# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_BIF-41
_database_code_depnum_ccdc_archive 'CCDC 1436999'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H32 B2 Co2 N16 O11'
_chemical_formula_weight         932.20

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'
Co Co 0.3494 0.9721 '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           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   26.1535(10)
_cell_length_b                   13.6168(5)
_cell_length_c                   17.1807(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.056(3)
_cell_angle_gamma                90.00
_cell_volume                     4946.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9133
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4171
_reflns_number_gt                2815
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1550P)²+0.0000P] where P=(Fo²+2Fc²)/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         4171
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0717
_refine_ls_wR_factor_ref         0.2375
_refine_ls_wR_factor_gt          0.2146
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.004

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.12292(3) 0.22335(6) 0.18843(5) 0.0251(3) Uani 1 1 d . . .
O21 O 0.1189(2) 0.3533(4) 0.1112(4) 0.0545(13) Uani 1 1 d . . .
O39 O 0.0976(3) 0.3691(4) 0.2146(4) 0.0652(15) Uani 1 1 d . . .
N1 N 0.2195(2) 0.2447(4) 0.3035(3) 0.0298(11) Uani 1 1 d . . .
N3 N 0.0261(2) 0.1964(3) 0.0753(3) 0.0289(11) Uani 1 1 d . . .
N5 N -0.0749(2) 0.1545(3) 0.0005(3) 0.0274(11) Uani 1 1 d . . .
N7 N 0.1497(2) 0.1219(4) 0.1291(3) 0.0315(11) Uani 1 1 d . . .
N9 N 0.3116(2) 0.3090(3) 0.4199(3) 0.0250(10) Uani 1 1 d . . .
N11 N 0.1148(2) 0.1393(4) 0.2833(3) 0.0299(11) Uani 1 1 d . . .
N12 N 0.1251(2) 0.1054(3) 0.4183(3) 0.0276(11) Uani 1 1 d . . .
N14 N 0.1536(2) -0.0160(3) 0.0644(3) 0.0263(11) Uani 1 1 d . . .
C1 C 0.0822(5) 0.5114(6) 0.1194(6) 0.090(3) Uani 1 1 d . . .
H1A H 0.0682 0.5416 0.1563 0.108 Uiso 1 1 calc R . .
H1B H 0.1199 0.5479 0.1347 0.108 Uiso 1 1 calc R . .
C2 C 0.0306(4) 0.5211(6) 0.0142(7) 0.083(3) Uani 1 1 d . . .
H2A H 0.0244 0.5916 -0.0035 0.100 Uiso 1 1 calc R . .
H2B H 0.0438 0.4877 -0.0226 0.100 Uiso 1 1 calc R . .
C19 C 0.3163(3) 0.2075(4) 0.4304(4) 0.0363(15) Uani 1 1 d . . .
H19 H 0.3524 0.1713 0.4787 0.044 Uiso 1 1 calc R . .
C22 C -0.0185(2) 0.1664(4) 0.0849(4) 0.0290(13) Uani 1 1 d . . .
H22 H -0.0110 0.1548 0.1454 0.035 Uiso 1 1 calc R . .
C25 C -0.0657(3) 0.1820(5) -0.0678(4) 0.0347(14) Uani 1 1 d . . .
H25 H -0.0970 0.1835 -0.1355 0.042 Uiso 1 1 calc R . .
C27 C 0.2519(3) 0.3244(4) 0.3410(4) 0.0309(13) Uani 1 1 d . . .
H27 H 0.2353 0.3878 0.3155 0.037 Uiso 1 1 calc R . .
C29 C 0.1235(3) 0.0354(4) 0.0930(4) 0.0295(13) Uani 1 1 d . . .
H29 H 0.0874 0.0120 0.0879 0.035 Uiso 1 1 calc R . .
C31 C -0.0047(3) 0.2063(5) -0.0215(4) 0.0365(15) Uani 1 1 d . . .
H31 H 0.0143 0.2274 -0.0517 0.044 Uiso 1 1 calc R . .
C32 C 0.2605(3) 0.1708(5) 0.3599(4) 0.0395(16) Uani 1 1 d . . .
H32 H 0.2504 0.1028 0.3500 0.047 Uiso 1 1 calc R . .
C35 C 0.1333(3) 0.1716(4) 0.3682(4) 0.0298(13) Uani 1 1 d . . .
H35 H 0.1506 0.2351 0.3919 0.036 Uiso 1 1 calc R . .
