#------------------------------------------------------------------------------
#$Date: 2023-02-09 12:15:12 +0200 (Thu, 09 Feb 2023) $
#$Revision: 280846 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/67/8106743.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_8106743
loop_
_publ_author_name
'Liu, Yingfan'
'Mao, Kaiming'
'Li, Xiaochuan'
'Son, Young-A'
_publ_section_title
;
 Crystal structure of
 bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-9,9-dioctylfluorene,
 C41H64B2O4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              987
_journal_page_last               989
_journal_paper_doi               10.1515/ncrs-2017-0120
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C41 H64 B2 O4'
_chemical_formula_sum            'C41 H64 B2 O4'
_chemical_formula_weight         642.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                110.394(3)
_cell_angle_beta                 90.1700(10)
_cell_angle_gamma                115.623(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8189(8)
_cell_length_b                   13.4808(9)
_cell_length_c                   14.1592(12)
_cell_measurement_reflns_used    4766
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.10
_cell_measurement_theta_min      2.58
_cell_volume                     2033.5(3)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40607
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.560
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.064
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         8001
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0562
_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)+(0.0816P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4054
_reflns_number_total             8001
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2017-0120_suppl.cif
_cod_data_source_block           cnu1271
_cod_database_code               8106743
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H20C-H22F
 2 with sigma of 0.01
3. Rigid bond restraints
 C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C21A(0.5) H21D(0.5)
 H21E(0.5) H21F(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C22A(0.5) H22D(0.5)
 H22E(0.5) H22F(0.5)
 Fixed U11: C20(0.124802)
6.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
6.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C47(H47A,
 H47B,H47C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C9(H9), C13(H13)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C22(H22A,H22B,H22C), C22A(H22D,
 H22E,H22F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B14 B 0.4188(2) 0.3316(3) 0.0820(2) 0.0507(7) Uani 1 1 d . . . . .
B23 B 1.1053(2) 0.2639(2) 0.32668(18) 0.0424(6) Uani 1 1 d . . . . .
C1 C 0.53085(18) 0.34476(19) 0.13781(15) 0.0428(5) Uani 1 1 d . . . . .
C2 C 0.59989(18) 0.44522(19) 0.22562(16) 0.0460(5) Uani 1 1 d . . . . .
H2 H 0.5763 0.5042 0.2520 0.055 Uiso 1 1 calc R . . . .
C3 C 0.70155(18) 0.46007(18) 0.27455(15) 0.0436(5) Uani 1 1 d . . . . .
H3 H 0.7462 0.5280 0.3329 0.052 Uiso 1 1 calc R . . . .
C4 C 0.73628(16) 0.37159(17) 0.23516(14) 0.0355(5) Uani 1 1 d . . . . .
C5 C 0.83877(16) 0.36287(17) 0.26961(13) 0.0345(5) Uani 1 1 d . . . . .
C6 C 0.93078(18) 0.43936(18) 0.35139(14) 0.0423(5) Uani 1 1 d . . . . .
H6 H 0.9356 0.5117 0.3950 0.051 Uiso 1 1 calc R . . . .
C7 C 1.01530(18) 0.40692(18) 0.36736(15) 0.0432(5) Uani 1 1 d . . . . .
H7 H 1.0772 0.4587 0.4226 0.052 Uiso 1 1 calc R . . . .
C8 C 1.01160(17) 0.29945(18) 0.30392(14) 0.0391(5) Uani 1 1 d . . . . .
C9 C 0.91865(17) 0.22411(18) 0.21986(15) 0.0401(5) Uani 1 1 d . . . . .
H9 H 0.9148 0.1526 0.1752 0.048 Uiso 1 1 calc R . . . .
C10 C 0.83319(16) 0.25494(17) 0.20289(14) 0.0359(5) Uani 1 1 d . . . . .
C11 C 0.72402(16) 0.18556(17) 0.11911(14) 0.0367(5) Uani 1 1 d . . . . .
