# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_I-Urea_L

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H10 I2 N2 O'
_chemical_formula_sum            'C13 H10 I2 N2 O'
_chemical_formula_weight         464.03

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_symmetry_space_group_name_Hall  '-C 2yc'
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                   29.2420(9)
_cell_length_b                   4.64140(10)
_cell_length_c                   10.1031(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.122(2)
_cell_angle_gamma                90.00
_cell_volume                     1367.68(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5600
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864.0
_exptl_absorpt_coefficient_mu    4.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9542
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         28.30
_reflns_number_total             1694
_reflns_number_gt                1541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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+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    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1694
_refine_ls_number_parameters     83
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.1052
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_restrained_S_all      0.909
_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
I1 I 0.205031(7) 0.01985(4) 0.65499(2) 0.05062(15) Uani 1 1 d . . .
C1 C 0.07132(7) 0.3864(4) 0.39087(19) 0.0304(4) Uani 1 1 d . . .
C7 C 0.0000 0.3447(6) 0.2500 0.0303(6) Uani 1 2 d S . .
C5 C 0.10419(9) 0.0721(6) 0.5619(2) 0.0387(5) Uani 1 1 d . . .
H5 H 0.1007 -0.0694 0.6256 0.046 Uiso 1 1 calc R . .
C6 C 0.06646(7) 0.1789(5) 0.4876(2) 0.0367(5) Uani 1 1 d . . .
H6 H 0.0374 0.1106 0.5027 0.044 Uiso 1 1 calc R . .
C4 C 0.14752(7) 0.1782(5) 0.5407(2) 0.0335(4) Uani 1 1 d . . .
N2 N 0.03334(9) 0.5050(3) 0.3155(3) 0.0378(6) Uani 1 1 d . . .
H2N H 0.0312 0.6895 0.3107 0.045 Uiso 1 1 calc R . .
O1 O 0.0000 0.0789(5) 0.2500 0.0436(6) Uani 1 2 d S . .
C3 C 0.15294(8) 0.3866(6) 0.4464(2) 0.0397(5) Uani 1 1 d . . .
H2 H 0.1820 0.4596 0.4342 0.048 Uiso 1 1 calc R . .
C2 C 0.11496(12) 0.4885(5) 0.3690(3) 0.0412(7) Uani 1 1 d . . .
H1 H 0.1187 0.6242 0.3029 0.049 Uiso 1 1 calc R . .


_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
I1 C4 2.103(2) . ?
C1 C6 1.387(3) . ?
C1 C2 1.394(4) . ?
C1 N2 1.413(3) . ?
C7 O1 1.234(3) . ?
C7 N2 1.360(3) . ?
C7 N2 1.360(3) 2 ?
C5 C6 1.381(3) . ?
C5 C4 1.390(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C4 C3 1.375(3) . ?
N2 H2N 0.8600 . ?
C3 C2 1.394(4) . ?
C3 H2 0.9300 . ?
C2 H1 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
C6 C1 C2 119.3(2) . . ?
C6 C1 N2 122.3(2) . . ?
C2 C1 N2 118.4(2) . . ?
O1 C7 N2 123.17(13) . . ?
O1 C7 N2 123.17(13) . 2 ?
N2 C7 N2 113.7(3) . 2 ?
C6 C5 C4 119.3(2) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.9(2) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C3 C4 C5 120.5(2) . . ?
C3 C4 I1 119.93(15) . . ?
C5 C4 I1 119.54(17) . . ?
C7 N2 C1 123.90(18) . . ?
C7 N2 H2N 118.0 . . ?
C1 N2 H2N 118.0 . . ?
C4 C3 C2 120.0(2) . . ?
C4 C3 H2 120.0 . . ?
C2 C3 H2 120.0 . . ?
C1 C2 C3 119.8(2) . . ?
C1 C2 H1 120.1 . . ?
C3 C2 H1 120.1 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.319
_refine_diff_density_min         -1.832
_refine_diff_density_rms         0.205
_database_code_depnum_ccdc_archive 'CCDC 973820'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_I-U_HCO3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H10 I2 N2 O, C16 H36 N, C H O3'
_chemical_formula_sum            'C30 H47 I2 N3 O4'
_chemical_formula_weight         767.51

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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2'
_symmetry_space_group_name_Hall  'C 2y'

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                   23.9471(7)
_cell_length_b                   8.3931(2)
_cell_length_c                   17.0344(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.4510(10)
_cell_angle_gamma                90.00
_cell_volume                     3402.07(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8754
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      23.64

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544.0
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_T_max  0.658

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19895
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         28.28
_reflns_number_total             8369
_reflns_number_gt                4629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. The following restraints
 were applied (given as SHELXL lines):
 DFIX 1.500 0.01 C28 C29  C29 C30
 DFIX 1.500 0.01 C27 C28D  C28D C29C  C29C C30C
 SIMU 0.005 C28 C29 C30 C28D C29C C30C 
;

