Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Martin Schroder'
'A. Blake'
'Neil Champness'
'Alessandra Garau'
'Caitlin Horn'
'Vito Lippolis'
'Claire Wilson'

_publ_contact_author_name        'Prof Martin Schroder'
_publ_contact_author_address     
;
School of Chemistry
University of Nottingham
University Park
Nottingham
NG7 2RD
UNITED KINGDOM
;

_publ_contact_author_email       M.SCHRODER@NOTTINGHAM.AC.UK

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Helical templating of polyiodide networks at a
binuclear metallo complex
;

data_NIN8II
_database_code_CSD               198624

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;  
?  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H24 I12 N10 Ni'
_chemical_formula_weight         2058.06

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'
Ni Ni 0.3393 1.1124 '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   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                   13.497(2)
_cell_length_b                   35.962(6)
_cell_length_c                   20.498(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.127(3)
_cell_angle_gamma                90.00
_cell_volume                     9456(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    606
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.15

_exptl_crystal_description       'Irregular block'
_exptl_crystal_colour            Red-black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7312
_exptl_absorpt_coefficient_mu    8.278
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_T_max  0.316
_exptl_absorpt_process_details   ?

_exptl_special_details           
;  
?  
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        none
_diffrn_reflns_number            9308
_diffrn_reflns_av_R_equivalents  0.117
_diffrn_reflns_av_sigmaI/netI    0.081
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_theta_max         26.00
_reflns_number_total             9308
_reflns_number_gt                5350
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'

