# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               J.Mater.Chem.
_journal_coden_cambridge         1145
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       hongyuzhang@jlu.edu.cn
_publ_contact_author_name        'Hongyu Zhang'
loop_
_publ_author_name
'Hongyu Zhang'
'Di Li'
'Kai Wang'
'Shuo Huang'
'Songnan Qu'
'Xingyuan Liu'
'Yue Wang'

data_1
_database_code_depnum_ccdc_archive 'CCDC 823398'
#TrackingRef '1 and 2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H30 B2 N2 O4'
_chemical_formula_weight         672.32

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'
N N 0.0061 0.0033 '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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.220(5)
_cell_length_b                   8.960(7)
_cell_length_c                   13.113(7)
_cell_angle_alpha                74.48(2)
_cell_angle_beta                 75.97(2)
_cell_angle_gamma                65.43(3)
_cell_volume                     836.7(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             350
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9692
_exptl_absorpt_correction_T_max  0.9961
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8244
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_sigmaI/netI    0.1309
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3776
_reflns_number_gt                1768
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_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^)+(0.0591P)^2^+0.0000P] 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    riding
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3776
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1801
_refine_ls_R_factor_gt           0.0786
_refine_ls_wR_factor_ref         0.1631
_refine_ls_wR_factor_gt          0.1304
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
B1 B 0.2542(5) 0.2609(5) 0.2127(3) 0.0348(8) Uani 1 1 d . . .
C1 C 1.1497(4) 0.3338(4) -0.1357(2) 0.0345(7) Uani 1 1 d . . .
C2 C 1.3265(4) 0.2248(4) -0.1380(2) 0.0429(8) Uani 1 1 d . . .
H2 H 1.3598 0.1155 -0.1000 0.051 Uiso 1 1 calc R . .
C3 C 1.4513(5) 0.2899(5) -0.2013(3) 0.0486(9) Uani 1 1 d . . .
H3 H 1.5738 0.2235 -0.2047 0.058 Uiso 1 1 calc R . .
C4 C 1.3987(4) 0.4514(5) -0.2595(3) 0.0487(9) Uani 1 1 d . . .
H4 H 1.4876 0.4895 -0.3015 0.058 Uiso 1 1 calc R . .
C5 C 1.2190(4) 0.5591(4) -0.2580(2) 0.0450(8) Uani 1 1 d . . .
H5 H 1.1849 0.6673 -0.2977 0.054 Uiso 1 1 calc R . .
C6 C 1.0939(4) 0.4949(4) -0.1935(2) 0.0345(7) Uani 1 1 d . . .
C7 C 0.8556(4) 0.4466(4) -0.1007(2) 0.0336(7) Uani 1 1 d . . .
C8 C 0.6740(4) 0.4685(4) -0.0506(2) 0.0341(7) Uani 1 1 d . . .
C9 C 0.6252(4) 0.3357(4) 0.0104(2) 0.0384(8) Uani 1 1 d . . .
H9 H 0.7108 0.2270 0.0161 0.046 Uiso 1 1 calc R . .
C10 C 0.4509(4) 0.3651(4) 0.0620(2) 0.0354(8) Uani 1 1 d . . .
C11 C 0.1735(4) 0.1176(4) 0.2391(2) 0.0337(7) Uani 1 1 d . . .
C12 C 0.1060(5) 0.0892(4) 0.1616(3) 0.0495(9) Uani 1 1 d . . .
H12 H 0.1163 0.1493 0.0921 0.059 Uiso 1 1 calc R . .
C13 C 0.0241(5) -0.0251(5) 0.1842(3) 0.0590(10) Uani 1 1 d . . .
H13 H -0.0215 -0.0394 0.1307 0.071 Uiso 1 1 calc R . .
C14 C 0.0100(5) -0.1176(5) 0.2852(3) 0.0648(11) Uani 1 1 d . . .
H14 H -0.0455 -0.1945 0.3006 0.078 Uiso 1 1 calc R . .
C15 C 0.0778(5) -0.0962(5) 0.3629(3) 0.0617(11) Uani 1 1 d . . .