C41 C 0.2026(3) 0.0438(5) 0.0831(5) 0.0374(15) Uani 1 1 d . . .
H41 H 0.2326 0.0290 0.0704 0.045 Uiso 1 1 calc R . .
C44 C 0.0933(3) 0.0462(5) 0.2776(4) 0.0372(15) Uani 1 1 d . . .
H44 H 0.0763 0.0032 0.2241 0.045 Uiso 1 1 calc R . .
C46 C 0.0998(3) 0.0248(5) 0.3596(4) 0.0411(16) Uani 1 1 d . . .
H46 H 0.0888 -0.0355 0.3741 0.049 Uiso 1 1 calc R . .
C47 C 0.1994(3) 0.1274(5) 0.1228(4) 0.0387(15) Uani 1 1 d . . .
H47 H 0.2274 0.1816 0.1433 0.046 Uiso 1 1 calc R . .
C50 C 0.1007(3) 0.4043(5) 0.1509(6) 0.059(2) Uani 1 1 d . . .
B37 B -0.1358(3) 0.1173(5) -0.0163(4) 0.0235(14) Uani 1 1 d . . .
O1 O 0.1709(12) 0.4127(18) 0.0242(16) 0.375(12) Uiso 1 1 d . . .
O2 O 0.4077(12) 0.0348(19) 0.6533(16) 0.393(12) Uiso 1 1 d . . .
O3 O -0.1891(16) 0.174(2) -0.338(2) 0.464(16) Uiso 1 1 d . . .
O4 O 0.5000 -0.167(5) 0.7500 0.66(4) Uiso 1 2 d S . .


_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
Co1 N7 2.069(5) . ?
Co1 N11 2.102(5) . ?
Co1 N1 2.121(4) . ?
Co1 N3 2.128(4) . ?
Co1 O21 2.178(5) . ?
Co1 O39 2.221(5) . ?
O21 C50 1.248(9) . ?
O39 C50 1.241(10) . ?
N1 C27 1.291(7) . ?
N1 C32 1.369(8) . ?
N3 C22 1.335(7) . ?
N3 C31 1.363(7) . ?
N5 C22 1.336(7) . ?
N5 C25 1.382(7) . ?
N5 B37 1.529(7) . ?
N7 C29 1.320(7) . ?
N7 C47 1.367(7) . ?
N9 C27 1.352(7) . ?
N9 C19 1.390(7) . ?
N9 B37 1.526(7) 8_556 ?
N11 C35 1.315(7) . ?
N11 C44 1.367(8) . ?
N12 C35 1.347(7) . ?
N12 C46 1.370(8) . ?
N12 B37 1.544(7) 2 ?
N14 C29 1.345(7) . ?
N14 C41 1.388(7) . ?
N14 B37 1.532(8) 5 ?
C1 C2 1.495(12) . ?
C1 C50 1.532(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.488(17) 5_565 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C19 C32 1.328(8) . ?
C19 H19 0.9500 . ?
C22 H22 0.9500 . ?
C25 C31 1.338(8) . ?
C25 H25 0.9500 . ?
C27 H27 0.9500 . ?
C29 H29 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C35 H35 0.9500 . ?
C41 C47 1.356(9) . ?
C41 H41 0.9500 . ?
C44 C46 1.348(8) . ?
C44 H44 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
B37 N9 1.526(7) 8_455 ?
B37 N14 1.532(8) 5 ?
B37 N12 1.544(7) 2 ?

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
N7 Co1 N11 103.7(2) . . ?
N7 Co1 N1 89.28(18) . . ?
N11 Co1 N1 87.73(18) . . ?
N7 Co1 N3 90.04(18) . . ?
N11 Co1 N3 90.30(17) . . ?
N1 Co1 N3 177.71(18) . . ?
N7 Co1 O21 98.7(2) . . ?
N11 Co1 O21 157.6(2) . . ?
N1 Co1 O21 93.46(18) . . ?
N3 Co1 O21 88.81(17) . . ?
N7 Co1 O39 157.6(2) . . ?
N11 Co1 O39 98.7(2) . . ?
N1 Co1 O39 91.28(19) . . ?
N3 Co1 O39 90.18(19) . . ?
O21 Co1 O39 58.9(2) . . ?
C50 O21 Co1 90.9(5) . . ?
C50 O39 Co1 89.1(5) . . ?
C27 N1 C32 104.8(5) . . ?
C27 N1 Co1 130.6(4) . . ?
C32 N1 Co1 124.4(4) . . ?
C22 N3 C31 104.4(4) . . ?