_refine_special_details          
;  
?  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.052P)^2^+1669P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9308
_refine_ls_number_parameters     443
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.149
_refine_ls_R_factor_gt           0.095
_refine_ls_wR_factor_ref         0.239
_refine_ls_wR_factor_gt          0.216
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.021
_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
Ni1 Ni 1.0522(2) 0.87506(8) 0.35698(16) 0.0256(6) Uani 1 1 d U . .
I1 I 0.7716(2) 0.79964(6) 0.66733(18) 0.0849(9) Uani 1 1 d U . .
I2 I 0.64861(19) 0.79186(6) 0.52908(17) 0.0789(9) Uani 1 1 d U . .
I3 I 0.53424(19) 0.79360(6) 0.36614(13) 0.0630(6) Uani 1 1 d U . .
I4 I 0.55646(14) 0.87641(5) 0.36700(10) 0.0429(4) Uani 1 1 d U . .
I5 I 0.57741(17) 0.95641(5) 0.37261(11) 0.0547(5) Uani 1 1 d U . .
I6 I 0.62721(16) 0.95767(6) 0.54994(14) 0.0653(7) Uani 1 1 d U . .
I7 I 0.64773(16) 0.94980(5) 0.68799(14) 0.0640(7) Uani 1 1 d U . .
I10 I 0.92197(16) 0.80643(5) 0.85281(11) 0.0508(5) Uani 1 1 d U . .
I9 I 0.80687(15) 0.87350(6) 0.86012(10) 0.0469(5) Uani 1 1 d U . .
I8 I 0.68456(15) 0.94285(5) 0.86098(11) 0.0476(5) Uani 1 1 d U . .
I11 I 0.90414(14) 0.98605(5) 0.96076(10) 0.0406(4) Uani 1 1 d . . .
I12 I 0.80635(14) 0.76313(5) 0.95891(10) 0.0420(4) Uani 1 1 d . . .
N1 N 1.1225(11) 0.8418(4) 0.2878(7) 0.026(3) Uani 1 1 d DU . .
C1 C 1.1894(12) 0.8539(4) 0.2555(8) 0.020(4) Uani 1 1 d DU . .
C2 C 1.2560(14) 0.8307(5) 0.2340(9) 0.041(6) Uani 1 1 d DU . .
H2B H 1.3022 0.8401 0.2113 0.049 Uiso 1 1 calc R . .
C3 C 1.2511(14) 0.7931(5) 0.2474(10) 0.037(6) Uani 1 1 d DU . .
H3A H 1.2951 0.7761 0.2340 0.045 Uiso 1 1 calc R . .
C4 C 1.1842(14) 0.7806(4) 0.2795(9) 0.033(5) Uani 1 1 d DU . .
H4A H 1.1803 0.7548 0.2885 0.040 Uiso 1 1 calc R . .
C5 C 1.1223(13) 0.8054(4) 0.2988(8) 0.031(5) Uani 1 1 d DU . .
C6 C 0.9654(17) 0.8124(6) 0.4060(16) 0.039(6) Uani 1 1 d U . .
H6B H 0.9471 0.7876 0.4130 0.046 Uiso 1 1 calc R . .
N2 N 1.0615(15) 0.7940(5) 0.3376(10) 0.027(4) Uani 1 1 d U . .
H2A H 1.0502 0.7702 0.3421 0.033 Uiso 1 1 calc R . .
N3 N 1.0198(15) 0.8193(5) 0.3684(9) 0.027(3) Uani 1 1 d U . .
N4 N 0.9641(13) 0.8775(4) 0.4266(9) 0.027(3) Uani 1 1 d DU . .
C7 C 0.9297(15) 0.8440(4) 0.4398(11) 0.029(4) Uani 1 1 d DU . .
C8 C 0.8570(19) 0.8388(5) 0.4748(14) 0.041(6) Uani 1 1 d DU . .
H8A H 0.8307 0.8149 0.4802 0.049 Uiso 1 1 calc R . .
C9 C 0.826(2) 0.8706(6) 0.5011(14) 0.050(7) Uani 1 1 d DU . .
H9A H 0.7798 0.8687 0.5279 0.060 Uiso 1 1 calc R . .
C10 C 0.8600(17) 0.9041(5) 0.4886(13) 0.037(6) Uani 1 1 d DU . .
H10A H 0.8356 0.9260 0.5045 0.045 Uiso 1 1 calc R . .
C11 C 0.9300(18) 0.9066(5) 0.4532(13) 0.039(5) Uani 1 1 d DU . .
H11A H 0.9558 0.9305 0.4471 0.047 Uiso 1 1 calc R . .
N5 N 0.9148(11) 0.9072(4) 0.2914(10) 0.027(3) Uani 1 1 d DU . .
C12 C 0.8178(13) 0.8943(4) 0.2602(12) 0.029(5) Uani 1 1 d DU . .
C13 C 0.7293(13) 0.9167(5) 0.2390(13) 0.035(6) Uani 1 1 d DU . .
H13A H 0.6621 0.9066 0.2169 0.042 Uiso 1 1 calc R . .
C14 C 0.7447(14) 0.9544(5) 0.2517(13) 0.038(6) Uani 1 1 d DU . .
H14A H 0.6865 0.9707 0.2417 0.046 Uiso 1 1 calc R . .
C15 C 0.8420(14) 0.9680(4) 0.2782(12) 0.031(5) Uani 1 1 d DU . .
H15A H 0.8538 0.9941 0.2811 0.037 Uiso 1 1 calc R . .
C16 C 0.9230(13) 0.9438(4) 0.3008(11) 0.030(5) Uani 1 1 d DU . .
N6 N 1.0217(15) 0.9561(5) 0.3333(11) 0.036(5) Uani 1 1 d U . .
H6A H 1.0366 0.9799 0.3338 0.043 Uiso 1 1 calc R . .
N7 N 1.0969(15) 0.9310(5) 0.3650(11) 0.034(4) Uani 1 1 d U . .
C17 C 1.1899(17) 0.9384(6) 0.4027(13) 0.026(4) Uani 1 1 d U . .
H17A H 1.2148 0.9632 0.4112 0.031 Uiso 1 1 calc R . .
N8 N 1.2061(11) 0.8732(4) 0.4238(10) 0.030(4) Uani 1 1 d DU . .
C18 C 1.2556(13) 0.9063(4) 0.4319(11) 0.024(4) Uani 1 1 d DU . .
C19 C 1.3605(14) 0.9114(5) 0.4687(12) 0.031(5) Uani 1 1 d DU . .
H19A H 1.3922 0.9352 0.4739 0.037 Uiso 1 1 calc R . .
C20 C 1.4160(14) 0.8799(5) 0.4971(11) 0.032(5) Uani 1 1 d DU . .
H20A H 1.4870 0.8819 0.5244 0.039 Uiso 1 1 calc R . .
C21 C 1.3691(14) 0.8464(5) 0.4861(12) 0.037(6) Uani 1 1 d DU . .
H21A H 1.4081 0.8245 0.5027 0.044 Uiso 1 1 calc R . .
C22 C 1.2655(14) 0.8441(5) 0.4512(13) 0.035(6) Uani 1 1 d DU . .
H22A H 1.2336 0.8203 0.4460 0.042 Uiso 1 1 calc R . .
N1S N 0.534(2) 0.7859(6) 0.8426(13) 0.055(7) Uani 1 1 d U . .
C1S C 0.502(2) 0.8145(7) 0.8355(13) 0.042(7) Uani 1 1 d U . .
C2S C 0.467(2) 0.8529(8) 0.8268(19) 0.061(9) Uani 1 1 d U . .
H2S1 H 0.5259 0.8696 0.8471 0.091 Uiso 1 1 calc R . .
H2S2 H 0.4137 0.8566 0.8497 0.091 Uiso 1 1 calc R . .
H2S3 H 0.4369 0.8585 0.7778 0.091 Uiso 1 1 calc R . .
N2S N 1.0652(19) 0.9647(6) 0.8422(16) 0.058(8) Uani 1 1 d U . .
C3S C 1.088(2) 0.9357(7) 0.8347(16) 0.045(7) Uani 1 1 d U . .
C4S C 1.113(3) 0.8978(7) 0.8208(19) 0.062(10) Uani 1 1 d U . .
H4SA H 1.1673 0.8880 0.8608 0.093 Uiso 1 1 calc R . .
H4SB H 1.1379 0.8976 0.7808 0.093 Uiso 1 1 calc R . .
H4SC H 1.0504 0.8822 0.8116 0.093 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0299(15) 0.0144(13) 0.0339(17) 0.0024(12) 0.0118(13) -0.0007(11)
I1 0.0685(15) 0.0320(11) 0.169(3) 0.0327(14) 0.0580(17) 0.0061(10)
I2 0.0743(16) 0.0266(10) 0.167(3) 0.0164(13) 0.0825(17) 0.0051(10)
I3 0.0799(16) 0.0358(10) 0.0828(16) -0.0040(11) 0.0394(13) -0.0074(10)
I4 0.0434(10) 0.0440(10) 0.0438(10) -0.0019(9) 0.0169(8) 0.0037(8)
I5 0.0674(14) 0.0360(10) 0.0624(13) 0.0024(10) 0.0226(11) 0.0029(9)
I6 0.0417(11) 0.0327(10) 0.111(2) -0.0069(11) 0.0092(12) -0.0024(8)
I7 0.0461(11) 0.0225(9) 0.120(2) -0.0123(11) 0.0211(12) -0.0056(8)
I10 0.0494(11) 0.0393(10) 0.0680(14) -0.0017(10) 0.0247(10) 0.0009(9)
I9 0.0478(11) 0.0469(10) 0.0461(11) 0.0017(9) 0.0146(9) -0.0114(9)
I8 0.0445(11) 0.0360(10) 0.0614(13) -0.0002(9) 0.0152(9) 0.0008(8)
I11 0.0428(10) 0.0321(9) 0.0464(11) 0.0126(8) 0.0131(8) 0.0017(7)
I12 0.0446(10) 0.0315(9) 0.0515(11) -0.0133(8) 0.0171(9) -0.0037(8)
N1 0.030(10) 0.015(6) 0.033(9) -0.001(6) 0.008(7) 0.000(6)
C1 0.024(11) 0.013(8) 0.019(11) -0.004(8) -0.001(7) -0.003(7)
C2 0.054(17) 0.016(9) 0.063(19) 0.002(11) 0.032(13) 0.007(10)
C3 0.050(15) 0.014(8) 0.052(17) 0.009(11) 0.022(12) 0.006(10)
C4 0.046(15) 0.014(8) 0.041(15) -0.013(10) 0.016(11) -0.009(8)
C5 0.037(13) 0.019(7) 0.036(14) 0.000(9) 0.011(9) -0.002(8)
C6 0.020(12) 0.015(7) 0.09(2) 0.007(10) 0.027(12) -0.003(9)
N2 0.032(10) 0.012(6) 0.035(11) 0.001(7) 0.007(7) -0.004(7)
N3 0.037(10) 0.018(6) 0.021(10) -0.001(6) 0.003(7) -0.003(6)
N4 0.035(9) 0.022(7) 0.025(8) -0.008(7) 0.009(7) -0.008(7)
C7 0.013(11) 0.032(8) 0.041(14) 0.008(9) 0.005(8) -0.001(8)
C8 0.053(17) 0.021(9) 0.059(18) 0.016(11) 0.031(13) 0.005(10)
C9 0.061(19) 0.046(12) 0.050(18) -0.017(13) 0.028(13) -0.010(13)
C10 0.026(13) 0.034(9) 0.053(17) -0.018(12) 0.014(10) 0.005(10)
C11 0.035(14) 0.042(10) 0.042(15) -0.008(11) 0.013(10) 0.004(11)
N5 0.030(6) 0.016(6) 0.035(10) 0.004(7) 0.011(6) 0.000(5)
C12 0.029(8) 0.027(10) 0.033(13) 0.000(10) 0.011(8) 0.000(6)
C13 0.027(9) 0.031(10) 0.049(16) -0.021(12) 0.015(10) 0.008(8)
C14 0.034(8) 0.030(9) 0.048(16) 0.007(12) 0.008(11) 0.010(9)
C15 0.034(8) 0.015(8) 0.044(15) 0.006(10) 0.014(10) 0.004(6)
C16 0.034(8) 0.023(7) 0.023(12) -0.005(9) -0.005(9) 0.005(6)
N6 0.033(8) 0.017(7) 0.050(13) 0.006(9) 0.001(8) -0.003(6)
N7 0.031(7) 0.015(6) 0.054(14) 0.004(7) 0.011(7) 0.003(5)
C17 0.026(8) 0.010(7) 0.049(15) 0.006(8) 0.024(8) 0.000(6)
N8 0.032(6) 0.017(6) 0.037(10) 0.000(7) 0.003(6) -0.003(5)
C18 0.033(8) 0.014(7) 0.029(12) 0.004(8) 0.017(8) -0.001(6)
C19 0.033(9) 0.022(9) 0.039(15) 0.005(10) 0.013(9) -0.008(7)
C20 0.040(11) 0.026(10) 0.031(13) -0.002(10) 0.011(10) -0.002(7)
C21 0.041(10) 0.028(9) 0.037(15) 0.016(11) 0.006(11) 0.001(9)
C22 0.037(9) 0.021(9) 0.046(16) 0.013(10) 0.009(10) -0.002(7)
N1S 0.09(2) 0.029(10) 0.055(16) -0.003(11) 0.033(15) 0.014(12)
C1S 0.07(2) 0.025(10) 0.026(13) -0.010(11) 0.009(13) 0.005(12)
C2S 0.054(19) 0.028(11) 0.09(3) 0.014(16) 0.014(18) 0.005(12)
N2S 0.053(15) 0.011(8) 0.12(2) 0.025(12) 0.043(16) 0.016(10)
C3S 0.048(17) 0.023(10) 0.07(2) 0.000(13) 0.031(15) 0.015(12)
C4S 0.08(2) 0.014(10) 0.11(3) 0.016(14) 0.05(2) 0.017(14)