H15 H 0.0701 -0.1599 0.4314 0.074 Uiso 1 1 calc R . .
C16 C 0.1584(5) 0.0205(4) 0.3403(2) 0.0464(9) Uani 1 1 d . . .
H16 H 0.2034 0.0338 0.3945 0.056 Uiso 1 1 calc R . .
C17 C 0.3227(4) 0.2792(4) 0.3107(2) 0.0352(7) Uani 1 1 d . . .
C18 C 0.2162(5) 0.3874(5) 0.3814(3) 0.0516(10) Uani 1 1 d . . .
H18 H 0.1006 0.4610 0.3683 0.062 Uiso 1 1 calc R . .
C19 C 0.2783(5) 0.3883(6) 0.4713(3) 0.0623(11) Uani 1 1 d . . .
H19 H 0.2047 0.4621 0.5169 0.075 Uiso 1 1 calc R . .
C20 C 0.4483(6) 0.2797(6) 0.4921(3) 0.0618(11) Uani 1 1 d . . .
H20 H 0.4898 0.2787 0.5523 0.074 Uiso 1 1 calc R . .
C21 C 0.5563(5) 0.1729(5) 0.4236(3) 0.0570(10) Uani 1 1 d . . .
H21 H 0.6719 0.0999 0.4370 0.068 Uiso 1 1 calc R . .
C22 C 0.4941(5) 0.1734(4) 0.3351(2) 0.0461(9) Uani 1 1 d . . .
H22 H 0.5698 0.0999 0.2898 0.055 Uiso 1 1 calc R . .
N1 N 0.9031(3) 0.5635(3) -0.16918(18) 0.0342(6) Uani 1 1 d . . .
O1 O 0.9968(3) 0.3037(3) -0.07691(15) 0.0387(5) Uani 1 1 d . . .
O2 O 0.4006(3) 0.2363(3) 0.11633(15) 0.0372(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 0.0239(19) 0.035(2) 0.0352(18) -0.0025(15) -0.0025(15) -0.0042(17)
C1 0.0298(18) 0.041(2) 0.0343(16) -0.0036(14) -0.0010(13) -0.0185(17)
C2 0.0293(19) 0.037(2) 0.055(2) -0.0068(16) -0.0074(15) -0.0057(17)
C3 0.034(2) 0.053(3) 0.057(2) -0.0146(18) -0.0059(16) -0.0115(19)
C4 0.033(2) 0.050(3) 0.061(2) -0.0118(19) 0.0019(16) -0.018(2)
C5 0.036(2) 0.041(2) 0.0531(19) -0.0035(16) -0.0007(15) -0.0158(18)
C6 0.0284(18) 0.040(2) 0.0347(15) -0.0060(14) -0.0042(13) -0.0134(16)
C7 0.0342(18) 0.0288(19) 0.0343(15) -0.0005(13) -0.0079(13) -0.0102(16)
C8 0.0292(18) 0.035(2) 0.0357(15) -0.0043(14) -0.0006(13) -0.0133(16)
C9 0.0308(19) 0.035(2) 0.0415(16) -0.0044(14) -0.0035(14) -0.0071(16)
C10 0.039(2) 0.037(2) 0.0308(15) -0.0031(14) -0.0038(14) -0.0178(18)
C11 0.0263(17) 0.0323(19) 0.0357(15) -0.0011(13) -0.0029(13) -0.0084(15)
C12 0.059(2) 0.045(2) 0.0481(19) -0.0035(17) -0.0153(17) -0.021(2)
C13 0.060(3) 0.046(3) 0.079(3) -0.015(2) -0.020(2) -0.021(2)
C14 0.061(3) 0.051(3) 0.092(3) -0.013(2) -0.005(2) -0.033(2)
C15 0.073(3) 0.051(3) 0.060(2) 0.0037(19) -0.001(2) -0.035(2)
C16 0.053(2) 0.047(2) 0.0400(17) -0.0008(16) -0.0058(15) -0.024(2)
C17 0.0346(18) 0.0328(19) 0.0377(16) -0.0006(14) -0.0049(14) -0.0159(16)
C18 0.038(2) 0.060(3) 0.053(2) -0.0140(19) -0.0021(17) -0.015(2)
C19 0.059(3) 0.083(3) 0.049(2) -0.027(2) 0.0040(19) -0.028(3)
C20 0.068(3) 0.080(3) 0.043(2) -0.002(2) -0.0173(19) -0.035(3)
C21 0.054(2) 0.060(3) 0.055(2) 0.0019(19) -0.0237(19) -0.019(2)
C22 0.047(2) 0.040(2) 0.0464(19) -0.0032(16) -0.0143(16) -0.0117(19)
N1 0.0257(14) 0.0318(17) 0.0373(13) 0.0001(11) -0.0022(11) -0.0088(13)
O1 0.0316(13) 0.0330(14) 0.0425(12) -0.0003(10) -0.0044(9) -0.0084(11)
O2 0.0334(12) 0.0310(14) 0.0407(11) -0.0005(9) -0.0006(9) -0.0122(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
B1 O2 1.511(4) . ?