_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)+(0.0650P)²+0.6092P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.01(3)
_refine_ls_number_reflns         6242
_refine_ls_number_parameters     384
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1203
_refine_ls_wR_factor_gt          0.1107
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.070
_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
C28 C 0.5643(7) 0.009(2) 0.3864(9) 0.104(3) Uani 0.61 1 d PDU A 1
H28A H 0.5911 -0.0601 0.4170 0.124 Uiso 0.61 1 calc PR A 1
H28B H 0.5415 -0.0566 0.3482 0.124 Uiso 0.61 1 calc PR A 1
C29 C 0.5950(8) 0.1326(17) 0.3441(9) 0.103(3) Uani 0.61 1 d PDU A 1
H29A H 0.5683 0.2082 0.3186 0.124 Uiso 0.61 1 calc PR A 1
H29B H 0.6206 0.1904 0.3822 0.124 Uiso 0.61 1 calc PR A 1
C30 C 0.6276(7) 0.0577(18) 0.2833(9) 0.107(3) Uani 0.61 1 d PDU A 1
H30A H 0.6454 0.1395 0.2556 0.161 Uiso 0.61 1 calc PR A 1
H30B H 0.6024 -0.0021 0.2465 0.161 Uiso 0.61 1 calc PR A 1
H30C H 0.6556 -0.0122 0.3090 0.161 Uiso 0.61 1 calc PR A 1
C28D C 0.5400(13) 0.010(3) 0.3666(11) 0.105(4) Uani 0.39 1 d PDU A 2
H28C H 0.5641 -0.0800 0.3822 0.126 Uiso 0.39 1 calc PR A 2
H28D H 0.5052 -0.0331 0.3406 0.126 Uiso 0.39 1 calc PR A 2
C29C C 0.5675(9) 0.102(3) 0.3053(14) 0.105(3) Uani 0.39 1 d PDU A 2
H29C H 0.5602 0.0493 0.2545 0.126 Uiso 0.39 1 calc PR A 2
H29D H 0.5518 0.2084 0.3003 0.126 Uiso 0.39 1 calc PR A 2
C30C C 0.6295(10) 0.112(4) 0.3287(17) 0.111(4) Uani 0.39 1 d PDU A 2
H30D H 0.6366 0.1661 0.3784 0.167 Uiso 0.39 1 calc PR A 2
H30E H 0.6468 0.1691 0.2891 0.167 Uiso 0.39 1 calc PR A 2
H30F H 0.6449 0.0061 0.3337 0.167 Uiso 0.39 1 calc PR A 2
I2 I 0.192727(17) 0.32763(5) 0.11286(3) 0.08485(19) Uani 1 1 d . . .
I1 I 0.73749(2) 0.49435(9) 0.54592(3) 0.1004(2) Uani 1 1 d . . .
C8 C 0.3833(2) 0.5021(8) 0.2066(3) 0.0485(12) Uani 1 1 d . . .
C2 C 0.5665(3) 0.5081(8) 0.4330(3) 0.0577(14) Uani 1 1 d . . .
H2 H 0.5312 0.4853 0.4482 0.069 Uiso 1 1 calc R . .
C3 C 0.6131(3) 0.4871(9) 0.4859(3) 0.0629(15) Uani 1 1 d . . .
H3 H 0.6095 0.4465 0.5358 0.076 Uiso 1 1 calc R . .
C11 C 0.2744(2) 0.4037(8) 0.1518(4) 0.0590(15) Uani 1 1 d . . .
C12 C 0.3063(2) 0.4895(9) 0.1040(4) 0.0648(15) Uani 1 1 d . . .
H12 H 0.2913 0.5142 0.0527 0.078 Uiso 1 1 calc R . .
C1 C 0.5708(2) 0.5635(7) 0.3565(3) 0.0504(14) Uani 1 1 d . . .
C13 C 0.3593(2) 0.5386(8) 0.1308(3) 0.0573(15) Uani 1 1 d . . .
H13 H 0.3797 0.5975 0.0976 0.069 Uiso 1 1 calc R . .
C4 C 0.6656(3) 0.5259(8) 0.4654(3) 0.0624(16) Uani 1 1 d . . .
C7 C 0.4725(2) 0.5202(8) 0.2963(3) 0.0519(13) Uani 1 1 d . . .
C5 C 0.6703(3) 0.5855(9) 0.3894(4) 0.0686(18) Uani 1 1 d . . .
H5 H 0.7053 0.6138 0.3751 0.082 Uiso 1 1 calc R . .
C10 C 0.2971(3) 0.3708(8) 0.2272(4) 0.073(2) Uani 1 1 d . . .
H10 H 0.2762 0.3136 0.2604 0.088 Uiso 1 1 calc R . .
C9 C 0.3510(3) 0.4217(9) 0.2551(4) 0.0681(18) Uani 1 1 d . . .
H9 H 0.3653 0.4008 0.3071 0.082 Uiso 1 1 calc R . .
N2 N 0.43865(19) 0.5545(6) 0.2291(3) 0.0541(12) Uani 1 1 d . . .
H2N H 0.4528 0.6159 0.1960 0.065 Uiso 1 1 calc R . .
N1 N 0.52454(19) 0.5863(6) 0.2987(3) 0.0568(12) Uani 1 1 d . . .
H1N H 0.5298 0.6494 0.2604 0.068 Uiso 1 1 calc R . .
O1 O 0.45760(17) 0.4375(6) 0.3500(2) 0.0718(13) Uani 1 1 d . . .
N3 N 0.5000 0.2130(7) 0.0000 0.0573(18) Uani 1 2 d S . .
C15 C 0.4528(3) 0.3224(9) -0.0354(4) 0.0680(16) Uani 1 1 d . . .
H15A H 0.4451 0.3983 0.0050 0.082 Uiso 1 1 calc R . .
H15B H 0.4667 0.3825 -0.0778 0.082 Uiso 1 1 calc R . .
C16 C 0.3979(3) 0.2464(8) -0.0675(4) 0.0746(19) Uani 1 1 d . . .
H16A H 0.3807 0.1959 -0.0250 0.090 Uiso 1 1 calc R . .
H16B H 0.4045 0.1655 -0.1061 0.090 Uiso 1 1 calc R . .
C19 C 0.4801(3) 0.1012(7) 0.0619(3) 0.0619(17) Uani 1 1 d . . .
H19B H 0.4513 0.0316 0.0360 0.074 Uiso 1 1 calc R . .
H19A H 0.5114 0.0347 0.0826 0.074 Uiso 1 1 calc R . .
C20 C 0.4567(4) 0.1819(9) 0.1304(4) 0.083(2) Uani 1 1 d . . .
H20B H 0.4300 0.2637 0.1109 0.100 Uiso 1 1 calc R . .
H20A H 0.4868 0.2319 0.1645 0.100 Uiso 1 1 calc R . .
C6 C 0.6232(2) 0.6020(8) 0.3361(4) 0.0616(17) Uani 1 1 d . . .
H6 H 0.6267 0.6397 0.2855 0.074 Uiso 1 1 calc R . .
O3 O 0.48630(15) 0.6715(5) 0.0903(2) 0.0552(9) Uani 1 1 d . . .
O2 O 0.5580(2) 0.7553(7) 0.1730(2) 0.0794(13) Uani 1 1 d . . .
C14 C 0.5356(2) 0.7240(7) 0.1063(3) 0.0502(14) Uani 1 1 d . . .
O4 O 0.56578(15) 0.7513(5) 0.0466(2) 0.0558(10) Uani 1 1 d . . .
H4O H 0.5494 0.7142 0.0058 0.084 Uiso 1 1 calc R . .
N4 N 0.5000 -0.0160(9) 0.5000 0.0652(19) Uani 1 2 d S . .
C24 C 0.4049(3) -0.0406(10) 0.4119(4) 0.084(2) Uani 1 1 d . . .
H24A H 0.3831 0.0116 0.4492 0.100 Uiso 1 1 calc R . .
H24B H 0.4175 0.0401 0.3772 0.100 Uiso 1 1 calc R . .
C17 C 0.3596(3) 0.3738(9) -0.1057(6) 0.099(3) Uani 1 1 d . . .
H17A H 0.3751 0.4134 -0.1521 0.119 Uiso 1 1 calc R . .
H17B H 0.3584 0.4619 -0.0690 0.119 Uiso 1 1 calc R . .
C18 C 0.3000(4) 0.3156(16) -0.1298(6) 0.121(3) Uani 1 1 d . . .
H18A H 0.3003 0.2361 -0.1702 0.181 Uiso 1 1 calc R . .
H18B H 0.2769 0.4035 -0.1496 0.181 Uiso 1 1 calc R . .
H18C H 0.2850 0.2704 -0.0847 0.181 Uiso 1 1 calc R . .
C22 C 0.3729(5) -0.0038(18) 0.1331(7) 0.138(4) Uani 1 1 d . . .
H22A H 0.3447 0.0772 0.1335 0.207 Uiso 1 1 calc R . .
H22B H 0.3609 -0.0981 0.1583 0.207 Uiso 1 1 calc R . .
H22C H 0.3788 -0.0280 0.0796 0.207 Uiso 1 1 calc R . .
C21 C 0.4272(5) 0.0550(11) 0.1772(5) 0.105(3) Uani 1 1 d . . .
H21A H 0.4523 -0.0347 0.1885 0.126 Uiso 1 1 calc R . .
H21B H 0.4194 0.1003 0.2272 0.126 Uiso 1 1 calc R . .
C25 C 0.3682(3) -0.1619(13) 0.3635(5) 0.096(2) Uani 1 1 d . . .
H25A H 0.3888 -0.2038 0.3222 0.115 Uiso 1 1 calc R . .
H25B H 0.3604 -0.2500 0.3975 0.115 Uiso 1 1 calc R . .
C23 C 0.4555(3) -0.1240(8) 0.4562(4) 0.0720(19) Uani 1 1 d . . .
H23B H 0.4734 -0.1878 0.4187 0.086 Uiso 1 1 calc R . .
H23A H 0.4420 -0.1965 0.4943 0.086 Uiso 1 1 calc R . .
C26 C 0.3137(4) -0.0932(17) 0.3266(6) 0.133(4) Uani 1 1 d . . .
H26B H 0.2967 -0.0322 0.3653 0.199 Uiso 1 1 calc R . .
H26A H 0.2888 -0.1780 0.3076 0.199 Uiso 1 1 calc R . .
H26C H 0.3205 -0.0254 0.2833 0.199 Uiso 1 1 calc R . .
C27 C 0.5264(4) 0.0913(9) 0.4418(5) 0.084(2) Uani 1 1 d D . .
H27B H 0.5485 0.1722 0.4718 0.100 Uiso 1 1 calc R A 1
H27A H 0.4963 0.1455 0.4093 0.100 Uiso 1 1 calc R A 1


_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
C28 C29 1.505(9) . ?
C28 C27 1.546(17) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.502(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C28D C29C 1.507(10) . ?
C28D C27 1.519(10) . ?
C28D H28C 0.9700 . ?
C28D H28D 0.9700 . ?
C29C C30C 1.495(10) . ?
C29C H29C 0.9700 . ?
C29C H29D 0.9700 . ?
C30C H30D 0.9600 . ?
C30C H30E 0.9600 . ?
C30C H30F 0.9600 . ?
I2 C11 2.094(6) . ?
I1 C4 2.093(6) . ?
C8 C9 1.371(8) . ?
C8 C13 1.389(8) . ?
C8 N2 1.407(7) . ?
C2 C3 1.365(8) . ?
C2 C1 1.399(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(9) . ?
C3 H3 0.9300 . ?
C11 C10 1.365(9) . ?
C11 C12 1.379(9) . ?
C12 C13 1.364(8) . ?
C12 H12 0.9300 . ?
C1 C6 1.376(8) . ?
C1 N1 1.410(7) . ?
C13 H13 0.9300 . ?
C4 C5 1.405(8) . ?
C7 O1 1.233(7) . ?
C7 N2 1.359(7) . ?
C7 N1 1.360(7) . ?
C5 C6 1.375(9) . ?
C5 H5 0.9300 . ?
C10 C9 1.393(9) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
N2 H2N 0.8600 . ?
N1 H1N 0.8600 . ?
N3 C15 1.526(8) . ?
N3 C15 1.526(8) 2_655 ?
N3 C19 1.528(7) 2_655 ?
N3 C19 1.528(7) . ?
C15 C16 1.508(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.509(10) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C19 C20 1.510(9) . ?
C19 H19B 0.9700 . ?
C19 H19A 0.9700 . ?
C20 C21 1.549(11) . ?
C20 H20B 0.9700 . ?
C20 H20A 0.9700 . ?
C6 H6 0.9300 . ?
O3 C14 1.261(6) . ?
O2 C14 1.229(7) . ?
C14 O4 1.333(7) . ?
O4 H4O 0.8200 . ?
N4 C27 1.527(8) . ?
N4 C27 1.527(8) 2_656 ?
N4 C23 1.528(8) . ?
N4 C23 1.528(8) 2_656 ?
C24 C25 1.524(12) . ?
C24 C23 1.525(10) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C17 C18 1.521(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C22 C21 1.508(14) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C25 C26 1.500(11) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23A 0.9700 . ?
C26 H26B 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27B 0.9700 . ?
C27 H27A 0.9700 . ?

