68.59(11) . .
C1 C2 C3 121.2(5) . .
C1 C2 C2 117.9(5) . 5
C3 C2 C2 120.8(5) . 5
C1 C2 K3 96.6(3) . 3
C3 C2 K3 70.2(3) . 3
C2 C2 K3 106.7(4) 5 3
C1 C2 K2 62.5(3) . .
C3 C2 K2 134.1(4) . .
C2 C2 K2 77.64(8) 5 .
K3 C2 K2 64.08(9) 3 .
C8 C3 C4 118.2(6) . .
C8 C3 C2 120.7(5) . .
C4 C3 C2 121.1(5) . .
C8 C3 K3 88.2(4) . 3
C4 C3 K3 97.2(4) . 3
C2 C3 K3 83.6(3) . 3
C5 C4 C3 120.4(6) . .
C5 C4 K3 106.4(6) . 3
C3 C4 K3 59.2(3) . 3
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
K3 C4 H4 103.4 3 .
C4 C5 C6 122.1(7) . .
C4 C5 H5 119.0 . .
C6 C5 H5 119.0 . .
C7 C6 C5 118.1(7) . .
C7 C6 H6 121.0 . .
C5 C6 H6 121.0 . .
C6 C7 C8 122.2(7) . .
C6 C7 H7 118.9 . .
C8 C7 H7 118.9 . .
C7 C8 C3 119.1(6) . .
C7 C8 B1 123.3(6) . .
C3 C8 B1 117.6(5) . .
C7 C8 K3 107.5(5) . 3
C3 C8 K3 66.6(3) . 3
B1 C8 K3 95.6(4) . 3
C10 C9 C14 119.0(6) . .
C10 C9 B1 122.0(6) . .
C14 C9 B1 118.9(6) . .
C11 C10 C9 120.0(7) . .
C11 C10 C15 119.7(7) . .
C9 C10 C15 120.4(6) . .
C12 C11 C10 122.1(9) . .
C12 C11 H11 118.9 . .
C10 C11 H11 118.9 . .
C11 C12 C13 117.6(8) . .
C11 C12 C18 122.0(11) . .
C13 C12 C18 120.3(10) . .
C12 C13 C14 123.3(9) . .
C12 C13 H13 118.3 . .
C14 C13 H13 118.3 . .
C13 C14 C9 117.8(8) . .
C13 C14 C21 121.4(8) . .
C9 C14 C21 120.8(6) . .
C16 C15 C10 112.2(7) . .
C16 C15 C17 110.3(7) . .
C10 C15 C17 112.3(6) . .
C16 C15 H15 107.3 . .
C10 C15 H15 107.3 . .
C17 C15 H15 107.3 . .
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 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C20 C18 C19 119.9(13) . .
C20 C18 C12 114.9(13) . .
C19 C18 C12 114.4(13) . .
C20 C18 H18 101.1 . .
C19 C18 H18 101.1 . .
C12 C18 H18 101.1 . .
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 . .
C18 C20 H20A 109.5 . .
C18 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C18 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C14 C21 C23 113.5(8) . .
C14 C21 C22 111.7(8) . .
C23 C21 C22 110.5(8) . .
C14 C21 H21 106.9 . .
C23 C21 H21 106.9 . .
C22 C21 H21 106.9 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
O1 B1 C8 117.5(5) . .
O1 B1 C9 118.6(5) . .
C8 B1 C9 123.9(5) . .
C2A O3 C2A 94.7 . 2
C2A O3 C2A 94.7 . 3
C2A O3 C2A 94.7 2 3
C2A O3 K1 121.849(13) . .
C2A O3 K1 121.847(13) 2 .
C2A O3 K1 121.847(13) 3 .
O3 C2A C3A 112.1 . .
C3A C2A C2A 75.0 . 2
C3A C2A C2A 90.0 . 3
C2A C2A C2A 60.0 2 3
O3 C2A C3A 81.1 . 3
C3A C2A C3A 53.3 . 3
C2A C2A C3A 73.6 2 3
C3A C2A K1 150.01(1) . .