B1 C17 1.593(4) . ?
B1 C11 1.601(5) . ?
B1 N1 1.630(4) 2_665 ?
C1 C2 1.371(4) . ?
C1 C6 1.379(4) . ?
C1 O1 1.396(3) . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.383(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 N1 1.414(4) . ?
C7 N1 1.312(4) . ?
C7 O1 1.346(4) . ?
C7 C8 1.431(4) . ?
C8 C9 1.396(4) . ?
C8 C10 1.408(4) 2_665 ?
C9 C10 1.375(4) . ?
C9 H9 0.9300 . ?
C10 O2 1.350(3) . ?
C10 C8 1.408(4) 2_665 ?
C11 C16 1.388(4) . ?
C11 C12 1.392(4) . ?
C12 C13 1.379(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.368(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.362(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.391(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.390(4) . ?
C17 C18 1.396(4) . ?
C18 C19 1.395(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.373(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.370(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.374(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N1 B1 1.630(4) 2_665 ?

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
O2 B1 C17 111.4(2) . . ?
O2 B1 C11 109.7(3) . . ?
C17 B1 C11 114.8(3) . . ?
O2 B1 N1 102.8(2) . 2_665 ?
C17 B1 N1 110.0(3) . 2_665 ?
C11 B1 N1 107.4(2) . 2_665 ?
C2 C1 C6 124.5(3) . . ?
C2 C1 O1 127.2(3) . . ?
C6 C1 O1 108.2(3) . . ?
C1 C2 C3 114.8(3) . . ?
C1 C2 H2 122.6 . . ?
C3 C2 H2 122.6 . . ?
C2 C3 C4 121.7(3) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 122.8(3) . . ?
C3 C4 H4 118.6 . . ?
C5 C4 H4 118.6 . . ?
C6 C5 C4 115.7(3) . . ?
C6 C5 H5 122.2 . . ?
C4 C5 H5 122.2 . . ?
C1 C6 C5 120.5(3) . . ?
C1 C6 N1 106.6(2) . . ?
C5 C6 N1 132.9(3) . . ?
N1 C7 O1 113.3(3) . . ?
N1 C7 C8 124.4(3) . . ?
O1 C7 C8 122.2(3) . . ?
C9 C8 C10 122.0(3) . 2_665 ?
C9 C8 C7 122.6(3) . . ?
C10 C8 C7 115.3(3) 2_665 . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
O2 C10 C9 120.4(3) . . ?
O2 C10 C8 121.7(3) . 2_665 ?
C9 C10 C8 117.8(3) . 2_665 ?
C16 C11 C12 116.0(3) . . ?
C16 C11 B1 122.8(3) . . ?
C12 C11 B1 121.1(3) . . ?
C13 C12 C11 122.3(3) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 119.5(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 121.8(3) . . ?
C11 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C22 C17 C18 115.8(3) . . ?
C22 C17 B1 119.7(3) . . ?
C18 C17 B1 124.3(3) . . ?
C19 C18 C17 121.9(3) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C20 C19 C18 119.8(4) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C21 C20 C19 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 120.2(4) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C17 122.8(3) . . ?
C21 C22 H22 118.6 . . ?
C17 C22 H22 118.6 . . ?
