# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 2001

data_swb21 

_database_code_CSD	167765


_journal_coden_Cambridge      207

_publ_requested_journal       'Perkin Transactions 1'

loop_
_publ_author_name
'Cosway, Sarah'
'Jones, Raymond H. V.'
'Leung, Wilson'
'Wills, M.'

_publ_contact_author_name     	'Dr M Wills'  
_publ_contact_author_address 
;
Department of Chemistry
University of Warwick
Coventry
CV4 7AL
UK
;

_publ_contact_author_email       'M.WILLS@WARWICK.AC.UK'

_publ_section_title		
;
Synthesis of Benzazaphospholidine Ligands via an Intramolecular
Cyclisation Reaction
;

_audit_creation_method            SHELXL

_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ?

_chemical_formula_moiety          ? 
_chemical_formula_structural      ?

_chemical_formula_analytical      ? 
_chemical_formula_sum 
'C18 H21 B Br N O P' 
_chemical_formula_weight          389.05 
_chemical_melting_point		? 
_chemical_compound_source         ? 

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' 
'P'  'P'   0.1023 0.0942 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Br' 'Br'  -0.2901   2.4595 
'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

loop_ 
_symmetry_equiv_pos_as_xyz

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


_cell_length_a                    27.0233(2) 
_cell_length_b			  14.3417(3) 
_cell_length_c                    20.1259(4)

_cell_angle_alpha                 90.00 
_cell_angle_beta		  96.7510(10) 
_cell_angle_gamma                 90.00 
_cell_volume			  7745.9(2) 
_cell_formula_units_Z             16

_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used	  ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max	  ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour 		  ? 
_exptl_crystal_size_max           0.60 
_exptl_crystal_size_mid		  0.20 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas 	  ? 
_exptl_crystal_density_diffrn     1.334

_exptl_crystal_density_method     ? 
_exptl_crystal_F_000		  3184 
_exptl_absorpt_coefficient_mu     2.208

_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min	  0.5156 
_exptl_absorpt_correction_T_max   0.8381 

_exptl_special_details

; 
? 
; 

_diffrn_ambient_temperature       180(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
? 
_diffrn_measurement_method        ? 
_diffrn_standards_number
? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time
? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number
19561 
_diffrn_reflns_av_R_equivalents   0.0402

_diffrn_reflns_av_sigmaI/netI     0.1045 
_diffrn_reflns_limit_h_min
-34 
_diffrn_reflns_limit_h_max        31 
_diffrn_reflns_limit_k_min
-17 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min
-15 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min
1.02 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total
13053 
_reflns_number_observed           7522

_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection
? 
_computing_cell_refinement        ? 
_computing_data_reduction
? 
_computing_structure_solution     'SHELXS-96 (Sheldrick, 1990)'

_computing_structure_refinement   'SHELXL-96 (Sheldrick, 1996)'

_computing_molecular_graphics     ? 
_computing_publication_material   ? 


_refine_special_details 
; 
Refinement of F^2^ against ALL reflections.
Weighted R-factors wR and all 
goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for
calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0453P)^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     ? 
_refine_ls_extinction_method
none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details

'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack    0.018(8) 
_refine_ls_number_reflns
13053 
_refine_ls_number_parameters      840

_refine_ls_number_restraints      46 
_refine_ls_R_factor_all
0.1126 
_refine_ls_R_factor_obs           0.0521 
_refine_ls_wR_factor_all
0.1167 
_refine_ls_wR_factor_obs          0.0954

_refine_ls_goodness_of_fit_all    0.947 
_refine_ls_goodness_of_fit_obs
1.042 
_refine_ls_restrained_S_all       0.945 
_refine_ls_restrained_S_obs
1.039 
_refine_ls_shift/esd_max          0.001

_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 

_atom_site_calc_flag 
_atom_site_refinement_flags 

_atom_site_disorder_group 
Br1 Br 0.16586(3) 0.23469(6) -0.01438(4)
0.0527(3) Uani 1 d . . 
Br2 Br 0.29604(4) 0.15700(8) 0.00107(5) 0.0854(4)
Uani 1 d . . 
Br3 Br 0.20894(3) -0.08639(7) -0.50467(4) 0.0715(4) Uani 1 d
. . 
Br4 Br 0.34299(3) -0.01342(6) -0.48408(4) 0.0540(3) Uani 1 d . . 
P1 P
0.11310(6) 0.07711(13) 0.24063(9) 0.0245(4) Uani 1 d . . 
P2 P 0.39382(6)
0.07719(13) -0.23346(9) 0.0260(5) Uani 1 d . . 
P3 P 0.11149(6)
-0.17244(13) -0.26968(9) 0.0274(5) Uani 1 d . . 
P4 P 0.38434(6)
-0.17074(13) -0.74255(9) 0.0230(4) Uani 1 d . . 
O11 O 0.06462(16)
0.1191(3) 0.2680(2) 0.0330(12) Uani 1 d . . 
O21 O 0.43915(15) 0.1266(3)
-0.2634(2) 0.0275(11) Uani 1 d . . 
O31 O 0.06543(15) -0.1234(3) -0.2403(2)
0.0299(12) Uani 1 d . . 
O41 O 0.43240(15) -0.1263(3) -0.7685(2) 0.0270(11)
Uani 1 d . . 
N11 N 0.10425(18) 0.1305(4) 0.1673(2) 0.0221(13) Uani 1 d . .

N21 N 0.40176(18) 0.1323(4) -0.1609(2) 0.0237(13) Uani 1 d . . 
N31 N
0.10494(18) -0.1128(4) -0.3414(2) 0.0248(14) Uani 1 d . . 
N41 N
0.39267(18) -0.1213(4) -0.6682(2) 0.0244(13) Uani 1 d . . 
B1 B 0.1134(3)
-0.0552(6) 0.2437(5) 0.042(2) Uani 1 d D . 
H1A H 0.1475(7) -0.0818(8)
0.2244(6) 0.063 Uiso 1 calc RD . 
H1B H 0.0800(7) -0.0824(8) 0.2123(7)
0.063 Uiso 1 calc RD . 
H1C H 0.1128(3) -0.0786(7) 0.2962(10) 0.063 Uiso 1
calc RD . 
B2 B 0.3995(3) -0.0544(6) -0.2330(5) 0.045(2) Uani 1 d D . 
H2A
H 0.3671(6) -0.0854(8) -0.2118(6) 0.067 Uiso 1 calc RD . 
H2B H 0.4345(7)
-0.0751(7) -0.2018(7) 0.067 Uiso 1 calc RD . 
H2C H 0.4004(3) -0.0798(8)
-0.2850(10) 0.067 Uiso 1 calc RD . 
B3 B 0.1060(3) -0.3032(6) -0.2732(4)
0.040(2) Uani 1 d D . 
H3A H 0.1386(7) -0.3327(8) -0.2937(6) 0.061 Uiso 1
calc RD . 
H3B H 0.0718(7) -0.3228(7) -0.3055(7) 0.061 Uiso 1 calc RD .