_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
Ni1 N3 2.080(18) . ?
Ni1 N7 2.091(19) . ?
Ni1 N8 2.104(14) . ?
Ni1 N4 2.124(14) . ?
Ni1 N5 2.242(15) . ?
Ni1 N1 2.277(14) . ?
I1 I2 2.817(5) . ?
I3 I4 2.992(3) . ?
I4 I5 2.890(3) . ?
I6 I7 2.770(4) . ?
I10 I9 2.898(3) . ?
I9 I8 2.994(3) . ?
I11 I11 2.775(4) 5_777 ?
I12 I12 2.764(4) 7_667 ?
N1 C5 1.329(15) . ?
N1 C1 1.346(15) . ?
C1 C2 1.395(17) . ?
C1 C12 1.48(2) 2_755 ?
C2 C3 1.384(17) . ?
C3 C4 1.349(18) . ?
C4 C5 1.361(18) . ?
C5 N2 1.37(2) . ?
C6 N3 1.24(3) . ?
C6 C7 1.48(3) . ?
N2 N3 1.33(3) . ?
N4 C11 1.329(15) . ?
N4 C7 1.348(15) . ?
C7 C8 1.396(17) . ?
C8 C9 1.385(18) . ?
C9 C10 1.346(18) . ?
C10 C11 1.362(18) . ?
N5 C16 1.330(15) . ?
N5 C12 1.348(15) . ?
C12 C13 1.394(17) . ?
C12 C1 1.48(2) 2_755 ?
C13 C14 1.385(17) . ?
C14 C15 1.348(18) . ?
C15 C16 1.363(18) . ?
C16 N6 1.36(3) . ?
N6 N7 1.36(3) . ?
N7 C17 1.28(3) . ?
C17 C18 1.47(3) . ?
N8 C22 1.330(15) . ?
N8 C18 1.349(15) . ?
C18 C19 1.394(17) . ?
C19 C20 1.383(17) . ?
C20 C21 1.347(18) . ?
C21 C22 1.360(18) . ?
N1S C1S 1.11(3) . ?
C1S C2S 1.45(4) . ?
N2S C3S 1.11(3) . ?
C3S C4S 1.45(3) . ?

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
N3 Ni1 N7 169.5(8) . . ?
N3 Ni1 N8 95.5(7) . . ?
N7 Ni1 N8 77.1(7) . . ?
N3 Ni1 N4 77.5(7) . . ?
N7 Ni1 N4 96.7(7) . . ?
N8 Ni1 N4 102.1(8) . . ?
N3 Ni1 N5 113.6(7) . . ?
N7 Ni1 N5 73.5(7) . . ?
N8 Ni1 N5 150.7(5) . . ?
N4 Ni1 N5 81.4(7) . . ?
N3 Ni1 N1 72.9(7) . . ?
N7 Ni1 N1 112.8(7) . . ?
N8 Ni1 N1 82.6(7) . . ?
N4 Ni1 N1 150.3(5) . . ?
N5 Ni1 N1 108.9(6) . . ?
I5 I4 I3 178.01(10) . . ?
I10 I9 I8 177.51(10) . . ?
C5 N1 C1 116.0(12) . . ?
C5 N1 Ni1 112.9(10) . . ?
C1 N1 Ni1 127.5(10) . . ?
N1 C1 C2 123.9(12) . . ?
N1 C1 C12 114.5(14) . 2_755 ?
C2 C1 C12 121.5(14) . 2_755 ?
C3 C2 C1 116.5(13) . . ?
C4 C3 C2 120.1(14) . . ?
C3 C4 C5 119.2(13) . . ?
N1 C5 C4 124.1(14) . . ?
N1 C5 N2 115.2(15) . . ?
C4 C5 N2 120.4(15) . . ?
N3 C6 C7 118(2) . . ?
N3 N2 C5 119.3(17) . . ?
C6 N3 N2 125(2) . . ?
C6 N3 Ni1 116.5(16) . . ?
N2 N3 Ni1 118.2(15) . . ?
C11 N4 C7 116.0(13) . . ?
C11 N4 Ni1 130.2(12) . . ?
C7 N4 Ni1 113.5(11) . . ?
N4 C7 C8 124.3(13) . . ?
N4 C7 C6 114.0(16) . . ?
C8 C7 C6 121.3(16) . . ?
C9 C8 C7 116.0(13) . . ?
C10 C9 C8 120.1(14) . . ?
C9 C10 C11 119.8(14) . . ?
N4 C11 C10 123.6(14) . . ?
C16 N5 C12 115.8(12) . . ?
C16 N5 Ni1 114.0(11) . . ?
C12 N5 Ni1 127.3(11) . . ?
N5 C12 C13 124.0(13) . . ?
N5 C12 C1 115.4(13) . 2_755 ?
C13 C12 C1 120.4(13) . 2_755 ?
C14 C13 C12 116.4(13) . . ?
C15 C14 C13 120.1(14) . . ?
C14 C15 C16 118.9(13) . . ?
N5 C16 C15 124.2(14) . . ?
N5 C16 N6 114.7(15) . . ?
C15 C16 N6 121.1(16) . . ?
C16 N6 N7 119.1(18) . . ?
C17 N7 N6 126.3(19) . . ?
C17 N7 Ni1 117.0(15) . . ?
N6 N7 Ni1 116.5(15) . . ?
N7 C17 C18 115.8(18) . . ?
C22 N8 C18 115.5(12) . . ?
C22 N8 Ni1 130.0(11) . . ?
C18 N8 Ni1 113.7(11) . . ?
N8 C18 C19 124.3(13) . . ?
N8 C18 C17 115.6(15) . . ?
C19 C18 C17 120.0(15) . . ?
C20 C19 C18 116.4(13) . . ?
C21 C20 C19 119.8(14) . . ?
C20 C21 C22 119.6(14) . . ?
N8 C22 C21 124.1(14) . . ?
N1S C1S C2S 177(4) . . ?
N2S C3S C4S 177(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ni1 N1 C5 -10.5(9) . . . . ?
N7 Ni1 N1 C5 160.2(9) . . . . ?
N8 Ni1 N1 C5 87.6(9) . . . . ?
N4 Ni1 N1 C5 -13.7(16) . . . . ?
N5 Ni1 N1 C5 -120.2(9) . . . . ?
N3 Ni1 N1 C1 -168.1(12) . . . . ?
N7 Ni1 N1 C1 2.6(13) . . . . ?
N8 Ni1 N1 C1 -70.0(11) . . . . ?
N4 Ni1 N1 C1 -171.4(13) . . . . ?
N5 Ni1 N1 C1 82.2(11) . . . . ?
C5 N1 C1 C2 0.0(3) . . . . ?
Ni1 N1 C1 C2 157.1(11) . . . . ?
C5 N1 C1 C12 175.9(15) . . . 2_755 ?
Ni1 N1 C1 C12 -27.0(15) . . . 2_755 ?
N1 C1 C2 C3 -0.1(3) . . . . ?
C12 C1 C2 C3 -175.7(16) 2_755 . . . ?
C1 C2 C3 C4 0.3(7) . . . . ?
C2 C3 C4 C5 -0.4(9) . . . . ?
C1 N1 C5 C4 -0.2(7) . . . . ?
Ni1 N1 C5 C4 -160.6(10) . . . . ?
C1 N1 C5 N2 173.7(16) . . . . ?
Ni1 N1 C5 N2 13.3(14) . . . . ?
C3 C4 C5 N1 0.4(10) . . . . ?
C3 C4 C5 N2 -173.2(17) . . . . ?
N1 C5 N2 N3 -9(2) . . . . ?
C4 C5 N2 N3 165.3(15) . . . . ?
C7 C6 N3 N2 177(2) . . . . ?
C7 C6 N3 Ni1 -1(3) . . . . ?
C5 N2 N3 C6 -178(2) . . . . ?
C5 N2 N3 Ni1 -1(2) . . . . ?
N7 Ni1 N3 C6 59(5) . . . . ?
N8 Ni1 N3 C6 103(2) . . . . ?
N4 Ni1 N3 C6 1.8(19) . . . . ?
N5 Ni1 N3 C6 -73(2) . . . . ?
N1 Ni1 N3 C6 -176(2) . . . . ?
N7 Ni1 N3 N2 -119(4) . . . . ?
N8 Ni1 N3 N2 -74.4(16) . . . . ?
N4 Ni1 N3 N2 -175.6(17) . . . . ?
N5 Ni1 N3 N2 109.8(16) . . . . ?
N1 Ni1 N3 N2 6.1(14) . . . . ?
N3 Ni1 N4 C11 -175(2) . . . . ?
N7 Ni1 N4 C11 13(2) . . . . ?
N8 Ni1 N4 C11 92(2) . . . . ?
N5 Ni1 N4 C11 -59(2) . . . . ?
N1 Ni1 N4 C11 -172.2(18) . . . . ?
N3 Ni1 N4 C7 -2.8(15) . . . . ?
N7 Ni1 N4 C7 -174.0(16) . . . . ?
N8 Ni1 N4 C7 -95.8(16) . . . . ?
N5 Ni1 N4 C7 113.9(16) . . . . ?
N1 Ni1 N4 C7 0(2) . . . . ?
C11 N4 C7 C8 4(3) . . . . ?
Ni1 N4 C7 C8 -169(2) . . . . ?
C11 N4 C7 C6 177(2) . . . . ?
Ni1 N4 C7 C6 3(3) . . . . ?
N3 C6 C7 N4 -2(3) . . . . ?
N3 C6 C7 C8 171(2) . . . . ?
N4 C7 C8 C9 -5(4) . . . . ?
C6 C7 C8 C9 -177(3) . . . . ?
C7 C8 C9 C10 4(4) . . . . ?
C8 C9 C10 C11 -3(4) . . . . ?
C7 N4 C11 C10 -4(4) . . . . ?
Ni1 N4 C11 C10 169.0(19) . . . . ?
C9 C10 C11 N4 3(4) . . . . ?
N3 Ni1 N5 C16 159.8(16) . . . . ?
N7 Ni1 N5 C16 -12.0(17) . . . . ?
N8 Ni1 N5 C16 -12(3) . . . . ?
N4 Ni1 N5 C16 87.6(17) . . . . ?
N1 Ni1 N5 C16 -121.1(16) . . . . ?
N3 Ni1 N5 C12 0(2) . . . . ?
N7 Ni1 N5 C12 -172(2) . . . . ?
N8 Ni1 N5 C12 -171.6(18) . . . . ?
N4 Ni1 N5 C12 -72.2(19) . . . . ?
N1 Ni1 N5 C12 79.1(19) . . . . ?
C16 N5 C12 C13 -1(4) . . . . ?
Ni1 N5 C12 C13 158.8(19) . . . . ?
C16 N5 C12 C1 175(2) . . . 2_755 ?
Ni1 N5 C12 C1 -26(3) . . . 2_755 ?
N5 C12 C13 C14 0(4) . . . . ?
C1 C12 C13 C14 -176(2) 2_755 . . . ?
C12 C13 C14 C15 5(4) . . . . ?
C13 C14 C15 C16 -9(4) . . . . ?
C12 N5 C16 C15 -3(4) . . . . ?
Ni1 N5 C16 C15 -166(2) . . . . ?
C12 N5 C16 N6 179(2) . . . . ?
Ni1 N5 C16 N6 17(3) . . . . ?
C14 C15 C16 N5 8(4) . . . . ?
C14 C15 C16 N6 -174(2) . . . . ?
N5 C16 N6 N7 -13(3) . . . . ?
C15 C16 N6 N7 169(2) . . . . ?
C16 N6 N7 C17 -173(2) . . . . ?
C16 N6 N7 Ni1 2(3) . . . . ?
N3 Ni1 N7 C17 46(5) . . . . ?
N8 Ni1 N7 C17 0.9(18) . . . . ?
N4 Ni1 N7 C17 101.8(19) . . . . ?
N5 Ni1 N7 C17 -179(2) . . . . ?
N1 Ni1 N7 C17 -75(2) . . . . ?
N3 Ni1 N7 N6 -129(4) . . . . ?
N8 Ni1 N7 N6 -174.7(19) . . . . ?
N4 Ni1 N7 N6 -73.8(18) . . . . ?
N5 Ni1 N7 N6 5.2(17) . . . . ?
N1 Ni1 N7 N6 109.2(17) . . . . ?
N6 N7 C17 C18 179(2) . . . . ?
Ni1 N7 C17 C18 4(3) . . . . ?
N3 Ni1 N8 C22 12(2) . . . . ?
N7 Ni1 N8 C22 -175(2) . . . . ?
N4 Ni1 N8 C22 90(2) . . . . ?
N5 Ni1 N8 C22 -175.7(19) . . . . ?
N1 Ni1 N8 C22 -60(2) . . . . ?
N3 Ni1 N8 C18 -178.4(16) . . . . ?
N7 Ni1 N8 C18 -5.8(16) . . . . ?
N4 Ni1 N8 C18 -100.1(16) . . . . ?
N5 Ni1 N8 C18 -6(3) . . . . ?
N1 Ni1 N8 C18 109.7(17) . . . . ?
C22 N8 C18 C19 -3(4) . . . . ?
Ni1 N8 C18 C19 -174.1(19) . . . . ?
C22 N8 C18 C17 -179(2) . . . . ?
Ni1 N8 C18 C17 10(3) . . . . ?
N7 C17 C18 N8 -9(3) . . . . ?
N7 C17 C18 C19 174(2) . . . . ?
N8 C18 C19 C20 1(4) . . . . ?
C17 C18 C19 C20 177(2) . . . . ?
C18 C19 C20 C21 3(4) . . . . ?
C19 C20 C21 C22 -5(4) . . . . ?
C18 N8 C22 C21 1(4) . . . . ?
Ni1 N8 C22 C21 170(2) . . . . ?
C20 C21 C22 N8 3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.55
_refine_diff_density_min         -2.30
_refine_diff_density_rms         0.38