C7 N1 C6 106.4(3) . . ?
C7 N1 B1 119.0(2) . 2_665 ?
C6 N1 B1 134.4(2) . 2_665 ?
C7 O1 C1 105.4(2) . . ?
C10 O2 B1 119.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.054

###End

data_2
_database_code_depnum_ccdc_archive 'CCDC 823399'
#TrackingRef '1 and 2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H30 B2 N2 O2 S2'
_chemical_formula_weight         704.44

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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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                   9.813(7)
_cell_length_b                   10.072(6)
_cell_length_c                   10.185(6)
_cell_angle_alpha                85.79(2)
_cell_angle_beta                 77.07(2)
_cell_angle_gamma                63.68(2)
_cell_volume                     879.0(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             366
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9606
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8711
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3993
_reflns_number_gt                2521
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_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^)+(0.0501P)^2^+0.1332P] 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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3993
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1230
_refine_ls_wR_factor_gt          0.1064
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
B1 B 0.1101(3) 0.7415(3) 0.1786(2) 0.0358(6) Uani 1 1 d . . .
C1 C 0.2147(3) 0.4252(2) 0.4410(2) 0.0381(5) Uani 1 1 d . . .
C2 C 0.2691(3) 0.3741(3) 0.5590(2) 0.0486(6) Uani 1 1 d . . .
H2 H 0.2772 0.2835 0.5937 0.058 Uiso 1 1 calc R . .
C3 C 0.3102(3) 0.4619(3) 0.6218(2) 0.0546(7) Uani 1 1 d . . .
H3 H 0.3490 0.4297 0.6996 0.066 Uiso 1 1 calc R . .
C4 C 0.2949(3) 0.5985(3) 0.5710(3) 0.0585(7) Uani 1 1 d . . .
H4 H 0.3210 0.6570 0.6173 0.070 Uiso 1 1 calc R . .
C5 C 0.2424(3) 0.6498(3) 0.4545(2) 0.0518(6) Uani 1 1 d . . .
H5 H 0.2341 0.7408 0.4208 0.062 Uiso 1 1 calc R . .
C6 C 0.2020(3) 0.5605(2) 0.3886(2) 0.0381(5) Uani 1 1 d . . .
C7 C 0.1113(2) 0.4869(2) 0.2361(2) 0.0346(5) Uani 1 1 d . . .
C8 C 0.0499(2) 0.4941(2) 0.1178(2) 0.0339(5) Uani 1 1 d . . .
C9 C 0.0543(2) 0.6021(2) 0.0240(2) 0.0343(5) Uani 1 1 d . . .
C10 C 0.0050(2) 0.6062(2) -0.0941(2) 0.0361(5) Uani 1 1 d . . .
H10 H 0.0085 0.6762 -0.1579 0.043 Uiso 1 1 calc R . .
C11 C -0.0599(3) 0.8681(2) 0.2422(2) 0.0383(5) Uani 1 1 d . . .
C12 C -0.1209(3) 0.9001(3) 0.3794(2) 0.0527(7) Uani 1 1 d . . .
H12 H -0.0595 0.8470 0.4402 0.063 Uiso 1 1 calc R . .
C13 C -0.2700(4) 1.0087(3) 0.4285(3) 0.0675(8) Uani 1 1 d . . .
H13 H -0.3080 1.0259 0.5209 0.081 Uiso 1 1 calc R . .
C14 C -0.3615(3) 1.0908(3) 0.3409(4) 0.0707(9) Uani 1 1 d . . .
H14 H -0.4620 1.1631 0.3734 0.085 Uiso 1 1 calc R . .
C15 C -0.3041(3) 1.0657(3) 0.2060(3) 0.0759(10) Uani 1 1 d . . .
H15 H -0.3645 1.1227 0.1458 0.091 Uiso 1 1 calc R . .
C16 C -0.1559(3) 0.9554(3) 0.1581(3) 0.0610(8) Uani 1 1 d . . .
H16 H -0.1194 0.9394 0.0655 0.073 Uiso 1 1 calc R . .
C17 C 0.2544(3) 0.7809(2) 0.1611(2) 0.0355(5) Uani 1 1 d . . .
