# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005



data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Todd Marder'
'Andrei S. Batsanov'
'David N. Coventry'
'Andres Eduardo Goeta'
'Judith A.K. Howard'
'Robin N Perutz'

_publ_contact_author_name        'Prof Todd Marder'
_publ_contact_author_address     
;
Department of Chemistry
University of Durham
South Road
Durham
DH1  3LE
;

_publ_contact_author_email       TODD.MARDER@DURHAM.AC.UK

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Selective Ir-Catalysed Borylation of Polycyclic
Aromatic Hydrocarbons: Structures of Naphthalene-2,6-bis(boronate),
Pyrene-2,7-bis(boronate) and Perylene-2,5,8,11-tetra(boronate) esters
;

#==============================================

data_(1B'2)
_database_code_depnum_ccdc_archive 'CCDC 263078'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2,6-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)naphthalene
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H30 B2 O4'
_chemical_formula_sum            'C22 H30 B2 O4'
_chemical_formula_weight         380.08

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.501(1)
_cell_length_b                   16.249(2)
_cell_length_c                   10.146(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.70(1)
_cell_angle_gamma                90.00
_cell_volume                     1056.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    997
_cell_measurement_theta_min      10.22
_cell_measurement_theta_max      24.82

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             408
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.0300
1.00 0.00 -1.00 0.0300
0.00 1.00 0.00 0.1200
0.00 -1.00 0.00 0.1200
0.00 0.00 1.00 0.1200
0.00 0.00 -1.00 0.1200

_exptl_special_details           
;The data collection nominally covered full sphere
of reciprocal space, by a combination of 5 sets of \w scans;
each set at different \f and/or 2\q angles and each
scan (10 sec exposure) covering 0.3\% in \w. Crystal to
detector distance 4.84 cm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            14776
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         29.99
_reflns_number_total             3082
_reflns_number_gt                2138
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_structure_solution    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 5.10 (Bruker, 1997)'
_computing_publication_material  'SHELXTL version 5.10 (Bruker, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.
O(1), O(2), C(6), C(7), C(9) and C(11) with their hydrogens are
disordered between positions A (85%) and B (15%).
Disordered H atoms - riding (constr), other - refall.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0367P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3082
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1315
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1A O 0.05579(18) 0.13297(8) 0.63244(11) 0.0269(3) Uani 0.85 1 d P A 1
O2A O 0.36379(17) 0.14875(7) 0.55316(11) 0.0259(3) Uani 0.85 1 d P A 1
O1B O 0.0984(11) 0.1658(5) 0.6570(7) 0.0300(17) Uiso 0.15 1 d P A 2
O2B O 0.3172(11) 0.1123(5) 0.5269(7) 0.0300(15) Uiso 0.15 1 d P A 2
B B 0.2659(2) 0.11682(9) 0.65079(14) 0.0248(3) Uani 1 1 d . . .
C1 C 0.2916(2) 0.05567(7) 0.88438(12) 0.0245(3) Uani 1 1 d . . .
H1 H 0.150(2) 0.0737(8) 0.8897(13) 0.012(3) Uiso 1 1 d . . .
C2 C 0.3842(2) 0.06872(7) 0.77359(12) 0.0244(3) Uani 1 1 d . A .
C3 C 0.5913(2) 0.03933(8) 0.77555(12) 0.0284(3) Uani 1 1 d . . .
H3 H 0.661(2) 0.0491(10) 0.6960(16) 0.032(4) Uiso 1 1 d . . .
C4 C 0.6964(2) -0.00170(8) 0.88494(13) 0.0275(3) Uani 1 1 d . A .
H4 H 0.841(3) -0.0236(9) 0.8899(16) 0.031(4) Uiso 1 1 d . . .
C5 C 0.60291(19) -0.01468(7) 0.99979(12) 0.0229(3) Uani 1 1 d . . .
C6A C 0.0010(2) 0.16798(9) 0.49768(13) 0.0241(3) Uani 0.85 1 d P A 1
C7A C 0.2129(2) 0.20461(9) 0.47441(13) 0.0225(3) Uani 0.85 1 d P A 1
C6B C 0.0621(14) 0.2126(6) 0.5298(9) 0.0292(17) Uiso 0.15 1 d P A 2
C7B C 0.1518(14) 0.1536(6) 0.4346(9) 0.0281(17) Uiso 0.15 1 d P A 2
C8 C -0.1718(2) 0.23018(9) 0.49682(14) 0.0335(3) Uani 1 1 d . . .
H81 H -0.1988 0.2526 0.4079 0.050 Uiso 1 1 d R A .
H82 H -0.2883 0.1997 0.5140 0.050 Uiso 1 1 d R . .
H83 H -0.1336 0.2704 0.5577 0.050 Uiso 1 1 d R . .
C9A C -0.0753(4) 0.09686(12) 0.4048(2) 0.0355(5) Uani 0.85 1 d P A 1
H91 H 0.0374 0.0681 0.3886 0.053 Uiso 0.85 1 d PR A 1
H92 H -0.1208 0.1168 0.3168 0.053 Uiso 0.85 1 d PR A 1
H93 H -0.2018 0.0691 0.4316 0.053 Uiso 0.85 1 d PR A 1
C9B C -0.005(2) 0.0861(10) 0.3809(15) 0.045(4) Uiso 0.15 1 d P A 2
H91B H -0.0552 0.0590 0.4559 0.068 Uiso 0.15 1 d PR A 2
H92B H 0.0628 0.0454 0.3313 0.068 Uiso 0.15 1 d PR A 2
H93B H -0.1237 0.1106 0.3212 0.068 Uiso 0.15 1 d PR A 2
C10 C 0.2480(2) 0.20309(9) 0.32988(13) 0.0336(3) Uani 1 1 d . . .
H101 H 0.1448 0.2341 0.2767 0.050 Uiso 1 1 d R A .
H102 H 0.3784 0.2305 0.3334 0.050 Uiso 1 1 d R . .
H103 H 0.2516 0.1500 0.2886 0.050 Uiso 1 1 d R . .
C11A C 0.2555(3) 0.28980(11) 0.53433(18) 0.0295(4) Uani 0.85 1 d P A 1
H111 H 0.1666 0.3296 0.4780 0.044 Uiso 0.85 1 d PR A 1
H112 H 0.2270 0.2910 0.6222 0.044 Uiso 0.85 1 d PR A 1
H113 H 0.4138 0.3077 0.5307 0.044 Uiso 0.85 1 d PR A 1
C11B C 0.1844(18) 0.2943(7) 0.5580(12) 0.031(3) Uiso 0.15 1 d P A 2
H114 H 0.3342 0.2824 0.5792 0.046 Uiso 0.15 1 d PR A 2
H115 H 0.1400 0.3225 0.6339 0.046 Uiso 0.15 1 d PR A 2
H116 H 0.1568 0.3296 0.4787 0.046 Uiso 0.15 1 d PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0301(6) 0.0289(6) 0.0199(5) 0.0097(5) -0.0011(4) -0.0010(5)
O2 0.0273(6) 0.0265(6) 0.0220(5) 0.0085(4) -0.0012(4) 0.0048(4)
B 0.0316(7) 0.0206(6) 0.0202(6) 0.0016(5) -0.0019(5) 0.0003(5)
C1 0.0272(6) 0.0206(5) 0.0235(6) 0.0019(5) -0.0024(5) 0.0006(5)
C2 0.0313(6) 0.0195(5) 0.0198(5) 0.0026(4) -0.0034(5) -0.0008(4)
C3 0.0349(7) 0.0278(6) 0.0214(6) 0.0036(5) 0.0019(5) 0.0029(5)
C4 0.0286(7) 0.0286(6) 0.0243(6) 0.0032(5) 0.0015(5) 0.0032(5)
C5 0.0280(6) 0.0181(5) 0.0207(6) 0.0007(4) -0.0012(4) -0.0015(4)
C6A 0.0282(7) 0.0234(7) 0.0184(6) 0.0062(5) -0.0026(5) -0.0002(6)
C7A 0.0257(7) 0.0223(7) 0.0175(6) 0.0057(5) -0.0019(5) 0.0025(5)
C8 0.0308(7) 0.0384(8) 0.0303(7) 0.0095(6) 0.0022(5) 0.0064(6)
C9A 0.0442(12) 0.0267(9) 0.0291(9) 0.0039(7) -0.0121(9) -0.0063(8)
C10 0.0366(7) 0.0425(8) 0.0215(6) 0.0077(6) 0.0040(5) 0.0054(6)
C11A 0.0350(10) 0.0238(8) 0.0273(8) 0.0030(6) -0.0019(8) -0.0020(7)