H3C H 0.1043(3) -0.3307(8) -0.2223(10) 0.061 Uiso 1 calc R . 
B4 B
0.3846(3) -0.3016(5) -0.7485(4) 0.037(2) Uani 1 d D . 
H4A H 0.3509(7)
-0.3296(8) -0.7301(5) 0.055 Uiso 1 calc RD . 
H4B H 0.4177(7) -0.3293(8)
-0.7179(7) 0.055 Uiso 1 calc RD . 
H4C H 0.3854(3) -0.3225(7) -0.8009(10)
0.055 Uiso 1 calc R . 
C101 C 0.1681(2) 0.1276(5) 0.2873(3) 0.0255(17) Uani
1 d . . 
C102 C 0.1819(2) 0.2205(5) 0.2775(3) 0.0324(19) Uani 1 d . . 
H10A
H 0.1627 0.2579 0.2450 0.039 Uiso 1 calc R . 
C103 C 0.2232(3) 0.2576(6)
0.3148(4) 0.043(2) Uani 1 d . . 
H10B H 0.2319 0.3210 0.3090 0.052 Uiso 1
calc R . 
C104 C 0.2519(3) 0.2027(6) 0.3605(4) 0.056(2) Uani 1 d . . 
H10C
H 0.2804 0.2284 0.3862 0.067 Uiso 1 calc R . 
C105 C 0.2393(3) 0.1104(6)
0.3689(4) 0.052(2) Uani 1 d . . 
H10D H 0.2596 0.0723 0.3996 0.062 Uiso 1
calc R . 
C106 C 0.1976(2) 0.0736(5) 0.3329(3) 0.0383(19) Uani 1 d . .

H10E H 0.1889 0.0104 0.3395 0.046 Uiso 1 calc R . 
C107 C 0.0467(2)
0.2007(5) 0.2315(3) 0.0331(19) Uani 1 d . . 
H10F H 0.0602 0.2572 0.2554
0.040 Uiso 1 calc R . 
H10G H 0.0099 0.2030 0.2283 0.040 Uiso 1 calc R .

C108 C 0.0629(2) 0.1988(5) 0.1616(3) 0.0262(17) Uani 1 d . . 
C109 C
0.0220(2) 0.1721(5) 0.1046(3) 0.0327(18) Uani 1 d . . 
C110 C -0.0043(2)
0.0793(5) 0.1172(4) 0.049(2) Uani 1 d . . 
H11A H 0.0207 0.0314 0.1306
0.073 Uiso 1 calc R . 
H11B H -0.0248 0.0597 0.0761 0.073 Uiso 1 calc R .

H11C H -0.0257 0.0880 0.1528 0.073 Uiso 1 calc R . 
C111 C -0.0164(3)
0.2507(5) 0.0952(4) 0.049(2) Uani 1 d . . 
H11D H 0.0003 0.3091 0.0859
0.073 Uiso 1 calc R . 
H11E H -0.0324 0.2577 0.1362 0.073 Uiso 1 calc R .

H11F H -0.0416 0.2357 0.0577 0.073 Uiso 1 calc R . 
C112 C 0.1426(2)
0.1410(5) 0.1221(3) 0.0295(18) Uani 1 d . . 
C113 C 0.1338(2) 0.0799(5)
0.0604(3) 0.0272(17) Uani 1 d . . 
C114 C 0.1182(2) -0.0125(5) 0.0639(3)
0.0358(17) Uani 1 d . . 
H11G H 0.1091 -0.0355 0.1051 0.043 Uiso 1 calc R .

C115 C 0.1156(3) -0.0709(6) 0.0098(4) 0.047(2) Uani 1 d . . 
H11I H 0.1054
-0.1338 0.0145 0.056 Uiso 1 calc R . 
C116 C 0.1273(3) -0.0406(7)
-0.0505(4) 0.055(3) Uani 1 d . . 
H11J H 0.1248 -0.0817 -0.0878 0.066 Uiso
1 calc R . 
C117 C 0.1427(3) 0.0500(7) -0.0569(4) 0.050(2) Uani 1 d . .

H11H H 0.1508 0.0724 -0.0988 0.060 Uiso 1 calc R . 
C118 C 0.1462(2)
0.1083(5) -0.0017(4) 0.0359(19) Uani 1 d . . 
C201 C 0.3363(2) 0.1193(5)
-0.2780(3) 0.0285(18) Uani 1 d . . 
C202 C 0.3193(2) 0.2094(5) -0.2665(3)
0.034(2) Uani 1 d . . 
H20C H 0.3378 0.2482 -0.2344 0.041 Uiso 1 calc R .

C203 C 0.2755(3) 0.2425(6) -0.3019(3) 0.044(2) Uani 1 d . . 
H20D H 0.2638
0.3035 -0.2941 0.052 Uiso 1 calc R . 
C204 C 0.2492(3) 0.1848(7) -0.3485(4)
0.056(3) Uani 1 d . . 
H20E H 0.2195 0.2069 -0.3735 0.068 Uiso 1 calc R .

C205 C 0.2653(3) 0.0970(6) -0.3590(4) 0.054(2) Uani 1 d . . 
H20F H 0.2465
0.0581 -0.3908 0.065 Uiso 1 calc R . 
C206 C 0.3087(2) 0.0637(5) -0.3240(3)
0.0380(19) Uani 1 d . . 
H20G H 0.3195 0.0021 -0.3319 0.046 Uiso 1 calc R .

C207 C 0.4493(2) 0.2169(5) -0.2316(3) 0.0328(19) Uani 1 d . . 
H20A H
0.4300 0.2659 -0.2579 0.039 Uiso 1 calc R . 
H20B H 0.4851 0.2319 -0.2304
0.039 Uiso 1 calc R . 
C208 C 0.4350(2) 0.2151(5) -0.1607(3) 0.0254(17)
Uani 1 d . . 
C209 C 0.4794(2) 0.2069(5) -0.1041(3) 0.0324(19) Uani 1 d . .

C210 C 0.5055(3) 0.3016(6) -0.0958(4) 0.050(2) Uani 1 d . . 
H21A H 0.5325
0.2983 -0.0588 0.075 Uiso 1 calc R . 
H21B H 0.4815 0.3494 -0.0862 0.075
Uiso 1 calc R . 
H21C H 0.5194 0.3176 -0.1372 0.075 Uiso 1 calc R . 
C211 C
0.5158(3) 0.1308(6) -0.1186(4) 0.054(2) Uani 1 d . . 
H21D H 0.5433 0.1285
-0.0823 0.082 Uiso 1 calc R . 
H21E H 0.5290 0.1443 -0.1609 0.082 Uiso 1
calc R . 
H21F H 0.4986 0.0705 -0.1219 0.082 Uiso 1 calc R . 
C212 C
0.3639(2) 0.1317(5) -0.1138(3) 0.0279(18) Uani 1 d . . 
H21K H 0.3317
0.1116 -0.1381 0.033 Uiso 1 calc R . 
H21L H 0.3596 0.1961 -0.0977 0.033
Uiso 1 calc R . 
C213 C 0.3765(2) 0.0680(5) -0.0532(3) 0.0258(16) Uani 1 d
. . 
C214 C 0.4132(2) 0.0014(5) -0.0519(3) 0.0373(19) Uani 1 d . . 
H21G H
0.4319 -0.0044 -0.0888 0.045 Uiso 1 calc R . 
C215 C 0.4233(3) -0.0572(5)
0.0026(4) 0.046(2) Uani 1 d . . 
H21H H 0.4486 -0.1032 0.0020 0.055 Uiso 1
calc R . 
C216 C 0.3979(3) -0.0507(5) 0.0572(4) 0.041(2) Uani 1 d . . 
H21I
H 0.4055 -0.0907 0.0946 0.049 Uiso 1 calc R . 
C217 C 0.3610(3) 0.0156(6)
0.0566(4) 0.045(2) Uani 1 d . . 
H21J H 0.3425 0.0217 0.0937 0.055 Uiso 1
calc R . 
C218 C 0.3511(2) 0.0733(5) 0.0014(4) 0.0385(19) Uani 1 d . .

