# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_L1-Cd
_database_code_depnum_ccdc_archive 'CCDC 989402'
_audit_update_record             
;
2014-03-02 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 Cd Cl2 N8 O2,2(H2O)'
_chemical_formula_sum            'C34 H40 Cd Cl2 N8 O4'

_chemical_formula_weight         808.05

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   18.0309(4)
_cell_length_b                   10.7197(4)
_cell_length_c                   20.3059(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.574(2)
_cell_angle_gamma                90.00
_cell_volume                     3649.88(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      26.62

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656.0
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_process_details   SADBAS

_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            22411
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4158
_reflns_number_gt                3086
_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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3766
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   0.783
_refine_ls_restrained_S_all      0.783
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.0000 0.74210(2) 0.2500 0.03786(12) Uani 1 2 d S . .
Cl2 Cl 1.05325(4) 0.86882(7) 0.17520(4) 0.0563(2) Uani 1 1 d . . .
C3 C 0.74959(16) 0.4146(3) -0.02889(15) 0.0493(6) Uani 1 1 d . . .
H3 H 0.7044 0.4434 -0.0219 0.059 Uiso 1 1 calc R . .
C9 C 1.06886(15) 0.4975(2) 0.17794(12) 0.0455(6) Uani 1 1 d . . .
H9 H 1.1108 0.4544 0.1721 0.055 Uiso 1 1 calc R . .
C2 C 0.82273(16) 0.4287(3) 0.02402(13) 0.0497(6) Uani 1 1 d . . .
H2 H 0.8258 0.4655 0.0664 0.060 Uiso 1 1 calc R . .
C8 C 0.98945(15) 0.4804(2) 0.12817(13) 0.0475(6) Uani 1 1 d . . .
H8 H 0.9481 0.5205 0.1367 0.057 Uiso 1 1 calc R . .
C7 C 0.97126(15) 0.4096(3) 0.06970(13) 0.0509(7) Uani 1 1 d . . .
H7 H 1.0136 0.3693 0.0630 0.061 Uiso 1 1 calc R . .
C6 C 0.88439(17) 0.3290(2) -0.04740(13) 0.0500(7) Uani 1 1 d . . .
H6 H 0.9296 0.2991 -0.0540 0.060 Uiso 1 1 calc R . .
C5 C 0.81120(17) 0.3129(3) -0.10027(14) 0.0549(7) Uani 1 1 d . . .
H5 H 0.8079 0.2714 -0.1415 0.066 Uiso 1 1 calc R . .
C1 C 0.89311(15) 0.3891(2) 0.01621(12) 0.0455(6) Uani 1 1 d . . .
C4 C 0.74133(16) 0.3576(2) -0.09369(13) 0.0484(6) Uani 1 1 d . . .
N1 N 1.08286(11) 0.57211(19) 0.23073(10) 0.0407(5) Uani 1 1 d . . .
N2 N 1.16155(12) 0.5822(2) 0.27667(10) 0.0411(5) Uani 1 1 d . . .
C10 C 1.17772(14) 0.6602(2) 0.33181(12) 0.0388(5) Uani 1 1 d . . .
O1 O 1.12653(12) 0.72642(18) 0.34215(10) 0.0473(5) Uani 1 1 d . . .
C11 C 1.26184(13) 0.6594(2) 0.38342(12) 0.0386(5) Uani 1 1 d . . .
C12 C 1.28833(19) 0.7507(2) 0.43435(18) 0.0501(7) Uani 1 1 d . . .
H12 H 1.2560 0.8184 0.4341 0.060 Uiso 1 1 calc R . .
N4 N 1.30564(14) 0.5624(3) 0.38037(12) 0.0615(7) Uani 1 1 d . . .
C13 C 1.3635(2) 0.7403(3) 0.48579(18) 0.0571(8) Uani 1 1 d . . .
H13 H 1.3825 0.8002 0.5212 0.068 Uiso 1 1 calc R . .
C14 C 1.40936(16) 0.6402(3) 0.48372(14) 0.0605(8) Uani 1 1 d . . .