_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
O1A B 1.3724(18) . ?
O1A C6A 1.4682(16) . ?
O2A B 1.3666(18) . ?
O2A C7A 1.4699(16) . ?
O1B B 1.359(7) . ?
O1B C6B 1.483(11) . ?
O2B B 1.355(7) . ?
O2B C7B 1.464(11) . ?
B C2 1.5595(17) . ?
C1 C2 1.3780(18) . ?
C1 C5 1.4224(16) 3_657 ?
C2 C3 1.4256(19) . ?
C3 C4 1.3737(17) . ?
C4 C5 1.4178(18) . ?
C5 C5 1.421(2) 3_657 ?
C5 C1 1.4224(16) 3_657 ?
C6A C8 1.510(2) . ?
C6A C9A 1.521(2) . ?
C6A C7A 1.555(2) . ?
C7A C11A 1.518(2) . ?
C7A C10 1.5217(19) . ?
C6B C8 1.528(9) . ?
C6B C7B 1.543(13) . ?
C6B C11B 1.548(15) . ?
C7B C9B 1.535(18) . ?
C7B C10 1.546(9) . ?

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
B O1A C6A 106.26(11) . . ?
B O2A C7A 106.19(11) . . ?
B O1B C6B 105.7(6) . . ?
B O2B C7B 107.4(6) . . ?
O2B B O1B 113.5(4) . . ?
O2B B O2A 29.7(3) . . ?
O1B B O2A 106.6(3) . . ?
O2B B O1A 106.2(3) . . ?
O1B B O1A 26.8(3) . . ?
O2A B O1A 113.80(11) . . ?
O2B B C2 123.2(3) . . ?
O1B B C2 123.2(3) . . ?
O2A B C2 122.82(12) . . ?
O1A B C2 123.36(12) . . ?
C2 C1 C5 122.01(12) . 3_657 ?
C1 C2 C3 118.58(11) . . ?
C1 C2 B 120.29(12) . . ?
C3 C2 B 121.11(11) . . ?
C4 C3 C2 120.91(12) . . ?
C3 C4 C5 120.84(12) . . ?
C4 C5 C5 119.12(13) . 3_657 ?
C4 C5 C1 122.35(12) . 3_657 ?
C5 C5 C1 118.53(14) 3_657 3_657 ?
O1A C6A C8 109.16(12) . . ?
O1A C6A C9 106.58(12) . . ?
C8 C6A C9 109.89(14) . . ?
O1A C6A C7A 101.99(10) . . ?
C8 C6A C7A 114.84(12) . . ?
C9 C6A C7A 113.70(15) . . ?
O2A C7A C11A 106.58(12) . . ?
O2A C7A C10 108.62(11) . . ?
C11A C7A C10 110.72(13) . . ?
O2A C7A C6A 102.01(10) . . ?
C11A C7A C6A 113.24(14) . . ?
C10 C7A C6A 114.87(11) . . ?
O1B C6B C8 107.0(6) . . ?
O1B C6B C7B 101.8(7) . . ?
C8 C6B C7B 116.5(7) . . ?
O1B C6B C11B 106.1(8) . . ?
C8 C6B C11B 110.0(7) . . ?
C7B C6B C11B 114.3(8) . . ?
O2B C7B C9B 105.8(9) . . ?
O2B C7B C6B 101.5(7) . . ?
C9B C7B C6B 111.6(8) . . ?
O2B C7B C10 109.9(6) . . ?
C9B C7B C10 116.7(8) . . ?
C6B C7B C10 110.2(7) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.048

#=============================================END

data_(2B2)
_database_code_depnum_ccdc_archive 'CCDC 263079'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;2,7-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-pyrene
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H32 B2 O4'
_chemical_formula_sum            'C28 H32 B2 O4'
_chemical_formula_weight         454.16
_chemical_absolute_configuration und

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.7931(5)
_cell_length_b                   17.790(2)
_cell_length_c                   20.368(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2461.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2981
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      29.84

_exptl_crystal_description       'thin needle'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 0.00 0.195
-1.00 0.00 0.00 0.195
0.00 -1.00 -1.00 0.030
0.00 1.00 1.00 0.030
0.00 -1.00 1.00 0.030
0.00 1.00 -1.00 0.030

_exptl_special_details           
;The data collection nominally covered over a hemisphere of reciprocal
space, by a combination of 3 sets of \w scans; each set at different
\f angles and each scan covering 0.3\% in \w. Crystal to detector
distance 4.84 cm. 7513 unique reflections before merging Friedel
equivalents.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART-6000 CCD Diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 5.6
_diffrn_standards_number         0
_diffrn_reflns_number            23207
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         30.51
_reflns_number_total             4237
_reflns_number_gt                2697
_reflns_threshold_expression     I>2\s(I)
_reflns_Friedel_coverage         0.77