C12 C 0.66874(17) 0.26940(17) 0.14778(14) 0.0358(5) Uani 1 1 d . . . . .
C13 C 0.56718(17) 0.25651(18) 0.09969(15) 0.0419(5) Uani 1 1 d . . . . .
H13 H 0.5225 0.1885 0.0414 0.050 Uiso 1 1 calc R . . . .
C16 C 0.2766(2) 0.3773(2) 0.04381(19) 0.0605(7) Uani 1 1 d . U . . .
C17 C 0.2540(3) 0.2544(3) -0.0353(2) 0.0860(9) Uani 1 1 d . U . . .
C19 C 0.1819(3) 0.3770(4) 0.1045(3) 0.1287(14) Uani 1 1 d . . . . .
H19A H 0.1115 0.3528 0.0597 0.193 Uiso 1 1 calc R . . . .
H19B H 0.1668 0.3222 0.1376 0.193 Uiso 1 1 calc R . . . .
H19C H 0.2063 0.4557 0.1553 0.193 Uiso 1 1 calc R . . . .
C20 C 0.3073(3) 0.4731(3) 0.0026(3) 0.1307(14) Uani 1 1 d . . . . .
H20A H 0.2410 0.4531 -0.0451 0.196 Uiso 1 1 calc R . . . .
H20B H 0.3275 0.5478 0.0580 0.196 Uiso 1 1 calc R . . . .
H20C H 0.3731 0.4795 -0.0317 0.196 Uiso 1 1 calc DR . . . .
C21 C 0.1453(7) 0.1481(8) -0.0010(6) 0.097(2) Uani 0.5 1 d . U P A 1
H21A H 0.1651 0.1669 0.0707 0.145 Uiso 0.5 1 calc GR . P A 1
H21B H 0.1391 0.0709 -0.0402 0.145 Uiso 0.5 1 calc GR . P A 1
H21C H 0.0715 0.1473 -0.0145 0.145 Uiso 0.5 1 calc GR . P A 1
C21A C 0.1502(9) 0.1600(9) -0.0709(10) 0.149(4) Uani 0.5 1 d . U P A 2
H21D H 0.1168 0.1411 -0.0151 0.224 Uiso 0.5 1 calc GR . P A 2
H21E H 0.1586 0.0936 -0.1177 0.224 Uiso 0.5 1 calc GR . P A 2
H21F H 0.0993 0.1764 -0.1061 0.224 Uiso 0.5 1 calc GR . P A 2
C22 C 0.2226(8) 0.2116(10) -0.1427(6) 0.107(3) Uani 0.5 1 d . U P A 1
H22A H 0.1638 0.2321 -0.1590 0.160 Uiso 0.5 1 calc GR . P A 1
H22B H 0.1918 0.1265 -0.1715 0.160 Uiso 0.5 1 calc GR . P A 1
H22C H 0.2908 0.2472 -0.1706 0.160 Uiso 0.5 1 calc GR . P A 1
C22A C 0.3034(8) 0.2875(9) -0.1406(6) 0.112(3) Uani 0.5 1 d . U P A 2
H22D H 0.2654 0.3284 -0.1575 0.168 Uiso 0.5 1 calc GR . P A 2
H22E H 0.2851 0.2148 -0.1980 0.168 Uiso 0.5 1 calc GR . P A 2
H22F H 0.3870 0.3376 -0.1240 0.168 Uiso 0.5 1 calc DGR . P A 2
C25 C 1.2684(2) 0.2753(2) 0.40343(17) 0.0545(6) Uani 1 1 d . . . . .
C26 C 1.2018(2) 0.1535(2) 0.31271(17) 0.0534(6) Uani 1 1 d . . . . .
C28 C 1.3033(3) 0.2699(3) 0.50190(19) 0.0934(10) Uani 1 1 d . . . . .
H28A H 1.3605 0.2408 0.4937 0.140 Uiso 1 1 calc R . . . .
H28B H 1.3366 0.3483 0.5553 0.140 Uiso 1 1 calc R . . . .