C301 C 0.1686(2) -0.1315(5) -0.2224(3) 0.0302(18) Uani 1 d . . 
C302 C
0.1871(3) -0.0423(5) -0.2304(3) 0.035(2) Uani 1 d . . 
H30A H 0.1705
-0.0013 -0.2627 0.042 Uiso 1 calc R . 
C303 C 0.2292(3) -0.0135(7)
-0.1918(4) 0.050(2) Uani 1 d . . 
H30B H 0.2409 0.0481 -0.1973 0.060 Uiso 1
calc R . 
C304 C 0.2550(3) -0.0702(7) -0.1458(4) 0.055(2) Uani 1 d . .

H30C H 0.2845 -0.0485 -0.1201 0.066 Uiso 1 calc R . 
C305 C 0.2378(3)
-0.1602(7) -0.1367(4) 0.058(2) Uani 1 d . . 
H30D H 0.2554 -0.2005 -0.1048
0.069 Uiso 1 calc R . 
C306 C 0.1942(3) -0.1905(5) -0.1753(4) 0.046(2) Uani
1 d . . 
H30E H 0.1821 -0.2517 -0.1693 0.055 Uiso 1 calc R . 
C307 C
0.0566(2) -0.0290(5) -0.2676(3) 0.0269(17) Uani 1 d . . 
C308 C 0.0707(2)
-0.0310(5) -0.3405(3) 0.0279(17) Uani 1 d . . 
C309 C 0.0265(2) -0.0393(5)
-0.3970(3) 0.0310(18) Uani 1 d . . 
C310 C -0.0105(3) -0.1139(5) -0.3838(4)
0.051(2) Uani 1 d . . 
H31G H -0.0379 -0.1146 -0.4203 0.077 Uiso 1 calc R .

H31H H -0.0237 -0.1009 -0.3415 0.077 Uiso 1 calc R . 
H31I H 0.0061
-0.1748 -0.3811 0.077 Uiso 1 calc R . 
C311 C 0.0002(3) 0.0562(5)
-0.4049(4) 0.047(2) Uani 1 d . . 
H31J H -0.0278 0.0525 -0.4406 0.071 Uiso
1 calc R . 
H31K H 0.0239 0.1036 -0.4165 0.071 Uiso 1 calc R . 
H31L H
-0.0123 0.0732 -0.3628 0.071 Uiso 1 calc R . 
C312 C 0.1410(2) -0.1139(4)
-0.3895(3) 0.0275(17) Uani 1 d . . 
H31A H 0.1735 -0.1346 -0.3663 0.033
Uiso 1 calc R . 
H31B H 0.1454 -0.0493 -0.4051 0.033 Uiso 1 calc R . 
C313
C 0.1282(2) -0.1750(4) -0.4498(3) 0.0248(16) Uani 1 d . . 
C314 C 0.0910(2)
-0.2409(5) -0.4533(3) 0.0323(18) Uani 1 d . . 
H31C H 0.0728 -0.2481
-0.4160 0.039 Uiso 1 calc R . 
C315 C 0.0790(3) -0.2968(5) -0.5082(4)
0.042(2) Uani 1 d . . 
H31D H 0.0527 -0.3408 -0.5085 0.050 Uiso 1 calc R .

C316 C 0.1049(3) -0.2892(5) -0.5627(4) 0.046(2) Uani 1 d . . 
H31E H
0.0969 -0.3286 -0.6004 0.056 Uiso 1 calc R . 
C317 C 0.1423(3) -0.2248(5)
-0.5626(4) 0.042(2) Uani 1 d . . 
H31F H 0.1603 -0.2182 -0.6002 0.050 Uiso
1 calc R . 
C318 C 0.1533(2) -0.1692(5) -0.5062(4) 0.0377(19) Uani 1 d . .

C401 C 0.3290(2) -0.1173(5) -0.7866(3) 0.0204(16) Uani 1 d . . 
C402 C
0.3162(2) -0.0251(5) -0.7753(3) 0.0318(18) Uani 1 d . . 
H40B H 0.3365
0.0113 -0.7434 0.038 Uiso 1 calc R . 
C403 C 0.2748(3) 0.0134(6) -0.8096(4)
0.042(2) Uani 1 d . . 
H40C H 0.2661 0.0759 -0.8005 0.050 Uiso 1 calc R .

C404 C 0.2454(3) -0.0369(6) -0.8572(4) 0.049(2) Uani 1 d . . 
H40D H
0.2171 -0.0091 -0.8820 0.059 Uiso 1 calc R . 
C405 C 0.2577(3) -0.1292(6)
-0.8685(4) 0.048(2) Uani 1 d . . 
H40E H 0.2371 -0.1650 -0.9005 0.057 Uiso
1 calc R . 
C406 C 0.2989(2) -0.1690(5) -0.8341(3) 0.0364(19) Uani 1 d . .

H40F H 0.3071 -0.2320 -0.8426 0.044 Uiso 1 calc R . 
C407 C 0.4500(3)
-0.0413(5) -0.7320(3) 0.039(2) Uani 1 d . . 
C408 C 0.4326(2) -0.0514(5)
-0.6619(3) 0.0285(18) Uani 1 d . . 
H40A H 0.4174 0.0094 -0.6509 0.034 Uiso
1 calc R . 
C409 C 0.4739(2) -0.0736(5) -0.6048(3) 0.0336(18) Uani 1 d . .

H40G H 0.4575 -0.0802 -0.5630 0.040 Uiso 1 calc R . 
C410 C 0.5099(3)
0.0085(5) -0.5942(4) 0.052(2) Uani 1 d . . 
H41A H 0.5349 -0.0044 -0.5560
0.079 Uiso 1 calc R . 
H41B H 0.4914 0.0650 -0.5853 0.079 Uiso 1 calc R .

H41C H 0.5265 0.0176 -0.6345 0.079 Uiso 1 calc R . 
C411 C 0.5004(3)
-0.1640(5) -0.6146(4) 0.052(2) Uani 1 d . . 
H41D H 0.5200 -0.1822 -0.5726
0.077 Uiso 1 calc R . 
H41E H 0.5225 -0.1560 -0.6494 0.077 Uiso 1 calc R .

H41F H 0.4758 -0.2127 -0.6283 0.077 Uiso 1 calc R . 
C412 C 0.3539(2)
-0.1184(5) -0.6229(3) 0.0328(19) Uani 1 d . . 
H41G H 0.3223 -0.1406
-0.6475 0.039 Uiso 1 calc R . 
H41H H 0.3490 -0.0527 -0.6101 0.039 Uiso 1
calc R . 
C413 C 0.3648(2) -0.1755(5) -0.5598(3) 0.0255(16) Uani 1 d . .