_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.28A (Bruker, 2001)'
_computing_structure_solution    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.
The boryl substituent at C(20) is conformationally disordered: the atoms
O(1) and O(2), and methyl groups C(1)H~3~ and C(3)H~3~ occupy two sets of
positions (A and B) with equal probabilities.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'undeterminable, Friedel equivalents merged, \Df" set to 0'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_number_reflns         4237
_refine_ls_number_parameters     329
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1138
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.1754(4) 0.02797(16) 0.59846(14) 0.0250(6) Uani 1 1 d D . .
B2 B 0.7445(4) 0.30599(15) 0.20604(13) 0.0224(6) Uani 1 1 d . . .
O1A O 0.2791(10) -0.0349(3) 0.6201(3) 0.0320(13) Uani 0.50 1 d PD A 1
O2A O -0.0073(9) 0.0339(3) 0.6225(3) 0.0313(13) Uani 0.50 1 d PD A 1
O1B O 0.2769(10) -0.0117(3) 0.6431(2) 0.0276(12) Uani 0.50 1 d PD A 2
O2B O -0.0239(9) 0.0123(3) 0.5989(3) 0.0277(11) Uani 0.50 1 d PD A 2
O3 O 0.6653(3) 0.36996(9) 0.17993(8) 0.0265(4) Uani 1 1 d . . .
O4 O 0.9007(3) 0.27847(9) 0.17169(8) 0.0284(4) Uani 1 1 d . . .
C1A C 0.1761(10) -0.1538(3) 0.6636(3) 0.0410(15) Uiso 0.50 1 d PD A 1
H11A H 0.3123 -0.1682 0.6732 0.062 Uiso 0.50 1 d PR A 1
H12A H 0.1428 -0.1687 0.6186 0.062 Uiso 0.50 1 d PR A 1
H13A H 0.0873 -0.1791 0.6944 0.062 Uiso 0.50 1 d PR A 1
C1B C 0.1949(10) -0.1429(3) 0.6335(3) 0.0382(15) Uiso 0.50 1 d PD A 2
H11B H 0.1715 -0.1351 0.5865 0.057 Uiso 0.50 1 d PR A 2
H12B H 0.1073 -0.1825 0.6497 0.057 Uiso 0.50 1 d PR A 2
H13B H 0.3322 -0.1580 0.6403 0.057 Uiso 0.50 1 d PR A 2
C2 C 0.1544(4) -0.06996(13) 0.67061(12) 0.0276(6) Uani 1 1 d D . .
C3A C 0.2531(11) -0.0467(4) 0.7368(3) 0.0494(17) Uiso 0.50 1 d PD A 1
H31A H 0.2425 0.0079 0.7425 0.074 Uiso 0.50 1 d PR A 1
H32A H 0.3922 -0.0612 0.7362 0.074 Uiso 0.50 1 d PR A 1
H33A H 0.1865 -0.0721 0.7733 0.074 Uiso 0.50 1 d PR A 1
C3B C 0.1906(10) -0.0791(3) 0.7418(2) 0.0356(14) Uiso 0.50 1 d PD A 2
H31B H 0.1656 -0.0313 0.7642 0.053 Uiso 0.50 1 d PR A 2
H32B H 0.3276 -0.0942 0.7489 0.053 Uiso 0.50 1 d PR A 2
H33B H 0.1025 -0.1178 0.7594 0.053 Uiso 0.50 1 d PR A 2
C4 C -0.1967(5) -0.09132(19) 0.62462(18) 0.0550(9) Uani 1 1 d . . .
H41 H -0.3224 -0.0661 0.6162 0.083 Uiso 1 1 d R A .
H42 H -0.1405 -0.1087 0.5830 0.083 Uiso 1 1 d R . .
H43 H -0.2184 -0.1344 0.6537 0.083 Uiso 1 1 d R . .
C5 C -0.0561(4) -0.03707(13) 0.65675(13) 0.0287(6) Uani 1 1 d . A .
C6 C -0.1558(6) -0.0025(2) 0.71590(17) 0.0609(10) Uani 1 1 d . . .
H61 H -0.2795 0.0211 0.7022 0.091 Uiso 1 1 d R A .
H62 H -0.1835 -0.0417 0.7484 0.091 Uiso 1 1 d R . .
H63 H -0.0691 0.0355 0.7354 0.091 Uiso 1 1 d R . .
C7 C 0.6218(5) 0.34855(19) 0.06500(13) 0.0442(8) Uani 1 1 d . . .
H71 H 0.4922 0.3724 0.0690 0.066 Uiso 1 1 d R . .
H72 H 0.6749 0.3578 0.0210 0.066 Uiso 1 1 d R . .
H73 H 0.6088 0.2943 0.0721 0.066 Uiso 1 1 d R . .
C8 C 0.7600(4) 0.38127(14) 0.11603(11) 0.0259(5) Uani 1 1 d . . .
C9 C 0.7866(5) 0.46483(15) 0.10511(14) 0.0407(7) Uani 1 1 d . . .
H91 H 0.6574 0.4893 0.1037 0.061 Uiso 1 1 d R . .
H92 H 0.8645 0.4861 0.1411 0.061 Uiso 1 1 d R . .
H93 H 0.8552 0.4732 0.0634 0.061 Uiso 1 1 d R . .
C10 C 1.0280(5) 0.29890(16) 0.06203(13) 0.0406(8) Uani 1 1 d . . .
H101 H 1.1531 0.2734 0.0710 0.061 Uiso 1 1 d R . .
H102 H 0.9305 0.2620 0.0473 0.061 Uiso 1 1 d R . .
H103 H 1.0474 0.3368 0.0277 0.061 Uiso 1 1 d R . .
C11 C 0.9557(4) 0.33679(14) 0.12409(12) 0.0252(5) Uani 1 1 d . . .
C12 C 1.1186(4) 0.38194(18) 0.15583(14) 0.0395(7) Uani 1 1 d . . .
H121 H 1.2277 0.3484 0.1674 0.059 Uiso 1 1 d R . .
H122 H 1.1653 0.4203 0.1250 0.059 Uiso 1 1 d R . .
H123 H 1.0685 0.4064 0.1956 0.059 Uiso 1 1 d R . .
C13 C 0.6628(4) 0.26769(13) 0.26918(12) 0.0234(5) Uani 1 1 d . . .
C14 C 0.7679(4) 0.20973(12) 0.29981(11) 0.0229(5) Uani 1 1 d . . .
H14 H 0.8913 0.1948 0.2822 0.027 Uiso 1 1 d R . .
C15 C 0.6953(4) 0.17334(12) 0.35586(11) 0.0199(5) Uani 1 1 d . . .
C16 C 0.8017(4) 0.11462(13) 0.38816(12) 0.0239(5) Uani 1 1 d . . .
H16 H 0.9254 0.0992 0.3711 0.029 Uiso 1 1 d R . .
C17 C 0.7299(4) 0.08047(13) 0.44246(12) 0.0241(5) Uani 1 1 d . . .
H17 H 0.8058 0.0425 0.4633 0.029 Uiso 1 1 d R . .
C18 C 0.5413(4) 0.10035(13) 0.46920(11) 0.0217(5) Uani 1 1 d . A .
C19 C 0.4591(4) 0.06363(13) 0.52326(12) 0.0241(5) Uani 1 1 d . . .
H19 H 0.5334 0.0258 0.5449 0.029 Uiso 1 1 d R A .
C20 C 0.2706(4) 0.08077(14) 0.54632(11) 0.0239(5) Uani 1 1 d . A .
C21 C 0.1657(4) 0.13916(12) 0.51625(11) 0.0222(5) Uani 1 1 d . . .
H21 H 0.0387 0.1520 0.5323 0.027 Uiso 1 1 d R A .
C22 C 0.2440(4) 0.17899(13) 0.46286(11) 0.0198(5) Uani 1 1 d . A .
C23 C 0.1395(4) 0.23944(13) 0.43130(11) 0.0220(5) Uani 1 1 d . . .
H23 H 0.0148 0.2543 0.4479 0.026 Uiso 1 1 d R A .
C24 C 0.2145(4) 0.27524(13) 0.37846(12) 0.0234(5) Uani 1 1 d . A .
H24 H 0.1421 0.3151 0.3590 0.028 Uiso 1 1 d R . .
C25 C 0.4018(4) 0.25445(12) 0.35130(11) 0.0206(5) Uani 1 1 d . . .
C26 C 0.4815(4) 0.28924(13) 0.29574(11) 0.0226(5) Uani 1 1 d . A .
H26 H 0.4104 0.3289 0.2754 0.027 Uiso 1 1 d R . .
C27 C 0.5101(4) 0.19549(12) 0.38164(11) 0.0182(5) Uani 1 1 d . A .
C28 C 0.4319(4) 0.15853(12) 0.43804(11) 0.0193(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
B1 0.0308(16) 0.0247(14) 0.0195(13) -0.0002(11) 0.0040(13) -0.0015(12)
B2 0.0244(15) 0.0225(13) 0.0203(13) -0.0001(11) -0.0003(12) -0.0028(12)
O1A 0.031(2) 0.031(3) 0.034(3) 0.013(2) 0.007(3) -0.001(2)
O2A 0.041(3) 0.019(3) 0.033(3) 0.0056(19) 0.021(3) 0.006(2)
O1B 0.025(2) 0.033(3) 0.025(3) 0.0065(19) 0.001(2) -0.007(2)
O2B 0.032(2) 0.021(3) 0.031(3) 0.0065(18) 0.006(2) 0.001(2)
O3 0.0290(10) 0.0299(9) 0.0205(9) 0.0059(7) 0.0068(8) 0.0033(8)
O4 0.0338(10) 0.0264(9) 0.0251(9) 0.0059(7) 0.0079(8) 0.0027(8)
C2 0.0327(14) 0.0237(12) 0.0263(13) 0.0056(10) 0.0054(12) -0.0014(11)
C4 0.0426(19) 0.059(2) 0.063(2) -0.0131(17) -0.0182(18) 0.0139(17)
C5 0.0343(15) 0.0213(12) 0.0306(14) 0.0075(10) 0.0116(12) 0.0006(11)
C6 0.049(2) 0.066(2) 0.068(2) -0.0255(19) 0.019(2) 0.0066(19)
C7 0.0298(16) 0.077(2) 0.0261(14) 0.0028(15) -0.0053(13) -0.0092(16)
C8 0.0257(13) 0.0336(13) 0.0183(11) 0.0056(10) 0.0022(11) -0.0001(11)
C9 0.0508(19) 0.0343(15) 0.0371(16) 0.0142(13) 0.0095(15) 0.0079(14)
C10 0.0508(19) 0.0422(17) 0.0289(14) 0.0063(13) 0.0153(15) 0.0107(15)
C11 0.0266(13) 0.0281(13) 0.0210(12) 0.0068(10) 0.0057(11) -0.0007(11)
C12 0.0297(15) 0.0528(18) 0.0362(16) 0.0109(14) -0.0053(13) -0.0082(14)
C13 0.0261(13) 0.0208(12) 0.0233(12) 0.0005(10) 0.0010(11) -0.0033(10)
C14 0.0246(13) 0.0224(12) 0.0216(12) -0.0021(10) 0.0021(11) -0.0018(10)
C15 0.0238(13) 0.0179(11) 0.0182(11) -0.0011(9) 0.0009(10) -0.0027(10)
C16 0.0201(12) 0.0226(12) 0.0292(13) 0.0024(10) 0.0014(11) 0.0016(10)
C17 0.0236(13) 0.0217(12) 0.0269(13) 0.0039(10) -0.0040(11) -0.0009(10)
C18 0.0235(13) 0.0217(12) 0.0199(12) 0.0001(9) -0.0022(11) -0.0035(10)
C19 0.0255(13) 0.0221(12) 0.0249(13) 0.0033(10) -0.0015(11) -0.0016(10)
C20 0.0283(14) 0.0241(12) 0.0193(12) -0.0010(9) 0.0016(11) -0.0062(11)
C21 0.0227(13) 0.0240(12) 0.0200(12) -0.0018(9) 0.0028(10) -0.0022(10)
C22 0.0234(12) 0.0196(11) 0.0165(11) -0.0050(9) 0.0005(10) -0.0028(10)
C23 0.0217(13) 0.0231(12) 0.0212(11) -0.0035(10) 0.0046(11) 0.0027(10)
C24 0.0248(13) 0.0213(12) 0.0241(12) 0.0011(9) -0.0003(11) 0.0034(10)
C25 0.0244(13) 0.0198(11) 0.0175(11) -0.0007(9) -0.0009(10) -0.0006(10)
C26 0.0252(13) 0.0216(12) 0.0208(12) 0.0018(9) -0.0015(11) 0.0022(10)
C27 0.0227(12) 0.0170(11) 0.0147(11) -0.0028(8) -0.0012(10) -0.0025(9)
C28 0.0229(13) 0.0180(11) 0.0168(11) -0.0035(9) -0.0016(10) -0.0026(10)