data_NI2LIX
_database_code_CSD               198625

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;  
?  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H42 I13 N18 Ni2'
_chemical_formula_weight         2638.12

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'
Ni Ni 0.3393 1.1124 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.429(1)
_cell_length_b                   15.266(1)
_cell_length_c                   18.172(1)
_cell_angle_alpha                79.363(1)
_cell_angle_beta                 86.971(1)
_cell_angle_gamma                73.100(1)
_cell_volume                     3503.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6232
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.73

_exptl_crystal_description       sphenoid
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    2.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2402
_exptl_absorpt_coefficient_mu    6.312
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_process_details   '(SHELXTL version 6.12; Bruker, 2001)'

_exptl_special_details           
;  
?  
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        none
_diffrn_reflns_number            33302
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_av_sigmaI/netI    0.045
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         29.15
_reflns_number_total             16910
_reflns_number_gt                13360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'

_refine_special_details          
;  
?
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.056P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16910
_refine_ls_number_parameters     732
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.977
_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
I1 I 0.14384(3) 0.63794(3) -0.02691(2) 0.03558(10) Uani 1 1 d . . .
I2 I 0.13854(3) 0.46543(3) 0.08523(2) 0.03006(9) Uani 1 1 d . . .
I3 I 0.12558(3) 0.30855(3) 0.19278(2) 0.03911(11) Uani 1 1 d . . .
I4 I 0.05999(4) 0.11658(3) 0.31549(2) 0.04267(11) Uani 1 1 d . . .
I5 I 0.10438(3) 0.01067(3) 0.19928(2) 0.02948(9) Uani 1 1 d . . .
I6 I 0.15695(3) -0.10596(3) 0.07512(2) 0.03476(10) Uani 1 1 d . . .
I7 I 0.36544(3) 0.12717(3) 0.36679(2) 0.03358(10) Uani 1 1 d . . .
I8 I 0.53876(3) 0.13864(3) 0.45570(2) 0.02883(9) Uani 1 1 d . . .
I9 I 0.69718(3) 0.15421(3) 0.54902(3) 0.04642(12) Uani 1 1 d . . .
I10 I -0.05504(4) 0.66224(3) 0.59445(2) 0.04223(11) Uani 1 1 d . . .
I11 I 0.08331(4) 0.64723(3) 0.47381(3) 0.04230(11) Uani 1 1 d . . .
I12 I 0.22459(3) 0.66686(4) 0.33319(3) 0.04796(12) Uani 1 1 d . . .
I13 I 0.41345(3) 0.54350(3) 0.45385(2) 0.03550(10) Uani 1 1 d . . .
Ni1 Ni 0.75732(5) 0.88872(5) 0.25491(3) 0.01807(14) Uani 1 1 d . . .
Ni2 Ni 0.66757(5) 0.63929(5) 0.19805(4) 0.01960(14) Uani 1 1 d . . .
N1 N 0.7141(3) 1.0364(3) 0.2251(2) 0.0232(9) Uani 1 1 d . . .
N2 N 0.8543(3) 0.9105(3) 0.1690(2) 0.0214(9) Uani 1 1 d . . .
N3 N 0.9286(3) 0.8362(3) 0.1506(2) 0.0264(10) Uani 1 1 d . . .
H3A H 0.9685 0.8410 0.1109 0.032 Uiso 1 1 calc R . .
N4 N 0.8583(3) 0.7501(3) 0.2465(2) 0.0208(9) Uani 1 1 d . . .
N5 N 0.6846(3) 0.6794(3) 0.3040(2) 0.0212(9) Uani 1 1 d . . .
N6 N 0.5059(3) 0.7066(3) 0.3034(3) 0.0264(10) Uani 1 1 d . . .
H6A H 0.4435 0.7271 0.3224 0.032 Uiso 1 1 calc R . .
N7 N 0.5189(3) 0.6883(3) 0.2334(2) 0.0225(9) Uani 1 1 d . . .
N8 N 0.5804(3) 0.6278(3) 0.1102(2) 0.0221(9) Uani 1 1 d . . .
N9 N 0.8553(3) 0.8900(3) 0.3411(2) 0.0220(9) Uani 1 1 d . . .
N10 N 0.6600(3) 0.8975(3) 0.3448(2) 0.0195(9) Uani 1 1 d . . .
N11 N 0.5580(3) 0.9097(3) 0.3320(2) 0.0245(10) Uani 1 1 d . . .
H11A H 0.5113 0.9167 0.3679 0.029 Uiso 1 1 calc R . .
N12 N 0.6112(3) 0.8836(3) 0.2125(2) 0.0192(9) Uani 1 1 d . . .
N13 N 0.7199(3) 0.7447(3) 0.1175(2) 0.0200(9) Uani 1 1 d . . .
N14 N 0.8511(3) 0.6128(3) 0.1027(3) 0.0262(10) Uani 1 1 d . . .
H14A H 0.9086 0.5835 0.0816 0.031 Uiso 1 1 calc R . .
N15 N 0.8067(3) 0.5677(3) 0.1605(2) 0.0226(9) Uani 1 1 d . . .
N16 N 0.6899(3) 0.5023(3) 0.2598(2) 0.0249(10) Uani 1 1 d . . .
C1 C 0.6445(4) 1.1000(4) 0.2564(3) 0.0272(12) Uani 1 1 d . . .
H1A H 0.6011 1.0797 0.2948 0.033 Uiso 1 1 calc R . .
C2 C 0.6320(5) 1.1949(4) 0.2357(3) 0.0329(13) Uani 1 1 d . . .
H2A H 0.5818 1.2381 0.2601 0.039 Uiso 1 1 calc R . .
C3 C 0.6930(5) 1.2254(4) 0.1795(3) 0.0370(15) Uani 1 1 d . . .
H3B H 0.6863 1.2899 0.1649 0.044 Uiso 1 1 calc R . .
C4 C 0.7650(5) 1.1600(4) 0.1445(3) 0.0346(14) Uani 1 1 d . . .
H4A H 0.8072 1.1790 0.1047 0.042 Uiso 1 1 calc R . .
C5 C 0.7735(4) 1.0668(4) 0.1687(3) 0.0255(12) Uani 1 1 d . . .
C6 C 0.8503(4) 0.9930(4) 0.1381(3) 0.0267(12) Uani 1 1 d . . .
H6B H 0.8945 1.0061 0.0976 0.032 Uiso 1 1 calc R . .
C7 C 0.9376(4) 0.7519(4) 0.1984(3) 0.0260(12) Uani 1 1 d . . .
C8 C 1.0235(4) 0.6754(4) 0.1943(3) 0.0321(14) Uani 1 1 d . . .