C414 C 0.3780(2) -0.2681(5) -0.5631(3) 0.0365(17) Uani 1 d . . 
H41I H
0.3829 -0.2944 -0.6051 0.044 Uiso 1 calc R . 
C415 C 0.3843(2) -0.3233(6)
-0.5068(4) 0.045(2) Uani 1 d . . 
H41J H 0.3928 -0.3872 -0.5108 0.054 Uiso
1 calc R . 
C416 C 0.3786(3) -0.2880(7) -0.4463(4) 0.051(2) Uani 1 d . .

H41K H 0.3837 -0.3268 -0.4078 0.061 Uiso 1 calc R . 
C417 C 0.3659(3)
-0.1985(7) -0.4396(4) 0.045(2) Uani 1 d . . 
H41L H 0.3618 -0.1738 -0.3968
0.054 Uiso 1 calc R . 
C418 C 0.3587(2) -0.1422(5) -0.4962(4) 0.0337(19)
Uani 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 
Br1 0.0581(6) 0.0607(7)
0.0402(6) 0.0165(4) 0.0092(4) -0.0055(5) 
Br2 0.0920(8) 0.1061(10)
0.0685(8) 0.0377(6) 0.0533(6) 0.0615(7) 
Br3 0.0763(7) 0.0909(9) 0.0542(7)
-0.0178(5) 0.0356(5) -0.0439(6) 
Br4 0.0593(6) 0.0589(7) 0.0440(6)
-0.0222(4) 0.0068(4) 0.0031(5) 
P1 0.0271(10) 0.0214(11) 0.0253(11)
0.0016(9) 0.0045(8) -0.0005(8) 
P2 0.0329(11) 0.0205(11) 0.0255(12)
-0.0034(9) 0.0070(8) -0.0001(9) 
P3 0.0335(11) 0.0187(11) 0.0311(12)
0.0010(9) 0.0089(8) -0.0012(9) 
P4 0.0294(10) 0.0181(11) 0.0222(11)
-0.0012(9) 0.0059(8) 0.0024(8) 
O11 0.036(3) 0.036(3) 0.029(3) 0.006(2)
0.013(2) 0.001(2) 
O21 0.032(3) 0.027(3) 0.026(3) -0.005(2) 0.014(2)
-0.001(2) 
O31 0.027(3) 0.033(3) 0.032(3) 0.003(2) 0.015(2) -0.005(2) 
O41
0.029(3) 0.029(3) 0.025(3) -0.002(2) 0.010(2) 0.000(2) 
N11 0.026(3)
0.025(3) 0.015(3) 0.002(3) 0.004(2) 0.004(3) 
N21 0.031(3) 0.025(3)
0.015(3) -0.001(3) 0.003(2) -0.004(3) 
N31 0.028(3) 0.022(3) 0.027(3)
-0.006(3) 0.009(2) -0.003(3) 
N41 0.024(3) 0.023(3) 0.028(3) -0.001(3)
0.007(2) -0.001(2) 
B1 0.046(6) 0.022(5) 0.057(6) 0.000(4) 0.002(4)
-0.004(4) 
B2 0.058(6) 0.018(5) 0.062(7) -0.004(4) 0.022(5) -0.005(4) 
B3
0.052(6) 0.022(5) 0.049(6) 0.000(4) 0.010(4) -0.007(4) 
B4 0.060(6)
0.013(5) 0.037(6) -0.002(4) 0.005(4) 0.001(4) 
C101 0.034(4) 0.029(4)
0.013(4) 0.001(3) 0.003(3) 0.001(3) 
C102 0.038(4) 0.032(5) 0.028(5)
0.002(4) 0.006(3) -0.003(4) 
C103 0.052(5) 0.040(5) 0.038(5) -0.001(4)
0.004(4) -0.018(4) 
C104 0.039(5) 0.071(7) 0.054(6) 0.004(5) -0.013(4)
-0.015(5) 
C105 0.051(5) 0.050(6) 0.050(6) 0.013(5) -0.009(4) -0.001(4)

C106 0.037(5) 0.043(5) 0.032(5) 0.007(4) -0.004(3) -0.004(4) 
C107
0.039(4) 0.030(5) 0.030(5) -0.005(4) 0.004(3) 0.008(3) 
C108 0.025(4)
0.033(5) 0.022(4) 0.001(3) 0.006(3) 0.014(3) 
C109 0.032(4) 0.024(4)
0.040(5) 0.001(4) -0.002(3) 0.004(3) 
C110 0.028(4) 0.054(6) 0.063(6)
-0.005(5) -0.005(4) 0.004(4) 
C111 0.043(5) 0.053(6) 0.048(5) 0.012(5)
0.001(4) 0.013(4) 
C112 0.038(4) 0.037(5) 0.017(4) -0.014(3) 0.014(3)
-0.007(3) 
C113 0.017(4) 0.038(5) 0.027(4) 0.002(4) 0.003(3) 0.008(3) 
C114
0.041(4) 0.039(5) 0.027(4) -0.006(4) 0.001(3) 0.002(4) 
C115 0.050(5)
0.047(5) 0.042(6) -0.004(5) -0.001(4) 0.009(4) 
C116 0.052(6) 0.071(8)
0.041(6) -0.033(5) -0.005(4) 0.006(5) 
C117 0.045(5) 0.087(8) 0.021(5)
-0.004(5) 0.015(4) 0.007(5) 
C118 0.035(4) 0.044(5) 0.028(5) 0.002(4)
0.003(3) 0.004(3) 
C201 0.023(4) 0.033(5) 0.032(5) -0.007(4) 0.010(3)
-0.005(3) 
C202 0.030(4) 0.045(6) 0.028(5) -0.007(4) 0.004(3) -0.001(4)

C203 0.039(5) 0.058(6) 0.034(5) -0.011(5) 0.004(4) 0.011(4) 
C204 0.031(5)
0.095(8) 0.041(6) -0.006(5) -0.001(4) 0.009(5) 
C205 0.044(5) 0.073(7)
0.044(6) -0.024(5) 0.001(4) -0.010(5) 
C206 0.037(5) 0.041(5) 0.037(5)
-0.017(4) 0.010(4) -0.009(4) 
C207 0.034(4) 0.026(5) 0.038(5) 0.009(4)
0.003(3) -0.001(3) 
C208 0.034(4) 0.024(5) 0.020(4) 0.003(3) 0.009(3)
-0.004(3) 
C209 0.024(4) 0.038(5) 0.032(5) -0.002(4) -0.008(3) -0.009(3)

C210 0.054(5) 0.064(6) 0.031(5) 0.001(4) -0.003(4) -0.035(4) 
C211
0.046(5) 0.065(6) 0.052(6) 0.017(5) 0.003(4) -0.002(5) 
C212 0.023(4)
0.032(5) 0.029(4) -0.001(4) 0.006(3) 0.002(3) 
C213 0.026(4) 0.030(4)
0.023(4) 0.001(3) 0.007(3) -0.010(3) 
C214 0.045(5) 0.044(5) 0.027(4)
0.007(4) 0.017(3) 0.006(4) 
C215 0.045(5) 0.044(5) 0.050(6) 0.014(4)
0.019(4) 0.008(4) 
C216 0.056(5) 0.037(5) 0.030(5) 0.018(4) 0.006(4)
-0.004(4) 
C217 0.049(5) 0.055(6) 0.037(5) 0.004(4) 0.022(4) -0.005(4)