_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
B1 O2A 1.339(6) . ?
B1 O1B 1.342(6) . ?
B1 O2B 1.382(7) . ?
B1 O1A 1.393(6) . ?
B1 C20 1.558(4) . ?
B2 O4 1.362(3) . ?
B2 O3 1.366(3) . ?
B2 C13 1.558(4) . ?
O1A C2 1.472(7) . ?
O2A C5 1.480(6) . ?
O1B C2 1.442(7) . ?
O2B C5 1.486(6) . ?
O3 C8 1.466(3) . ?
O4 C11 1.468(3) . ?
C1A C2 1.505(6) . ?
C1A H11A 0.9800 . ?
C1A H12A 0.9800 . ?
C1A H13A 0.9800 . ?
C1A H12B 0.7478 . ?
C1A H13B 1.1638 . ?
C1B C2 1.528(6) . ?
C1B H11A 1.2213 . ?
C1B H12A 0.6532 . ?
C1B H13A 1.5780 . ?
C1B H11B 0.9800 . ?
C1B H12B 0.9800 . ?
C1B H13B 0.9800 . ?
C2 C3B 1.480(5) . ?
C2 C5 1.571(4) . ?
C2 C3A 1.562(7) . ?
C3A H31A 0.9800 . ?
C3A H32A 0.9800 . ?
C3A H33A 0.9800 . ?
C3A H31B 0.8596 . ?
C3A H32B 1.0161 . ?
C3B H31A 1.5871 . ?
C3B H32A 1.4110 . ?
C3B H33A 0.6543 . ?
C3B H31B 0.9800 . ?
C3B H32B 0.9800 . ?
C3B H33B 0.9800 . ?
C4 C5 1.507(4) . ?
C4 H41 0.9801 . ?
C4 H42 0.9800 . ?
C4 H43 0.9801 . ?
C5 C6 1.512(4) . ?
C6 H61 0.9801 . ?
C6 H62 0.9802 . ?
C6 H63 0.9802 . ?
C7 C8 1.517(4) . ?
C7 H71 0.9800 . ?
C7 H72 0.9800 . ?
C7 H73 0.9800 . ?
C8 C9 1.514(4) . ?
C8 C11 1.556(4) . ?
C9 H91 0.9800 . ?
C9 H92 0.9801 . ?
C9 H93 0.9800 . ?
C10 C11 1.514(3) . ?
C10 H101 0.9800 . ?
C10 H102 0.9800 . ?
C10 H103 0.9800 . ?
C11 C12 1.513(4) . ?
C12 H121 0.9800 . ?
C12 H122 0.9800 . ?
C12 H123 0.9800 . ?
C13 C26 1.399(4) . ?
C13 C14 1.401(3) . ?
C14 C15 1.402(3) . ?
C14 H14 0.9500 . ?
C15 C27 1.419(3) . ?
C15 C16 1.431(3) . ?
C16 C17 1.353(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.437(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(3) . ?
C18 C28 1.423(3) . ?
C19 C20 1.398(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.401(3) . ?
C21 C22 1.403(3) . ?
C21 H21 0.9500 . ?
C22 C28 1.420(3) . ?
C22 C23 1.440(3) . ?
C23 C24 1.350(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.436(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.399(3) . ?
C25 C27 1.422(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.426(3) . ?