H14 H 1.4603 0.6304 0.5178 0.073 Uiso 1 1 calc R . .
C16 C 1.37890(18) 0.5543(4) 0.43043(16) 0.0771(11) Uani 1 1 d . . .
H16 H 1.4107 0.4869 0.4290 0.093 Uiso 1 1 calc R . .
N3 N 0.66841(15) 0.3502(3) -0.14830(13) 0.0715(8) Uani 1 1 d . . .
C18 C 0.5980(2) 0.4022(4) -0.14070(19) 0.0860(11) Uani 1 1 d . . .
H18A H 0.5825 0.3510 -0.1092 0.129 Uiso 1 1 calc R . .
H18B H 0.5554 0.4050 -0.1862 0.129 Uiso 1 1 calc R . .
H18C H 0.6093 0.4851 -0.1218 0.129 Uiso 1 1 calc R . .
C17 C 0.6547(3) 0.2634(3) -0.2056(2) 0.0819(13) Uani 1 1 d . . .
H17A H 0.6835 0.2900 -0.2346 0.123 Uiso 1 1 calc R . .
H17B H 0.5987 0.2604 -0.2337 0.123 Uiso 1 1 calc R . .
H17C H 0.6727 0.1820 -0.1868 0.123 Uiso 1 1 calc R . .
O2 O 0.26570(14) 0.4363(3) 0.22612(15) 0.0648(6) Uani 1 1 d . . .
H2N H 1.2032(18) 0.544(2) 0.2714(14) 0.039(7) Uiso 1 1 d . . .
H2O H 0.279(2) 0.459(4) 0.2006(18) 0.068(14) Uiso 1 1 d . . .
H3O H 0.309(3) 0.425(4) 0.264(2) 0.113(16) Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.3654(19) 2_755 ?
Cd1 O1 2.3654(19) . ?
Cd1 N1 2.477(2) 2_755 ?
Cd1 N1 2.477(2) . ?
Cd1 Cl2 2.4793(7) 2_755 ?
Cd1 Cl2 2.4793(7) . ?
C3 C2 1.369(4) . ?
C3 C4 1.408(4) . ?
C9 N1 1.285(3) . ?
C9 C8 1.429(3) . ?
C2 C1 1.401(4) . ?
C8 C7 1.344(3) . ?
C7 C1 1.445(3) . ?
C6 C5 1.372(4) . ?
C6 C1 1.400(3) . ?
C5 C4 1.399(4) . ?
C4 N3 1.376(3) . ?
N1 N2 1.386(3) . ?
N2 C10 1.341(3) . ?
C10 O1 1.242(3) . ?
C10 C11 1.493(3) . ?
C11 N4 1.321(3) . ?
C11 C12 1.375(4) . ?
C12 C13 1.378(5) . ?
N4 C16 1.341(3) . ?
C13 C14 1.365(4) . ?
C14 C16 1.372(4) . ?
N3 C17 1.438(4) . ?
N3 C18 1.446(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O1 171.85(10) 2_755 . ?
O1 Cd1 N1 67.07(6) 2_755 2_755 ?
O1 Cd1 N1 106.57(7) . 2_755 ?
O1 Cd1 N1 106.57(7) 2_755 . ?
O1 Cd1 N1 67.07(6) . . ?
N1 Cd1 N1 85.28(9) 2_755 . ?
O1 Cd1 Cl2 92.60(6) 2_755 2_755 ?
O1 Cd1 Cl2 91.86(5) . 2_755 ?
N1 Cd1 Cl2 85.08(5) 2_755 2_755 ?
N1 Cd1 Cl2 153.11(5) . 2_755 ?
O1 Cd1 Cl2 91.86(5) 2_755 . ?
O1 Cd1 Cl2 92.60(6) . . ?
N1 Cd1 Cl2 153.11(5) 2_755 . ?
N1 Cd1 Cl2 85.08(5) . . ?
Cl2 Cd1 Cl2 113.55(4) 2_755 . ?
C2 C3 C4 121.4(3) . . ?