H8A H 1.0762 0.6786 0.1577 0.039 Uiso 1 1 calc R . .
C9 C 1.0295(5) 0.5956(4) 0.2444(4) 0.0359(15) Uani 1 1 d . . .
H9A H 1.0887 0.5431 0.2446 0.043 Uiso 1 1 calc R . .
C10 C 0.9495(4) 0.5906(4) 0.2954(3) 0.0315(13) Uani 1 1 d . . .
H10A H 0.9529 0.5353 0.3304 0.038 Uiso 1 1 calc R . .
C11 C 0.8658(4) 0.6676(4) 0.2938(3) 0.0232(11) Uani 1 1 d . . .
C12 C 0.7723(4) 0.6685(3) 0.3416(3) 0.0228(11) Uani 1 1 d . . .
C13 C 0.7762(5) 0.6637(4) 0.4181(3) 0.0316(13) Uani 1 1 d . . .
H13A H 0.8403 0.6528 0.4430 0.038 Uiso 1 1 calc R . .
C14 C 0.6831(5) 0.6752(4) 0.4576(3) 0.0333(14) Uani 1 1 d . . .
H14B H 0.6829 0.6722 0.5103 0.040 Uiso 1 1 calc R . .
C15 C 0.5919(5) 0.6910(4) 0.4206(3) 0.0302(13) Uani 1 1 d . . .
H15A H 0.5275 0.7011 0.4467 0.036 Uiso 1 1 calc R . .
C16 C 0.5955(4) 0.6917(4) 0.3441(3) 0.0242(11) Uani 1 1 d . . .
C17 C 0.4438(4) 0.6913(4) 0.1913(3) 0.0260(12) Uani 1 1 d . . .
H17A H 0.3729 0.7116 0.2056 0.031 Uiso 1 1 calc R . .
C18 C 0.4760(4) 0.6612(4) 0.1200(3) 0.0255(12) Uani 1 1 d . . .
C19 C 0.4052(5) 0.6629(4) 0.0663(3) 0.0329(13) Uani 1 1 d . . .
H19A H 0.3324 0.6855 0.0744 0.040 Uiso 1 1 calc R . .
C20 C 0.4429(5) 0.6310(5) 0.0008(3) 0.0365(15) Uani 1 1 d . . .
H20A H 0.3960 0.6332 -0.0373 0.044 Uiso 1 1 calc R . .
C21 C 0.5481(5) 0.5961(4) -0.0089(3) 0.0322(13) Uani 1 1 d . . .
H21A H 0.5751 0.5723 -0.0529 0.039 Uiso 1 1 calc R . .
C22 C 0.6146(5) 0.5965(4) 0.0474(3) 0.0282(12) Uani 1 1 d . . .
H22A H 0.6875 0.5733 0.0404 0.034 Uiso 1 1 calc R . .
C23 C 0.9560(4) 0.8836(4) 0.3380(3) 0.0266(12) Uani 1 1 d . . .
H23A H 0.9927 0.8732 0.2929 0.032 Uiso 1 1 calc R . .
C24 C 1.0094(5) 0.8917(4) 0.3984(3) 0.0322(13) Uani 1 1 d . . .
H24A H 1.0815 0.8874 0.3943 0.039 Uiso 1 1 calc R . .
C25 C 0.9583(5) 0.9057(4) 0.4635(3) 0.0331(14) Uani 1 1 d . . .
H25A H 0.9939 0.9126 0.5049 0.040 Uiso 1 1 calc R . .
C26 C 0.8537(5) 0.9097(4) 0.4692(3) 0.0284(12) Uani 1 1 d . . .
H26A H 0.8168 0.9184 0.5146 0.034 Uiso 1 1 calc R . .
C27 C 0.8045(4) 0.9008(4) 0.4074(3) 0.0232(11) Uani 1 1 d . . .
C28 C 0.6936(4) 0.9067(4) 0.4059(3) 0.0234(11) Uani 1 1 d . . .
H28A H 0.6498 0.9168 0.4481 0.028 Uiso 1 1 calc R . .
C29 C 0.5314(4) 0.9106(4) 0.2594(3) 0.0210(11) Uani 1 1 d . . .
C30 C 0.4271(4) 0.9354(4) 0.2385(3) 0.0263(12) Uani 1 1 d . . .
H30A H 0.3731 0.9534 0.2733 0.032 Uiso 1 1 calc R . .
C31 C 0.4047(4) 0.9332(4) 0.1662(3) 0.0312(13) Uani 1 1 d . . .
H31A H 0.3346 0.9525 0.1496 0.037 Uiso 1 1 calc R . .
C32 C 0.4855(4) 0.9023(4) 0.1173(3) 0.0268(12) Uani 1 1 d . . .
H32A H 0.4710 0.8984 0.0676 0.032 Uiso 1 1 calc R . .
C33 C 0.5858(4) 0.8777(4) 0.1420(3) 0.0214(11) Uani 1 1 d . . .
C34 C 0.6747(4) 0.8371(4) 0.0951(3) 0.0219(11) Uani 1 1 d . . .
C35 C 0.7067(4) 0.8907(4) 0.0334(3) 0.0284(12) Uani 1 1 d . . .
H35A H 0.6719 0.9551 0.0192 0.034 Uiso 1 1 calc R . .
C36 C 0.7925(5) 0.8461(5) -0.0072(3) 0.0329(14) Uani 1 1 d . . .
H36A H 0.8164 0.8803 -0.0500 0.039 Uiso 1 1 calc R . .
C37 C 0.8418(4) 0.7533(4) 0.0150(3) 0.0281(12) Uani 1 1 d . . .
H37A H 0.9001 0.7224 -0.0117 0.034 Uiso 1 1 calc R . .
C38 C 0.8038(4) 0.7056(4) 0.0781(3) 0.0219(11) Uani 1 1 d . . .
C39 C 0.8430(4) 0.4813(4) 0.1868(3) 0.0285(12) Uani 1 1 d . . .
H39A H 0.9062 0.4446 0.1690 0.034 Uiso 1 1 calc R . .
C40 C 0.7832(4) 0.4426(4) 0.2446(3) 0.0296(13) Uani 1 1 d . . .
C41 C 0.8177(5) 0.3518(4) 0.2825(4) 0.0382(15) Uani 1 1 d . . .
H41A H 0.8832 0.3119 0.2712 0.046 Uiso 1 1 calc R . .
C42 C 0.7542(6) 0.3209(4) 0.3370(4) 0.0414(16) Uani 1 1 d . . .
H42A H 0.7755 0.2588 0.3637 0.050 Uiso 1 1 calc R . .
C43 C 0.6614(6) 0.3792(4) 0.3526(3) 0.0397(15) Uani 1 1 d . . .
H43A H 0.6177 0.3587 0.3905 0.048 Uiso 1 1 calc R . .
C44 C 0.6309(5) 0.4699(4) 0.3120(3) 0.0326(13) Uani 1 1 d . . .
H44A H 0.5650 0.5100 0.3224 0.039 Uiso 1 1 calc R . .
N1S N 0.5578(4) 0.1125(4) 0.0658(3) 0.0422(14) Uani 1 1 d D . .
C1S C 0.4883(5) 0.1498(4) 0.0959(3) 0.0402(15) Uani 1 1 d D . .
C2S C 0.3944(5) 0.2012(5) 0.1334(4) 0.0480(18) Uani 1 1 d D . .
H2S1 H 0.4055 0.2578 0.1452 0.072 Uiso 1 1 calc R . .
H2S2 H 0.3815 0.1617 0.1798 0.072 Uiso 1 1 calc R . .
H2S3 H 0.3342 0.2180 0.1001 0.072 Uiso 1 1 calc R . .
N2S N 0.4650(7) 0.4316(6) 0.1928(5) 0.088(3) Uani 1 1 d D . .
C3S C 0.4055(7) 0.4218(6) 0.2376(5) 0.062(3) Uani 1 1 d D . .
C4S C 0.3357(8) 0.4013(7) 0.2973(5) 0.082(3) Uani 1 1 d D . .
H4S1 H 0.3468 0.3339 0.3097 0.124 Uiso 1 1 calc R . .
H4S2 H 0.2636 0.4319 0.2811 0.124 Uiso 1 1 calc R . .
H4S3 H 0.3495 0.4242 0.3416 0.124 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0333(2) 0.0337(2) 0.0398(2) -0.00376(18) 0.00450(17) -0.01217(17)
I2 0.02590(19) 0.0372(2) 0.02643(19) -0.01192(16) 0.00637(14) -0.00525(16)
I3 0.0348(2) 0.0422(2) 0.0299(2) 0.00029(18) 0.00670(17) 0.00003(18)
I4 0.0646(3) 0.0321(2) 0.0281(2) -0.00465(17) 0.0038(2) -0.0099(2)