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
O2A B1 O1B 105.6(4) . . ?
O2A B1 O2B 26.5(2) . . ?
O1B B1 O2B 113.1(4) . . ?
O2A B1 O1A 114.6(4) . . ?
O1B B1 O1A 26.3(2) . . ?
O2B B1 O1A 109.3(4) . . ?
O2A B1 C20 125.9(3) . . ?
O1B B1 C20 124.5(4) . . ?
O2B B1 C20 122.2(3) . . ?
O1A B1 C20 119.3(4) . . ?
O4 B2 O3 114.0(2) . . ?
O4 B2 C13 123.0(2) . . ?
O3 B2 C13 123.1(2) . . ?
B1 O1A C2 105.7(4) . . ?
B1 O2A C5 108.2(4) . . ?
B1 O1B C2 110.2(5) . . ?
B1 O2B C5 105.6(4) . . ?
B2 O3 C8 106.70(19) . . ?
B2 O4 C11 106.46(19) . . ?
C2 C1A H11A 109.4 . . ?
C2 C1A H12A 109.5 . . ?
H11A C1A H12A 109.5 . . ?
C2 C1A H13A 109.5 . . ?
H11A C1A H13A 109.5 . . ?
H12A C1A H13A 109.5 . . ?
C2 C1A H12B 130.7 . . ?
H11A C1A H12B 119.1 . . ?
H12A C1A H12B 47.0 . . ?
H13A C1A H12B 62.9 . . ?
C2 C1A H13B 101.0 . . ?
H11A C1A H13B 37.2 . . ?
H12A C1A H13B 79.2 . . ?
H13A C1A H13B 142.4 . . ?
H12B C1A H13B 111.8 . . ?
C2 C1B H11A 95.9 . . ?
C2 C1B H12A 136.6 . . ?
H11A C1B H12A 113.8 . . ?
C2 C1B H13A 82.7 . . ?
H11A C1B H13A 68.4 . . ?
H12A C1B H13A 80.1 . . ?
C2 C1B H11B 109.5 . . ?
H11A C1B H11B 143.6 . . ?
H12A C1B H11B 63.8 . . ?
H13A C1B H11B 138.7 . . ?
C2 C1B H12B 109.5 . . ?
H11A C1B H12B 84.7 . . ?
H12A C1B H12B 47.4 . . ?
H13A C1B H12B 32.8 . . ?
H11B C1B H12B 109.5 . . ?
C2 C1B H13B 109.5 . . ?
H11A C1B H13B 35.3 . . ?
H12A C1B H13B 113.0 . . ?
H13A C1B H13B 102.5 . . ?
H11B C1B H13B 109.5 . . ?
H12B C1B H13B 109.5 . . ?
O1B C2 O1A 24.8(2) . . ?
O1B C2 C3B 111.3(4) . . ?
O1A C2 C3B 129.5(4) . . ?
O1B C2 C1A 128.2(4) . . ?
O1A C2 C1A 107.3(4) . . ?
C3B C2 C1A 88.2(4) . . ?
O1B C2 C1B 108.3(3) . . ?
O1A C2 C1B 84.8(3) . . ?
C3B C2 C1B 111.2(4) . . ?
C1A C2 C1B 25.0(3) . . ?
O1B C2 C5 100.8(3) . . ?
O1A C2 C5 103.9(3) . . ?
C3B C2 C5 111.6(3) . . ?
C1A C2 C5 116.2(3) . . ?
C1B C2 C5 113.1(3) . . ?
O1B C2 C3A 84.1(4) . . ?
O1A C2 C3A 104.2(4) . . ?
C3B C2 C3A 27.3(3) . . ?
C1A C2 C3A 107.6(4) . . ?
C1B C2 C3A 125.2(4) . . ?
C5 C2 C3A 116.5(3) . . ?
C2 C3A H31A 109.5 . . ?
C2 C3A H32A 109.4 . . ?
H31A C3A H32A 109.5 . . ?
C2 C3A H33A 109.5 . . ?
H31A C3A H33A 109.5 . . ?
H32A C3A H33A 109.5 . . ?
C2 C3A H31B 110.4 . . ?
H31A C3A H31B 63.7 . . ?
H32A C3A H31B 139.4 . . ?
H33A C3A H31B 48.4 . . ?
C2 C3A H32B 101.7 . . ?
H31A C3A H32B 146.3 . . ?
H32A C3A H32B 45.8 . . ?
H33A C3A H32B 70.3 . . ?
H31B C3A H32B 116.9 . . ?
C2 C3B H31A 86.5 . . ?
C2 C3B H32A 93.3 . . ?
H31A C3B H32A 64.2 . . ?
C2 C3B H33A 158.9 . . ?
H31A C3B H33A 79.3 . . ?
H32A C3B H33A 94.4 . . ?
C2 C3B H31B 109.4 . . ?
H31A C3B H31B 35.7 . . ?
H32A C3B H31B 90.6 . . ?
H33A C3B H31B 51.0 . . ?
C2 C3B H32B 109.5 . . ?
H31A C3B H32B 93.1 . . ?
H32A C3B H32B 31.9 . . ?
H33A C3B H32B 87.0 . . ?
H31B C3B H32B 109.5 . . ?
C2 C3B H33B 109.5 . . ?
H31A C3B H33B 144.8 . . ?
H32A C3B H33B 141.3 . . ?
H33A C3B H33B 75.5 . . ?
H31B C3B H33B 109.5 . . ?
H32B C3B H33B 109.5 . . ?
C5 C4 H41 109.5 . . ?
C5 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
C5 C4 H43 109.5 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O2A C5 O2B 24.3(2) . . ?
O2A C5 C4 118.9(3) . . ?
O2B C5 C4 97.4(3) . . ?
O2A C5 C6 97.4(3) . . ?
O2B C5 C6 117.2(3) . . ?
C4 C5 C6 108.8(3) . . ?
O2A C5 C2 101.5(3) . . ?
O2B C5 C2 103.2(3) . . ?
C4 C5 C2 114.6(2) . . ?
C6 C5 C2 114.6(3) . . ?
C5 C6 H61 109.4 . . ?
C5 C6 H62 109.6 . . ?
H61 C6 H62 109.4 . . ?
C5 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
C8 C7 H71 109.5 . . ?
C8 C7 H72 109.5 . . ?
H71 C7 H72 109.5 . . ?
C8 C7 H73 109.4 . . ?
H71 C7 H73 109.5 . . ?
H72 C7 H73 109.5 . . ?
O3 C8 C9 108.5(2) . . ?
O3 C8 C7 106.5(2) . . ?
C9 C8 C7 110.5(2) . . ?
O3 C8 C11 102.21(18) . . ?
C9 C8 C11 114.4(2) . . ?
C7 C8 C11 114.0(2) . . ?
C8 C9 H91 109.5 . . ?
C8 C9 H92 109.5 . . ?
H91 C9 H92 109.5 . . ?
C8 C9 H93 109.4 . . ?
H91 C9 H93 109.5 . . ?
H92 C9 H93 109.5 . . ?
C11 C10 H101 109.4 . . ?
C11 C10 H102 109.6 . . ?
H101 C10 H102 109.5 . . ?
C11 C10 H103 109.5 . . ?
H101 C10 H103 109.5 . . ?
H102 C10 H103 109.5 . . ?
O4 C11 C12 106.2(2) . . ?
O4 C11 C10 108.6(2) . . ?
C12 C11 C10 110.8(2) . . ?
O4 C11 C8 102.22(19) . . ?
C12 C11 C8 113.6(2) . . ?
C10 C11 C8 114.5(2) . . ?
C11 C12 H121 109.5 . . ?
C11 C12 H122 109.4 . . ?
H121 C12 H122 109.5 . . ?
C11 C12 H123 109.5 . . ?
H121 C12 H123 109.5 . . ?
H122 C12 H123 109.5 . . ?
C26 C13 C14 118.6(2) . . ?
C26 C13 B2 120.9(2) . . ?
C14 C13 B2 120.5(2) . . ?
C13 C14 C15 121.5(2) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.3 . . ?
C14 C15 C27 119.0(2) . . ?