C22 N3 Co1 126.6(4) . . ?
C31 N3 Co1 128.9(4) . . ?
C22 N5 C25 104.8(5) . . ?
C22 N5 B37 127.4(5) . . ?
C25 N5 B37 127.8(4) . . ?
C29 N7 C47 105.5(5) . . ?
C29 N7 Co1 126.4(4) . . ?
C47 N7 Co1 128.0(4) . . ?
C27 N9 C19 104.2(5) . . ?
C27 N9 B37 129.7(5) . 8_556 ?
C19 N9 B37 126.0(5) . 8_556 ?
C35 N11 C44 104.8(5) . . ?
C35 N11 Co1 122.7(4) . . ?
C44 N11 Co1 132.5(4) . . ?
C35 N12 C46 104.8(5) . . ?
C35 N12 B37 129.2(5) . 2 ?
C46 N12 B37 125.9(5) . 2 ?
C29 N14 C41 105.7(5) . . ?
C29 N14 B37 127.5(5) . 5 ?
C41 N14 B37 126.8(5) . 5 ?
C2 C1 C50 112.6(7) . . ?
C2 C1 H1A 109.1 . . ?
C50 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C50 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 113.2(11) 5_565 . ?
C2 C2 H2A 108.9 5_565 . ?
C1 C2 H2A 108.9 . . ?
C2 C2 H2B 108.9 5_565 . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.8 . . ?
C32 C19 N9 106.9(5) . . ?
C32 C19 H19 126.6 . . ?
N9 C19 H19 126.6 . . ?
N3 C22 N5 112.9(5) . . ?
N3 C22 H22 123.5 . . ?
N5 C22 H22 123.5 . . ?
C31 C25 N5 107.7(5) . . ?
C31 C25 H25 126.1 . . ?
N5 C25 H25 126.1 . . ?
N1 C27 N9 113.6(5) . . ?
N1 C27 H27 123.2 . . ?
N9 C27 H27 123.2 . . ?
N7 C29 N14 112.4(5) . . ?
N7 C29 H29 123.8 . . ?
N14 C29 H29 123.8 . . ?
C25 C31 N3 110.1(5) . . ?
C25 C31 H31 125.0 . . ?
N3 C31 H31 125.0 . . ?
C19 C32 N1 110.5(5) . . ?
C19 C32 H32 124.7 . . ?
N1 C32 H32 124.7 . . ?
N11 C35 N12 113.2(5) . . ?
N11 C35 H35 123.4 . . ?
N12 C35 H35 123.4 . . ?
C47 C41 N14 106.6(5) . . ?
C47 C41 H41 126.7 . . ?
N14 C41 H41 126.7 . . ?
C46 C44 N11 109.4(5) . . ?
C46 C44 H44 125.3 . . ?
N11 C44 H44 125.3 . . ?
C44 C46 N12 107.8(5) . . ?
C44 C46 H46 126.1 . . ?
N12 C46 H46 126.1 . . ?
C41 C47 N7 109.7(5) . . ?
C41 C47 H47 125.1 . . ?
N7 C47 H47 125.1 . . ?
O39 C50 O21 120.8(7) . . ?
O39 C50 C1 120.6(9) . . ?
O21 C50 C1 118.6(9) . . ?
N9 B37 N14 110.2(4) 8_455 5 ?
N9 B37 N5 108.5(5) 8_455 . ?
N14 B37 N5 110.6(4) 5 . ?
N9 B37 N12 111.1(4) 8_455 2 ?
N14 B37 N12 107.2(5) 5 2 ?
N5 B37 N12 109.2(4) . 2 ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.130
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_BIF-42
_database_code_depnum_ccdc_archive 'CCDC 1437000'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H24 B Cd N9 O4'
_chemical_formula_weight         589.70

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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                   9.003(5)
_cell_length_b                   17.382(11)
_cell_length_c                   17.057(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.595(10)
_cell_angle_gamma                90.00
_cell_volume                     2583(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    6078
_cell_measurement_theta_min      2.3435
_cell_measurement_theta_max      27.6178

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1500
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7183
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15833
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4481
_reflns_number_gt                3699
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1000P)²+6.4432P] where P=(Fo²+2Fc²)/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         4481
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1942
_refine_ls_wR_factor_gt          0.1850
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.003
_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
Cd1 Cd 0.38438(5) 0.06015(3) 0.21475(3) 0.0286(2) Uani 1 1 d . . .