C18 C 0.4033(3) 0.6735(3) 0.1077(2) 0.0483(6) Uani 1 1 d . . .
H18 H 0.4167 0.5791 0.0882 0.058 Uiso 1 1 calc R . .
C19 C 0.5315(3) 0.7017(3) 0.0827(3) 0.0556(7) Uani 1 1 d . . .
H19 H 0.6293 0.6274 0.0457 0.067 Uiso 1 1 calc R . .
C20 C 0.5155(3) 0.8389(3) 0.1120(3) 0.0607(7) Uani 1 1 d . . .
H20 H 0.6021 0.8582 0.0960 0.073 Uiso 1 1 calc R . .
C21 C 0.3712(3) 0.9472(3) 0.1651(3) 0.0614(8) Uani 1 1 d . . .
H21 H 0.3594 1.0408 0.1850 0.074 Uiso 1 1 calc R . .
C22 C 0.2421(3) 0.9188(3) 0.1894(2) 0.0479(6) Uani 1 1 d . . .
H22 H 0.1448 0.9942 0.2256 0.057 Uiso 1 1 calc R . .
N1 N 0.1429(2) 0.59296(19) 0.27005(17) 0.0353(4) Uani 1 1 d . . .
O1 O 0.11679(18) 0.69188(16) 0.04159(14) 0.0398(4) Uani 1 1 d . . .
S1 S 0.15289(7) 0.33958(6) 0.34172(6) 0.04273(19) 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 0.0435(15) 0.0394(13) 0.0305(13) 0.0016(11) -0.0090(11) -0.0230(12)
C1 0.0360(13) 0.0414(12) 0.0315(11) -0.0027(10) -0.0070(9) -0.0118(10)
C2 0.0495(15) 0.0526(14) 0.0388(13) 0.0052(11) -0.0137(11) -0.0166(12)
C3 0.0559(17) 0.0741(18) 0.0400(14) 0.0087(13) -0.0209(12) -0.0301(14)
C4 0.0713(19) 0.0794(19) 0.0467(15) 0.0030(14) -0.0244(14) -0.0471(16)
C5 0.0645(18) 0.0625(15) 0.0434(14) 0.0066(12) -0.0190(13) -0.0386(14)
C6 0.0359(13) 0.0484(13) 0.0316(11) -0.0004(10) -0.0081(10) -0.0191(10)
C7 0.0347(12) 0.0379(11) 0.0293(11) -0.0030(9) -0.0041(9) -0.0148(10)
C8 0.0340(12) 0.0364(11) 0.0285(11) -0.0032(9) -0.0056(9) -0.0129(9)
C9 0.0329(12) 0.0373(11) 0.0315(11) -0.0041(10) -0.0041(9) -0.0148(10)
C10 0.0427(13) 0.0371(11) 0.0299(11) 0.0007(9) -0.0054(10) -0.0198(10)
C11 0.0427(14) 0.0404(12) 0.0402(12) -0.0010(10) -0.0084(10) -0.0255(10)
C12 0.0615(18) 0.0445(13) 0.0447(15) 0.0028(12) -0.0067(13) -0.0190(13)
C13 0.071(2) 0.0558(16) 0.0591(18) -0.0113(15) 0.0152(16) -0.0245(15)
C14 0.0413(16) 0.0615(18) 0.096(2) -0.0248(18) -0.0031(16) -0.0121(14)
C15 0.0555(19) 0.0723(19) 0.086(2) -0.0142(18) -0.0333(17) -0.0051(15)
C16 0.0508(17) 0.0696(17) 0.0520(16) -0.0068(14) -0.0194(13) -0.0117(14)
C17 0.0405(13) 0.0405(11) 0.0276(11) -0.0003(9) -0.0063(9) -0.0198(10)
C18 0.0474(15) 0.0498(14) 0.0476(14) -0.0060(12) -0.0045(12) -0.0229(12)
C19 0.0394(15) 0.0669(17) 0.0535(16) 0.0020(14) -0.0050(12) -0.0194(13)
C20 0.0566(18) 0.084(2) 0.0581(17) 0.0090(15) -0.0104(14) -0.0480(16)
C21 0.069(2) 0.0587(16) 0.0727(19) -0.0022(15) -0.0107(15) -0.0437(16)
C22 0.0473(15) 0.0477(13) 0.0498(14) -0.0052(12) -0.0034(12) -0.0241(12)
N1 0.0382(11) 0.0396(10) 0.0304(9) -0.0020(8) -0.0061(8) -0.0192(8)
O1 0.0520(10) 0.0478(9) 0.0306(8) 0.0015(7) -0.0085(7) -0.0320(8)
S1 0.0535(4) 0.0381(3) 0.0373(3) 0.0018(2) -0.0147(3) -0.0185(3)

_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 O1 1.495(3) . ?