I5 0.02654(19) 0.0346(2) 0.02742(19) -0.00328(16) 0.00518(15) -0.01128(16)
I6 0.0302(2) 0.0453(2) 0.0339(2) -0.01541(18) 0.01004(16) -0.01536(18)
I7 0.0337(2) 0.0396(2) 0.0290(2) -0.01187(17) 0.00085(16) -0.00948(17)
I8 0.0318(2) 0.0285(2) 0.02647(19) -0.00868(15) 0.00655(15) -0.00782(16)
I9 0.0340(2) 0.0510(3) 0.0559(3) -0.0118(2) -0.0099(2) -0.0116(2)
I10 0.0542(3) 0.0369(2) 0.0308(2) -0.00232(18) -0.00245(19) -0.0075(2)
I11 0.0454(3) 0.0380(2) 0.0414(2) -0.01165(19) -0.00573(19) -0.0048(2)
I12 0.0363(2) 0.0724(3) 0.0392(2) -0.0199(2) -0.00041(19) -0.0155(2)
I13 0.0348(2) 0.0393(2) 0.0347(2) -0.00581(18) 0.00700(17) -0.01588(18)
Ni1 0.0170(3) 0.0209(3) 0.0154(3) -0.0030(3) 0.0027(2) -0.0047(3)
Ni2 0.0179(3) 0.0214(3) 0.0185(3) -0.0058(3) 0.0020(3) -0.0030(3)
N1 0.025(2) 0.027(2) 0.018(2) -0.0020(18) -0.0003(18) -0.0077(19)
N2 0.019(2) 0.029(2) 0.018(2) -0.0045(19) -0.0008(17) -0.0090(19)
N3 0.021(2) 0.035(3) 0.022(2) -0.010(2) 0.0096(18) -0.005(2)
N4 0.020(2) 0.025(2) 0.018(2) -0.0055(18) -0.0019(17) -0.0067(18)
N5 0.026(2) 0.018(2) 0.020(2) -0.0072(18) 0.0038(18) -0.0051(18)
N6 0.020(2) 0.035(3) 0.026(2) -0.013(2) 0.0101(19) -0.008(2)
N7 0.023(2) 0.021(2) 0.022(2) -0.0057(18) 0.0058(18) -0.0046(18)
N8 0.022(2) 0.024(2) 0.021(2) -0.0046(18) 0.0018(18) -0.0081(19)
N9 0.023(2) 0.024(2) 0.020(2) -0.0034(18) 0.0051(17) -0.0079(19)
N10 0.023(2) 0.017(2) 0.018(2) -0.0030(17) 0.0042(17) -0.0058(18)
N11 0.022(2) 0.027(2) 0.023(2) -0.0045(19) 0.0087(18) -0.0067(19)
N12 0.017(2) 0.020(2) 0.019(2) -0.0033(17) 0.0034(16) -0.0031(17)
N13 0.018(2) 0.025(2) 0.018(2) -0.0062(18) -0.0006(17) -0.0059(18)
N14 0.016(2) 0.032(3) 0.027(2) -0.008(2) 0.0069(18) -0.0017(19)
N15 0.018(2) 0.028(2) 0.020(2) -0.0072(19) -0.0003(17) -0.0027(19)
N16 0.027(2) 0.026(2) 0.022(2) -0.0087(19) 0.0004(19) -0.006(2)
C1 0.034(3) 0.026(3) 0.020(3) -0.001(2) -0.001(2) -0.008(2)
C2 0.042(4) 0.025(3) 0.030(3) -0.008(2) -0.005(3) -0.005(3)
C3 0.055(4) 0.024(3) 0.033(3) -0.001(3) -0.011(3) -0.014(3)
C4 0.044(4) 0.032(3) 0.029(3) 0.003(3) -0.002(3) -0.018(3)
C5 0.028(3) 0.031(3) 0.018(3) 0.004(2) -0.005(2) -0.015(2)
C6 0.024(3) 0.037(3) 0.018(3) 0.002(2) 0.001(2) -0.012(2)
C7 0.020(3) 0.038(3) 0.023(3) -0.014(2) -0.001(2) -0.008(2)
C8 0.022(3) 0.045(4) 0.030(3) -0.017(3) 0.004(2) -0.004(3)
C9 0.029(3) 0.031(3) 0.042(4) -0.014(3) -0.010(3) 0.008(3)
C10 0.030(3) 0.032(3) 0.029(3) -0.013(3) -0.008(2) 0.004(3)
C11 0.026(3) 0.024(3) 0.021(3) -0.008(2) -0.005(2) -0.006(2)
C12 0.031(3) 0.014(2) 0.022(3) -0.003(2) -0.001(2) -0.005(2)
C13 0.039(3) 0.029(3) 0.027(3) -0.004(2) -0.004(3) -0.011(3)
C14 0.052(4) 0.034(3) 0.016(3) -0.005(2) 0.005(3) -0.016(3)
C15 0.043(3) 0.026(3) 0.025(3) -0.008(2) 0.010(3) -0.015(3)
C16 0.033(3) 0.018(3) 0.023(3) -0.006(2) 0.008(2) -0.010(2)
C17 0.018(3) 0.024(3) 0.034(3) -0.006(2) 0.003(2) -0.003(2)
C18 0.022(3) 0.024(3) 0.029(3) -0.004(2) 0.002(2) -0.004(2)
C19 0.023(3) 0.032(3) 0.041(4) -0.003(3) -0.005(3) -0.004(2)
C20 0.038(4) 0.043(4) 0.031(3) -0.004(3) -0.013(3) -0.015(3)
C21 0.042(4) 0.034(3) 0.023(3) -0.003(2) -0.002(3) -0.014(3)
C22 0.030(3) 0.033(3) 0.023(3) -0.010(2) 0.001(2) -0.009(3)
C23 0.024(3) 0.031(3) 0.026(3) -0.001(2) -0.002(2) -0.011(2)
C24 0.030(3) 0.034(3) 0.032(3) 0.002(3) -0.009(2) -0.012(3)
C25 0.041(3) 0.040(4) 0.022(3) -0.003(3) -0.011(3) -0.016(3)
C26 0.038(3) 0.033(3) 0.016(3) -0.004(2) -0.002(2) -0.013(3)
C27 0.033(3) 0.016(2) 0.019(3) -0.001(2) 0.002(2) -0.006(2)
C28 0.026(3) 0.026(3) 0.018(3) -0.005(2) 0.006(2) -0.007(2)
C29 0.022(3) 0.018(3) 0.023(3) -0.005(2) 0.002(2) -0.006(2)
C30 0.017(3) 0.027(3) 0.033(3) -0.009(2) 0.006(2) -0.003(2)
C31 0.013(3) 0.035(3) 0.042(4) -0.008(3) -0.004(2) -0.001(2)
C32 0.026(3) 0.029(3) 0.025(3) -0.007(2) -0.003(2) -0.005(2)
C33 0.020(3) 0.020(3) 0.024(3) -0.004(2) 0.001(2) -0.006(2)
C34 0.022(3) 0.028(3) 0.019(3) -0.006(2) 0.001(2) -0.011(2)
C35 0.033(3) 0.025(3) 0.025(3) -0.004(2) 0.004(2) -0.005(2)
C36 0.039(3) 0.044(4) 0.018(3) -0.005(3) 0.008(2) -0.019(3)
C37 0.024(3) 0.037(3) 0.025(3) -0.012(3) 0.008(2) -0.009(2)
C38 0.015(2) 0.032(3) 0.020(3) -0.009(2) 0.0006(19) -0.005(2)
C39 0.022(3) 0.027(3) 0.034(3) -0.010(2) -0.003(2) 0.000(2)
C40 0.030(3) 0.028(3) 0.029(3) -0.009(2) -0.005(2) -0.001(2)
C41 0.041(4) 0.028(3) 0.041(4) -0.005(3) -0.010(3) -0.002(3)
C42 0.058(4) 0.025(3) 0.037(4) 0.000(3) -0.008(3) -0.008(3)
C43 0.059(4) 0.033(3) 0.029(3) 0.002(3) 0.002(3) -0.022(3)
C44 0.039(3) 0.030(3) 0.031(3) -0.008(3) 0.003(3) -0.011(3)
N1S 0.034(3) 0.059(4) 0.033(3) -0.016(3) -0.001(2) -0.007(3)
C1S 0.050(4) 0.040(4) 0.033(3) -0.001(3) -0.012(3) -0.019(3)
C2S 0.058(5) 0.046(4) 0.033(4) -0.012(3) 0.010(3) -0.003(3)
N2S 0.124(8) 0.068(6) 0.064(6) -0.008(5) -0.035(5) -0.014(5)
C3S 0.078(7) 0.047(5) 0.056(5) -0.015(4) -0.035(5) -0.002(5)
C4S 0.097(8) 0.060(6) 0.100(8) -0.025(6) -0.014(6) -0.028(6)