C218 0.038(4) 0.042(5) 0.036(5) 0.011(4) 0.005(3) 0.008(4) 
C301 0.030(4)
0.043(5) 0.018(4) -0.001(4) 0.005(3) 0.004(4) 
C302 0.035(4) 0.034(5)
0.036(5) 0.005(4) 0.004(3) -0.002(4) 
C303 0.043(5) 0.059(6) 0.046(6)
0.005(5) -0.002(4) -0.019(5) 
C304 0.035(5) 0.092(8) 0.036(5) 0.005(5)
-0.001(4) -0.016(5) 
C305 0.042(5) 0.080(7) 0.048(6) 0.012(5) -0.003(4)
0.003(5) 
C306 0.050(5) 0.037(5) 0.049(6) 0.011(4) 0.004(4) 0.010(4) 
C307
0.039(4) 0.018(4) 0.026(4) 0.005(3) 0.013(3) 0.001(3) 
C308 0.036(4)
0.024(4) 0.024(4) -0.006(3) 0.004(3) 0.011(3) 
C309 0.030(4) 0.033(5)
0.028(4) 0.000(4) -0.006(3) 0.003(3) 
C310 0.035(5) 0.064(6) 0.053(6)
-0.016(5) -0.001(4) -0.003(4) 
C311 0.045(5) 0.055(6) 0.041(5) 0.006(4)
0.005(4) 0.022(4) 
C312 0.035(4) 0.026(5) 0.023(4) -0.001(3) 0.011(3)
0.000(3) 
C313 0.035(4) 0.019(4) 0.021(4) -0.005(3) 0.006(3) 0.010(3) 
C314
0.044(5) 0.022(4) 0.032(4) -0.008(3) 0.011(3) -0.005(3) 
C315 0.051(5)
0.019(4) 0.056(6) -0.018(4) 0.004(4) -0.006(4) 
C316 0.054(5) 0.049(6)
0.035(5) -0.018(4) 0.003(4) 0.009(4) 
C317 0.050(5) 0.051(6) 0.026(5)
-0.014(4) 0.013(4) 0.008(4) 
C318 0.029(4) 0.038(5) 0.045(5) -0.002(4)
0.003(4) 0.002(4) 
C401 0.020(4) 0.021(4) 0.021(4) 0.005(3) 0.007(3)
0.003(3) 
C402 0.041(4) 0.024(5) 0.031(5) -0.002(4) 0.004(3) 0.000(4) 
C403
0.041(5) 0.043(5) 0.043(5) 0.003(4) 0.007(4) 0.014(4) 
C404 0.038(5)
0.052(6) 0.056(6) -0.004(5) 0.004(4) 0.015(4) 
C405 0.034(5) 0.066(6)
0.040(5) -0.014(5) -0.010(4) -0.001(4) 
C406 0.036(4) 0.033(5) 0.040(5)
-0.004(4) 0.005(4) 0.001(4) 
C407 0.062(5) 0.036(6) 0.020(4) -0.012(4)
0.016(3) -0.009(4) 
C408 0.035(4) 0.012(4) 0.037(5) -0.001(3) 0.002(3)
-0.002(3) 
C409 0.041(5) 0.033(5) 0.026(4) 0.005(4) -0.003(3) -0.004(4)

C410 0.058(6) 0.049(6) 0.047(5) -0.011(5) -0.010(4) -0.022(4) 
C411
0.040(5) 0.041(5) 0.069(6) 0.010(4) -0.017(4) 0.004(4) 
C412 0.034(4)
0.035(5) 0.031(5) -0.005(4) 0.014(3) -0.002(3) 
C413 0.016(3) 0.036(5)
0.025(4) 0.009(4) 0.003(3) -0.008(3) 
C414 0.041(4) 0.043(5) 0.026(4)
-0.001(4) 0.007(3) 0.002(4) 
C415 0.048(5) 0.037(5) 0.049(6) 0.015(4)
0.002(4) -0.006(4) 
C416 0.056(5) 0.075(8) 0.023(5) 0.024(5) 0.006(4)
-0.007(5) 
C417 0.042(5) 0.081(7) 0.012(4) 0.004(4) 0.007(3) -0.011(5)

C418 0.021(4) 0.040(5) 0.041(5) -0.011(4) 0.005(3) -0.011(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

Br1 C118 1.914(7) . ? 
Br2 C218 1.911(7) . ? 
Br3 C318 1.914(7) . ? 
Br4
C418 1.918(7) . ? 
P1 O11 1.597(5) . ? 
P1 N11 1.655(5) . ? 
P1 C101
1.814(7) . ? 
P1 B1 1.898(9) . ? 
P2 O21 1.593(4) . ? 
P2 N21 1.653(5) . ?

P2 C201 1.804(7) . ? 
P2 B2 1.893(9) . ? 
P3 O31 1.602(4) . ? 
P3 N31
1.669(5) . ? 
P3 C301 1.813(7) . ? 
P3 B3 1.882(8) . ? 
P4 O41 1.589(4) . ?

P4 N41 1.647(5) . ? 
P4 C401 1.815(6) . ? 
P4 B4 1.881(8) . ? 
O11 C107
1.434(7) . ? 
O21 C207 1.457(7) . ? 
O31 C307 1.469(7) . ? 
O41 C407
1.473(7) . ? 
N11 C112 1.465(7) . ? 
N11 C108 1.480(7) . ? 
N21 C212
1.475(7) . ? 
N21 C208 1.488(7) . ? 
N31 C312 1.454(7) . ? 
N31 C308
1.497(8) . ? 
N41 C412 1.467(7) . ? 
N41 C408 1.468(7) . ? 
C101 C106
1.380(9) . ? 
C101 C102 1.405(9) . ? 
C102 C103 1.375(9) . ? 
C103 C104
1.378(10) . ? 
C104 C105 1.383(10) . ? 
C105 C106 1.370(9) . ? 
C107 C108
1.521(9) . ? 
C108 C109 1.545(9) . ? 
C109 C111 1.529(9) . ? 
C109 C110
1.544(10) . ? 
C112 C113 1.515(9) . ? 
C113 C118 1.392(9) . ? 
C113 C114
1.396(9) . ? 
C114 C115 1.370(9) . ? 
C115 C116 1.360(10) . ? 
C116 C117
1.377(11) . ? 
C117 C118 1.385(10) . ? 
C201 C206 1.375(9) . ? 
C201 C202
1.400(9) . ? 
C202 C203 1.392(9) . ? 
C203 C204 1.382(11) . ? 
C204 C205
1.357(11) . ? 
C205 C206 1.379(10) . ? 
C207 C208 1.522(9) . ? 
C208 C209
1.559(8) . ? 
C209 C211 1.521(10) . ? 
C209 C210 1.532(9) . ? 
C212 C213
1.529(8) . ? 
C213 C218 1.364(9) . ? 
C213 C214 1.375(8) . ? 
C214 C215
1.383(9) . ? 
C215 C216 1.367(9) . ? 
C216 C217 1.376(10) . ? 
C217 C218
1.386(9) . ? 
C301 C302 1.390(9) . ? 
C301 C306 1.393(9) . ? 
C302 C303
1.363(9) . ? 
C303 C304 1.361(11) . ? 
C304 C305 1.390(12) . ? 
C305 C306
1.402(10) . ? 
C307 C308 1.558(9) . ? 
C308 C309 1.553(8) . ? 
C309 C310
1.510(9) . ? 
C309 C311 1.544(9) . ? 
C312 C313 1.503(8) . ? 
C313 C314
1.375(8) . ? 
C313 C318 1.391(9) . ? 
C314 C315 1.373(8) . ? 
C315 C316
1.373(10) . ? 
C316 C317 1.368(10) . ? 
C317 C318 1.391(9) . ? 
C401 C402
1.393(9) . ? 
C401 C406 1.395(9) . ? 
C402 C403 1.361(9) . ? 
C403 C404
1.376(10) . ? 
C404 C405 1.389(10) . ? 
C405 C406 1.366(9) . ? 
C407 C408
1.546(9) . ? 
C408 C409 1.537(8) . ? 
C409 C411 1.506(10) . ? 
C409 C410
1.527(10) . ? 
C412 C413 1.510(8) . ? 
C413 C414 1.379(9) . ? 
C413 C418
1.395(9) . ? 
C414 C415 1.375(9) . ? 
C415 C416 1.346(10) . ? 
C416 C417
1.339(11) . ? 
C417 C418 1.390(10) . ? 

