# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Org.Biomol.Chem.
_journal_coden_cambridge         0177

_publ_contact_author_name        'Hiroyuki Furuta'
_publ_contact_author_email       hfuruta@cstf.kyushu-u.ac.jp
_publ_contact_author_fax         +81-92-802-2865
_publ_contact_author_phone       +81-92-802-2865
_publ_contact_letter             
;
ENTER TEXT OF LETTER
;
_publ_requested_category         CO
_publ_requested_coeditor_name    ?
_publ_author_name                'Hiroyuki Furuta'
#==============================================================================

data_N-SEM-NCTPP
_database_code_depnum_ccdc_archive 'CCDC 856308'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H44 N4 O Si'
_chemical_formula_sum            'C50 H44 N4 O Si'
_chemical_formula_weight         744.98

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'
Si Si 0.0817 0.0704 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   10.344(4)
_cell_length_b                   13.082(5)
_cell_length_c                   14.935(6)
_cell_angle_alpha                85.488(9)
_cell_angle_beta                 83.720(8)
_cell_angle_gamma                80.284(9)
_cell_volume                     1976.4(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2222
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      23.2

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71069
_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            11471
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.1553
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7315
_reflns_number_gt                3229
_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    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7315
_refine_ls_number_parameters     508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1653
_refine_ls_wR_factor_gt          0.1426
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_restrained_S_all      0.854
_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
C1 C 0.8877(4) 0.4687(3) 0.1719(2) 0.0367(9) Uani 1 1 d . . .
H68 H 0.9010 0.4981 0.2250 0.044 Uiso 1 1 calc R . .
C2 C 0.7772(3) 0.4998(2) 0.1224(2) 0.0317(8) Uani 1 1 d . . .
C3 C 0.8019(4) 0.4380(2) 0.0480(2) 0.0337(9) Uani 1 1 d . . .
H78 H 0.7465 0.4422 0.0015 0.040 Uiso 1 1 calc R . .
C4 C 0.9188(4) 0.3702(3) 0.0525(2) 0.0327(9) Uani 1 1 d . . .
C5 C 0.9818(3) 0.2940(3) -0.0092(2) 0.0326(9) Uani 1 1 d . . .
C6 C 0.9508(3) 0.2991(3) -0.0980(2) 0.0350(9) Uani 1 1 d . . .
C7 C 1.0041(4) 0.2215(3) -0.1619(2) 0.0391(9) Uani 1 1 d . . .
H45 H 1.0634 0.1601 -0.1509 0.047 Uiso 1 1 calc R . .
C8 C 0.9522(4) 0.2539(3) -0.2404(2) 0.0431(10) Uani 1 1 d . . .
H46 H 0.9691 0.2200 -0.2947 0.052 Uiso 1 1 calc R . .
C9 C 0.8656(4) 0.3513(3) -0.2245(2) 0.0354(9) Uani 1 1 d . . .
C10 C 0.7896(4) 0.4122(3) -0.2900(2) 0.0374(9) Uani 1 1 d . . .
C11 C 0.6944(4) 0.4983(3) -0.2722(2) 0.0368(9) Uani 1 1 d . . .
C12 C 0.6306(4) 0.5675(3) -0.3397(2) 0.0464(11) Uani 1 1 d . . .
H69 H 0.6444 0.5605 -0.4023 0.056 Uiso 1 1 calc R . .
C13 C 0.5477(4) 0.6441(3) -0.2979(2) 0.0429(10) Uani 1 1 d . . .
H70 H 0.4951 0.6998 -0.3270 0.051 Uiso 1 1 calc R . .
C14 C 0.5525(3) 0.6271(2) -0.2019(2) 0.0324(9) Uani 1 1 d . . .
C15 C 0.4820(3) 0.6898(2) -0.1369(2) 0.0338(9) Uani 1 1 d . . .
C16 C 0.4955(3) 0.6757(2) -0.0419(2) 0.0326(9) Uani 1 1 d . . .
C17 C 0.4095(4) 0.7310(3) 0.0273(2) 0.0400(9) Uani 1 1 d . . .
H71 H 0.3327 0.7793 0.0191 0.048 Uiso 1 1 calc R . .
C18 C 0.4608(4) 0.6998(3) 0.1059(2) 0.0379(9) Uani 1 1 d . . .