N1 C9 C8 120.6(2) . . ?
C3 C2 C1 121.9(2) . . ?
C7 C8 C9 123.6(3) . . ?
C8 C7 C1 127.1(2) . . ?
C5 C6 C1 122.0(3) . . ?
C6 C5 C4 121.5(2) . . ?
C6 C1 C2 116.4(2) . . ?
C6 C1 C7 120.7(2) . . ?
C2 C1 C7 122.9(2) . . ?
N3 C4 C5 122.0(2) . . ?
N3 C4 C3 121.3(3) . . ?
C5 C4 C3 116.6(2) . . ?
C9 N1 N2 116.6(2) . . ?
C9 N1 Cd1 130.10(16) . . ?
N2 N1 Cd1 111.33(14) . . ?
C10 N2 N1 117.7(2) . . ?
O1 C10 N2 123.4(2) . . ?
O1 C10 C11 120.7(2) . . ?
N2 C10 C11 115.8(2) . . ?
C10 O1 Cd1 117.87(15) . . ?
N4 C11 C12 123.2(2) . . ?
N4 C11 C10 116.2(2) . . ?
C12 C11 C10 120.4(2) . . ?
C11 C12 C13 119.0(3) . . ?
C11 N4 C16 117.0(2) . . ?
C14 C13 C12 118.6(3) . . ?
C13 C14 C16 118.7(3) . . ?
N4 C16 C14 123.5(3) . . ?
C4 N3 C17 121.2(3) . . ?
C4 N3 C18 120.6(2) . . ?
C17 N3 C18 116.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.054
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_L1
_database_code_depnum_ccdc_archive 'CCDC 989403'
_audit_update_record             
;
2014-03-02 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H18 N4 O'
_chemical_formula_sum            'C17 H18 N4 O'

_chemical_formula_weight         294.35

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   5.9895(4)
_cell_length_b                   14.7978(8)
_cell_length_c                   17.8142(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.481(6)
_cell_angle_gamma                90.00
_cell_volume                     1568.81(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.23

_exptl_crystal_description       neddle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624.0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_T_max  0.989
_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            6970
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         28.72
_reflns_number_total             5103
_reflns_number_gt                2513
_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)+(0.1795P)²+0.7995P] 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(5)
_refine_ls_number_reflns         7981
_refine_ls_number_parameters     401
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.3180
_refine_ls_wR_factor_gt          0.2489
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_restrained_S_all      0.932
_refine_ls_shift/su_max          0.003
_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
N6 N 0.3143(12) 0.4875(4) 0.1084(3) 0.0632(16) Uani 1 1 d . . .
H6NA H 0.1874 0.5148 0.0993 0.076 Uiso 1 1 calc R . .
N7 N 0.3228(11) 0.4023(4) 0.1423(3) 0.0650(17) Uani 1 1 d . . .
C23 C 0.5012(13) 0.5273(5) 0.0900(4) 0.0544(17) Uani 1 1 d . . .
O2 O 0.6890(10) 0.4978(4) 0.1053(3) 0.0820(17) Uani 1 1 d . . .
N5 N 0.2423(10) 0.6296(5) 0.0176(4) 0.0690(18) Uani 1 1 d . . .
C22 C 0.4570(12) 0.6130(5) 0.0464(3) 0.0546(18) Uani 1 1 d . . .
O1 O 1.4874(11) 0.7120(5) 0.2362(4) 0.112(3) Uani 1 1 d . . .
N3 N 1.1124(13) 0.6140(5) 0.2627(4) 0.0780(19) Uani 1 1 d . . .
N2 N 1.1152(13) 0.6882(5) 0.2149(4) 0.077(2) Uani 1 1 d . . .
H2NA H 0.9914 0.7044 0.1893 0.093 Uiso 1 1 calc R . .
C24 C 0.1342(14) 0.3755(5) 0.1639(4) 0.0621(19) Uani 1 1 d . . .
H24 H 0.0104 0.4139 0.1592 0.074 Uiso 1 1 calc R . .