C14 C15 C16 122.2(2) . . ?
C27 C15 C16 118.7(2) . . ?
C17 C16 C15 121.4(2) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 121.4(2) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C19 C18 C28 118.9(2) . . ?
C19 C18 C17 122.7(2) . . ?
C28 C18 C17 118.4(2) . . ?
C18 C19 C20 121.9(2) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.0 . . ?
C19 C20 C21 118.8(2) . . ?
C19 C20 B1 118.5(2) . . ?
C21 C20 B1 122.3(2) . . ?
C20 C21 C22 121.4(2) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C21 C22 C28 119.2(2) . . ?
C21 C22 C23 122.4(2) . . ?
C28 C22 C23 118.4(2) . . ?
C24 C23 C22 121.5(2) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 121.3(2) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.4 . . ?
C26 C25 C27 118.5(2) . . ?
C26 C25 C24 122.7(2) . . ?
C27 C25 C24 118.7(2) . . ?
C13 C26 C25 122.2(2) . . ?
C13 C26 H26 118.9 . . ?
C25 C26 H26 119.0 . . ?
C15 C27 C25 120.2(2) . . ?
C15 C27 C28 120.0(2) . . ?
C25 C27 C28 119.8(2) . . ?
C22 C28 C18 119.8(2) . . ?
C22 C28 C27 120.2(2) . . ?
C18 C28 C27 120.0(2) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2A B1 O1A C2 -7.0(5) . . . . ?
O1B B1 O1A C2 68.1(10) . . . . ?
O2B B1 O1A C2 -35.1(5) . . . . ?
C20 B1 O1A C2 177.3(3) . . . . ?
O1B B1 O2A C5 -36.2(5) . . . . ?
O2B B1 O2A C5 74.4(9) . . . . ?
O1A B1 O2A C5 -9.8(5) . . . . ?
C20 B1 O2A C5 165.5(3) . . . . ?
O2A B1 O1B C2 37.9(4) . . . . ?
O2B B1 O1B C2 10.9(5) . . . . ?
O1A B1 O1B C2 -76.3(11) . . . . ?
C20 B1 O1B C2 -163.5(3) . . . . ?
O2A B1 O2B C5 -71.1(9) . . . . ?
O1B B1 O2B C5 7.4(5) . . . . ?
O1A B1 O2B C5 35.5(4) . . . . ?
C20 B1 O2B C5 -178.0(2) . . . . ?
O4 B2 O3 C8 8.7(3) . . . . ?
C13 B2 O3 C8 -171.0(2) . . . . ?
O3 B2 O4 C11 10.9(3) . . . . ?
C13 B2 O4 C11 -169.4(2) . . . . ?
B1 O1B C2 O1A 77.0(10) . . . . ?
B1 O1B C2 C3B -141.3(4) . . . . ?
B1 O1B C2 C1A 113.5(5) . . . . ?
B1 O1B C2 C1B 96.1(5) . . . . ?
B1 O1B C2 C5 -22.8(4) . . . . ?
B1 O1B C2 C3A -138.7(4) . . . . ?
B1 O1A C2 O1B -66.2(9) . . . . ?
B1 O1A C2 C3B -114.6(5) . . . . ?
B1 O1A C2 C1A 143.0(4) . . . . ?
B1 O1A C2 C1B 132.0(4) . . . . ?
B1 O1A C2 C5 19.5(4) . . . . ?
B1 O1A C2 C3A -103.0(4) . . . . ?
B1 O2A C5 O2B -76.0(9) . . . . ?
B1 O2A C5 C4 -105.9(4) . . . . ?
B1 O2A C5 C6 137.8(4) . . . . ?
B1 O2A C5 C2 20.8(4) . . . . ?
B1 O2B C5 O2A 67.9(9) . . . . ?
B1 O2B C5 C4 -138.2(3) . . . . ?
B1 O2B C5 C6 106.2(4) . . . . ?
B1 O2B C5 C2 -20.7(4) . . . . ?
O1B C2 C5 O2A 1.0(3) . . . . ?
O1A C2 C5 O2A -24.2(3) . . . . ?
C3B C2 C5 O2A 119.3(4) . . . . ?
C1A C2 C5 O2A -141.7(4) . . . . ?
C1B C2 C5 O2A -114.4(4) . . . . ?
C3A C2 C5 O2A 89.7(4) . . . . ?
O1B C2 C5 O2B 25.8(3) . . . . ?
O1A C2 C5 O2B 0.6(3) . . . . ?
C3B C2 C5 O2B 144.1(4) . . . . ?
C1A C2 C5 O2B -116.9(4) . . . . ?
C1B C2 C5 O2B -89.6(4) . . . . ?
C3A C2 C5 O2B 114.6(4) . . . . ?
O1B C2 C5 C4 130.4(3) . . . . ?
O1A C2 C5 C4 105.2(3) . . . . ?
C3B C2 C5 C4 -111.3(4) . . . . ?
C1A C2 C5 C4 -12.3(4) . . . . ?
C1B C2 C5 C4 15.0(4) . . . . ?
C3A C2 C5 C4 -140.8(4) . . . . ?
O1B C2 C5 C6 -102.8(3) . . . . ?
O1A C2 C5 C6 -127.9(3) . . . . ?
C3B C2 C5 C6 15.5(4) . . . . ?
C1A C2 C5 C6 114.5(4) . . . . ?
C1B C2 C5 C6 141.8(4) . . . . ?
C3A C2 C5 C6 -14.0(4) . . . . ?
B2 O3 C8 C9 -144.2(2) . . . . ?
B2 O3 C8 C7 96.8(2) . . . . ?
B2 O3 C8 C11 -23.0(2) . . . . ?
B2 O4 C11 C12 95.0(2) . . . . ?
B2 O4 C11 C10 -145.7(2) . . . . ?
B2 O4 C11 C8 -24.3(2) . . . . ?
O3 C8 C11 O4 28.5(2) . . . . ?
C9 C8 C11 O4 145.5(2) . . . . ?
C7 C8 C11 O4 -86.0(2) . . . . ?
O3 C8 C11 C12 -85.5(2) . . . . ?
C9 C8 C11 C12 31.6(3) . . . . ?
C7 C8 C11 C12 160.0(2) . . . . ?
O3 C8 C11 C10 145.7(2) . . . . ?
C9 C8 C11 C10 -97.2(3) . . . . ?
C7 C8 C11 C10 31.2(3) . . . . ?
O4 B2 C13 C26 -167.9(2) . . . . ?
O3 B2 C13 C26 11.8(4) . . . . ?
O4 B2 C13 C14 10.8(4) . . . . ?
O3 B2 C13 C14 -169.5(2) . . . . ?
C26 C13 C14 C15 0.1(3) . . . . ?
B2 C13 C14 C15 -178.6(2) . . . . ?
C16 C17 C18 C19 176.8(2) . . . . ?
C16 C17 C18 C28 -1.4(3) . . . . ?
C28 C18 C19 C20 2.0(4) . . . . ?
C17 C18 C19 C20 -176.3(2) . . . . ?
C18 C19 C20 C21 -3.3(3) . . . . ?
C18 C19 C20 B1 169.2(2) . . . . ?
O2A B1 C20 C19 -175.8(4) . . . . ?
O1B B1 C20 C19 29.9(4) . . . . ?
O2B B1 C20 C19 -144.0(3) . . . . ?
O1A B1 C20 C19 -0.6(4) . . . . ?
O2A B1 C20 C21 -3.5(5) . . . . ?
O1B B1 C20 C21 -157.8(3) . . . . ?
O2B B1 C20 C21 28.2(4) . . . . ?
O1A B1 C20 C21 171.6(3) . . . . ?
C19 C20 C21 C22 1.6(3) . . . . ?
B1 C20 C21 C22 -170.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.050