N3 N 0.7621(7) -0.0950(3) 0.1794(3) 0.0310(13) Uani 1 1 d . . .
C1AA C 0.6892(10) -0.0442(5) 0.2829(5) 0.0416(18) Uani 1 1 d . . .
H1AA H 0.6827 -0.0322 0.3363 0.050 Uiso 1 1 calc R . .
C3AA C 0.6928(8) 0.1675(4) 0.2698(5) 0.0371(17) Uani 1 1 d . . .
H3AA H 0.7462 0.1302 0.2466 0.045 Uiso 1 1 calc R . .
N6 N 0.5423(7) 0.1614(3) 0.2743(4) 0.0323(13) Uani 1 1 d . . .
N7 N 0.0021(6) -0.1122(3) 0.1286(3) 0.0298(13) Uani 1 1 d . . .
N8 N 0.2550(7) 0.1515(3) -0.0408(3) 0.0307(13) Uani 1 1 d . . .
C9 C 0.0714(9) -0.0486(4) 0.1689(5) 0.0353(17) Uani 1 1 d . . .
H9 H 0.0294 -0.0187 0.2047 0.042 Uiso 1 1 calc R . .
C10 C 0.6420(8) -0.0474(4) 0.1528(5) 0.0318(15) Uani 1 1 d . . .
H10 H 0.5967 -0.0378 0.0971 0.038 Uiso 1 1 calc R . .
N12 N 0.6381(6) 0.2723(3) 0.3302(3) 0.0296(13) Uani 1 1 d . . .
O13 O 0.2064(7) 0.0875(3) 0.2932(3) 0.0484(14) Uani 1 1 d . . .
C14 C 0.7525(9) 0.2347(4) 0.3033(5) 0.0368(17) Uani 1 1 d . . .
H14 H 0.8538 0.2528 0.3077 0.044 Uiso 1 1 calc R . .
N15 N 0.2041(7) -0.0339(4) 0.1521(4) 0.0379(14) Uani 1 1 d . . .
C16 C 0.5132(8) 0.2251(4) 0.3108(4) 0.0327(16) Uani 1 1 d . . .
H16 H 0.4174 0.2364 0.3220 0.039 Uiso 1 1 calc R . .
N17 N 0.3511(7) 0.1192(4) 0.0892(4) 0.0391(15) Uani 1 1 d . . .
N19 N 0.5935(7) -0.0155(3) 0.2121(4) 0.0350(14) Uani 1 1 d . . .
C20 C 0.1003(9) -0.1377(4) 0.0834(5) 0.0402(18) Uani 1 1 d . . .
H20 H 0.0845 -0.1808 0.0481 0.048 Uiso 1 1 calc R . .
O21 O 0.3884(7) 0.0052(4) 0.3466(4) 0.0573(16) Uani 1 1 d . . .
C22 C 0.7936(9) -0.0921(5) 0.2637(4) 0.0429(19) Uani 1 1 d . . .
H22 H 0.8735 -0.1187 0.3008 0.052 Uiso 1 1 calc R . .
C23 C 0.2451(8) 0.1050(4) 0.0216(4) 0.0333(16) Uani 1 1 d . . .
H23 H 0.1694 0.0660 0.0172 0.040 Uiso 1 1 calc R . .
C24 C 0.0453(10) 0.0483(5) 0.4111(5) 0.049(2) Uani 1 1 d . . .
H24 H -0.0007 0.0842 0.3702 0.059 Uiso 1 1 calc R . .
C25 C -0.0343(9) 0.0271(5) 0.4698(5) 0.0448(19) Uani 1 1 d . . .
C26 C 0.2231(9) -0.0900(5) 0.0988(5) 0.0423(18) Uani 1 1 d . . .
H26 H 0.3089 -0.0945 0.0762 0.051 Uiso 1 1 calc R . .
C27 C 0.1867(9) 0.0185(5) 0.4116(5) 0.0441(19) Uani 1 1 d . . .
B28 B 0.8446(9) -0.1463(4) 0.1294(5) 0.0302(17) Uani 1 1 d . . .
C30 C 0.2570(10) -0.0347(6) 0.4737(5) 0.052(2) Uani 1 1 d . . .
H30 H 0.3561 -0.0547 0.4758 0.062 Uiso 1 1 calc R . .
C40 C 0.4361(11) 0.1785(5) 0.0694(5) 0.062(3) Uani 1 1 d . . .
H40 H 0.5221 0.2019 0.1055 0.075 Uiso 1 1 calc R . .