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 
O11 P1 N11 95.4(2) . .
? 
O11 P1 C101 109.1(3) . . ? 
N11 P1 C101 107.6(3) . . ? 
O11 P1 B1
111.5(3) . . ? 
N11 P1 B1 119.4(3) . . ? 
C101 P1 B1 112.4(4) . . ? 
O21 P2
N21 95.5(2) . . ? 
O21 P2 C201 108.6(3) . . ? 
N21 P2 C201 107.1(3) . . ?

O21 P2 B2 112.3(3) . . ? 
N21 P2 B2 118.0(4) . . ? 
C201 P2 B2 113.6(4) .
. ? 
O31 P3 N31 94.9(2) . . ? 
O31 P3 C301 108.3(3) . . ? 
N31 P3 C301
106.6(3) . . ? 
O31 P3 B3 112.9(3) . . ? 
N31 P3 B3 118.6(3) . . ? 
C301 P3
B3 113.7(4) . . ? 
O41 P4 N41 95.5(2) . . ? 
O41 P4 C401 109.1(3) . . ?

N41 P4 C401 106.2(3) . . ? 
O41 P4 B4 111.7(3) . . ? 
N41 P4 B4 119.1(3) .
. ? 
C401 P4 B4 113.5(3) . . ? 
C107 O11 P1 111.8(4) . . ? 
C207 O21 P2
110.0(4) . . ? 
C307 O31 P3 111.5(4) . . ? 
C407 O41 P4 113.3(4) . . ?

C112 N11 C108 117.8(5) . . ? 
C112 N11 P1 124.2(4) . . ? 
C108 N11 P1
113.8(4) . . ? 
C212 N21 C208 117.9(5) . . ? 
C212 N21 P2 122.5(4) . . ?

C208 N21 P2 113.5(4) . . ? 
C312 N31 C308 118.8(5) . . ? 
C312 N31 P3
124.0(4) . . ? 
C308 N31 P3 113.2(4) . . ? 
C412 N41 C408 119.9(5) . . ?

C412 N41 P4 123.1(4) . . ? 
C408 N41 P4 113.2(4) . . ? 
C106 C101 C102
118.9(6) . . ? 
C106 C101 P1 119.7(6) . . ? 
C102 C101 P1 121.4(5) . . ?

C103 C102 C101 120.1(7) . . ? 
C102 C103 C104 120.0(8) . . ? 
C103 C104
C105 120.1(7) . . ? 
C106 C105 C104 120.2(8) . . ? 
C105 C106 C101 120.7(7)
. . ? 
O11 C107 C108 110.1(5) . . ? 
N11 C108 C107 103.7(5) . . ? 
N11 C108
C109 111.1(5) . . ? 
C107 C108 C109 115.7(5) . . ? 
C111 C109 C110 109.6(5)
. . ? 
C111 C109 C108 108.9(6) . . ? 
C110 C109 C108 113.2(6) . . ? 
N11
C112 C113 113.3(5) . . ? 
C118 C113 C114 115.5(6) . . ? 
C118 C113 C112
122.4(7) . . ? 
C114 C113 C112 121.7(6) . . ? 
C115 C114 C113 121.9(7) . .
? 
C116 C115 C114 121.2(8) . . ? 
C115 C116 C117 119.4(8) . . ? 
C116 C117
C118 119.1(7) . . ? 
C117 C118 C113 122.9(7) . . ? 
C117 C118 Br1 117.3(6)
. . ? 
C113 C118 Br1 119.7(6) . . ? 
C206 C201 C202 118.9(6) . . ? 
C206
C201 P2 120.6(6) . . ? 
C202 C201 P2 120.5(5) . . ? 
C203 C202 C201
120.5(7) . . ? 
C204 C203 C202 118.7(8) . . ? 
C205 C204 C203 120.8(8) . .
? 
C204 C205 C206 120.7(8) . . ? 
C201 C206 C205 120.3(7) . . ? 
O21 C207
C208 110.0(5) . . ? 
N21 C208 C207 103.4(5) . . ? 
N21 C208 C209 110.6(5) .
. ? 
C207 C208 C209 115.3(5) . . ? 
C211 C209 C210 110.8(6) . . ? 
C211
C209 C208 112.0(6) . . ? 
C210 C209 C208 108.6(6) . . ? 
N21 C212 C213
114.2(5) . . ? 
C218 C213 C214 116.9(6) . . ? 
C218 C213 C212 121.5(6) . .
? 
C214 C213 C212 121.6(6) . . ? 
C213 C214 C215 120.9(6) . . ? 
C216 C215
C214 121.7(7) . . ? 
C215 C216 C217 118.2(7) . . ? 
C216 C217 C218 119.5(7)
. . ? 
C213 C218 C217 123.0(7) . . ? 
C213 C218 Br2 119.8(5) . . ? 
C217
C218 Br2 117.1(5) . . ? 
C302 C301 C306 118.7(6) . . ? 
C302 C301 P3
122.3(6) . . ? 
C306 C301 P3 119.0(6) . . ? 
C303 C302 C301 120.1(7) . . ?

C304 C303 C302 122.2(9) . . ? 
C303 C304 C305 119.5(8) . . ? 
C304 C305
C306 119.1(8) . . ? 
C301 C306 C305 120.5(8) . . ? 
O31 C307 C308 106.7(5)
. . ? 
N31 C308 C309 110.7(5) . . ? 
N31 C308 C307 104.2(5) . . ? 
C309
C308 C307 116.1(5) . . ? 
C310 C309 C311 109.9(6) . . ? 
C310 C309 C308
113.2(6) . . ? 
C311 C309 C308 108.2(6) . . ? 
N31 C312 C313 115.8(5) . . ?

C314 C313 C318 115.0(6) . . ? 
C314 C313 C312 122.6(6) . . ? 
C318 C313
C312 122.3(6) . . ? 
C315 C314 C313 123.0(6) . . ? 
C316 C315 C314 120.2(7)
. . ? 
C317 C316 C315 119.8(7) . . ? 
C316 C317 C318 118.4(7) . . ? 
C313
C318 C317 123.6(7) . . ? 
C313 C318 Br3 118.8(5) . . ? 
C317 C318 Br3
117.4(6) . . ? 
C402 C401 C406 118.7(6) . . ? 
C402 C401 P4 121.9(5) . . ?