N1 N 1.0570(11) 0.8346(5) 0.1284(4) 0.076(2) Uani 1 1 d . . .
C27 C -0.1059(14) 0.1685(6) 0.2524(4) 0.061(2) Uani 1 1 d . . .
C25 C 0.1165(14) 0.2871(6) 0.1951(4) 0.0630(19) Uani 1 1 d . . .
H25 H 0.2390 0.2482 0.1965 0.076 Uiso 1 1 calc R . .
C5 C 1.2668(15) 0.8199(6) 0.1611(4) 0.070(2) Uani 1 1 d . . .
C6 C 1.2999(16) 0.7354(6) 0.2070(5) 0.075(2) Uani 1 1 d . . .
C10 C 0.6243(14) 0.3973(6) 0.3706(4) 0.069(2) Uani 1 1 d . . .
N8 N -0.2240(16) -0.0851(6) 0.3507(5) 0.102(3) Uani 1 1 d . . .
C30 C -0.1896(15) -0.0018(6) 0.3183(5) 0.073(2) Uani 1 1 d . . .
C19 C 0.3715(14) 0.7653(6) -0.0370(4) 0.072(2) Uani 1 1 d . . .
H19 H 0.3370 0.8171 -0.0655 0.087 Uiso 1 1 calc R . .
C18 C 0.2093(13) 0.7043(7) -0.0237(5) 0.076(2) Uani 1 1 d . . .
H18 H 0.0636 0.7161 -0.0453 0.092 Uiso 1 1 calc R . .
C26 C -0.0677(14) 0.2586(6) 0.2220(4) 0.066(2) Uani 1 1 d . . .
H26 H -0.1851 0.2998 0.2215 0.079 Uiso 1 1 calc R . .
C29 C -0.0027(14) 0.0131(6) 0.2812(5) 0.077(2) Uani 1 1 d . . .
H29 H 0.0995 -0.0336 0.2778 0.092 Uiso 1 1 calc R . .
C21 C 0.6297(13) 0.6702(6) 0.0360(4) 0.064(2) Uani 1 1 d . . .
H21 H 0.7749 0.6573 0.0576 0.077 Uiso 1 1 calc R . .
C7 C 0.9126(17) 0.5813(6) 0.2688(5) 0.071(2) Uani 1 1 d . . .
H7 H 0.7891 0.6063 0.2398 0.085 Uiso 1 1 calc R . .
C11 C 0.7748(14) 0.3586(6) 0.4281(4) 0.072(2) Uani 1 1 d . . .
H11 H 0.9172 0.3837 0.4386 0.086 Uiso 1 1 calc R . .
C20 C 0.5877(14) 0.7468(6) -0.0066(5) 0.080(2) Uani 1 1 d . . .
H20 H 0.7043 0.7858 -0.0147 0.096 Uiso 1 1 calc R . .
C8 C 0.8784(17) 0.5083(6) 0.3189(5) 0.076(2) Uani 1 1 d . . .
H8 H 1.0023 0.4857 0.3493 0.091 Uiso 1 1 calc R . .
C9 C 0.6843(16) 0.4721(7) 0.3241(5) 0.078(3) Uani 1 1 d . . .
H9 H 0.5652 0.4978 0.2934 0.093 Uiso 1 1 calc R . .
C12 C 0.7188(14) 0.2849(7) 0.4692(4) 0.076(2) Uani 1 1 d . . .
H12 H 0.8250 0.2603 0.5056 0.092 Uiso 1 1 calc R . .
C13 C 0.5048(15) 0.2464(7) 0.4569(4) 0.077(2) Uani 1 1 d . . .
N4 N 0.4502(14) 0.1705(7) 0.4969(4) 0.098(3) Uani 1 1 d . . .
C3 C 1.4021(16) 0.9583(8) 0.1179(5) 0.086(3) Uani 1 1 d . . .
H3 H 1.5171 1.0003 0.1168 0.104 Uiso 1 1 calc R . .
C31 C -0.3317(15) 0.0722(7) 0.3238(6) 0.085(3) Uani 1 1 d . . .