C2A C2A K1 74.996(11) 2 .
C2A C2A K1 74.995(11) 3 .
C3A C2A K1 116.92(2) 3 .
O3 C2A H2A 109.2 . .
C3A C2A H2A 109.2 . .
C2A C2A H2A 144.1 2 .
C2A C2A H2A 84.1 3 .
C3A C2A H2A 80.9 3 .
K1 C2A H2A 95.2 . .
O3 C2A H2B 109.2 . .
C3A C2A H2B 109.1 . .
C2A C2A H2B 103.8 2 .
C2A C2A H2B 151.5 3 .
C3A C2A H2B 162.4 3 .
K1 C2A H2B 78.2 . .
H2A C2A H2B 107.9 . .
C2A C3A C3A 83.3 . 3
C2A C3A C3A 100.4 . 2
C3A C3A C3A 60.0 3 2
C2A C3A C2A 63.1 . 2
C3A C3A C2A 78.6 3 2
C2A C3A H3A 111.7 . .
C3A C3A H3A 65.9 3 .
C3A C3A H3A 111.7 2 .
C2A C3A H3A 144.5 2 .
C2A C3A H3B 111.7 . .
C3A C3A H3B 164.5 3 .
C3A C3A H3B 111.7 2 .
C2A C3A H3B 104.5 2 .
H3A C3A H3B 109.5 . .
C2A C3A H3C 114.7 . .
C3A C3A H3C 114.7 3 .
C3A C3A H3C 144.0 2 .
C2A C3A H3C 166.5 2 .
H3A C3A H3C 48.9 . .
H3B C3A H3C 63.2 . .
C2A C3A H3D 114.8 . .
C3A C3A H3D 114.7 3 .
C3A C3A H3D 55.3 2 .
C2A C3A H3D 61.1 2 .
H3A C3A H3D 133.3 . .
H3B C3A H3D 56.6 . .
H3C C3A H3D 111.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O3 2.660(2) .
K1 O2 2.778(4) 3
K1 O2 2.778(4) 2
K1 O2 2.778(4) .
K1 O1 2.812(3) 2
K1 O1 2.812(3) .
K1 O1 2.812(3) 3
K1 C1 3.217(5) .
K1 C1 3.217(5) 2
K1 C1 3.217(5) 3
K1 C2A 3.460(2) 2
K1 C2A 3.460(2) 3
K2 O2 2.647(3) 5
K2 O2 2.647(3) 2
K2 O2 2.647(3) 6
K2 O2 2.647(3) 4
K2 O2 2.647(3) 3
K2 O2 2.647(3) .
K2 C1 3.094(5) 6
K2 C1 3.094(5) 2
K2 C1 3.094(5) 4
K2 C1 3.094(5) .
K2 C1 3.094(5) 5
K2 C1 3.094(5) 3
K3 O2 2.679(4) .
K3 O2 2.679(4) 4
K3 C3 3.016(6) 5
K3 C3 3.016(6) 2
K3 C2 3.185(6) 5
K3 C2 3.185(5) 2
K3 C8 3.284(6) 2
K3 C8 3.284(6) 5
K3 C4 3.485(7) 2
K3 C4 3.485(7) 5
O1 B1 1.356(7) .
O1 C1 1.392(6) .
O2 C1 1.255(6) .
C1 C2 1.379(7) .
C2 C3 1.411(7) .
C2 C2 1.490(10) 5
C2 K3 3.185(5) 3
C3 C8 1.400(8) .
C3 C4 1.409(8) .
C3 K3 3.016(6) 3
C4 C5 1.344(9) .
C4 K3 3.485(7) 3
C4 H4 0.9500 .
C5 C6 1.396(10) .
C5 H5 0.9500 .
C6 C7 1.348(9) .
C6 H6 0.9500 .
C7 C8 1.397(8) .
C7 H7 0.9500 .
C8 B1 1.503(9) .
C8 K3 3.284(6) 3
C9 C10 1.385(9) .