C406 C401 P4 119.4(5) . . ? 
C403 C402 C401 120.6(7) . . ? 
C402 C403 C404
120.9(8) . . ? 
C403 C404 C405 118.9(7) . . ? 
C406 C405 C404 120.8(7) . .
? 
C405 C406 C401 120.0(7) . . ? 
O41 C407 C408 105.2(5) . . ? 
N41 C408
C409 112.7(5) . . ? 
N41 C408 C407 106.5(5) . . ? 
C409 C408 C407 115.5(6)
. . ? 
C411 C409 C410 112.2(6) . . ? 
C411 C409 C408 113.2(6) . . ? 
C410
C409 C408 109.8(6) . . ? 
N41 C412 C413 115.1(5) . . ? 
C414 C413 C418
115.6(6) . . ? 
C414 C413 C412 120.6(6) . . ? 
C418 C413 C412 123.6(7) . .
? 
C415 C414 C413 121.6(7) . . ? 
C416 C415 C414 120.8(8) . . ? 
C417 C416
C415 120.6(8) . . ? 
C416 C417 C418 119.2(7) . . ? 
C417 C418 C413 122.2(7)
. . ? 
C417 C418 Br4 117.8(6) . . ? 
C413 C418 Br4 119.9(6) . . ? 

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 
N11 P1 O11 C107
-19.1(5) . . . . ? 
C101 P1 O11 C107 91.6(5) . . . . ? 
B1 P1 O11 C107
-143.6(5) . . . . ? 
N21 P2 O21 C207 -25.4(4) . . . . ? 
C201 P2 O21 C207
84.7(4) . . . . ? 
B2 P2 O21 C207 -148.8(5) . . . . ? 
N31 P3 O31 C307
-27.5(4) . . . . ? 
C301 P3 O31 C307 81.8(5) . . . . ? 
B3 P3 O31 C307
-151.4(4) . . . . ? 
N41 P4 O41 C407 -21.7(5) . . . . ? 
C401 P4 O41 C407
87.5(5) . . . . ? 
B4 P4 O41 C407 -146.0(5) . . . . ? 
O11 P1 N11 C112
163.9(5) . . . . ? 
C101 P1 N11 C112 51.9(6) . . . . ? 
B1 P1 N11 C112
-77.7(6) . . . . ? 
O11 P1 N11 C108 7.4(5) . . . . ? 
C101 P1 N11 C108
-104.6(5) . . . . ? 
B1 P1 N11 C108 125.8(5) . . . . ? 
O21 P2 N21 C212
166.7(5) . . . . ? 
C201 P2 N21 C212 55.3(6) . . . . ? 
B2 P2 N21 C212
-74.4(6) . . . . ? 
O21 P2 N21 C208 14.8(4) . . . . ? 
C201 P2 N21 C208
-96.6(5) . . . . ? 
B2 P2 N21 C208 133.7(5) . . . . ? 
O31 P3 N31 C312
170.3(5) . . . . ? 
C301 P3 N31 C312 59.6(6) . . . . ? 
B3 P3 N31 C312
-70.2(6) . . . . ? 
O31 P3 N31 C308 13.1(4) . . . . ? 
C301 P3 N31 C308
-97.6(5) . . . . ? 
B3 P3 N31 C308 132.6(5) . . . . ? 
O41 P4 N41 C412
166.3(5) . . . . ? 
C401 P4 N41 C412 54.6(6) . . . . ? 
B4 P4 N41 C412
-75.0(6) . . . . ? 
O41 P4 N41 C408 8.7(4) . . . . ? 
C401 P4 N41 C408
-103.1(4) . . . . ? 
B4 P4 N41 C408 127.3(5) . . . . ? 
O11 P1 C101 C106
108.0(6) . . . . ? 
N11 P1 C101 C106 -149.6(6) . . . . ? 
B1 P1 C101 C106
-16.2(7) . . . . ? 
O11 P1 C101 C102 -72.9(6) . . . . ? 
N11 P1 C101 C102
29.5(6) . . . . ? 
B1 P1 C101 C102 162.9(6) . . . . ? 
C106 C101 C102
C103 -2.4(11) . . . . ? 
P1 C101 C102 C103 178.4(5) . . . . ? 
C101 C102
C103 C104 1.9(12) . . . . ? 
C102 C103 C104 C105 0.0(13) . . . . ? 
C103
C104 C105 C106 -1.5(14) . . . . ? 
C104 C105 C106 C101 0.9(13) . . . . ? 

C102 C101 C106 C105 1.0(11) . . . . ? 
P1 C101 C106 C105 -179.9(6) . . . .
? 
P1 O11 C107 C108 25.2(6) . . . . ? 
C112 N11 C108 C107 -152.6(5) . . .
. ? 
P1 N11 C108 C107 5.5(6) . . . . ? 
C112 N11 C108 C109 82.5(7) . . .
. ? 
P1 N11 C108 C109 -119.4(5) . . . . ? 
O11 C107 C108 N11 -18.4(7) . .
. . ? 
O11 C107 C108 C109 103.6(6) . . . . ? 
N11 C108 C109 C111
-173.1(5) . . . . ? 
C107 C108 C109 C111 69.1(8) . . . . ? 
N11 C108 C109
C110 64.7(7) . . . . ? 
C107 C108 C109 C110 -53.2(8) . . . . ? 
C108 N11
C112 C113 -96.4(7) . . . . ? 
P1 N11 C112 C113 108.0(6) . . . . ? 
N11
C112 C113 C118 145.4(6) . . . . ? 
N11 C112 C113 C114 -42.3(8) . . . . ? 

C118 C113 C114 C115 0.3(10) . . . . ? 
C112 C113 C114 C115 -172.5(6) . . .
. ? 
C113 C114 C115 C116 -1.3(11) . . . . ? 
C114 C115 C116 C117 1.0(12)
. . . . ? 
C115 C116 C117 C118 0.3(12) . . . . ? 
C116 C117 C118 C113
-1.4(11) . . . . ? 
C116 C117 C118 Br1 -178.0(6) . . . . ? 
C114 C113
C118 C117 1.1(10) . . . . ? 
C112 C113 C118 C117 173.8(6) . . . . ? 
C114
C113 C118 Br1 177.7(5) . . . . ? 
C112 C113 C118 Br1 -9.6(8) . . . . ? 

O21 P2 C201 C206 105.7(6) . . . . ? 
N21 P2 C201 C206 -152.2(6) . . . . ?

B2 P2 C201 C206 -20.1(7) . . . . ? 
O21 P2 C201 C202 -73.7(6) . . . . ?

N21 P2 C201 C202 28.3(6) . . . . ? 
B2 P2 C201 C202 160.5(6) . . . . ? 