H31 H -0.4566 0.0663 0.3501 0.103 Uiso 1 1 calc R . .
C33 C -0.0851(17) -0.1591(7) 0.3427(7) 0.103(3) Uani 1 1 d . . .
H33B H -0.0883 -0.1739 0.2902 0.154 Uiso 1 1 calc R . .
H33A H -0.1371 -0.2098 0.3695 0.154 Uiso 1 1 calc R . .
H33C H 0.0659 -0.1445 0.3630 0.154 Uiso 1 1 calc R . .
C14 C 0.3518(13) 0.2854(7) 0.4005(5) 0.078(3) Uani 1 1 d . . .
H14 H 0.2078 0.2618 0.3902 0.094 Uiso 1 1 calc R . .
C1 C 1.0268(18) 0.9113(7) 0.0881(5) 0.087(3) Uani 1 1 d . . .
H1 H 0.8842 0.9227 0.0635 0.105 Uiso 1 1 calc R . .
C28 C 0.0362(15) 0.0946(7) 0.2492(5) 0.077(3) Uani 1 1 d . . .
H28 H 0.1635 0.1011 0.2242 0.093 Uiso 1 1 calc R . .
C32 C -0.2902(14) 0.1528(6) 0.2914(5) 0.077(2) Uani 1 1 d . . .
H32 H -0.3907 0.1999 0.2956 0.092 Uiso 1 1 calc R . .
C4 C 1.4373(16) 0.8791(8) 0.1568(5) 0.085(3) Uani 1 1 d . . .
H4 H 1.5798 0.8656 0.1806 0.101 Uiso 1 1 calc R . .
C15 C 0.4152(14) 0.3580(7) 0.3609(4) 0.074(2) Uani 1 1 d . . .
H15 H 0.3091 0.3828 0.3246 0.088 Uiso 1 1 calc R . .
C2 C 1.1927(17) 0.9742(8) 0.0805(5) 0.091(3) Uani 1 1 d . . .
H2 H 1.1637 1.0257 0.0510 0.109 Uiso 1 1 calc R . .
C16 C 0.610(2) 0.1336(9) 0.5565(6) 0.127(5) Uani 1 1 d . . .
H16B H 0.7293 0.1038 0.5346 0.191 Uiso 1 1 calc R . .
H16A H 0.5351 0.0909 0.5856 0.191 Uiso 1 1 calc R . .
H16C H 0.6708 0.1816 0.5888 0.191 Uiso 1 1 calc R . .
C17 C 0.2406(18) 0.1243(9) 0.4815(7) 0.123(4) Uani 1 1 d . . .
H17A H 0.1219 0.1618 0.4959 0.185 Uiso 1 1 calc R . .
H17B H 0.2456 0.0690 0.5097 0.185 Uiso 1 1 calc R . .
H17C H 0.2136 0.1112 0.4285 0.185 Uiso 1 1 calc R . .
C34 C -0.409(2) -0.0968(10) 0.3938(8) 0.149(6) Uani 1 1 d . . .
H34C H -0.4139 -0.0472 0.4284 0.224 Uiso 1 1 calc R . .
H34B H -0.3913 -0.1524 0.4216 0.224 Uiso 1 1 calc R . .
H34A H -0.5466 -0.0986 0.3604 0.224 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
N6 C23 1.338(9) . ?
N6 N7 1.396(9) . ?
N7 C24 1.296(10) . ?
C23 O2 1.209(8) . ?
C23 C22 1.495(10) . ?
N5 C18 1.330(10) . ?
N5 C22 1.352(9) . ?
C22 C21 1.366(11) . ?
O1 C6 1.232(10) . ?
N3 C7 1.306(12) . ?
N3 N2 1.391(10) . ?
N2 C6 1.328(11) . ?
C24 C25 1.431(11) . ?
N1 C1 1.345(12) . ?
N1 C5 1.342(10) . ?
C27 C32 1.389(11) . ?
C27 C28 1.390(11) . ?
C27 C26 1.467(11) . ?
C25 C26 1.320(11) . ?