C9 C14 1.405(9) .
C9 B1 1.575(8) .
C10 C11 1.383(9) .
C10 C15 1.513(10) .
C11 C12 1.358(12) .
C11 H11 0.9500 .
C12 C13 1.362(12) .
C12 C18 1.520(11) .
C13 C14 1.393(10) .
C13 H13 0.9500 .
C14 C21 1.500(11) .
C15 C16 1.508(10) .
C15 C17 1.514(10) .
C15 H15 1.0000 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 C20 1.316(18) .
C18 C19 1.365(19) .
C18 H18 1.0000 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 C23 1.502(11) .
C21 C22 1.502(12) .
C21 H21 1.0000 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
O3 C2A 1.2177 .
O3 C2A 1.2177 2
O3 C2A 1.2177 3
C2A C3A 1.3426 .
C2A H2A 0.9695 .
C2A H2B 0.9704 .
C3A C3A 1.5657 3
C3A C3A 1.5658 2
C3A H3A 0.9700 .
C3A H3B 0.9700 .
C3A H3C 0.9700 .
C3A H3D 0.9700 .
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
K2 O2 C1 C2 -67.7(6) . .
K3 O2 C1 C2 20.5(7) . .
K1 O2 C1 C2 -150.8(5) . .
K2 O2 C1 O1 110.3(4) . .
K3 O2 C1 O1 -161.5(3) . .
K1 O2 C1 O1 27.2(4) . .
K3 O2 C1 K2 88.2(3) . .
K1 O2 C1 K2 -83.07(14) . .
K2 O2 C1 K1 83.07(14) . .
K3 O2 C1 K1 171.2(4) . .
B1 O1 C1 O2 -179.3(5) . .
K1 O1 C1 O2 -26.6(4) . .
B1 O1 C1 C2 -1.1(7) . .
K1 O1 C1 C2 151.6(4) . .
B1 O1 C1 K2 -114.4(5) . .
K1 O1 C1 K2 38.3(3) . .
B1 O1 C1 K1 -152.7(5) . .
O2 C1 C2 C3 178.8(5) . .
O1 C1 C2 C3 0.9(8) . .
K2 C1 C2 C3 127.1(5) . .
K1 C1 C2 C3 82.4(10) . .
O2 C1 C2 C2 -5.0(8) . 5
O1 C1 C2 C2 177.1(4) . 5
K2 C1 C2 C2 -56.7(5) . 5
K1 C1 C2 C2 -101.3(9) . 5
O2 C1 C2 K3 107.9(5) . 3
O1 C1 C2 K3 -70.0(4) . 3
K2 C1 C2 K3 56.21(18) . 3
K1 C1 C2 K3 11.6(9) . 3
O2 C1 C2 K2 51.7(5) . .
O1 C1 C2 K2 -126.2(5) . .
K1 C1 C2 K2 -44.6(8) . .
C1 C2 C3 C8 -1.7(9) . .
C2 C2 C3 C8 -177.8(5) 5 .
K3 C2 C3 C8 84.0(6) 3 .
K2 C2 C3 C8 78.8(7) . .
C1 C2 C3 C4 179.8(6) . .
C2 C2 C3 C4 3.6(9) 5 .
K3 C2 C3 C4 -94.5(6) 3 .
K2 C2 C3 C4 -99.8(7) . .
C1 C2 C3 K3 -85.7(5) . 3
C2 C2 C3 K3 98.2(5) 5 3
K2 C2 C3 K3 -5.2(4) . 3
C8 C3 C4 C5 0.0(11) . .
C2 C3 C4 C5 178.7(7) . .
K3 C3 C4 C5 91.8(7) 3 .
C8 C3 C4 K3 -91.7(6) . 3
C2 C3 C4 K3 86.9(5) . 3
C3 C4 C5 C6 0.7(14) . .
K3 C4 C5 C6 64.1(10) 3 .
C4 C5 C6 C7 -0.8(15) . .
C5 C6 C7 C8 0.2(14) . .