H28C H 1.2353 0.2172 0.5198 0.140 Uiso 1 1 calc R . . . .
C29 C 1.3734(2) 0.3652(2) 0.3767(2) 0.0840(9) Uani 1 1 d . . . . .
H29A H 1.4336 0.3401 0.3669 0.126 Uiso 1 1 calc R . . . .
H29B H 1.3487 0.3696 0.3149 0.126 Uiso 1 1 calc R . . . .
H29C H 1.4040 0.4423 0.4316 0.126 Uiso 1 1 calc R . . . .
C30 C 1.1272(3) 0.0520(3) 0.3440(3) 0.0944(10) Uani 1 1 d . . . . .
H30A H 1.1772 0.0358 0.3804 0.142 Uiso 1 1 calc R . . . .
H30B H 1.0768 0.0736 0.3875 0.142 Uiso 1 1 calc R . . . .
H30C H 1.0801 -0.0180 0.2841 0.142 Uiso 1 1 calc R . . . .
C31 C 1.2774(3) 0.1186(3) 0.2397(2) 0.0857(9) Uani 1 1 d . . . . .
H31A H 1.3318 0.1056 0.2743 0.129 Uiso 1 1 calc R . . . .
H31B H 1.2282 0.0467 0.1820 0.129 Uiso 1 1 calc R . . . .
H31C H 1.3203 0.1815 0.2165 0.129 Uiso 1 1 calc R . . . .
C32 C 0.64306(18) 0.06334(18) 0.12105(15) 0.0451(5) Uani 1 1 d . . . . .
H32A H 0.5726 0.0262 0.0700 0.054 Uiso 1 1 calc R . . . .
H32B H 0.6825 0.0140 0.1002 0.054 Uiso 1 1 calc R . . . .
C33 C 0.6059(2) 0.0619(2) 0.22192(17) 0.0582(6) Uani 1 1 d . U . . .
H33A H 0.5606 0.1055 0.2411 0.070 Uiso 1 1 calc R . . . .
H33B H 0.6754 0.1021 0.2746 0.070 Uiso 1 1 calc R . . . .
C34 C 0.5324(2) -0.0643(2) 0.21643(19) 0.0709(7) Uani 1 1 d . U . . .
H34A H 0.4594 -0.1008 0.1687 0.085 Uiso 1 1 calc R . . . .
H34B H 0.5744 -0.1099 0.1887 0.085 Uiso 1 1 calc R . . . .
C35 C 0.5037(3) -0.0741(2) 0.3143(2) 0.0841(9) Uani 1 1 d . . . . .
H35A H 0.4543 -0.0360 0.3384 0.101 Uiso 1 1 calc R . . . .
H35B H 0.5761 -0.0302 0.3643 0.101 Uiso 1 1 calc R . . . .
C36 C 0.4411(3) -0.2016(2) 0.3098(2) 0.0811(8) Uani 1 1 d . . . . .
H36A H 0.3660 -0.2441 0.2637 0.097 Uiso 1 1 calc R . . . .
H36B H 0.4879 -0.2416 0.2816 0.097 Uiso 1 1 calc R . . . .
C37 C 0.4203(2) -0.2088(2) 0.4117(2) 0.0770(8) Uani 1 1 d . . . . .
H37A H 0.3723 -0.1700 0.4392 0.092 Uiso 1 1 calc R . . . .
H37B H 0.4953 -0.1646 0.4582 0.092 Uiso 1 1 calc R . . . .
C38 C 0.3612(2) -0.3331(2) 0.4095(2) 0.0750(8) Uani 1 1 d . . . . .
H38A H 0.4097 -0.3718 0.3837 0.090 Uiso 1 1 calc R . . . .
H38B H 0.2865 -0.3782 0.3624 0.090 Uiso 1 1 calc R . . . .
C39 C 0.3398(3) -0.3364(3) 0.5130(2) 0.0921(9) Uani 1 1 d . . . . .