H72 H 0.4264 0.7222 0.1633 0.045 Uiso 1 1 calc R . .
C19 C 0.5784(3) 0.6254(2) 0.0856(2) 0.0312(8) Uani 1 1 d . . .
C20 C 0.6695(4) 0.5803(2) 0.1456(2) 0.0337(9) Uani 1 1 d . . .
N1 N 0.9709(3) 0.3915(2) 0.13257(18) 0.0355(7) Uani 1 1 d . . .
N2 N 0.8645(3) 0.3767(2) -0.13874(18) 0.0351(7) Uani 1 1 d . . .
N3 N 0.6456(3) 0.5388(2) -0.19117(18) 0.0359(8) Uani 1 1 d . . .
H79 H 0.6701 0.5123 -0.1393 0.043 Uiso 1 1 calc R . .
N4 N 0.5958(3) 0.6100(2) -0.00607(18) 0.0343(7) Uani 1 1 d . . .
C21 C 1.0807(3) 0.2018(3) 0.0180(2) 0.0315(8) Uani 1 1 d . . .
C22 C 1.0393(4) 0.1187(3) 0.0688(3) 0.0478(10) Uani 1 1 d . . .
H47 H 0.9501 0.1219 0.0908 0.057 Uiso 1 1 calc R . .
C23 C 1.1288(5) 0.0308(3) 0.0871(3) 0.0603(12) Uani 1 1 d . . .
H48 H 1.0994 -0.0266 0.1201 0.072 Uiso 1 1 calc R . .
C24 C 1.2601(5) 0.0257(3) 0.0580(3) 0.0588(13) Uani 1 1 d . . .
H49 H 1.3203 -0.0341 0.0722 0.071 Uiso 1 1 calc R . .
C25 C 1.3029(4) 0.1079(3) 0.0084(3) 0.0518(11) Uani 1 1 d . . .
H50 H 1.3924 0.1048 -0.0125 0.062 Uiso 1 1 calc R . .
C26 C 1.2133(4) 0.1958(3) -0.0107(2) 0.0466(10) Uani 1 1 d . . .
H51 H 1.2432 0.2528 -0.0439 0.056 Uiso 1 1 calc R . .
C27 C 0.8145(4) 0.3809(3) -0.3853(2) 0.0449(10) Uani 1 1 d . . .
C28 C 0.9355(5) 0.3839(3) -0.4341(3) 0.0620(13) Uani 1 1 d . . .
H52 H 1.0034 0.4045 -0.4064 0.074 Uiso 1 1 calc R . .
C29 C 0.9590(6) 0.3566(4) -0.5245(3) 0.0780(15) Uani 1 1 d . . .
H53 H 1.0409 0.3608 -0.5574 0.094 Uiso 1 1 calc R . .
C30 C 0.8613(7) 0.3241(3) -0.5636(3) 0.0773(17) Uani 1 1 d . . .
H54 H 0.8759 0.3051 -0.6237 0.093 Uiso 1 1 calc R . .
C31 C 0.7426(6) 0.3191(3) -0.5158(3) 0.0709(15) Uani 1 1 d . . .
H55 H 0.6761 0.2964 -0.5435 0.085 Uiso 1 1 calc R . .
C32 C 0.7173(5) 0.3468(3) -0.4265(3) 0.0549(12) Uani 1 1 d . . .
H56 H 0.6347 0.3425 -0.3945 0.066 Uiso 1 1 calc R . .
C33 C 0.3872(4) 0.7813(3) -0.1694(2) 0.0383(9) Uani 1 1 d . . .
C34 C 0.2845(4) 0.7711(3) -0.2185(2) 0.0460(10) Uani 1 1 d . . .
H57 H 0.2677 0.7044 -0.2275 0.055 Uiso 1 1 calc R . .
C35 C 0.2063(4) 0.8572(3) -0.2546(3) 0.0530(11) Uani 1 1 d . . .
H58 H 0.1381 0.8485 -0.2886 0.064 Uiso 1 1 calc R . .
C36 C 0.2274(4) 0.9551(3) -0.2413(3) 0.0525(11) Uani 1 1 d . . .
H59 H 0.1752 1.0136 -0.2670 0.063 Uiso 1 1 calc R . .
C37 C 0.3253(4) 0.9671(3) -0.1900(3) 0.0554(12) Uani 1 1 d . . .