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
C29 C28 C27 109.5(11) . . ?
C29 C28 H28A 109.8 . . ?
C27 C28 H28A 109.8 . . ?
C29 C28 H28B 109.8 . . ?
C27 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
C30 C29 C28 111.1(11) . . ?
C30 C29 H29A 109.4 . . ?
C28 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29C C28D C27 120.4(18) . . ?
C29C C28D H28C 107.2 . . ?
C27 C28D H28C 107.2 . . ?
C29C C28D H28D 107.2 . . ?
C27 C28D H28D 107.2 . . ?
H28C C28D H28D 106.8 . . ?
C30C C29C C28D 110(2) . . ?
C30C C29C H29C 109.7 . . ?
C28D C29C H29C 109.7 . . ?
C30C C29C H29D 109.7 . . ?
C28D C29C H29D 109.7 . . ?
H29C C29C H29D 108.2 . . ?
C29C C30C H30D 109.5 . . ?
C29C C30C H30E 109.5 . . ?
H30D C30C H30E 109.5 . . ?
C29C C30C H30F 109.5 . . ?
H30D C30C H30F 109.5 . . ?
H30E C30C H30F 109.5 . . ?
C9 C8 C13 117.8(5) . . ?
C9 C8 N2 124.6(5) . . ?
C13 C8 N2 117.5(5) . . ?
C3 C2 C1 121.0(6) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C10 C11 C12 118.3(5) . . ?
C10 C11 I2 119.7(5) . . ?
C12 C11 I2 122.0(5) . . ?
C13 C12 C11 121.1(6) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C6 C1 C2 118.6(5) . . ?
C6 C1 N1 117.3(5) . . ?
C2 C1 N1 124.1(5) . . ?
C12 C13 C8 121.1(6) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
C3 C4 C5 119.0(5) . . ?
C3 C4 I1 120.7(4) . . ?
C5 C4 I1 120.3(5) . . ?
O1 C7 N2 123.3(5) . . ?
O1 C7 N1 123.3(5) . . ?
N2 C7 N1 113.3(5) . . ?
C6 C5 C4 120.0(6) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C11 C10 C9 120.9(6) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C8 C9 C10 120.7(6) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C7 N2 C8 128.1(5) . . ?
C7 N2 H2N 115.9 . . ?
C8 N2 H2N 115.9 . . ?
C7 N1 C1 127.6(5) . . ?
C7 N1 H1N 116.2 . . ?
C1 N1 H1N 116.2 . . ?
C15 N3 C15 106.0(6) . 2_655 ?
C15 N3 C19 111.8(4) . 2_655 ?
C15 N3 C19 111.6(4) 2_655 2_655 ?
C15 N3 C19 111.6(4) . . ?
C15 N3 C19 111.8(4) 2_655 . ?
C19 N3 C19 104.2(6) 2_655 . ?
C16 C15 N3 117.7(6) . . ?
C16 C15 H15A 107.9 . . ?
N3 C15 H15A 107.9 . . ?
C16 C15 H15B 107.9 . . ?
N3 C15 H15B 107.9 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 C17 108.7(6) . . ?
C15 C16 H16A 110.0 . . ?
C17 C16 H16A 110.0 . . ?
C15 C16 H16B 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H16A C16 H16B 108.3 . . ?
C20 C19 N3 115.4(5) . . ?
C20 C19 H19B 108.4 . . ?
N3 C19 H19B 108.4 . . ?
C20 C19 H19A 108.4 . . ?
N3 C19 H19A 108.4 . . ?
H19B C19 H19A 107.5 . . ?
C19 C20 C21 108.7(6) . . ?
C19 C20 H20B 110.0 . . ?
C21 C20 H20B 110.0 . . ?
C19 C20 H20A 110.0 . . ?
C21 C20 H20A 110.0 . . ?
H20B C20 H20A 108.3 . . ?
C5 C6 C1 120.9(6) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O2 C14 O3 125.1(6) . . ?
O2 C14 O4 116.8(5) . . ?
O3 C14 O4 118.0(5) . . ?
C14 O4 H4O 109.5 . . ?
C27 N4 C27 107.8(7) . 2_656 ?
C27 N4 C23 110.5(4) . . ?
C27 N4 C23 110.5(4) 2_656 . ?
C27 N4 C23 110.5(4) . 2_656 ?
C27 N4 C23 110.5(4) 2_656 2_656 ?
C23 N4 C23 107.3(7) . 2_656 ?
C25 C24 C23 109.8(6) . . ?
C25 C24 H24A 109.7 . . ?
C23 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 . . ?
C23 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C16 C17 C18 113.3(8) . . ?
C16 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C22 C21 C20 112.7(8) . . ?
C22 C21 H21A 109.1 . . ?
C20 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C26 C25 C24 113.0(9) . . ?
C26 C25 H25A 109.0 . . ?
C24 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
C24 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C24 C23 N4 116.2(5) . . ?
C24 C23 H23B 108.2 . . ?
N4 C23 H23B 108.2 . . ?
C24 C23 H23A 108.2 . . ?
N4 C23 H23A 108.2 . . ?
H23B C23 H23A 107.4 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
C28D C27 N4 115.3(11) . . ?
C28D C27 C28 24.0(15) . . ?
N4 C27 C28 116.5(8) . . ?
C28D C27 H27B 127.0 . . ?
N4 C27 H27B 108.2 . . ?
C28 C27 H27B 108.2 . . ?
C28D C27 H27A 86.9 . . ?
N4 C27 H27A 108.2 . . ?
C28 C27 H27A 108.2 . . ?
H27B C27 H27A 107.3 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 973821'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_I-U_AcO

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, C13 H10 I2 N2 O, C2 H3 O2'
_chemical_formula_sum            'C31 H49 I2 N3 O3'
_chemical_formula_weight         765.55

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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   8.8809(3)
_cell_length_b                   21.0697(6)
_cell_length_c                   18.9452(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.815(2)
_cell_angle_gamma                90.00
_cell_volume                     3512.06(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      23.12

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544.0
_exptl_absorpt_coefficient_mu    1.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43647
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         28.35
_reflns_number_total             8711
_reflns_number_gt                4605
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. The following restraints
 were applied (given as SHELXL lines):
EADP C17 C17A
EADP C21 C21A
EADP C26 C26A
EADP C30 C30A
DFIX 1.500 0.01 C16 C17  C17 C18  C18 C19
DFIX 1.500 0.01 C16 C17A  C17A C18A  C18A C19A
DFIX 1.500 0.01 C20 C21  C21 C22  C22 C23
DFIX 1.500 0.01 N3 C24  C24 C25  C25 C26  C26 C27
DFIX 1.500 0.01 C28 C29  C29 C30  C30 C31
DFIX 1.54 0.001 C20 C21A  C28 C29A  C24 C25A
SIMU 0.005 C17 C18 C19 C17A C18A C19A
SIMU 0.005 C21 C22 C23 C21A C22B C23A
SIMU 0.005 C25 C26 C27 C25A C26A C27A
SIMU 0.005 C29 C30 C31 C29A C30A C31A
ISOR 0.01 C17A C18A C19A
ISOR 0.01 C21A C22B C23A
ISOR 0.01 C25A C26A C27A
ISOR 0.01 C29A C30A C31A 
;