H39A H 0.3019 -0.4178 0.5071 0.138 Uiso 1 1 calc R . . . .
H39B H 0.4136 -0.2935 0.5596 0.138 Uiso 1 1 calc R . . . .
H39C H 0.2903 -0.2999 0.5383 0.138 Uiso 1 1 calc R . . . .
C40 C 0.75755(18) 0.16616(18) 0.01183(14) 0.0440(5) Uani 1 1 d . . . . .
H40A H 0.8015 0.1211 0.0017 0.053 Uiso 1 1 calc R . . . .
H40B H 0.6855 0.1170 -0.0388 0.053 Uiso 1 1 calc R . . . .
C41 C 0.8289(2) 0.27638(19) -0.00976(16) 0.0500(6) Uani 1 1 d . . . . .
H41A H 0.8982 0.3297 0.0435 0.060 Uiso 1 1 calc R . . . .
H41B H 0.7824 0.3177 -0.0077 0.060 Uiso 1 1 calc R . . . .
C42 C 0.8669(2) 0.2475(2) -0.11318(16) 0.0537(6) Uani 1 1 d . . . . .
H42A H 0.9119 0.2049 -0.1147 0.064 Uiso 1 1 calc R . . . .
H42B H 0.7969 0.1938 -0.1656 0.064 Uiso 1 1 calc R . . . .
C43 C 0.9392(2) 0.3519(2) -0.14103(18) 0.0635(7) Uani 1 1 d . . . . .
H43A H 1.0040 0.4108 -0.0847 0.076 Uiso 1 1 calc R . . . .
H43B H 0.8908 0.3883 -0.1492 0.076 Uiso 1 1 calc R . . . .
C44 C 0.9887(2) 0.3206(2) -0.23837(18) 0.0670(7) Uani 1 1 d . . . . .
H44A H 1.0462 0.3942 -0.2427 0.080 Uiso 1 1 calc R . . . .
H44B H 1.0299 0.2765 -0.2329 0.080 Uiso 1 1 calc R . . . .
C45 C 0.8997(2) 0.2484(2) -0.33625(17) 0.0636(7) Uani 1 1 d . . . . .
H45A H 0.8659 0.2968 -0.3465 0.076 Uiso 1 1 calc R . . . .
H45B H 0.8366 0.1800 -0.3286 0.076 Uiso 1 1 calc R . . . .
C46 C 0.9472(2) 0.2041(3) -0.4314(2) 0.0755(8) Uani 1 1 d . . . . .
H46A H 1.0088 0.2725 -0.4403 0.091 Uiso 1 1 calc R . . . .
H46B H 0.9825 0.1571 -0.4209 0.091 Uiso 1 1 calc R . . . .
C47 C 0.8568(3) 0.1301(3) -0.5276(2) 0.1083(12) Uani 1 1 d . . . . .
H47A H 0.8932 0.1055 -0.5842 0.162 Uiso 1 1 calc R . . . .
H47B H 0.7963 0.0610 -0.5204 0.162 Uiso 1 1 calc R . . . .
H47C H 0.8227 0.1764 -0.5399 0.162 Uiso 1 1 calc R . . . .
O15 O 0.37965(15) 0.41385(17) 0.11384(14) 0.0836(6) Uani 1 1 d . U . . .
O18 O 0.35014(15) 0.23786(16) -0.00405(13) 0.0765(5) Uani 1 1 d . . . . .
O24 O 1.18142(12) 0.31967(13) 0.41708(10) 0.0534(4) Uani 1 1 d . . . . .
O27 O 1.12032(13) 0.17268(13) 0.25826(11) 0.0572(4) Uani 1 1 d . . . . .
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'
B B 0.0013 0.0007 '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'
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
O15 B14 C1 123.5(2) . .
O18 B14 C1 124.0(2) . .
O18 B14 O15 112.4(2) . .
O24 B23 C8 123.6(2) . .
O24 B23 O27 112.73(19) . .