H60 H 0.3385 1.0341 -0.1791 0.067 Uiso 1 1 calc R . .
C38 C 0.4047(4) 0.8813(3) -0.1544(2) 0.0497(11) Uani 1 1 d . . .
H61 H 0.4717 0.8908 -0.1196 0.060 Uiso 1 1 calc R . .
C39 C 0.6606(4) 0.6189(3) 0.2380(2) 0.0353(9) Uani 1 1 d . . .
C40 C 0.6562(4) 0.7224(3) 0.2521(2) 0.0475(11) Uani 1 1 d . . .
H73 H 0.6518 0.7712 0.2024 0.057 Uiso 1 1 calc R . .
C41 C 0.6580(4) 0.7568(3) 0.3370(3) 0.0545(12) Uani 1 1 d . . .
H74 H 0.6568 0.8277 0.3440 0.065 Uiso 1 1 calc R . .
C42 C 0.6616(5) 0.6884(3) 0.4105(3) 0.0643(14) Uani 1 1 d . . .
H75 H 0.6620 0.7117 0.4684 0.077 Uiso 1 1 calc R . .
C43 C 0.6647(5) 0.5847(3) 0.3989(2) 0.0706(15) Uani 1 1 d . . .
H76 H 0.6670 0.5368 0.4493 0.085 Uiso 1 1 calc R . .
C44 C 0.6644(4) 0.5504(3) 0.3140(2) 0.0483(11) Uani 1 1 d . . .
H77 H 0.6668 0.4792 0.3074 0.058 Uiso 1 1 calc R . .
C45 C 1.0925(4) 0.3466(3) 0.1685(3) 0.0472(10) Uani 1 1 d . . .
H62 H 1.1585 0.3205 0.1200 0.057 Uiso 1 1 calc R . .
H63 H 1.1268 0.3986 0.1989 0.057 Uiso 1 1 calc R . .
O1 O 1.0637(3) 0.2634(2) 0.23105(17) 0.0511(7) Uani 1 1 d . . .
C46 C 1.1815(4) 0.2015(3) 0.2627(3) 0.0546(12) Uani 1 1 d . . .
H64 H 1.2337 0.2460 0.2880 0.066 Uiso 1 1 calc R . .
H65 H 1.2356 0.1665 0.2125 0.066 Uiso 1 1 calc R . .
C47 C 1.1402(4) 0.1222(3) 0.3341(3) 0.0670(13) Uani 1 1 d . . .
H66 H 1.0800 0.0843 0.3089 0.080 Uiso 1 1 calc R . .
H67 H 1.0902 0.1595 0.3846 0.080 Uiso 1 1 calc R . .
Si1 Si 1.27494(13) 0.02452(10) 0.38040(9) 0.0634(4) Uani 1 1 d . . .
C48 C 1.3288(5) -0.0784(4) 0.2998(4) 0.0935(18) Uani 1 1 d . . .
H36 H 1.3876 -0.1348 0.3275 0.140 Uiso 1 1 calc R . .
H37 H 1.3746 -0.0500 0.2459 0.140 Uiso 1 1 calc R . .
H38 H 1.2524 -0.1044 0.2839 0.140 Uiso 1 1 calc R . .
C49 C 1.4209(5) 0.0857(3) 0.3977(3) 0.0779(15) Uani 1 1 d . . .
H39 H 1.4876 0.0337 0.4231 0.117 Uiso 1 1 calc R . .
H40 H 1.3938 0.1410 0.4387 0.117 Uiso 1 1 calc R . .
H41 H 1.4569 0.1141 0.3402 0.117 Uiso 1 1 calc R . .
C50 C 1.2063(6) -0.0277(5) 0.4918(4) 0.117(2) Uani 1 1 d . . .
H42 H 1.1337 -0.0630 0.4834 0.175 Uiso 1 1 calc R . .
H43 H 1.1750 0.0291 0.5308 0.175 Uiso 1 1 calc R . .