_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+2.5737P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8377
_refine_ls_number_parameters     358
_refine_ls_number_restraints     397
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.2080
_refine_ls_wR_factor_gt          0.1786
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_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
C17 C 0.24054(4) 0.881456(15) 0.155681(19) 0.141(2) Uani 0.69 1 d PDU A 1
H17A H 0.1955 0.8462 0.1782 0.169 Uiso 0.69 1 calc PR A 1
H17B H 0.1587 0.9081 0.1332 0.169 Uiso 0.69 1 calc PR A 1
C18 C 0.32959(4) 0.856462(15) 0.099810(19) 0.147(3) Uani 0.69 1 d PRDU A 1
H18A H 0.2629 0.8420 0.0581 0.177 Uiso 0.69 1 d PR A 1
H18B H 0.3983 0.8884 0.0856 0.177 Uiso 0.69 1 d PR A 1
C19 C 0.41523(4) 0.802207(15) 0.137619(19) 0.161(4) Uani 0.69 1 d PRDU A 1
H19A H 0.5090 0.8175 0.1632 0.242 Uiso 0.69 1 calc PR A 1
H19B H 0.4366 0.7710 0.1034 0.242 Uiso 0.69 1 calc PR A 1
H19C H 0.3550 0.7834 0.1705 0.242 Uiso 0.69 1 calc PR A 1
C21 C 0.31813(4) 1.047662(15) 0.351678(19) 0.133(2) Uani 0.63 1 d PRDU A 1
H21A H 0.2615 1.0310 0.3879 0.159 Uiso 0.63 1 calc PR A 1
H21B H 0.2530 1.0763 0.3213 0.159 Uiso 0.63 1 calc PR A 1
C22 C 0.45851(4) 1.081419(15) 0.385383(19) 0.136(2) Uani 0.63 1 d PRDU A 1
H22A H 0.5281 1.0508 0.4103 0.163 Uiso 0.63 1 calc PR A 1
H22B H 0.5086 1.1009 0.3485 0.163 Uiso 0.63 1 calc PR A 1
C23 C 0.42235(4) 1.131484(15) 0.436805(19) 0.149(4) Uani 0.63 1 d PRDU A 1
H23A H 0.3623 1.1642 0.4114 0.224 Uiso 0.63 1 calc PR A 1
H23B H 0.5151 1.1494 0.4604 0.224 Uiso 0.63 1 calc PR A 1
H23C H 0.3664 1.1128 0.4715 0.224 Uiso 0.63 1 calc PR A 1
C25 C 0.17232(4) 1.055283(15) 0.180934(19) 0.137(3) Uani 0.69 1 d PRDU A 1
H25A H 0.2449 1.0480 0.1479 0.165 Uiso 0.69 1 calc PR A 1
H25B H 0.2228 1.0814 0.2192 0.165 Uiso 0.69 1 calc PR A 1
C26 C 0.04413(4) 1.093632(15) 0.142622(19) 0.141(2) Uani 0.69 1 d PRDU A 1
H26A H -0.0435 1.0917 0.1681 0.169 Uiso 0.69 1 calc PR A 1
H26B H 0.0745 1.1377 0.1396 0.169 Uiso 0.69 1 calc PR A 1
C27 C 0.00521(4) 1.066235(15) 0.069337(19) 0.162(4) Uani 0.69 1 d PRDU A 1
H27A H 0.0792 1.0797 0.0399 0.243 Uiso 0.69 1 calc PR A 1
H27B H -0.0937 1.0807 0.0489 0.243 Uiso 0.69 1 calc PR A 1
H27C H 0.0052 1.0207 0.0722 0.243 Uiso 0.69 1 calc PR A 1
C29 C 0.26167(4) 0.859867(15) 0.348264(19) 0.147(3) Uani 0.60 1 d PRDU A 1
H29A H 0.3570 0.8726 0.3759 0.177 Uiso 0.60 1 calc PR A 1
H29B H 0.2825 0.8281 0.3138 0.177 Uiso 0.60 1 calc PR A 1
C30 C 0.15483(4) 0.834138(15) 0.396129(19) 0.150(2) Uani 0.60 1 d PRDU A 1
H30A H 0.1516 0.8631 0.4357 0.180 Uiso 0.60 1 calc PR A 1
H30B H 0.0534 0.8318 0.3698 0.180 Uiso 0.60 1 calc PR A 1
C31 C 0.20069(4) 0.769552(15) 0.424655(19) 0.160(4) Uani 0.60 1 d PRDU A 1
H31A H 0.2691 0.7506 0.3957 0.241 Uiso 0.60 1 calc PR A 1
H31B H 0.1120 0.7434 0.4238 0.241 Uiso 0.60 1 calc PR A 1
H31C H 0.2503 0.7734 0.4727 0.241 Uiso 0.60 1 calc PR A 1
C17A C 0.27746(4) 0.853378(15) 0.193287(19) 0.141(2) Uani 0.31 1 d PRDU A 2
H17C H 0.2511 0.8344 0.2366 0.169 Uiso 0.31 1 calc PR A 2
H17D H 0.1836 0.8583 0.1610 0.169 Uiso 0.31 1 calc PR A 2
C18A C 0.37408(4) 0.806432(15) 0.160259(19) 0.147(3) Uani 0.31 1 d PRDU A 2
H18C H 0.4776 0.8089 0.1842 0.177 Uiso 0.31 1 calc PR A 2
H18D H 0.3367 0.7639 0.1670 0.177 Uiso 0.31 1 calc PR A 2
C19A C 0.37343(4) 0.818367(15) 0.082159(19) 0.153(4) Uani 0.31 1 d PRDU A 2
H19D H 0.2706 0.8231 0.0596 0.229 Uiso 0.31 1 calc PR A 2
H19E H 0.4199 0.7832 0.0612 0.229 Uiso 0.31 1 calc PR A 2
H19F H 0.4294 0.8564 0.0757 0.229 Uiso 0.31 1 calc PR A 2
C21A C 0.31343(4) 1.029680(15) 0.378912(19) 0.133(2) Uani 0.37 1 d PRDU A 2
H21C H 0.2302 1.0587 0.3643 0.159 Uiso 0.37 1 calc PR A 2
H21D H 0.2769 0.9968 0.4082 0.159 Uiso 0.37 1 calc PR A 2
C22B C 0.44219(4) 1.064878(15) 0.421222(19) 0.136(3) Uani 0.37 1 d PRU A 2
H22C H 0.4252 1.0702 0.4704 0.163 Uiso 0.37 1 calc PR A 2
H22D H 0.5382 1.0432 0.4200 0.163 Uiso 0.37 1 calc PR A 2
C23A C 0.43829(4) 1.127371(15) 0.383083(19) 0.138(4) Uani 0.37 1 d PRU A 2
H23D H 0.4168 1.1204 0.3326 0.207 Uiso 0.37 1 calc PR A 2
H23E H 0.5350 1.1480 0.3939 0.207 Uiso 0.37 1 calc PR A 2
H23F H 0.3605 1.1537 0.3983 0.207 Uiso 0.37 1 calc PR A 2
C25A C 0.20586(4) 1.021194(15) 0.145675(19) 0.137(3) Uani 0.31 1 d PRDU A 2
H25C H 0.2806 1.0543 0.1584 0.164 Uiso 0.31 1 calc PR A 2
H25D H 0.2492 0.9881 0.1190 0.164 Uiso 0.31 1 calc PR A 2
C26A C 0.06025(4) 1.046812(15) 0.106647(19) 0.141(2) Uani 0.31 1 d PRU A 2
H26C H 0.0409 1.0234 0.0622 0.169 Uiso 0.31 1 calc PR A 2
H26D H -0.0194 1.0350 0.1344 0.169 Uiso 0.31 1 calc PR A 2
C27A C 0.03616(4) 1.115597(15) 0.088017(19) 0.150(4) Uani 0.31 1 d PRU A 2
H27D H -0.0319 1.1340 0.1176 0.224 Uiso 0.31 1 calc PR A 2
H27E H -0.0068 1.1194 0.0389 0.224 Uiso 0.31 1 calc PR A 2
H27F H 0.1318 1.1375 0.0957 0.224 Uiso 0.31 1 calc PR A 2
C29A C 0.30220(4) 0.882213(15) 0.372050(19) 0.147(3) Uani 0.40 1 d PRDU A 2
H29C H 0.3562 0.8484 0.3515 0.176 Uiso 0.40 1 calc PR A 2
H29D H 0.3760 0.9137 0.3915 0.176 Uiso 0.40 1 calc PR A 2
C30A C 0.22286(4) 0.855927(15) 0.430694(19) 0.150(2) Uani 0.40 1 d PRU A 2
H30C H 0.2961 0.8383 0.4682 0.180 Uiso 0.40 1 calc PR A 2
H30D H 0.1661 0.8891 0.4509 0.180 Uiso 0.40 1 calc PR A 2
C31A C 0.11739(4) 0.805114(15) 0.397960(19) 0.150(4) Uani 0.40 1 d PRU A 2
H31D H 0.0313 0.8244 0.3699 0.224 Uiso 0.40 1 calc PR A 2
H31E H 0.0836 0.7799 0.4350 0.224 Uiso 0.40 1 calc PR A 2
H31F H 0.1699 0.7786 0.3681 0.224 Uiso 0.40 1 calc PR A 2
I2 I 0.34653(4) 1.263159(15) 0.098706(19) 0.0929(2) Uani 1 1 d R . .
I1 I 1.05570(4) 0.641817(15) 0.129138(19) 0.0891(2) Uani 1 1 d R . .
C7 C 0.70897(4) 0.953806(15) 0.141802(19) 0.0599(13) Uani 1 1 d R . .
C1 C 0.94928(4) 0.729287(15) 0.142813(19) 0.0707(16) Uani 1 1 d R . .
C11 C 0.46298(4) 1.177001(15) 0.120631(19) 0.0663(14) Uani 1 1 d R . .
C6 C 0.92009(4) 0.772895(15) 0.088683(19) 0.0718(16) Uani 1 1 d R . .
H6 H 0.9441 0.7633 0.0436 0.086 Uiso 1 1 calc R . .
C5 C 0.8548(7) 0.8312(3) 0.1009(3) 0.0698(16) Uani 1 1 d . . .
H5 H 0.8357 0.8603 0.0639 0.084 Uiso 1 1 calc R . .
C13 C 0.5377(6) 1.0727(3) 0.0879(3) 0.0669(15) Uani 1 1 d . . .
H13 H 0.5365 1.0410 0.0536 0.080 Uiso 1 1 calc R . .
C8 C 0.6148(6) 1.0632(3) 0.1560(3) 0.0599(13) Uani 1 1 d . . .
C9 C 0.6151(7) 1.1124(3) 0.2058(3) 0.0697(15) Uani 1 1 d . . .
H9 H 0.6673 1.1069 0.2514 0.084 Uiso 1 1 calc R . .
C4 C 0.8182(6) 0.8464(3) 0.1675(3) 0.0575(13) Uani 1 1 d . . .
C3 C 0.8473(7) 0.8012(3) 0.2212(3) 0.0742(16) Uani 1 1 d . . .
H3 H 0.8225 0.8102 0.2663 0.089 Uiso 1 1 calc R . .
C10 C 0.5406(8) 1.1681(3) 0.1891(3) 0.0771(17) Uani 1 1 d . . .
H10 H 0.5414 1.2000 0.2231 0.093 Uiso 1 1 calc R . .
C2 C 0.9116(8) 0.7436(3) 0.2093(4) 0.0817(18) Uani 1 1 d . . .
H2 H 0.9299 0.7142 0.2461 0.098 Uiso 1 1 calc R . .
C12 C 0.4619(7) 1.1302(3) 0.0712(3) 0.0674(15) Uani 1 1 d . . .
H12 H 0.4101 1.1364 0.0256 0.081 Uiso 1 1 calc R . .
N2 N 0.6866(5) 1.0066(2) 0.1798(2) 0.0622(11) Uani 1 1 d . . .
H2A H 0.7211 1.0051 0.2245 0.075 Uiso 1 1 calc R . .
N1 N 0.7623(5) 0.9046(2) 0.1858(2) 0.0648(12) Uani 1 1 d . . .
H1 H 0.7608 0.9108 0.2306 0.078 Uiso 1 1 calc R . .
O1 O 0.6875(5) 0.9502(2) 0.0773(2) 0.0773(12) Uani 1 1 d . . .
N3 N 0.2556(5) 0.9577(3) 0.2611(3) 0.0821(15) Uani 1 1 d D A .
C14 C 0.7858(6) 0.9604(3) 0.3599(3) 0.0631(14) Uani 1 1 d . . .
O2 O 0.8068(6) 1.0079(2) 0.3262(2) 0.0941(15) Uani 1 1 d . . .
O3 O 0.7321(7) 0.9110(2) 0.3327(2) 0.1031(17) Uani 1 1 d . . .
C15 C 0.8245(11) 0.9616(4) 0.4396(4) 0.116(3) Uani 1 1 d . . .
H15A H 0.8055 1.0032 0.4571 0.174 Uiso 1 1 calc R . .
H15B H 0.9299 0.9511 0.4525 0.174 Uiso 1 1 calc R . .
H15C H 0.7629 0.9311 0.4603 0.174 Uiso 1 1 calc R . .
C16 C 0.3392(9) 0.9195(4) 0.2120(4) 0.125(3) Uani 1 1 d D . .
H16A H 0.4071 0.8905 0.2406 0.150 Uiso 1 1 calc R A 1
H16B H 0.4016 0.9482 0.1883 0.150 Uiso 1 1 calc R A 1
C20 C 0.3679(7) 0.9995(4) 0.3126(3) 0.113(3) Uani 1 1 d D . .
H20A H 0.4254 0.9708 0.3461 0.136 Uiso 1 1 calc R A 1
H20B H 0.4396 1.0180 0.2841 0.136 Uiso 1 1 calc R A 1
C24 C 0.1405(7) 0.9948(4) 0.2111(3) 0.129(3) Uani 1 1 d D . .
H24A H 0.1070 0.9669 0.1713 0.155 Uiso 1 1 calc R A 1
H24B H 0.0533 1.0013 0.2361 0.155 Uiso 1 1 calc R A 1
C28 C 0.1873(6) 0.9128(4) 0.3135(3) 0.111(3) Uani 1 1 d D . .
H28A H 0.1585 0.9398 0.3509 0.133 Uiso 1 1 calc R A 1
H28B H 0.0933 0.8967 0.2876 0.133 Uiso 1 1 calc R A 1