O27 B23 C8 123.65(19) . .
C2 C1 B14 121.48(19) . .
C2 C1 C13 118.05(18) . .
C13 C1 B14 120.46(19) . .
C1 C2 H2 118.8 . .
C3 C2 C1 122.32(19) . .
C3 C2 H2 118.8 . .
C2 C3 H3 120.7 . .
C2 C3 C4 118.69(19) . .
C4 C3 H3 120.7 . .
C3 C4 C5 130.98(18) . .
C3 C4 C12 120.49(18) . .
C12 C4 C5 108.53(16) . .
C6 C5 C4 131.27(18) . .
C6 C5 C10 120.25(18) . .
C10 C5 C4 108.49(16) . .
C5 C6 H6 120.5 . .
C7 C6 C5 118.98(19) . .
C7 C6 H6 120.5 . .
C6 C7 H7 118.8 . .
C6 C7 C8 122.46(18) . .
C8 C7 H7 118.8 . .
C7 C8 B23 120.99(18) . .
C7 C8 C9 117.64(18) . .
C9 C8 B23 121.36(19) . .
C8 C9 H9 119.7 . .
C10 C9 C8 120.66(19) . .
C10 C9 H9 119.7 . .
C5 C10 C11 110.78(16) . .
C9 C10 C5 119.98(18) . .
C9 C10 C11 129.22(18) . .
C10 C11 C32 111.83(16) . .
C10 C11 C40 111.23(16) . .
C12 C11 C10 101.15(14) . .
C12 C11 C32 112.42(16) . .
C12 C11 C40 111.85(16) . .
C32 C11 C40 108.30(15) . .
C4 C12 C11 111.05(16) . .
C13 C12 C4 119.85(18) . .
C13 C12 C11 129.10(17) . .
C1 C13 H13 119.7 . .
C12 C13 C1 120.61(18) . .
C12 C13 H13 119.7 . .
C19 C16 C17 115.4(3) . .
C19 C16 C20 108.2(3) . .
C20 C16 C17 115.3(3) . .
O15 C16 C17 103.95(18) . .
O15 C16 C19 107.4(2) . .
O15 C16 C20 105.9(2) . .
C16 C17 C21 106.9(4) . .
C16 C17 C22A 102.3(4) . .
C21A C17 C16 124.7(6) . .
C21A C17 C22A 106.2(7) . .
C21A C17 O18 117.3(5) . .
C22 C17 C16 127.1(5) . .
C22 C17 C21 104.6(5) . .
C22 C17 O18 113.0(4) . .
O18 C17 C16 104.2(2) . .
O18 C17 C21 96.7(4) . .
O18 C17 C22A 97.7(3) . .
C16 C19 H19A 109.5 . .
C16 C19 H19B 109.5 . .
C16 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C16 C20 H20A 109.5 . .
C16 C20 H20B 109.5 . .
C16 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C17 C21 H21A 109.5 . .
C17 C21 H21B 109.5 . .
C17 C21 H21C 109.5 . .
H21A C21 H21B 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C17 C21A H21D 109.5 . .
C17 C21A H21E 109.5 . .
C17 C21A H21F 109.5 . .
H21D C21A H21E 109.5 . .
H21D C21A H21F 109.5 . .
H21E C21A H21F 109.5 . .
C17 C22 H22A 109.5 . .
C17 C22 H22B 109.5 . .
C17 C22 H22C 109.5 . .
H22A C22 H22B 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C17 C22A H22D 109.5 . .
C17 C22A H22E 109.5 . .
C17 C22A H22F 109.5 . .
H22D C22A H22E 109.5 . .
H22D C22A H22F 109.5 . .
H22E C22A H22F 109.5 . .
C28 C25 C26 115.4(2) . .
C28 C25 C29 110.6(2) . .
C29 C25 C26 112.9(2) . .
O24 C25 C26 102.17(16) . .
O24 C25 C28 108.81(19) . .
O24 C25 C29 106.06(19) . .