B1 C17 1.603(3) . ?
B1 C11 1.606(3) . ?
B1 N1 1.646(3) . ?
C1 C6 1.389(3) . ?
C1 C2 1.396(3) . ?
C1 S1 1.731(2) . ?
C2 C3 1.366(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C6 N1 1.410(3) . ?
C7 N1 1.324(3) . ?
C7 C8 1.447(3) . ?
C7 S1 1.718(2) . ?
C8 C10 1.394(3) 2_565 ?
C8 C9 1.403(3) . ?
C9 O1 1.339(2) . ?
C9 C10 1.385(3) . ?
C10 C8 1.394(3) 2_565 ?
C10 H10 0.9300 . ?
C11 C16 1.382(3) . ?
C11 C12 1.391(3) . ?
C12 C13 1.386(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.359(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.385(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C22 1.386(3) . ?
C17 C18 1.389(3) . ?
C18 C19 1.376(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.368(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.365(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.384(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?

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
O1 B1 C17 105.41(18) . . ?
O1 B1 C11 111.20(18) . . ?
C17 B1 C11 117.53(18) . . ?
O1 B1 N1 104.44(16) . . ?
C17 B1 N1 108.97(18) . . ?
C11 B1 N1 108.49(18) . . ?
C6 C1 C2 121.5(2) . . ?
C6 C1 S1 110.60(16) . . ?
C2 C1 S1 127.90(19) . . ?
C3 C2 C1 117.7(2) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 120.9(2) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 122.1(2) . . ?
C5 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
C4 C5 C6 117.6(2) . . ?
C4 C5 H5 121.2 . . ?
C6 C5 H5 121.2 . . ?
C1 C6 C5 120.3(2) . . ?
C1 C6 N1 112.90(19) . . ?
C5 C6 N1 126.8(2) . . ?
N1 C7 C8 122.4(2) . . ?
N1 C7 S1 114.53(16) . . ?
C8 C7 S1 123.08(16) . . ?
C10 C8 C9 120.99(19) 2_565 . ?
C10 C8 C7 121.7(2) 2_565 . ?
C9 C8 C7 117.23(19) . . ?
O1 C9 C10 119.8(2) . . ?
O1 C9 C8 121.27(18) . . ?
C10 C9 C8 118.72(19) . . ?
C9 C10 C8 120.3(2) . 2_565 ?
C9 C10 H10 119.9 . . ?
C8 C10 H10 119.9 2_565 . ?
C16 C11 C12 115.5(2) . . ?
C16 C11 B1 119.7(2) . . ?
C12 C11 B1 124.8(2) . . ?
C13 C12 C11 122.2(3) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 120.1(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 122.8(3) . . ?
C11 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
C22 C17 C18 116.1(2) . . ?
C22 C17 B1 124.7(2) . . ?
C18 C17 B1 119.1(2) . . ?
C19 C18 C17 122.3(2) . . ?
C19 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
C20 C19 C18 120.1(2) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 C19 119.2(3) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 120.6(2) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C21 C22 C17 121.6(2) . . ?
C21 C22 H22 119.2 . . ?
C17 C22 H22 119.2 . . ?
C7 N1 C6 111.79(18) . . ?
C7 N1 B1 120.44(17) . . ?
C6 N1 B1 127.77(17) . . ?
C9 O1 B1 121.97(17) . . ?
C7 S1 C1 90.17(11) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.046