_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
C17 C18 1.5003 . ?
C17 C16 1.515(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.5001 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 C20 1.364(4) . ?
C21 C22 1.5005 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.5000 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C25 C24 1.440(6) . ?
C25 C26 1.5003 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.4999 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 C28 1.413(4) . ?
C29 C30 1.5001 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.5000 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C17A C18A 1.5008 . ?
C17A C16 1.522(6) . ?
C17A H17C 0.9700 . ?
C17A H17D 0.9700 . ?
C18A C19A 1.5001 . ?
C18A H18C 0.9700 . ?
C18A H18D 0.9700 . ?
C19A H18A 1.1390 . ?
C19A H18B 1.4917 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C21A C22B 1.5003 . ?
C21A C20 1.5431(10) . ?
C21A H21C 0.9700 . ?
C21A H21D 0.9700 . ?
C22B C23A 1.5001 . ?
C22B H22C 0.9700 . ?
C22B H22D 0.9700 . ?
C23A H23D 0.9600 . ?
C23A H23E 0.9600 . ?
C23A H23F 0.9600 . ?
C25A C26A 1.5001 . ?
C25A C24 1.5427(10) . ?
C25A H25C 0.9700 . ?
C25A H25D 0.9700 . ?
C26A C27A 1.5001 . ?
C26A H26C 0.9700 . ?
C26A H26D 0.9700 . ?
C27A H27D 0.9600 . ?
C27A H27E 0.9600 . ?
C27A H27F 0.9600 . ?
C29A C30A 1.5001 . ?
C29A C28 1.5426(10) . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C30A C31A 1.5001 . ?
C30A H30C 0.9700 . ?
C30A H30D 0.9700 . ?
C31A H31D 0.9600 . ?
C31A H31E 0.9600 . ?
C31A H31F 0.9600 . ?
I2 C11 2.1025 . ?
I1 C1 2.1032 . ?
C7 O1 1.213(4) . ?
C7 N2 1.354(4) . ?
C7 N1 1.374(5) . ?
C1 C6 1.3751 . ?
C1 C2 1.379(7) . ?
C11 C12 1.359(6) . ?
C11 C10 1.396(6) . ?
C6 C5 1.392(6) . ?
C6 H6 0.9300 . ?
C5 C4 1.383(8) . ?
C5 H5 0.9300 . ?
C13 C8 1.391(8) . ?
C13 C12 1.401(8) . ?
C13 H13 0.9300 . ?
C8 N2 1.399(7) . ?
C8 C9 1.401(8) . ?
C9 C10 1.364(8) . ?
C9 H9 0.9300 . ?
C4 N1 1.385(7) . ?
C4 C3 1.392(8) . ?
C3 C2 1.373(9) . ?
C3 H3 0.9300 . ?
C10 H10 0.9300 . ?
C2 H2 0.9300 . ?
C12 H12 0.9300 . ?
N2 H2A 0.8600 . ?
N1 H1 0.8600 . ?
N3 C16 1.500(9) . ?
N3 C24 1.513(7) . ?
N3 C28 1.552(8) . ?
N3 C20 1.568(8) . ?
C14 O2 1.216(7) . ?
C14 O3 1.228(7) . ?
C14 C15 1.504(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?

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
C18 C17 C16 111.9(3) . . ?
C18 C17 H17A 109.2 . . ?
C16 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C16 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C17 102.3 . . ?
C19 C18 H18A 111.3 . . ?
C17 C18 H18A 111.3 . . ?
C19 C18 H18B 111.3 . . ?
C17 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
C20 C21 C22 105.8(3) . . ?
C20 C21 H21A 110.6 . . ?
C22 C21 H21A 110.6 . . ?
C20 C21 H21B 110.6 . . ?
C22 C21 H21B 110.6 . . ?
H21A C21 H21B 108.7 . . ?
C23 C22 C21 111.8 . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
C24 C25 C26 119.4(3) . . ?
C24 C25 H25A 107.5 . . ?
C26 C25 H25A 107.5 . . ?
C24 C25 H25B 107.5 . . ?
C26 C25 H25B 107.5 . . ?
H25A C25 H25B 107.0 . . ?
C27 C26 C25 107.7 . . ?
C27 C26 H26A 110.2 . . ?
C25 C26 H26A 110.2 . . ?
C27 C26 H26B 110.2 . . ?
C25 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
C28 C29 C30 105.9(3) . . ?
C28 C29 H29A 110.6 . . ?
C30 C29 H29A 110.6 . . ?
C28 C29 H29B 110.6 . . ?
C30 C29 H29B 110.6 . . ?
H29A C29 H29B 108.7 . . ?
C31 C30 C29 112.5 . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C18A C17A C16 119.5(3) . . ?
C18A C17A H17C 107.4 . . ?
C16 C17A H17C 107.4 . . ?
C18A C17A H17D 107.4 . . ?
C16 C17A H17D 107.4 . . ?
H17C C17A H17D 107.0 . . ?
C19A C18A C17A 112.0 . . ?
C19A C18A H18C 109.2 . . ?
C17A C18A H18C 109.2 . . ?
C19A C18A H18D 109.2 . . ?
C17A C18A H18D 109.2 . . ?
H18C C18A H18D 107.9 . . ?
C18A C19A H18A 110.9 . . ?
C18A C19A H18B 98.1 . . ?
H18A C19A H18B 72.5 . . ?
C18A C19A H19D 109.5 . . ?
C18A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C18A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C22B C21A C20 109.7(3) . . ?
C22B C21A H21C 109.7 . . ?
C20 C21A H21C 109.7 . . ?
C22B C21A H21D 109.7 . . ?
C20 C21A H21D 109.7 . . ?
H21C C21A H21D 108.2 . . ?
C23A C22B C21A 102.2 . . ?
C23A C22B H22C 111.3 . . ?
C21A C22B H22C 111.3 . . ?
C23A C22B H22D 111.3 . . ?
C21A C22B H22D 111.3 . . ?
H22C C22B H22D 109.2 . . ?
C22B C23A H23D 109.5 . . ?
C22B C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C22B C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C26A C25A C24 97.6(2) . . ?
C26A C25A H25C 112.2 . . ?
C24 C25A H25C 112.2 . . ?
C26A C25A H25D 112.2 . . ?
C24 C25A H25D 112.2 . . ?
H25C C25A H25D 109.8 . . ?
C27A C26A C25A 123.3 . . ?
C27A C26A H26C 106.5 . . ?
C25A C26A H26C 106.5 . . ?
C27A C26A H26D 106.5 . . ?
C25A C26A H26D 106.5 . . ?
H26C C26A H26D 106.5 . . ?
C26A C27A H27D 109.5 . . ?
C26A C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C26A C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C30A C29A C28 110.8(3) . . ?
C30A C29A H29C 109.5 . . ?
C28 C29A H29C 109.5 . . ?
C30A C29A H29D 109.5 . . ?
C28 C29A H29D 109.5 . . ?
H29C C29A H29D 108.1 . . ?
C31A C30A C29A 106.7 . . ?
C31A C30A H30C 110.4 . . ?
C29A C30A H30C 110.4 . . ?
C31A C30A H30D 110.4 . . ?
C29A C30A H30D 110.4 . . ?
H30C C30A H30D 108.6 . . ?
C30A C31A H31D 109.5 . . ?
C30A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C30A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
O1 C7 N2 125.0(3) . . ?
O1 C7 N1 123.9(3) . . ?
N2 C7 N1 111.1(3) . . ?
C6 C1 C2 119.4(3) . . ?
C6 C1 I1 122.4 . . ?
C2 C1 I1 118.2(3) . . ?
C12 C11 C10 119.9(4) . . ?
C12 C11 I2 122.2(2) . . ?
C10 C11 I2 117.8(3) . . ?
C1 C6 C5 120.4(2) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C4 C5 C6 120.7(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C8 C13 C12 119.7(5) . . ?
C8 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C8 N2 124.5(5) . . ?
C13 C8 C9 118.4(5) . . ?
N2 C8 C9 117.0(5) . . ?
C10 C9 C8 121.5(5) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C5 C4 N1 124.7(5) . . ?
C5 C4 C3 117.8(5) . . ?
N1 C4 C3 117.4(5) . . ?
C2 C3 C4 121.6(6) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C9 C10 C11 119.6(5) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C3 C2 C1 120.1(5) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C11 C12 C13 120.9(5) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C7 N2 C8 128.5(4) . . ?
C7 N2 H2A 115.8 . . ?
C8 N2 H2A 115.8 . . ?
C7 N1 C4 128.4(4) . . ?
C7 N1 H1 115.8 . . ?
C4 N1 H1 115.8 . . ?
C16 N3 C24 103.8(6) . . ?
C16 N3 C28 109.8(6) . . ?
C24 N3 C28 115.2(3) . . ?
C16 N3 C20 111.1(4) . . ?
C24 N3 C20 114.6(6) . . ?
C28 N3 C20 102.5(5) . . ?
O2 C14 O3 123.7(6) . . ?
O2 C14 C15 119.0(6) . . ?
O3 C14 C15 117.3(6) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 C17 115.7(5) . . ?
N3 C16 C17A 116.3(5) . . ?
C17 C16 C17A 36.44(13) . . ?
N3 C16 H16A 108.4 . . ?
C17 C16 H16A 108.4 . . ?
C17A C16 H16A 74.3 . . ?
N3 C16 H16B 108.4 . . ?
C17 C16 H16B 108.4 . . ?
C17A C16 H16B 132.2 . . ?
H16A C16 H16B 107.4 . . ?
C21 C20 C21A 24.7 . . ?
C21 C20 N3 122.0(5) . . ?
C21A C20 N3 119.6(4) . . ?
C21 C20 H20A 106.8 . . ?
C21A C20 H20A 85.4 . . ?
N3 C20 H20A 106.8 . . ?
C21 C20 H20B 106.8 . . ?
C21A C20 H20B 126.2 . . ?
N3 C20 H20B 106.8 . . ?
H20A C20 H20B 106.7 . . ?
C25 C24 N3 123.6(5) . . ?
C25 C24 C25A 41.09(7) . . ?
N3 C24 C25A 113.1(4) . . ?
C25 C24 H24A 106.4 . . ?
N3 C24 H24A 106.4 . . ?
C25A C24 H24A 72.7 . . ?
C25 C24 H24B 106.4 . . ?
N3 C24 H24B 106.4 . . ?
C25A C24 H24B 139.0 . . ?
H24A C24 H24B 106.5 . . ?
C29 C28 C29A 27.5 . . ?
C29 C28 N3 125.5(5) . . ?
C29A C28 N3 115.9(4) . . ?
C29 C28 H28A 105.9 . . ?
C29A C28 H28A 86.2 . . ?
N3 C28 H28A 105.9 . . ?
C29 C28 H28B 105.9 . . ?
C29A C28 H28B 131.0 . . ?
N3 C28 H28B 105.9 . . ?
H28A C28 H28B 106.3 . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 973822'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Br_Urea_L