_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 I2 3.0340(6) . ?
I2 I3 2.8398(6) . ?
I4 I5 2.8277(6) . ?
I5 I6 3.0566(5) . ?
I7 I8 2.9661(6) . ?
I8 I9 2.8778(6) . ?
I10 I11 2.7960(7) . ?
I11 I12 3.1233(7) . ?
I13 I13 2.7885(9) 2_666 ?
Ni1 N2 2.023(4) . ?
Ni1 N10 2.036(4) . ?
Ni1 N9 2.104(4) . ?
Ni1 N1 2.130(5) . ?
Ni1 N12 2.173(4) . ?
Ni1 N4 2.184(4) . ?
Ni2 N15 2.026(4) . ?
Ni2 N7 2.032(4) . ?
Ni2 N8 2.091(4) . ?
Ni2 N16 2.128(5) . ?
Ni2 N5 2.167(4) . ?
Ni2 N13 2.214(4) . ?
N1 C1 1.327(7) . ?
N1 C5 1.362(7) . ?
N2 C6 1.268(7) . ?
N2 N3 1.356(6) . ?
N3 C7 1.390(7) . ?
N4 C7 1.345(7) . ?
N4 C11 1.367(7) . ?
N5 C12 1.346(7) . ?
N5 C16 1.352(6) . ?
N6 N7 1.344(6) . ?
N6 C16 1.386(7) . ?
N7 C17 1.282(7) . ?
N8 C22 1.326(7) . ?
N8 C18 1.360(7) . ?
N9 C23 1.326(7) . ?
N9 C27 1.367(6) . ?
N10 C28 1.267(6) . ?
N10 N11 1.354(6) . ?
N11 C29 1.380(7) . ?
N12 C29 1.350(6) . ?
N12 C33 1.368(6) . ?
N13 C38 1.349(6) . ?
N13 C34 1.357(7) . ?
N14 N15 1.357(6) . ?
N14 C38 1.372(7) . ?
N15 C39 1.273(7) . ?
N16 C44 1.322(7) . ?
N16 C40 1.367(7) . ?
C1 C2 1.390(8) . ?
C2 C3 1.374(9) . ?
C3 C4 1.396(9) . ?
C4 C5 1.382(8) . ?
C5 C6 1.462(8) . ?
C7 C8 1.394(8) . ?
C8 C9 1.364(9) . ?
C9 C10 1.391(9) . ?
C10 C11 1.367(7) . ?
C11 C12 1.487(7) . ?
C12 C13 1.381(7) . ?
C13 C14 1.390(8) . ?
C14 C15 1.366(9) . ?
C15 C16 1.386(7) . ?
C17 C18 1.458(8) . ?
C18 C19 1.390(8) . ?
C19 C20 1.384(8) . ?
C20 C21 1.372(9) . ?
C21 C22 1.394(8) . ?
C23 C24 1.386(8) . ?
C24 C25 1.356(8) . ?
C25 C26 1.388(8) . ?
C26 C27 1.378(7) . ?
C27 C28 1.467(7) . ?
C29 C30 1.394(7) . ?
C30 C31 1.371(8) . ?
C31 C32 1.394(8) . ?
C32 C33 1.365(7) . ?
C33 C34 1.481(7) . ?
C34 C35 1.388(8) . ?
C35 C36 1.405(8) . ?
C36 C37 1.371(8) . ?
C37 C38 1.397(8) . ?
C39 C40 1.435(8) . ?
C40 C41 1.385(8) . ?
C41 C42 1.380(9) . ?
C42 C43 1.354(9) . ?
C43 C44 1.398(8) . ?
N1S C1S 1.117(6) . ?
C1S C2S 1.483(7) . ?
N2S C3S 1.131(7) . ?
C3S C4S 1.446(8) . ?