C206 C201 C202 C203 -0.8(10) . . . . ? 
P2 C201 C202 C203 178.7(5) . . . .
? 
C201 C202 C203 C204 -0.2(11) . . . . ? 
C202 C203 C204 C205 1.1(13) .
. . . ? 
C203 C204 C205 C206 -0.9(14) . . . . ? 
C202 C201 C206 C205
0.9(11) . . . . ? 
P2 C201 C206 C205 -178.6(6) . . . . ? 
C204 C205 C206
C201 -0.1(12) . . . . ? 
P2 O21 C207 C208 29.2(6) . . . . ? 
C212 N21
C208 C207 -153.1(5) . . . . ? 
P2 N21 C208 C207 0.2(6) . . . . ? 
C212
N21 C208 C209 82.9(6) . . . . ? 
P2 N21 C208 C209 -123.8(5) . . . . ? 

O21 C207 C208 N21 -17.5(6) . . . . ? 
O21 C207 C208 C209 103.3(6) . . . .
? 
N21 C208 C209 C211 69.7(7) . . . . ? 
C207 C208 C209 C211 -47.2(8) . .
. . ? 
N21 C208 C209 C210 -167.6(5) . . . . ? 
C207 C208 C209 C210
75.5(7) . . . . ? 
C208 N21 C212 C213 -104.8(6) . . . . ? 
P2 N21 C212
C213 104.5(6) . . . . ? 
N21 C212 C213 C218 166.5(6) . . . . ? 
N21 C212
C213 C214 -15.0(9) . . . . ? 
C218 C213 C214 C215 0.3(10) . . . . ? 
C212
C213 C214 C215 -178.4(6) . . . . ? 
C213 C214 C215 C216 -0.9(11) . . . . ?

C214 C215 C216 C217 0.9(12) . . . . ? 
C215 C216 C217 C218 -0.4(11) . .
. . ? 
C214 C213 C218 C217 0.3(11) . . . . ? 
C212 C213 C218 C217
178.9(6) . . . . ? 
C214 C213 C218 Br2 -175.1(5) . . . . ? 
C212 C213
C218 Br2 3.5(9) . . . . ? 
C216 C217 C218 C213 -0.2(11) . . . . ? 
C216
C217 C218 Br2 175.3(6) . . . . ? 
O31 P3 C301 C302 -73.9(6) . . . . ? 

N31 P3 C301 C302 27.2(7) . . . . ? 
B3 P3 C301 C302 159.7(6) . . . . ? 

O31 P3 C301 C306 104.6(6) . . . . ? 
N31 P3 C301 C306 -154.3(6) . . . . ?

B3 P3 C301 C306 -21.7(7) . . . . ? 
C306 C301 C302 C303 -1.0(11) . . . .
? 
P3 C301 C302 C303 177.5(6) . . . . ? 
C301 C302 C303 C304 1.4(13) . .
. . ? 
C302 C303 C304 C305 -0.9(13) . . . . ? 
C303 C304 C305 C306
0.0(13) . . . . ? 
C302 C301 C306 C305 0.2(11) . . . . ? 
P3 C301 C306
C305 -178.4(6) . . . . ? 
C304 C305 C306 C301 0.3(12) . . . . ? 
P3 O31
C307 C308 33.0(6) . . . . ? 
C312 N31 C308 C309 80.0(7) . . . . ? 
P3 N31
C308 C309 -121.5(5) . . . . ? 
C312 N31 C308 C307 -154.5(5) . . . . ? 
P3
N31 C308 C307 4.0(6) . . . . ? 
O31 C307 C308 N31 -21.7(6) . . . . ? 
O31
C307 C308 C309 100.3(6) . . . . ? 
N31 C308 C309 C310 71.8(7) . . . . ? 

C307 C308 C309 C310 -46.8(8) . . . . ? 
N31 C308 C309 C311 -166.2(5) . . .
. ? 
C307 C308 C309 C311 75.3(7) . . . . ? 
C308 N31 C312 C313 -102.7(6)
. . . . ? 
P3 N31 C312 C313 101.3(6) . . . . ? 
N31 C312 C313 C314
-13.6(9) . . . . ? 
N31 C312 C313 C318 166.5(6) . . . . ? 
C318 C313 C314
C315 -0.3(10) . . . . ? 
C312 C313 C314 C315 179.8(6) . . . . ? 
C313
C314 C315 C316 0.8(11) . . . . ? 
C314 C315 C316 C317 -1.0(11) . . . . ? 

C315 C316 C317 C318 0.7(11) . . . . ? 
C314 C313 C318 C317 0.1(10) . . . .
? 
C312 C313 C318 C317 179.9(6) . . . . ? 
C314 C313 C318 Br3 -175.5(5) .
. . . ? 
C312 C313 C318 Br3 4.3(9) . . . . ? 
C316 C317 C318 C313
-0.3(11) . . . . ? 
C316 C317 C318 Br3 175.3(5) . . . . ? 
O41 P4 C401
C402 -70.2(6) . . . . ? 
N41 P4 C401 C402 31.7(6) . . . . ? 
B4 P4 C401
C402 164.4(6) . . . . ? 
O41 P4 C401 C406 108.5(5) . . . . ? 
N41 P4 C401
C406 -149.6(5) . . . . ? 
B4 P4 C401 C406 -16.9(7) . . . . ? 
C406 C401
C402 C403 0.6(11) . . . . ? 
P4 C401 C402 C403 179.3(6) . . . . ? 
C401
C402 C403 C404 -1.5(12) . . . . ? 
C402 C403 C404 C405 2.0(12) . . . . ? 

C403 C404 C405 C406 -1.5(12) . . . . ? 
C404 C405 C406 C401 0.6(12) . . .
. ? 
C402 C401 C406 C405 -0.2(10) . . . . ? 
P4 C401 C406 C405 -178.9(6)
. . . . ? 
P4 O41 C407 C408 27.0(6) . . . . ? 
C412 N41 C408 C409 79.7(7)
. . . . ? 
P4 N41 C408 C409 -121.9(5) . . . . ? 
C412 N41 C408 C407
-152.6(6) . . . . ? 
P4 N41 C408 C407 5.8(6) . . . . ? 
O41 C407 C408 N41
-19.2(7) . . . . ? 
O41 C407 C408 C409 106.8(6) . . . . ? 
N41 C408 C409
C411 62.3(8) . . . . ? 
C407 C408 C409 C411 -60.5(8) . . . . ? 
N41 C408
C409 C410 -171.5(6) . . . . ? 
C407 C408 C409 C410 65.8(8) . . . . ? 

C408 N41 C412 C413 -91.3(7) . . . . ? 
P4 N41 C412 C413 112.5(6) . . . . ?

N41 C412 C413 C414 -52.0(8) . . . . ? 
N41 C412 C413 C418 133.2(6) . . .
. ? 
C418 C413 C414 C415 0.3(9) . . . . ? 
C412 C413 C414 C415 -174.9(6)
. . . . ? 
C413 C414 C415 C416 -1.2(10) . . . . ? 
C414 C415 C416 C417
1.1(11) . . . . ? 
C415 C416 C417 C418 -0.2(12) . . . . ? 
C416 C417 C418
C413 -0.8(10) . . . . ? 
C416 C417 C418 Br4 -177.7(6) . . . . ? 
C414
C413 C418 C417 0.7(9) . . . . ? 
C412 C413 C418 C417 175.7(6) . . . . ? 

C414 C413 C418 Br4 177.5(4) . . . . ? 
C412 C413 C418 Br4 -7.5(8) . . . .
? 

_refine_diff_density_max    1.043 
_refine_diff_density_min   -0.927

_refine_diff_density_rms    0.076