#============================================END

data_(3B4)
_database_code_depnum_ccdc_archive 'CCDC 263080'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2,5,8,11-tetrakis(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-
perylene, dichloromethane solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H56 B4 O8,2(C H2 Cl2)'
_chemical_formula_sum            'C46 H60 B4 Cl4 O8'
_chemical_formula_weight         925.98

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.6669(5)
_cell_length_b                   12.519(1)
_cell_length_c                   14.791(1)
_cell_angle_alpha                103.68(1)
_cell_angle_beta                 99.11(1)
_cell_angle_gamma                96.50(1)
_cell_volume                     1169.7(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2634
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;The data collection nominally covered full sphere of reciprocal
space, by a combination of 3 sets of \w scans; each set at different
\f angles and each scan (45 sec exposure) covering 0.3\% in \w.
Crystal to detector distance 4.83 cm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SMART 6000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 5.6
_diffrn_reflns_number            11294
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5352
_reflns_number_gt                3459
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_structure_solution    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.
Methyl groups refined as rotating bodies with common refined U(iso)
and C---H distance for all three H. Other H atoms - riding (constr).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5352
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1246
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      0.945
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.10284(10) -0.42101(6) 0.15505(5) 0.04108(19) Uani 1 1 d . . .
Cl2 Cl -0.25724(10) -0.34478(5) 0.22355(5) 0.03813(18) Uani 1 1 d . . .
O1 O -0.7153(2) 0.09077(13) 0.41670(11) 0.0273(4) Uani 1 1 d . . .
O2 O -0.5045(2) 0.06378(12) 0.30803(10) 0.0231(4) Uani 1 1 d . . .
O3 O 0.2467(2) 0.24548(12) 0.16008(10) 0.0210(3) Uani 1 1 d . . .
O4 O 0.5387(2) 0.37140(12) 0.18519(10) 0.0227(4) Uani 1 1 d . . .
C1 C -0.4790(3) 0.31785(17) 0.51274(14) 0.0168(4) Uani 1 1 d . . .
H1 H -0.6005 0.2931 0.5328 0.020 Uiso 1 1 d R . .
C2 C -0.4189(3) 0.24974(17) 0.43728(14) 0.0170(4) Uani 1 1 d . . .
C3 C -0.2378(3) 0.28861(17) 0.40863(14) 0.0175(4) Uani 1 1 d . . .
H3 H -0.1953 0.2418 0.3569 0.021 Uiso 1 1 d R . .
C4 C -0.1202(3) 0.39113(16) 0.45223(13) 0.0141(4) Uani 1 1 d . . .
C5 C 0.0678(3) 0.43110(16) 0.42037(13) 0.0145(4) Uani 1 1 d . . .
C6 C 0.1339(3) 0.36902(17) 0.34345(14) 0.0162(4) Uani 1 1 d . . .
H6 H 0.0566 0.2982 0.3104 0.019 Uiso 1 1 d R . .
C7 C 0.3125(3) 0.40664(17) 0.31175(14) 0.0169(4) Uani 1 1 d . . .
C8 C 0.4248(3) 0.50882(17) 0.36093(13) 0.0168(4) Uani 1 1 d . . .
H8 H 0.5466 0.5343 0.3415 0.020 Uiso 1 1 d R . .
C9 C 0.3643(3) 0.57665(17) 0.43913(13) 0.0158(4) Uani 1 1 d . . .
C10 C 0.1824(3) 0.53855(16) 0.46965(13) 0.0142(4) Uani 1 1 d . . .
C11 C -0.8129(3) -0.01131(18) 0.34533(16) 0.0235(5) Uani 1 1 d . . .
C12 C -0.6329(3) -0.04419(18) 0.29395(15) 0.0228(5) Uani 1 1 d . . .
C13 C -0.8950(4) -0.0945(2) 0.39487(17) 0.0322(6) Uani 1 1 d . . .
H13A H -0.7849(16) -0.1036(10) 0.4431(10) 0.038(4) Uiso 1 1 d R . .
H13B H -0.947(2) -0.1660(10) 0.3487(6) 0.038(4) Uiso 1 1 d R . .
H13C H -1.006(2) -0.0677(7) 0.4248(10) 0.038(4) Uiso 1 1 d R . .
C14 C -0.9875(4) 0.0206(2) 0.28161(19) 0.0370(6) Uani 1 1 d . . .
H14A H -1.0862(19) 0.0532(13) 0.3209(6) 0.043(4) Uiso 1 1 d R . .
H14B H -1.0616(19) -0.0475(10) 0.2317(10) 0.043(4) Uiso 1 1 d R . .
H14C H -0.9295(9) 0.0769(12) 0.2505(10) 0.043(4) Uiso 1 1 d R . .
C15 C -0.6966(4) -0.0979(2) 0.18859(17) 0.0365(6) Uani 1 1 d . . .
H15A H -0.769(2) -0.0484(9) 0.1581(5) 0.042(4) Uiso 1 1 d R . .
H15B H -0.787(2) -0.1683(12) 0.1782(2) 0.042(4) Uiso 1 1 d R . .
H15C H -0.5747(17) -0.1116(12) 0.1616(5) 0.042(4) Uiso 1 1 d R . .
C16 C -0.5028(4) -0.1148(2) 0.34011(19) 0.0323(6) Uani 1 1 d . . .
H16A H -0.377(2) -0.1208(11) 0.3125(9) 0.048(5) Uiso 1 1 d R . .
H16B H -0.5824(14) -0.1900(12) 0.3289(10) 0.048(5) Uiso 1 1 d R . .
H16C H -0.463(2) -0.0800(9) 0.4092(10) 0.048(5) Uiso 1 1 d R . .
C21 C 0.3168(3) 0.22622(18) 0.06980(14) 0.0199(5) Uani 1 1 d . . .
C22 C 0.5437(3) 0.28588(17) 0.09874(14) 0.0195(5) Uani 1 1 d . . .
C23 C 0.1785(4) 0.2800(2) 0.00761(16) 0.0334(6) Uani 1 1 d . . .
H23A H 0.033(2) 0.2477(10) 0.0020(9) 0.040(4) Uiso 1 1 d R . .
H23B H 0.2144(17) 0.2661(11) -0.0561(10) 0.040(4) Uiso 1 1 d R . .
H23C H 0.1979(18) 0.3611(12) 0.0364(7) 0.040(4) Uiso 1 1 d R . .
C24 C 0.2908(4) 0.1030(2) 0.02525(17) 0.0318(6) Uani 1 1 d . . .
H24A H 0.365(2) 0.0676(6) 0.0690(7) 0.043(5) Uiso 1 1 d R . .
H24B H 0.345(2) 0.0902(3) -0.0328(10) 0.043(5) Uiso 1 1 d R . .
H24C H 0.146(2) 0.0718(6) 0.0109(10) 0.043(5) Uiso 1 1 d R . .
C25 C 0.6944(4) 0.2119(2) 0.12701(17) 0.0308(6) Uani 1 1 d . . .
H25A H 0.827(2) 0.2567(7) 0.1561(10) 0.038(4) Uiso 1 1 d R . .
H25B H 0.7076(18) 0.1564(11) 0.0712(8) 0.038(4) Uiso 1 1 d R . .
H25C H 0.6445(14) 0.1753(11) 0.1717(10) 0.038(4) Uiso 1 1 d R . .
C26 C 0.6165(4) 0.3444(2) 0.02829(16) 0.0299(6) Uani 1 1 d . . .
H26A H 0.5328(19) 0.4013(12) 0.0204(8) 0.035(4) Uiso 1 1 d R . .
H26B H 0.604(2) 0.2906(8) -0.0323(9) 0.035(4) Uiso 1 1 d R . .
H26C H 0.759(2) 0.3786(12) 0.0516(6) 0.035(4) Uiso 1 1 d R . .
B1 B -0.5484(4) 0.1336(2) 0.38629(17) 0.0197(5) Uani 1 1 d . . .
B2 B 0.3690(4) 0.3390(2) 0.21901(16) 0.0184(5) Uani 1 1 d . . .
C1S C -0.0602(4) -0.4260(2) 0.23763(17) 0.0319(6) Uani 1 1 d . . .
H1S H -0.1227 -0.5042 0.2292 0.041 Uiso 1 1 d R . .
H2S H 0.0221 -0.3984 0.3027 0.041 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0395(4) 0.0380(4) 0.0532(4) 0.0183(3) 0.0169(3) 0.0118(3)
Cl2 0.0443(4) 0.0352(4) 0.0415(4) 0.0153(3) 0.0167(3) 0.0107(3)
O1 0.0265(9) 0.0203(8) 0.0306(9) -0.0042(7) 0.0136(7) -0.0028(7)
O2 0.0266(8) 0.0164(8) 0.0238(8) -0.0010(6) 0.0108(7) -0.0024(6)
O3 0.0209(8) 0.0223(8) 0.0177(7) -0.0008(6) 0.0093(6) -0.0001(6)
O4 0.0241(8) 0.0218(8) 0.0166(7) -0.0069(6) 0.0108(6) -0.0031(6)
C1 0.0160(10) 0.0163(11) 0.0189(10) 0.0052(8) 0.0060(8) 0.0012(8)
C2 0.0185(10) 0.0133(10) 0.0183(10) 0.0024(8) 0.0039(8) 0.0018(8)
C3 0.0207(11) 0.0169(11) 0.0138(10) -0.0003(8) 0.0054(8) 0.0057(9)
C4 0.0150(10) 0.0148(10) 0.0133(9) 0.0036(8) 0.0037(8) 0.0043(8)
C5 0.0145(10) 0.0144(10) 0.0144(10) 0.0024(8) 0.0031(8) 0.0043(8)
C6 0.0158(10) 0.0147(10) 0.0161(10) 0.0004(8) 0.0036(8) 0.0020(8)
C7 0.0194(11) 0.0179(11) 0.0142(10) 0.0024(8) 0.0061(8) 0.0056(8)
C8 0.0160(10) 0.0191(11) 0.0159(10) 0.0025(8) 0.0078(8) 0.0025(8)
C9 0.0166(10) 0.0159(10) 0.0145(10) 0.0034(8) 0.0032(8) 0.0026(8)
C10 0.0157(10) 0.0135(10) 0.0132(9) 0.0020(8) 0.0029(8) 0.0038(8)
C11 0.0210(11) 0.0146(11) 0.0297(12) -0.0043(9) 0.0075(9) -0.0017(9)
C12 0.0245(12) 0.0146(11) 0.0269(11) 0.0017(9) 0.0073(9) -0.0018(9)
C13 0.0358(14) 0.0254(13) 0.0342(13) 0.0044(10) 0.0144(11) -0.0036(11)
C14 0.0275(14) 0.0263(14) 0.0530(17) 0.0075(12) 0.0008(12) 0.0028(11)
C15 0.0522(17) 0.0245(13) 0.0264(13) -0.0022(10) 0.0125(12) -0.0077(12)
C16 0.0308(13) 0.0198(13) 0.0454(15) 0.0064(11) 0.0085(11) 0.0036(10)
C21 0.0227(11) 0.0194(11) 0.0180(10) 0.0003(8) 0.0111(9) 0.0036(9)
C22 0.0224(11) 0.0187(11) 0.0153(10) -0.0031(8) 0.0091(9) 0.0020(9)
C23 0.0297(13) 0.0485(17) 0.0226(12) 0.0075(11) 0.0055(10) 0.0113(12)
C24 0.0340(14) 0.0249(13) 0.0311(13) -0.0050(10) 0.0153(11) -0.0047(11)
C25 0.0231(12) 0.0394(15) 0.0277(12) 0.0006(11) 0.0068(10) 0.0104(11)
C26 0.0349(14) 0.0275(13) 0.0265(12) 0.0015(10) 0.0163(11) -0.0008(11)
B1 0.0211(13) 0.0179(12) 0.0196(12) 0.0030(9) 0.0046(10) 0.0033(10)
B2 0.0202(12) 0.0181(13) 0.0172(11) 0.0029(9) 0.0057(10) 0.0053(10)
C1S 0.0352(14) 0.0289(14) 0.0327(13) 0.0123(11) 0.0035(11) 0.0048(11)