C6 C7 C8 C3 0.5(12) . .
C6 C7 C8 B1 178.8(8) . .
C6 C7 C8 K3 -72.0(9) . 3
C4 C3 C8 C7 -0.6(10) . .
C2 C3 C8 C7 -179.2(6) . .
K3 C3 C8 C7 -97.8(6) 3 .
C4 C3 C8 B1 -179.0(6) . .
C2 C3 C8 B1 2.4(9) . .
K3 C3 C8 B1 83.9(6) 3 .
C4 C3 C8 K3 97.1(6) . 3
C2 C3 C8 K3 -81.5(5) . 3
C14 C9 C10 C11 -1.5(10) . .
B1 C9 C10 C11 -176.7(6) . .
C14 C9 C10 C15 177.7(6) . .
B1 C9 C10 C15 2.6(10) . .
C9 C10 C11 C12 -1.5(12) . .
C15 C10 C11 C12 179.3(8) . .
C10 C11 C12 C13 2.9(15) . .
C10 C11 C12 C18 -177.0(10) . .
C11 C12 C13 C14 -1.5(16) . .
C18 C12 C13 C14 178.4(10) . .
C12 C13 C14 C9 -1.4(14) . .
C12 C13 C14 C21 177.4(9) . .
C10 C9 C14 C13 2.8(11) . .
B1 C9 C14 C13 178.1(7) . .
C10 C9 C14 C21 -175.9(7) . .
B1 C9 C14 C21 -0.6(10) . .
C11 C10 C15 C16 -56.7(9) . .
C9 C10 C15 C16 124.0(7) . .
C11 C10 C15 C17 68.1(9) . .
C9 C10 C15 C17 -111.2(8) . .
C11 C12 C18 C20 -57.0(19) . .
C13 C12 C18 C20 123.1(15) . .
C11 C12 C18 C19 87(2) . .
C13 C12 C18 C19 -92.5(19) . .
C13 C14 C21 C23 40.1(12) . .
C9 C14 C21 C23 -141.2(8) . .
C13 C14 C21 C22 -85.7(10) . .
C9 C14 C21 C22 93.0(9) . .
C1 O1 B1 C8 1.9(9) . .
K1 O1 B1 C8 -138.5(5) . .
C1 O1 B1 C9 -177.6(5) . .
K1 O1 B1 C9 42.0(8) . .
C7 C8 B1 O1 179.2(6) . .
C3 C8 B1 O1 -2.5(9) . .
K3 C8 B1 O1 64.0(6) 3 .
C7 C8 B1 C9 -1.3(11) . .
C3 C8 B1 C9 177.0(6) . .
K3 C8 B1 C9 -116.6(6) 3 .
C10 C9 B1 O1 -98.3(8) . .
C14 C9 B1 O1 86.5(8) . .
C10 C9 B1 C8 82.2(9) . .
C14 C9 B1 C8 -92.9(8) . .
C2A O3 C2A C3A -31.3 2 .
C2A O3 C2A C3A 63.8 3 .
K1 O3 C2A C3A -163.734(6) . .
C2A O3 C2A C2A 95.2 3 2
K1 O3 C2A C2A -132.423(11) . 2
C2A O3 C2A C2A -95.2 2 3
K1 O3 C2A C2A 132.426(11) . 3
C2A O3 C2A C3A -75.5 2 3
C2A O3 C2A C3A 19.7 3 3
C2A O3 C2A K1 132.423(11) 2 .
C2A O3 C2A K1 -132.426(11) 3 .
O3 C2A C3A C3A -59.2 . 3
C2A C2A C3A C3A -80.5 2 3
C2A C2A C3A C3A -21.7 3 3
O3 C2A C3A C3A -1.4 . 2
C2A C2A C3A C3A -22.8 2 2
C2A C2A C3A C3A 36.0 3 2
C3A C2A C3A C3A 57.8 3 2
O3 C2A C3A C2A 21.4 . 2
C2A C2A C3A C2A 58.8 3 2
C3A C2A C3A C2A 80.5 3 2