C42 C 0.3788(11) 0.1986(5) -0.0094(5) 0.058(2) Uani 1 1 d . . .
H42 H 0.4171 0.2379 -0.0377 0.069 Uiso 1 1 calc R . .
C4AA C 0.2667(10) 0.0389(5) 0.3473(5) 0.0432(19) Uani 1 1 d . . .
C2AA C 0.1807(11) -0.0569(5) 0.5306(6) 0.055(2) Uani 1 1 d . . .
H2AA H 0.2275 -0.0931 0.5710 0.066 Uiso 1 1 calc R . .
N2 N 0.5140(15) -0.2297(7) 0.3730(7) 0.097(3) Uani 1 1 d . . .
C4 C 0.616(2) -0.1919(11) 0.4254(10) 0.130(7) Uani 1 1 d . . .
H4 H 0.6017 -0.1384 0.4320 0.157 Uiso 1 1 calc R . .
C2 C 0.5365(18) -0.3126(8) 0.3604(9) 0.110(5) Uani 1 1 d . . .
H2A H 0.6404 -0.3276 0.3899 0.166 Uiso 1 1 calc R . .
H2B H 0.5225 -0.3227 0.3025 0.166 Uiso 1 1 calc R . .
H2C H 0.4614 -0.3424 0.3805 0.166 Uiso 1 1 calc R . .
O1 O 0.3654(11) -0.2733(5) 0.1376(6) 0.122(4) Uani 1 1 d G . .
H1A H 0.4215 -0.2457 0.1746 0.183 Uiso 1 1 d G . .
H1B H 0.2770 -0.2781 0.1463 0.183 Uiso 1 1 d G . .
C0AA C 0.3730(19) -0.1927(12) 0.3242(8) 0.157(8) Uani 1 1 d G . .
H0AA H 0.2874 -0.2038 0.3483 0.236 Uiso 1 1 calc R . .
H0AB H 0.3496 -0.2130 0.2688 0.236 Uiso 1 1 calc R . .
H0AC H 0.3887 -0.1370 0.3231 0.236 Uiso 1 1 calc R . .
O4 O 0.7325(19) -0.2231(9) 0.4673(9) 0.174(6) Uani 1 1 d . . .


_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
Cd1 N19 2.306(6) . ?
Cd1 N17 2.326(6) . ?
Cd1 N6 2.328(6) . ?
Cd1 N15 2.361(6) . ?
Cd1 O13 2.380(5) . ?
Cd1 O21 2.436(6) . ?
Cd1 C4AA 2.753(8) . ?
N3 C10 1.346(9) . ?
N3 C22 1.394(9) . ?
N3 B28 1.549(9) . ?
C1AA C22 1.356(11) . ?
C1AA N19 1.389(10) . ?
C3AA C14 1.350(10) . ?
C3AA N6 1.380(9) . ?
N6 C16 1.329(9) . ?
N7 C9 1.367(9) . ?
N7 C20 1.384(9) . ?
N7 B28 1.540(9) 1_455 ?
N8 C23 1.358(9) . ?
N8 C42 1.378(10) . ?
N8 B28 1.553(10) 3_655 ?
C9 N15 1.322(9) . ?
C10 N19 1.320(9) . ?
N12 C16 1.363(9) . ?
N12 C14 1.392(9) . ?
N12 B28 1.564(9) 2_655 ?
O13 C4AA 1.268(10) . ?
N15 C26 1.373(10) . ?
N17 C23 1.321(9) . ?
N17 C40 1.376(10) . ?
C20 C26 1.353(11) . ?
O21 C4AA 1.245(10) . ?
C24 C27 1.372(12) . ?
C24 C25 1.419(11) . ?
C25 C2AA 1.415(12) 3_556 ?
C25 C25 1.416(17) 3_556 ?
C27 C30 1.428(12) . ?
C27 C4AA 1.499(10) . ?
B28 N7 1.540(9) 1_655 ?
B28 N8 1.553(10) 3_655 ?
B28 N12 1.564(9) 2_645 ?
C30 C2AA 1.376(12) . ?
C40 C42 1.359(12) . ?
C2AA C25 1.415(12) 3_556 ?
N2 C4 1.289(18) . ?
N2 C0AA 1.477(19) . ?
N2 C2 1.478(17) . ?
C4 O4 1.23(2) . ?

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
N19 Cd1 N17 98.6(2) . . ?
N19 Cd1 N6 91.6(2) . . ?
N17 Cd1 N6 89.5(2) . . ?
N19 Cd1 N15 93.9(2) . . ?