C30 C26 C25 114.0(2) . .
C30 C26 C31 110.2(2) . .
C31 C26 C25 114.9(2) . .
O27 C26 C25 102.29(16) . .
O27 C26 C30 106.31(19) . .
O27 C26 C31 108.29(19) . .
C25 C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
C25 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C25 C29 H29A 109.5 . .
C25 C29 H29B 109.5 . .
C25 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C26 C30 H30A 109.5 . .
C26 C30 H30B 109.5 . .
C26 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C26 C31 H31A 109.5 . .
C26 C31 H31B 109.5 . .
C26 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C11 C32 H32A 108.1 . .
C11 C32 H32B 108.1 . .
H32A C32 H32B 107.3 . .
C33 C32 C11 116.78(17) . .
C33 C32 H32A 108.1 . .
C33 C32 H32B 108.1 . .
C32 C33 H33A 109.2 . .
C32 C33 H33B 109.2 . .
C32 C33 C34 112.08(19) . .
H33A C33 H33B 107.9 . .
C34 C33 H33A 109.2 . .
C34 C33 H33B 109.2 . .
C33 C34 H34A 108.4 . .
C33 C34 H34B 108.4 . .
H34A C34 H34B 107.5 . .
C35 C34 C33 115.5(2) . .
C35 C34 H34A 108.4 . .
C35 C34 H34B 108.4 . .
C34 C35 H35A 108.5 . .
C34 C35 H35B 108.5 . .
C34 C35 C36 114.9(2) . .
H35A C35 H35B 107.5 . .
C36 C35 H35A 108.5 . .
C36 C35 H35B 108.5 . .
C35 C36 H36A 108.8 . .
C35 C36 H36B 108.8 . .
H36A C36 H36B 107.7 . .
C37 C36 C35 113.8(2) . .
C37 C36 H36A 108.8 . .
C37 C36 H36B 108.8 . .
C36 C37 H37A 108.6 . .
C36 C37 H37B 108.6 . .
C36 C37 C38 114.8(2) . .
H37A C37 H37B 107.6 . .
C38 C37 H37A 108.6 . .
C38 C37 H37B 108.6 . .
C37 C38 H38A 109.0 . .
C37 C38 H38B 109.0 . .
C37 C38 C39 113.0(2) . .
H38A C38 H38B 107.8 . .
C39 C38 H38A 109.0 . .
C39 C38 H38B 109.0 . .
C38 C39 H39A 109.5 . .
C38 C39 H39B 109.5 . .
C38 C39 H39C 109.5 . .
H39A C39 H39B 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
C11 C40 H40A 108.0 . .
C11 C40 H40B 108.0 . .
H40A C40 H40B 107.3 . .
C41 C40 C11 117.02(16) . .
C41 C40 H40A 108.0 . .
C41 C40 H40B 108.0 . .
C40 C41 H41A 109.1 . .
C40 C41 H41B 109.1 . .
C40 C41 C42 112.51(18) . .
H41A C41 H41B 107.8 . .
C42 C41 H41A 109.1 . .
C42 C41 H41B 109.1 . .
C41 C42 H42A 108.2 . .
C41 C42 H42B 108.2 . .
H42A C42 H42B 107.4 . .
C43 C42 C41 116.30(19) . .
C43 C42 H42A 108.2 . .
C43 C42 H42B 108.2 . .
C42 C43 H43A 108.7 . .
C42 C43 H43B 108.7 . .
C42 C43 C44 114.4(2) . .
H43A C43 H43B 107.6 . .
C44 C43 H43A 108.7 . .
C44 C43 H43B 108.7 . .
C43 C44 H44A 108.4 . .
C43 C44 H44B 108.4 . .
H44A C44 H44B 107.5 . .
C45 C44 C43 115.4(2) . .
C45 C44 H44A 108.4 . .
C45 C44 H44B 108.4 . .
C44 C45 H45A 108.5 . .
C44 C45 H45B 108.5 . .