_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
Cl1 C1S 1.766(2) . ?
Cl2 C1S 1.766(3) . ?
O1 B1 1.366(3) . ?
O1 C11 1.458(3) . ?
O2 B1 1.370(3) . ?
O2 C12 1.467(2) . ?
O3 B2 1.368(3) . ?
O3 C21 1.460(2) . ?
O4 B2 1.366(3) . ?
O4 C22 1.469(2) . ?
C1 C2 1.379(3) . ?
C1 C9 1.411(3) 2_566 ?
C2 C3 1.415(3) . ?
C2 B1 1.555(3) . ?
C3 C4 1.378(3) . ?
C4 C10 1.427(3) 2_566 ?
C4 C5 1.483(3) . ?
C5 C6 1.382(3) . ?
C5 C10 1.432(3) . ?
C6 C7 1.419(3) . ?
C7 C8 1.377(3) . ?
C7 B2 1.558(3) . ?
C8 C9 1.408(3) . ?
C9 C1 1.411(3) 2_566 ?
C9 C10 1.430(3) . ?
C10 C4 1.427(3) 2_566 ?
C11 C13 1.510(3) . ?
C11 C14 1.529(3) . ?
C11 C12 1.562(3) . ?
C12 C16 1.507(3) . ?
C12 C15 1.514(3) . ?
C21 C24 1.506(3) . ?
C21 C23 1.521(3) . ?
C21 C22 1.555(3) . ?
C22 C26 1.516(3) . ?
C22 C25 1.518(3) . ?

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
B1 O1 C11 107.42(16) . . ?
B1 O2 C12 106.55(16) . . ?
B2 O3 C21 106.80(15) . . ?
B2 O4 C22 107.61(16) . . ?
C2 C1 C9 121.54(18) . 2_566 ?
C1 C2 C3 118.12(18) . . ?
C1 C2 B1 120.17(18) . . ?
C3 C2 B1 121.71(18) . . ?
C4 C3 C2 123.06(18) . . ?
C3 C4 C10 118.76(17) . 2_566 ?
C3 C4 C5 122.29(17) . . ?
C10 C4 C5 118.95(17) 2_566 . ?
C6 C5 C10 118.84(17) . . ?
C6 C5 C4 122.18(18) . . ?
C10 C5 C4 118.97(17) . . ?
C5 C6 C7 122.76(19) . . ?
C8 C7 C6 118.07(18) . . ?
C8 C7 B2 120.91(18) . . ?
C6 C7 B2 120.81(18) . . ?
C7 C8 C9 121.94(18) . . ?
C8 C9 C1 121.04(18) . 2_566 ?
C8 C9 C10 119.50(18) . . ?
C1 C9 C10 119.46(18) 2_566 . ?
C4 C10 C9 119.05(18) 2_566 . ?
C4 C10 C5 122.07(17) 2_566 . ?
C9 C10 C5 118.87(17) . . ?
O1 C11 C13 108.62(18) . . ?
O1 C11 C14 106.29(18) . . ?
C13 C11 C14 111.06(19) . . ?
O1 C11 C12 102.20(16) . . ?
C13 C11 C12 114.81(19) . . ?
C14 C11 C12 113.04(19) . . ?
O2 C12 C16 107.19(18) . . ?
O2 C12 C15 108.66(17) . . ?
C16 C12 C15 109.8(2) . . ?
O2 C12 C11 102.48(16) . . ?
C16 C12 C11 113.23(19) . . ?
C15 C12 C11 114.9(2) . . ?
O3 C21 C24 109.55(17) . . ?
O3 C21 C23 105.89(17) . . ?
C24 C21 C23 109.7(2) . . ?
O3 C21 C22 102.88(15) . . ?
C24 C21 C22 114.60(18) . . ?
C23 C21 C22 113.56(18) . . ?
O4 C22 C26 107.85(17) . . ?
O4 C22 C25 106.77(17) . . ?
C26 C22 C25 111.04(18) . . ?
O4 C22 C21 102.06(15) . . ?
C26 C22 C21 114.97(18) . . ?
C25 C22 C21 113.29(18) . . ?
O1 B1 O2 113.57(19) . . ?
O1 B1 C2 122.87(19) . . ?
O2 B1 C2 123.55(19) . . ?
O4 B2 O3 113.25(18) . . ?
O4 B2 C7 123.26(19) . . ?
O3 B2 C7 123.35(19) . . ?
Cl2 C1S Cl1 111.59(13) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 B1 O1 -4.6(3) . . . . ?
C2 B1 O1 C11 172.6(2) . . . . ?
B1 O1 C11 C12 22.2(2) . . . . ?
O1 C11 C12 O2 -27.4(2) . . . . ?
C11 C12 O2 B1 23.2(2) . . . . ?
C12 O2 B1 O1 -10.4(3) . . . . ?
C6 C7 B2 O3 4.5(3) . . . . ?
C7 B2 O3 C21 163.3(2) . . . . ?
B2 O3 C21 C22 24.1(2) . . . . ?
O3 C21 C22 O4 -26.46(19) . . . . ?
C21 C22 O4 B2 20.0(2) . . . . ?
C22 O4 B2 O3 -5.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.061

#=============================================END