N17 Cd1 N15 88.5(2) . . ?
N6 Cd1 N15 174.4(2) . . ?
N19 Cd1 O13 142.5(2) . . ?
N17 Cd1 O13 118.8(2) . . ?
N6 Cd1 O13 91.6(2) . . ?
N15 Cd1 O13 84.8(2) . . ?
N19 Cd1 O21 88.4(2) . . ?
N17 Cd1 O21 172.9(2) . . ?
N6 Cd1 O21 91.6(2) . . ?
N15 Cd1 O21 89.7(2) . . ?
O13 Cd1 O21 54.2(2) . . ?
N19 Cd1 C4AA 115.1(2) . . ?
N17 Cd1 C4AA 146.0(3) . . ?
N6 Cd1 C4AA 93.6(2) . . ?
N15 Cd1 C4AA 85.2(2) . . ?
O13 Cd1 C4AA 27.4(2) . . ?
O21 Cd1 C4AA 26.9(2) . . ?
C10 N3 C22 105.3(6) . . ?
C10 N3 B28 128.6(6) . . ?
C22 N3 B28 126.0(6) . . ?
C22 C1AA N19 109.0(7) . . ?
C14 C3AA N6 109.6(6) . . ?
C16 N6 C3AA 105.9(6) . . ?
C16 N6 Cd1 131.6(5) . . ?
C3AA N6 Cd1 122.3(4) . . ?
C9 N7 C20 105.3(6) . . ?
C9 N7 B28 127.8(6) . 1_455 ?
C20 N7 B28 126.8(6) . 1_455 ?
C23 N8 C42 104.8(6) . . ?
C23 N8 B28 126.3(6) . 3_655 ?
C42 N8 B28 128.7(6) . 3_655 ?
N15 C9 N7 111.7(6) . . ?
N19 C10 N3 113.1(7) . . ?
C16 N12 C14 105.7(6) . . ?
C16 N12 B28 129.5(6) . 2_655 ?
C14 N12 B28 124.8(6) . 2_655 ?
C4AA O13 Cd1 92.9(5) . . ?
C3AA C14 N12 107.3(6) . . ?
C9 N15 C26 106.0(6) . . ?
C9 N15 Cd1 126.3(5) . . ?
C26 N15 Cd1 127.3(5) . . ?
N6 C16 N12 111.6(6) . . ?
C23 N17 C40 104.5(6) . . ?
C23 N17 Cd1 128.2(5) . . ?
C40 N17 Cd1 127.3(5) . . ?
C10 N19 C1AA 105.3(6) . . ?
C10 N19 Cd1 133.2(5) . . ?
C1AA N19 Cd1 121.2(5) . . ?
C26 C20 N7 107.5(7) . . ?
C4AA O21 Cd1 90.9(5) . . ?
C1AA C22 N3 107.4(7) . . ?
N17 C23 N8 113.4(6) . . ?
C27 C24 C25 122.0(8) . . ?
C2AA C25 C25 118.8(9) 3_556 3_556 ?
C2AA C25 C24 122.4(8) 3_556 . ?
C25 C25 C24 118.7(10) 3_556 . ?
C20 C26 N15 109.4(6) . . ?
C24 C27 C30 119.1(7) . . ?
C24 C27 C4AA 121.5(8) . . ?
C30 C27 C4AA 119.4(8) . . ?
N7 B28 N3 110.7(6) 1_655 . ?
N7 B28 N8 108.7(6) 1_655 3_655 ?
N3 B28 N8 109.2(6) . 3_655 ?
N7 B28 N12 111.3(6) 1_655 2_645 ?
N3 B28 N12 106.6(5) . 2_645 ?
N8 B28 N12 110.2(6) 3_655 2_645 ?
C2AA C30 C27 119.8(8) . . ?
C42 C40 N17 109.8(7) . . ?
C40 C42 N8 107.5(7) . . ?
O21 C4AA O13 121.6(7) . . ?
O21 C4AA C27 118.8(8) . . ?
O13 C4AA C27 119.6(7) . . ?
O21 C4AA Cd1 62.2(4) . . ?
O13 C4AA Cd1 59.7(4) . . ?
C27 C4AA Cd1 171.2(6) . . ?
C30 C2AA C25 121.6(9) . 3_556 ?
C4 N2 C0AA 122.1(15) . . ?
C4 N2 C2 119.8(15) . . ?
C0AA N2 C2 118.1(12) . . ?
O4 C4 N2 122.1(19) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.153


#end