C44 C45 C46 115.1(2) . .
H45A C45 H45B 107.5 . .
C46 C45 H45A 108.5 . .
C46 C45 H45B 108.5 . .
C45 C46 H46A 108.7 . .
C45 C46 H46B 108.7 . .
H46A C46 H46B 107.6 . .
C47 C46 C45 114.3(2) . .
C47 C46 H46A 108.7 . .
C47 C46 H46B 108.7 . .
C46 C47 H47A 109.5 . .
C46 C47 H47B 109.5 . .
C46 C47 H47C 109.5 . .
H47A C47 H47B 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
B14 O15 C16 109.82(19) . .
B14 O18 C17 109.5(2) . .
B23 O24 C25 107.42(16) . .
B23 O27 C26 107.42(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B14 C1 1.548(3) .
B14 O15 1.348(3) .
B14 O18 1.347(3) .
B23 C8 1.542(3) .
B23 O24 1.358(3) .
B23 O27 1.365(3) .
C1 C2 1.395(3) .
C1 C13 1.399(3) .
C2 H2 0.9300 .
C2 C3 1.375(3) .
C3 H3 0.9300 .
C3 C4 1.389(3) .
C4 C5 1.465(3) .
C4 C12 1.397(2) .
C5 C6 1.379(3) .
C5 C10 1.402(2) .
C6 H6 0.9300 .
C6 C7 1.376(3) .
C7 H7 0.9300 .
C7 C8 1.393(3) .
C8 C9 1.404(3) .
C9 H9 0.9300 .
C9 C10 1.376(3) .
C10 C11 1.525(2) .
C11 C12 1.523(3) .
C11 C32 1.531(3) .
C11 C40 1.544(3) .
C12 C13 1.380(3) .
C13 H13 0.9300 .
C16 C17 1.540(4) .
C16 C19 1.488(4) .
C16 C20 1.500(4) .
C16 O15 1.435(3) .
C17 C21 1.730(9) .
C17 C21A 1.315(9) .
C17 C22 1.411(8) .
C17 C22A 1.746(9) .
C17 O18 1.439(3) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C21A H21D 0.9600 .
C21A H21E 0.9600 .
C21A H21F 0.9600 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C22A H22D 0.9600 .
C22A H22E 0.9600 .
C22A H22F 0.9600 .
C25 C26 1.545(3) .
C25 C28 1.498(3) .
C25 C29 1.529(3) .
C25 O24 1.461(2) .
C26 C30 1.509(3) .
C26 C31 1.514(3) .
C26 O27 1.456(2) .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C32 C33 1.511(3) .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C33 C34 1.519(3) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C34 C35 1.470(3) .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
C35 C36 1.528(4) .
C36 H36A 0.9700 .
C36 H36B 0.9700 .
C36 C37 1.496(3) .
C37 H37A 0.9700 .
C37 H37B 0.9700 .
C37 C38 1.499(3) .
C38 H38A 0.9700 .
C38 H38B 0.9700 .
C38 C39 1.504(3) .
C39 H39A 0.9600 .
C39 H39B 0.9600 .
C39 H39C 0.9600 .
C40 H40A 0.9700 .
C40 H40B 0.9700 .
C40 C41 1.510(3) .
C41 H41A 0.9700 .
C41 H41B 0.9700 .
C41 C42 1.518(3) .
C42 H42A 0.9700 .
C42 H42B 0.9700 .
C42 C43 1.502(3) .
C43 H43A 0.9700 .
C43 H43B 0.9700 .
C43 C44 1.520(3) .
C44 H44A 0.9700 .
C44 H44B 0.9700 .
C44 C45 1.504(3) .
C45 H45A 0.9700 .
C45 H45B 0.9700 .
C45 C46 1.517(3) .
C46 H46A 0.9700 .
C46 H46B 0.9700 .
C46 C47 1.496(4) .
C47 H47A 0.9600 .
C47 H47B 0.9600 .
C47 H47C 0.9600 .