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H10 Br2 N2 O'
_chemical_formula_sum            'C13 H10 Br2 N2 O'
_chemical_formula_weight         370.03

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'
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'
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/c  '
_symmetry_space_group_name_Hall  '-C 2yc'
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                   28.0636(16)
_cell_length_b                   4.6085(3)
_cell_length_c                   10.0857(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.469(4)
_cell_angle_gamma                90.00
_cell_volume                     1298.46(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1632
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720.0
_exptl_absorpt_coefficient_mu    6.231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.106
_exptl_absorpt_correction_T_max  0.343
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8968
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         28.30
_reflns_number_total             1596
_reflns_number_gt                1040
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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+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    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1596
_refine_ls_number_parameters     83
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1119
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_restrained_S_all      0.920
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.294280(14) 0.01862(9) -0.16086(5) 0.0657(3) Uani 1 1 d . . .
C1 C 0.34764(11) 0.1660(7) -0.0517(3) 0.0395(7) Uani 1 1 d . . .
C5 C 0.43173(11) 0.1811(7) 0.0059(3) 0.0392(7) Uani 1 1 d . . .
H5 H 0.4624 0.1196 -0.0080 0.047 Uiso 1 1 calc R . .
C3 C 0.37980(14) 0.4787(7) 0.1213(4) 0.0469(9) Uani 1 1 d . . .
H3 H 0.3754 0.6158 0.1866 0.056 Uiso 1 1 calc R . .
C6 C 0.39282(13) 0.0689(7) -0.0714(4) 0.0448(8) Uani 1 1 d . . .
H6 H 0.3971 -0.0705 -0.1359 0.054 Uiso 1 1 calc R . .
C4 C 0.42558(10) 0.3834(6) 0.1036(3) 0.0343(7) Uani 1 1 d . . .
C2 C 0.34065(12) 0.3723(9) 0.0430(4) 0.0484(8) Uani 1 1 d . . .
H2 H 0.3100 0.4391 0.0541 0.058 Uiso 1 1 calc R . .
C7 C 0.5000 0.3470(9) 0.2500 0.0323(9) Uani 1 2 d S . .
N1 N 0.46507(11) 0.5084(5) 0.1822(3) 0.0397(7) Uani 1 1 d . . .
H1 H 0.4670 0.6944 0.1871 0.048 Uiso 1 1 calc R . .
O1 O 0.5000 0.0819(6) 0.2500 0.0435(9) Uani 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
Br1 C1 1.898(3) . ?
C1 C2 1.375(5) . ?
C1 C6 1.377(5) . ?
C5 C4 1.379(4) . ?
C5 C6 1.381(5) . ?
C5 H5 0.9300 . ?
C3 C2 1.380(5) . ?
C3 C4 1.385(5) . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C4 N1 1.422(4) . ?
C2 H2 0.9300 . ?
C7 O1 1.222(5) . ?
C7 N1 1.362(3) 2_655 ?
C7 N1 1.362(3) . ?
N1 H1 0.8600 . ?

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
C2 C1 C6 121.3(3) . . ?
C2 C1 Br1 119.6(2) . . ?
C6 C1 Br1 119.1(3) . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C1 C6 C5 119.1(3) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 N1 121.9(3) . . ?
C3 C4 N1 118.9(3) . . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
O1 C7 N1 123.11(18) . 2_655 ?
O1 C7 N1 123.11(18) . . ?
N1 C7 N1 113.8(4) 2_655 . ?
C7 N1 C4 123.0(2) . . ?
C7 N1 H1 118.5 . . ?
C4 N1 H1 118.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.078
_database_code_depnum_ccdc_archive 'CCDC 973823'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Br-U_AcO

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, C13 H10 Br2 N2 O, C2 H3 O2 '
_chemical_formula_sum            'C31 H49 Br2 N3 O3'
_chemical_formula_weight         671.53

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'
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'
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.5024(5)
_cell_length_b                   18.9054(10)
_cell_length_c                   19.3877(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.771(5)
_cell_angle_gamma                90.00
_cell_volume                     3432.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9985
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      23.23

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400.0
_exptl_absorpt_coefficient_mu    2.394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15160
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         28.69
_reflns_number_total             8817
_reflns_number_gt                5893
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. The following restraints
 were applied (given as SHELXL lines):  
EADP C26 C26A
EADP C30 C30A
DFIX 1.500 0.01 C17 C18  C18 C19
DFIX 1.500 0.01 C17 C18A  C18A C19A
DFIX 1.500 0.01 C20 C21  C21 C22  C22 C23
DFIX 1.500 0.01 C20 C21A  C21A C22A  C22A C23A
DFIX 1.500 0.01 C25 C26  C26 C27
DFIX 1.500 0.01 C25 C26A  C26A C27A
DFIX 1.500 0.01 C29 C30  C30 C31
DFIX 1.500 0.01 C29 C30A  C30A C31A
SIMU 0.005 C18 C19 C18A C19A
SIMU 0.005 C21 C22 C23 C21A C22A C23A
SIMU 0.005 C26 C27 C26A C27A
SIMU 0.005 C30 C31 C30A C31A
ISOR 0.01 C18A C19A
ISOR 0.01 C21A C22A C23A
ISOR 0.01 C26A C27A
ISOR 0.01 C30A C31A
;