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
I3 I2 I1 177.532(17) . . ?
I4 I5 I6 178.78(2) . . ?
I9 I8 I7 176.303(18) . . ?
I10 I11 I12 170.38(2) . . ?
N2 Ni1 N10 166.32(18) . . ?
N2 Ni1 N9 96.77(16) . . ?
N10 Ni1 N9 77.41(17) . . ?
N2 Ni1 N1 77.08(17) . . ?
N10 Ni1 N1 90.63(16) . . ?
N9 Ni1 N1 91.85(17) . . ?
N2 Ni1 N12 110.14(16) . . ?
N10 Ni1 N12 75.74(16) . . ?
N9 Ni1 N12 152.96(16) . . ?
N1 Ni1 N12 91.55(16) . . ?
N2 Ni1 N4 75.44(17) . . ?
N10 Ni1 N4 116.20(16) . . ?
N9 Ni1 N4 87.62(16) . . ?
N1 Ni1 N4 152.25(17) . . ?
N12 Ni1 N4 101.39(16) . . ?
N15 Ni2 N7 168.38(18) . . ?
N15 Ni2 N8 95.41(17) . . ?
N7 Ni2 N8 77.57(17) . . ?
N15 Ni2 N16 76.78(18) . . ?
N7 Ni2 N16 94.82(18) . . ?
N8 Ni2 N16 97.69(17) . . ?
N15 Ni2 N5 111.08(17) . . ?
N7 Ni2 N5 75.88(17) . . ?
N8 Ni2 N5 153.39(16) . . ?
N16 Ni2 N5 86.40(16) . . ?
N15 Ni2 N13 75.47(17) . . ?
N7 Ni2 N13 112.93(17) . . ?
N8 Ni2 N13 86.86(16) . . ?
N16 Ni2 N13 152.17(16) . . ?
N5 Ni2 N13 101.75(16) . . ?
C1 N1 C5 117.7(5) . . ?
C1 N1 Ni1 129.4(4) . . ?
C5 N1 Ni1 112.7(4) . . ?
C6 N2 N3 121.6(5) . . ?
C6 N2 Ni1 119.5(4) . . ?
N3 N2 Ni1 118.6(3) . . ?
N2 N3 C7 115.7(4) . . ?
C7 N4 C11 116.4(5) . . ?
C7 N4 Ni1 112.9(4) . . ?
C11 N4 Ni1 128.8(3) . . ?
C12 N5 C16 116.6(5) . . ?
C12 N5 Ni2 128.9(3) . . ?
C16 N5 Ni2 111.7(3) . . ?
N7 N6 C16 116.6(4) . . ?
C17 N7 N6 123.7(4) . . ?
C17 N7 Ni2 118.9(4) . . ?
N6 N7 Ni2 117.1(3) . . ?
C22 N8 C18 118.5(5) . . ?
C22 N8 Ni2 128.3(4) . . ?
C18 N8 Ni2 113.1(3) . . ?
C23 N9 C27 118.2(5) . . ?
C23 N9 Ni1 128.6(4) . . ?
C27 N9 Ni1 113.2(3) . . ?
C28 N10 N11 123.1(4) . . ?
C28 N10 Ni1 118.7(4) . . ?
N11 N10 Ni1 117.2(3) . . ?
N10 N11 C29 116.3(4) . . ?
C29 N12 C33 116.7(4) . . ?
C29 N12 Ni1 111.7(3) . . ?
C33 N12 Ni1 129.8(3) . . ?
C38 N13 C34 116.3(4) . . ?
C38 N13 Ni2 112.0(3) . . ?
C34 N13 Ni2 131.1(3) . . ?
N15 N14 C38 118.0(4) . . ?
C39 N15 N14 123.2(5) . . ?
C39 N15 Ni2 119.1(4) . . ?
N14 N15 Ni2 117.4(3) . . ?
C44 N16 C40 117.5(5) . . ?
C44 N16 Ni2 129.7(4) . . ?
C40 N16 Ni2 112.6(4) . . ?
N1 C1 C2 123.0(5) . . ?
C3 C2 C1 119.2(6) . . ?
C2 C3 C4 118.8(6) . . ?
C5 C4 C3 118.6(6) . . ?
N1 C5 C4 122.6(5) . . ?
N1 C5 C6 114.8(5) . . ?
C4 C5 C6 122.5(5) . . ?
N2 C6 C5 115.9(5) . . ?
N4 C7 N3 115.6(5) . . ?
N4 C7 C8 123.7(6) . . ?
N3 C7 C8 120.7(5) . . ?
C9 C8 C7 117.8(6) . . ?
C8 C9 C10 120.4(5) . . ?
C11 C10 C9 118.1(6) . . ?
C10 C11 N4 123.5(5) . . ?
C10 C11 C12 123.0(5) . . ?
N4 C11 C12 113.5(4) . . ?
N5 C12 C13 123.8(5) . . ?
N5 C12 C11 114.7(5) . . ?
C13 C12 C11 121.5(5) . . ?
C12 C13 C14 117.8(6) . . ?
C15 C14 C13 120.0(5) . . ?
C14 C15 C16 118.4(5) . . ?
N5 C16 N6 115.4(5) . . ?
N5 C16 C15 123.3(5) . . ?
N6 C16 C15 121.3(5) . . ?
N7 C17 C18 114.6(5) . . ?
N8 C18 C19 121.8(5) . . ?
N8 C18 C17 115.6(5) . . ?
C19 C18 C17 122.6(5) . . ?
C20 C19 C18 118.6(5) . . ?
C21 C20 C19 119.8(6) . . ?
C20 C21 C22 118.4(6) . . ?
N8 C22 C21 122.9(6) . . ?
N9 C23 C24 122.3(5) . . ?
C25 C24 C23 119.6(6) . . ?
C24 C25 C26 119.5(5) . . ?
C27 C26 C25 118.5(5) . . ?
N9 C27 C26 121.9(5) . . ?
N9 C27 C28 114.5(5) . . ?
C26 C27 C28 123.5(5) . . ?
N10 C28 C27 115.9(5) . . ?
N12 C29 N11 116.2(4) . . ?
N12 C29 C30 123.4(5) . . ?
N11 C29 C30 120.4(5) . . ?
C31 C30 C29 118.2(5) . . ?
C30 C31 C32 119.7(5) . . ?
C33 C32 C31 118.9(5) . . ?
C32 C33 N12 123.0(5) . . ?
C32 C33 C34 121.7(5) . . ?
N12 C33 C34 115.3(4) . . ?
N13 C34 C35 124.1(5) . . ?
N13 C34 C33 114.3(4) . . ?
C35 C34 C33 121.6(5) . . ?
C34 C35 C36 117.4(5) . . ?
C37 C36 C35 120.1(5) . . ?
C36 C37 C38 118.1(5) . . ?
N13 C38 N14 115.9(5) . . ?
N13 C38 C37 124.0(5) . . ?
N14 C38 C37 120.1(5) . . ?
N15 C39 C40 116.4(5) . . ?
N16 C40 C41 122.6(6) . . ?
N16 C40 C39 114.9(5) . . ?
C41 C40 C39 122.5(5) . . ?
C42 C41 C40 118.1(6) . . ?
C43 C42 C41 120.0(6) . . ?
C42 C43 C44 119.1(6) . . ?
N16 C44 C43 122.7(6) . . ?
N1S C1S C2S 178.0(7) . . ?
N2S C3S C4S 174.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.895
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         3.23
_refine_diff_density_min         -1.61
_refine_diff_density_rms         0.20