C5 C4 1.354(13) . ?
C5 C6 1.496(12) . ?
C10 C15 1.373(12) . ?
C10 C11 1.407(10) . ?
C10 C9 1.452(13) . ?
N8 C30 1.386(11) . ?
N8 C33 1.392(12) . ?
N8 C34 1.429(13) . ?
C30 C29 1.381(11) . ?
C30 C31 1.397(13) . ?
C19 C18 1.365(12) . ?
C19 C20 1.374(11) . ?
C29 C28 1.365(12) . ?
C21 C20 1.371(12) . ?
C7 C8 1.431(13) . ?
C11 C12 1.377(12) . ?
C8 C9 1.293(12) . ?
C12 C13 1.397(12) . ?
C13 N4 1.388(12) . ?
C13 C14 1.406(11) . ?
N4 C17 1.429(14) . ?
N4 C16 1.454(13) . ?
C3 C4 1.366(14) . ?
C3 C2 1.373(13) . ?
C31 C32 1.360(12) . ?
C14 C15 1.362(13) . ?
C1 C2 1.379(14) . ?

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
C23 N6 N7 120.8(7) . . ?
C24 N7 N6 114.5(7) . . ?
O2 C23 N6 124.7(7) . . ?
O2 C23 C22 122.0(7) . . ?
N6 C23 C22 113.3(7) . . ?
C18 N5 C22 115.9(7) . . ?
N5 C22 C21 122.6(7) . . ?
N5 C22 C23 117.2(7) . . ?
C21 C22 C23 120.2(7) . . ?
C7 N3 N2 114.7(7) . . ?
C6 N2 N3 123.2(7) . . ?
N7 C24 C25 120.0(7) . . ?
C1 N1 C5 115.6(8) . . ?
C32 C27 C28 114.4(8) . . ?
C32 C27 C26 120.2(7) . . ?
C28 C27 C26 125.3(7) . . ?
C26 C25 C24 122.3(8) . . ?
N1 C5 C4 123.1(8) . . ?
N1 C5 C6 115.6(8) . . ?
C4 C5 C6 121.2(8) . . ?
O1 C6 N2 122.6(9) . . ?
O1 C6 C5 121.5(9) . . ?
N2 C6 C5 115.9(8) . . ?
C15 C10 C11 114.8(8) . . ?
C15 C10 C9 122.1(8) . . ?
C11 C10 C9 123.1(8) . . ?
C30 N8 C33 122.5(8) . . ?
C30 N8 C34 119.5(9) . . ?
C33 N8 C34 117.9(9) . . ?
N8 C30 C29 120.6(9) . . ?
N8 C30 C31 123.2(8) . . ?
C29 C30 C31 116.2(8) . . ?
C18 C19 C20 117.2(8) . . ?
N5 C18 C19 125.5(8) . . ?
C25 C26 C27 126.5(8) . . ?
C28 C29 C30 121.8(8) . . ?
C22 C21 C20 119.5(8) . . ?
N3 C7 C8 121.9(9) . . ?
C12 C11 C10 122.3(8) . . ?
C19 C20 C21 119.3(8) . . ?
C9 C8 C7 123.4(9) . . ?
C8 C9 C10 129.8(8) . . ?
C11 C12 C13 121.0(8) . . ?
N4 C13 C12 121.0(8) . . ?
N4 C13 C14 121.8(9) . . ?
C12 C13 C14 117.2(8) . . ?
C13 N4 C17 122.8(9) . . ?
C13 N4 C16 120.4(9) . . ?
C17 N4 C16 116.9(9) . . ?
C4 C3 C2 118.3(10) . . ?
C32 C31 C30 121.0(8) . . ?
C15 C14 C13 119.8(8) . . ?
N1 C1 C2 124.6(10) . . ?
C29 C28 C27 122.9(8) . . ?
C31 C32 C27 123.6(8) . . ?
C5 C4 C3 120.6(9) . . ?
C14 C15 C10 124.9(8) . . ?
C3 C2 C1 117.7(10) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.72
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.038