_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)+(0.0500P)²+0.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7812
_refine_ls_number_parameters     430
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1652
_refine_ls_wR_factor_gt          0.1226
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C18 C 0.7335(13) 0.7048(5) 0.6022(7) 0.130(3) Uani 0.62 1 d PDU A 1
H18A H 0.6556 0.7298 0.5736 0.156 Uiso 0.62 1 calc PR A 1
H18B H 0.7761 0.7357 0.6400 0.156 Uiso 0.62 1 calc PR A 1
C19 C 0.8439(11) 0.6829(7) 0.5585(6) 0.129(3) Uani 0.62 1 d PDU A 1
H19A H 0.9316 0.6712 0.5888 0.194 Uiso 0.62 1 calc PR A 1
H19B H 0.8602 0.7212 0.5284 0.194 Uiso 0.62 1 calc PR A 1
H19C H 0.8100 0.6424 0.5307 0.194 Uiso 0.62 1 calc PR A 1
C21 C 0.6978(13) 0.6557(5) 0.8059(6) 0.126(3) Uani 0.61 1 d PDU B 1
H21A H 0.7921 0.6507 0.8338 0.151 Uiso 0.61 1 calc PR B 1
H21B H 0.7063 0.6872 0.7673 0.151 Uiso 0.61 1 calc PR B 1
C22 C 0.5992(14) 0.6907(7) 0.8513(6) 0.138(3) Uani 0.61 1 d PDU B 1
H22A H 0.6139 0.7414 0.8553 0.166 Uiso 0.61 1 calc PR B 1
H22B H 0.4993 0.6808 0.8342 0.166 Uiso 0.61 1 calc PR B 1
C23 C 0.6528(13) 0.6532(7) 0.9186(6) 0.146(3) Uani 0.61 1 d PDU B 1
H23A H 0.6734 0.6048 0.9090 0.219 Uiso 0.61 1 calc PR B 1
H23B H 0.5814 0.6549 0.9481 0.219 Uiso 0.61 1 calc PR B 1
H23C H 0.7383 0.6759 0.9418 0.219 Uiso 0.61 1 calc PR B 1
C26 C 0.9991(11) 0.4407(7) 0.8713(6) 0.142(2) Uani 0.65 1 d PDU C 1
H26A H 1.0454 0.4057 0.8461 0.171 Uiso 0.65 1 calc PR C 1
H26B H 1.0602 0.4821 0.8781 0.171 Uiso 0.65 1 calc PR C 1
C27 C 0.9825(13) 0.4110(7) 0.9416(6) 0.157(3) Uani 0.65 1 d PDU C 1
H27A H 0.9214 0.4414 0.9631 0.236 Uiso 0.65 1 calc PR C 1
H27B H 1.0745 0.4082 0.9710 0.236 Uiso 0.65 1 calc PR C 1
H27C H 0.9411 0.3647 0.9356 0.236 Uiso 0.65 1 calc PR C 1
C30 C 0.6420(12) 0.3809(6) 0.6184(7) 0.142(2) Uani 0.66 1 d PDU D 1
H30A H 0.6956 0.3460 0.5969 0.171 Uiso 0.66 1 calc PR D 1
H30B H 0.6063 0.3595 0.6575 0.171 Uiso 0.66 1 calc PR D 1
C31 C 0.5240(12) 0.4113(6) 0.5666(7) 0.143(3) Uani 0.66 1 d PDU D 1
H31A H 0.4425 0.4195 0.5888 0.215 Uiso 0.66 1 calc PR D 1
H31B H 0.4987 0.3787 0.5285 0.215 Uiso 0.66 1 calc PR D 1
H31C H 0.5545 0.4552 0.5492 0.215 Uiso 0.66 1 calc PR D 1
C18A C 0.737(2) 0.6717(10) 0.5718(8) 0.135(3) Uani 0.38 1 d PDU A 2
H18C H 0.7889 0.6364 0.5499 0.162 Uiso 0.38 1 calc PR A 2
H18D H 0.6569 0.6872 0.5370 0.162 Uiso 0.38 1 calc PR A 2
C19A C 0.833(2) 0.7337(9) 0.5921(11) 0.139(4) Uani 0.38 1 d PDU A 2
H19D H 0.8057 0.7571 0.6317 0.209 Uiso 0.38 1 calc PR A 2
H19E H 0.8255 0.7662 0.5536 0.209 Uiso 0.38 1 calc PR A 2
H19F H 0.9300 0.7176 0.6040 0.209 Uiso 0.38 1 calc PR A 2
C21A C 0.7201(18) 0.6273(9) 0.8356(8) 0.127(3) Uani 0.39 1 d PDU B 2
H21C H 0.7682 0.6671 0.8183 0.152 Uiso 0.39 1 calc PR B 2
H21D H 0.7900 0.5998 0.8668 0.152 Uiso 0.39 1 calc PR B 2
C22A C 0.602(2) 0.6530(10) 0.8738(12) 0.135(3) Uani 0.39 1 d PDU B 2
H22C H 0.5169 0.6595 0.8389 0.162 Uiso 0.39 1 calc PR B 2
H22D H 0.5816 0.6148 0.9041 0.162 Uiso 0.39 1 calc PR B 2
C23A C 0.621(2) 0.7184(10) 0.9170(11) 0.148(4) Uani 0.39 1 d PDU B 2
H23D H 0.6682 0.7069 0.9635 0.221 Uiso 0.39 1 calc PR B 2
H23E H 0.5297 0.7390 0.9190 0.221 Uiso 0.39 1 calc PR B 2
H23F H 0.6785 0.7516 0.8964 0.221 Uiso 0.39 1 calc PR B 2
C26A C 0.986(2) 0.4535(12) 0.8842(12) 0.142(2) Uani 0.35 1 d PDU C 2
H26C H 1.0723 0.4672 0.8669 0.171 Uiso 0.35 1 calc PR C 2
H26D H 0.9771 0.4826 0.9244 0.171 Uiso 0.35 1 calc PR C 2
C27A C 0.991(2) 0.3757(10) 0.9036(13) 0.149(4) Uani 0.35 1 d PDU C 2
H27D H 0.9272 0.3670 0.9361 0.223 Uiso 0.35 1 calc PR C 2
H27E H 1.0864 0.3631 0.9248 0.223 Uiso 0.35 1 calc PR C 2
H27F H 0.9624 0.3478 0.8622 0.223 Uiso 0.35 1 calc PR C 2
C30A C 0.663(2) 0.3869(10) 0.5995(14) 0.142(2) Uani 0.34 1 d PDU D 2
H30C H 0.7017 0.3877 0.5563 0.171 Uiso 0.34 1 calc PR D 2
H30D H 0.7019 0.3447 0.6243 0.171 Uiso 0.34 1 calc PR D 2
C31A C 0.509(2) 0.3724(12) 0.5781(14) 0.147(4) Uani 0.34 1 d PDU D 2
H31D H 0.4893 0.3244 0.5896 0.221 Uiso 0.34 1 calc PR D 2
H31E H 0.4827 0.3794 0.5286 0.221 Uiso 0.34 1 calc PR D 2
H31F H 0.4551 0.4040 0.6023 0.221 Uiso 0.34 1 calc PR D 2
Br1 Br 1.10557(6) 0.13047(3) 0.13309(4) 0.1032(3) Uani 1 1 d . . .
Br2 Br 0.31008(6) 0.75994(3) 0.09353(4) 0.1115(3) Uani 1 1 d . . .
O1 O 0.6908(3) 0.44132(18) 0.08638(19) 0.0813(10) Uani 1 1 d . . .
O2 O 0.8748(3) 0.4195(2) 0.33513(18) 0.0933(11) Uani 1 1 d . . .
N2 N 0.6673(3) 0.4995(2) 0.1874(2) 0.0650(10) Uani 1 1 d . . .
H2 H 0.6909 0.4970 0.2322 0.078 Uiso 1 1 calc R . .
O3 O 0.6830(3) 0.48398(19) 0.33258(18) 0.0891(11) Uani 1 1 d . . .
N1 N 0.7829(4) 0.3941(2) 0.1935(2) 0.0658(10) Uani 1 1 d . . .
H1 H 0.7872 0.4010 0.2377 0.079 Uiso 1 1 calc R . .
C7 C 0.7116(5) 0.4445(3) 0.1502(3) 0.0651(13) Uani 1 1 d . . .
N3 N 0.7443(4) 0.5471(2) 0.7318(2) 0.0767(12) Uani 1 1 d . A .
C11 C 0.4242(5) 0.6786(3) 0.1202(3) 0.0722(14) Uani 1 1 d . . .
C4 C 0.8498(4) 0.3326(3) 0.1744(3) 0.0633(13) Uani 1 1 d . . .
C15 C 0.7873(5) 0.4521(3) 0.3641(3) 0.0619(13) Uani 1 1 d . . .
C8 C 0.5882(4) 0.5594(3) 0.1613(3) 0.0598(12) Uani 1 1 d . . .
C1 C 0.9987(4) 0.2125(3) 0.1490(3) 0.0725(14) Uani 1 1 d . . .
C16 C 0.7958(5) 0.6005(3) 0.6838(3) 0.0927(17) Uani 1 1 d . A .
H16A H 0.8602 0.5768 0.6575 0.111 Uiso 1 1 calc R . .
H16B H 0.8503 0.6365 0.7123 0.111 Uiso 1 1 calc R . .
C5 C 0.8714(5) 0.3167(3) 0.1069(3) 0.0734(14) Uani 1 1 d . . .
H5 H 0.8356 0.3467 0.0701 0.088 Uiso 1 1 calc R . .
C9 C 0.5706(5) 0.6121(3) 0.2085(3) 0.0678(13) Uani 1 1 d . . .
H9 H 0.6154 0.6077 0.2548 0.081 Uiso 1 1 calc R . .
C14 C 0.8142(6) 0.4533(3) 0.4424(3) 0.0945(17) Uani 1 1 d . . .
H14A H 0.8099 0.4060 0.4599 0.142 Uiso 1 1 calc R . .
H14B H 0.7429 0.4818 0.4587 0.142 Uiso 1 1 calc R . .
H14C H 0.9070 0.4729 0.4589 0.142 Uiso 1 1 calc R . .
C12 C 0.4415(5) 0.6281(3) 0.0724(3) 0.0791(15) Uani 1 1 d . . .
H12 H 0.3981 0.6340 0.0260 0.095 Uiso 1 1 calc R . .
C13 C 0.5230(5) 0.5679(3) 0.0917(3) 0.0746(14) Uani 1 1 d . . .
H13 H 0.5339 0.5337 0.0585 0.090 Uiso 1 1 calc R . .
C6 C 0.9452(5) 0.2571(3) 0.0943(3) 0.0773(15) Uani 1 1 d . . .
H6 H 0.9592 0.2466 0.0491 0.093 Uiso 1 1 calc R . .
C10 C 0.4883(5) 0.6710(3) 0.1887(3) 0.0784(14) Uani 1 1 d . . .
H10 H 0.4763 0.7054 0.2215 0.094 Uiso 1 1 calc R . .
C28 C 0.6579(5) 0.4890(3) 0.6916(3) 0.0843(16) Uani 1 1 d . A .
H28A H 0.5723 0.5098 0.6649 0.101 Uiso 1 1 calc R . .
H28B H 0.6281 0.4563 0.7249 0.101 Uiso 1 1 calc R . .
C3 C 0.9021(5) 0.2854(3) 0.2280(3) 0.0734(14) Uani 1 1 d . . .
H3 H 0.8864 0.2945 0.2732 0.088 Uiso 1 1 calc R . .
C2 C 0.9759(5) 0.2262(3) 0.2153(3) 0.0773(14) Uani 1 1 d . . .
H2A H 1.0105 0.1954 0.2517 0.093 Uiso 1 1 calc R . .
C24 C 0.8791(5) 0.5181(3) 0.7767(3) 0.0923(17) Uani 1 1 d . A .
H24A H 0.9408 0.4996 0.7459 0.111 Uiso 1 1 calc R . .
H24B H 0.9291 0.5569 0.8028 0.111 Uiso 1 1 calc R . .
C20 C 0.6485(5) 0.5821(3) 0.7754(3) 0.105(2) Uani 1 1 d D . .
H20A H 0.6387 0.5509 0.8141 0.126 Uiso 1 1 calc R B 1
H20B H 0.5546 0.5873 0.7471 0.126 Uiso 1 1 calc R B 1
C17 C 0.6783(5) 0.6371(3) 0.6318(4) 0.122(2) Uani 1 1 d D . .
H17A H 0.6438 0.6050 0.5937 0.147 Uiso 1 1 calc R A 1
H17B H 0.5988 0.6487 0.6553 0.147 Uiso 1 1 calc R A 1
C29 C 0.7337(6) 0.4471(3) 0.6416(3) 0.114(2) Uani 1 1 d D . .
H29A H 0.8282 0.4332 0.6648 0.137 Uiso 1 1 calc R D 1
H29B H 0.7438 0.4758 0.6012 0.137 Uiso 1 1 calc R D 1
C25 C 0.8559(6) 0.4611(4) 0.8274(4) 0.135(3) Uani 1 1 d D . .
H25A H 0.8129 0.4201 0.8021 0.162 Uiso 1 1 calc R C 1
H25B H 0.7915 0.4779 0.8576 0.162 Uiso 1 1 calc R C 1


_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
C18 C19 1.514(8) . ?
C18 C17 1.530(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 C22 1.541(8) . ?
C21 C20 1.552(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.495(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C26 C27 1.508(9) . ?
C26 C25 1.528(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C30 C31 1.487(9) . ?
C30 C29 1.548(8) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C18A C19A 1.499(10) . ?
C18A C17 1.520(9) . ?
C18A H18C 0.9700 . ?
C18A H18D 0.9700 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C21A C20 1.511(9) . ?
C21A C22A 1.527(10) . ?
C21A H21C 0.9700 . ?
C21A H21D 0.9700 . ?
C22A C23A 1.488(10) . ?
C22A H22C 0.9700 . ?
C22A H22D 0.9700 . ?
C23A H23D 0.9600 . ?
C23A H23E 0.9600 . ?
C23A H23F 0.9600 . ?
C26A C27A 1.516(10) . ?
C26A C25 1.519(10) . ?
C26A H26C 0.9700 . ?
C26A H26D 0.9700 . ?
C27A H27D 0.9600 . ?
C27A H27E 0.9600 . ?
C27A H27F 0.9600 . ?
C30A C31A 1.479(10) . ?
C30A C29 1.492(10) . ?
C30A H30C 0.9700 . ?
C30A H30D 0.9700 . ?
C31A H31D 0.9600 . ?
C31A H31E 0.9600 . ?
C31A H31F 0.9600 . ?
Br1 C1 1.907(5) . ?
Br2 C11 1.902(5) . ?
O1 C7 1.220(5) . ?
O2 C15 1.244(5) . ?
N2 C7 1.372(5) . ?
N2 C8 1.404(5) . ?
N2 H2 0.8600 . ?
O3 C15 1.230(5) . ?
N1 C7 1.371(6) . ?
N1 C4 1.406(5) . ?
N1 H1 0.8600 . ?
N3 C20 1.498(5) . ?
N3 C28 1.506(6) . ?
N3 C16 1.510(6) . ?
N3 C24 1.523(6) . ?
C11 C12 1.360(6) . ?
C11 C10 1.371(6) . ?
C4 C5 1.391(6) . ?
C4 C3 1.395(6) . ?
C15 C14 1.496(6) . ?
C8 C9 1.382(6) . ?
C8 C13 1.397(6) . ?
C1 C2 1.365(7) . ?
C1 C6 1.382(7) . ?
C16 C17 1.537(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C5 C6 1.371(6) . ?
C5 H5 0.9300 . ?
C9 C10 1.378(6) . ?
C9 H9 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C12 C13 1.392(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C6 H6 0.9300 . ?
C10 H10 0.9300 . ?
C28 C29 1.525(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C3 C2 1.365(6) . ?
C3 H3 0.9300 . ?
C2 H2A 0.9300 . ?
C24 C25 1.499(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?

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
C19 C18 C17 107.2(8) . . ?
C19 C18 H18A 110.3 . . ?
C17 C18 H18A 110.3 . . ?
C19 C18 H18B 110.3 . . ?
C17 C18 H18B 110.3 . . ?
H18A C18 H18B 108.5 . . ?
C22 C21 C20 115.4(9) . . ?
C22 C21 H21A 108.4 . . ?
C20 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
C20 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C23 C22 C21 98.4(10) . . ?
C23 C22 H22A 112.1 . . ?
C21 C22 H22A 112.1 . . ?
C23 C22 H22B 112.1 . . ?
C21 C22 H22B 112.1 . . ?
H22A C22 H22B 109.7 . . ?
C27 C26 C25 112.2(9) . . ?
C27 C26 H26A 109.2 . . ?
C25 C26 H26A 109.2 . . ?
C27 C26 H26B 109.2 . . ?
C25 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
C31 C30 C29 101.9(9) . . ?
C31 C30 H30A 111.4 . . ?
C29 C30 H30A 111.4 . . ?
C31 C30 H30B 111.4 . . ?
C29 C30 H30B 111.4 . . ?
H30A C30 H30B 109.2 . . ?
C19A C18A C17 114.9(13) . . ?
C19A C18A H18C 108.5 . . ?
C17 C18A H18C 108.5 . . ?
C19A C18A H18D 108.5 . . ?
C17 C18A H18D 108.5 . . ?
H18C C18A H18D 107.5 . . ?
C18A C19A H19D 109.5 . . ?
C18A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C18A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C20 C21A C22A 106.4(11) . . ?
C20 C21A H21C 110.5 . . ?
C22A C21A H21C 110.5 . . ?
C20 C21A H21D 110.5 . . ?
C22A C21A H21D 110.5 . . ?
H21C C21A H21D 108.6 . . ?
C23A C22A C21A 120.5(15) . . ?
C23A C22A H22C 107.2 . . ?
C21A C22A H22C 107.2 . . ?
C23A C22A H22D 107.2 . . ?
C21A C22A H22D 107.2 . . ?
H22C C22A H22D 106.8 . . ?
C22A C23A H23D 109.5 . . ?
C22A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C22A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C27A C26A C25 105.0(15) . . ?
C27A C26A H26C 110.8 . . ?
C25 C26A H26C 110.8 . . ?
C27A C26A H26D 110.8 . . ?
C25 C26A H26D 110.8 . . ?
H26C C26A H26D 108.8 . . ?
C26A C27A H27D 109.5 . . ?
C26A C27A H27E 109.5 . . ?
H27D C27A H27E 109.5 . . ?
C26A C27A H27F 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C31A C30A C29 128.8(18) . . ?
C31A C30A H30C 105.1 . . ?
C29 C30A H30C 105.1 . . ?
C31A C30A H30D 105.1 . . ?
C29 C30A H30D 105.1 . . ?
H30C C30A H30D 105.9 . . ?
C30A C31A H31D 109.5 . . ?
C30A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C30A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C7 N2 C8 127.9(4) . . ?
C7 N2 H2 116.0 . . ?
C8 N2 H2 116.0 . . ?
C7 N1 C4 127.7(4) . . ?
C7 N1 H1 116.2 . . ?
C4 N1 H1 116.2 . . ?
O1 C7 N1 124.4(5) . . ?
O1 C7 N2 124.0(5) . . ?
N1 C7 N2 111.6(5) . . ?
C20 N3 C28 106.5(3) . . ?
C20 N3 C16 110.1(4) . . ?
C28 N3 C16 111.9(4) . . ?
C20 N3 C24 111.7(4) . . ?
C28 N3 C24 111.4(4) . . ?
C16 N3 C24 105.3(3) . . ?
C12 C11 C10 120.1(5) . . ?
C12 C11 Br2 120.7(4) . . ?
C10 C11 Br2 119.2(4) . . ?
C5 C4 C3 118.2(5) . . ?
C5 C4 N1 124.9(5) . . ?
C3 C4 N1 116.9(5) . . ?
O3 C15 O2 124.2(5) . . ?
O3 C15 C14 118.8(5) . . ?
O2 C15 C14 117.0(4) . . ?
C9 C8 C13 118.2(5) . . ?
C9 C8 N2 117.4(4) . . ?
C13 C8 N2 124.3(5) . . ?
C2 C1 C6 120.7(5) . . ?
C2 C1 Br1 118.7(5) . . ?
C6 C1 Br1 120.5(5) . . ?
N3 C16 C17 115.5(4) . . ?
N3 C16 H16A 108.4 . . ?
C17 C16 H16A 108.4 . . ?
N3 C16 H16B 108.4 . . ?
C17 C16 H16B 108.4 . . ?
H16A C16 H16B 107.5 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C10 C9 C8 121.7(5) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C8 119.3(5) . . ?
C12 C13 H13 120.3 . . ?
C8 C13 H13 120.3 . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
C11 C10 C9 119.5(5) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
N3 C28 C29 115.7(4) . . ?
N3 C28 H28A 108.4 . . ?
C29 C28 H28A 108.4 . . ?
N3 C28 H28B 108.4 . . ?
C29 C28 H28B 108.4 . . ?
H28A C28 H28B 107.4 . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C3 C2 C1 119.6(5) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C25 C24 N3 115.5(4) . . ?
C25 C24 H24A 108.4 . . ?
N3 C24 H24A 108.4 . . ?
C25 C24 H24B 108.4 . . ?
N3 C24 H24B 108.4 . . ?
H24A C24 H24B 107.5 . . ?
N3 C20 C21A 116.6(7) . . ?
N3 C20 C21 116.0(6) . . ?
C21A C20 C21 29.8(9) . . ?
N3 C20 H20A 108.3 . . ?
C21A C20 H20A 80.7 . . ?
C21 C20 H20A 108.3 . . ?
N3 C20 H20B 108.3 . . ?
C21A C20 H20B 129.1 . . ?
C21 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C18A C17 C18 32.9(7) . . ?
C18A C17 C16 112.2(10) . . ?
C18 C17 C16 111.4(7) . . ?
C18A C17 H17A 78.8 . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
C18A C17 H17B 132.6 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
C30A C29 C28 121.8(10) . . ?
C30A C29 C30 17.3(14) . . ?
C28 C29 C30 107.5(6) . . ?
C30A C29 H29A 109.9 . . ?
C28 C29 H29A 110.2 . . ?
C30 C29 H29A 110.2 . . ?
C30A C29 H29B 94.7 . . ?
C28 C29 H29B 110.2 . . ?
C30 C29 H29B 110.2 . . ?
H29A C29 H29B 108.5 . . ?
C24 C25 C26A 110.5(10) . . ?
C24 C25 C26 109.3(6) . . ?
C26A C25 C26 14.4(15) . . ?
C24 C25 H25A 109.8 . . ?
C26A C25 H25A 120.8 . . ?
C26 C25 H25A 109.8 . . ?
C24 C25 H25B 109.8 . . ?
C26A C25 H25B 96.5 . . ?
C26 C25 H25B 109.8 . . ?
H25A C25 H25B 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.69
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.052
_database_code_depnum_ccdc_archive 'CCDC 973825'