H44 H 1.2745 -0.0763 0.5193 0.175 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
C1 0.053(3) 0.030(2) 0.029(2) -0.0053(16) -0.0016(19) -0.0110(19)
C2 0.044(2) 0.0253(19) 0.0262(19) 0.0045(15) -0.0068(17) -0.0082(18)
C3 0.044(2) 0.032(2) 0.025(2) 0.0011(15) -0.0097(17) -0.0034(18)
C4 0.043(2) 0.038(2) 0.0200(18) 0.0005(15) -0.0063(17) -0.0124(19)
C5 0.036(2) 0.034(2) 0.029(2) 0.0007(16) -0.0021(17) -0.0122(18)
C6 0.040(2) 0.034(2) 0.032(2) -0.0043(16) -0.0037(18) -0.0094(18)
C7 0.047(2) 0.034(2) 0.037(2) -0.0060(17) -0.0085(19) -0.0008(18)
C8 0.056(3) 0.043(2) 0.031(2) -0.0133(17) -0.0082(19) -0.002(2)
C9 0.048(2) 0.033(2) 0.024(2) -0.0049(16) -0.0058(18) -0.0033(19)
C10 0.055(3) 0.034(2) 0.024(2) -0.0064(16) -0.0058(18) -0.0076(19)
C11 0.054(3) 0.034(2) 0.024(2) -0.0057(16) -0.0102(18) -0.0076(19)
C12 0.079(3) 0.033(2) 0.027(2) -0.0057(17) -0.012(2) -0.002(2)
C13 0.067(3) 0.035(2) 0.027(2) 0.0027(17) -0.018(2) -0.003(2)
C14 0.045(2) 0.027(2) 0.028(2) -0.0007(15) -0.0116(18) -0.0087(18)
C15 0.043(2) 0.0263(19) 0.034(2) 0.0014(16) -0.0106(18) -0.0062(17)
C16 0.043(2) 0.0238(19) 0.033(2) 0.0004(15) -0.0087(18) -0.0076(17)
C17 0.050(3) 0.032(2) 0.038(2) -0.0037(17) -0.0033(19) -0.0051(19)
C18 0.049(2) 0.038(2) 0.025(2) -0.0017(16) -0.0010(18) -0.0021(19)
C19 0.044(2) 0.0266(19) 0.0238(19) -0.0004(15) -0.0033(17) -0.0085(17)
C20 0.051(2) 0.0223(19) 0.028(2) 0.0027(15) -0.0049(18) -0.0062(18)
N1 0.0421(19) 0.0347(17) 0.0305(17) -0.0036(13) -0.0110(15) -0.0033(15)
N2 0.0438(19) 0.0363(17) 0.0250(17) -0.0022(13) -0.0078(14) -0.0033(15)
N3 0.050(2) 0.0337(17) 0.0246(17) -0.0003(13) -0.0119(15) -0.0045(15)
N4 0.0437(19) 0.0296(16) 0.0296(17) -0.0018(13) -0.0045(15) -0.0053(15)
C21 0.035(2) 0.033(2) 0.0267(19) -0.0059(16) -0.0035(17) -0.0037(18)
C22 0.045(3) 0.046(3) 0.051(3) 0.005(2) -0.002(2) -0.008(2)
C23 0.082(4) 0.038(3) 0.063(3) 0.008(2) -0.015(3) -0.014(3)
C24 0.075(4) 0.046(3) 0.053(3) -0.011(2) -0.029(3) 0.016(3)
C25 0.040(3) 0.067(3) 0.047(3) -0.011(2) -0.010(2) 0.005(2)
C26 0.049(3) 0.049(3) 0.042(2) -0.0012(18) -0.008(2) -0.008(2)
C27 0.058(3) 0.041(2) 0.032(2) -0.0021(18) -0.009(2) 0.006(2)
C28 0.083(4) 0.068(3) 0.034(3) -0.016(2) -0.001(2) -0.006(3)
C29 0.101(4) 0.073(3) 0.050(3) -0.011(2) 0.016(3) 0.006(3)
C30 0.130(5) 0.056(3) 0.039(3) -0.019(2) -0.019(3) 0.020(3)
C31 0.111(5) 0.052(3) 0.051(3) -0.017(2) -0.045(3) 0.010(3)
C32 0.080(3) 0.040(2) 0.046(3) -0.0073(19) -0.024(2) 0.000(2)
C33 0.055(3) 0.032(2) 0.029(2) -0.0034(16) -0.0083(19) -0.0053(19)
C34 0.050(3) 0.039(2) 0.052(3) -0.0040(18) -0.017(2) -0.008(2)
C35 0.049(3) 0.058(3) 0.052(3) -0.002(2) -0.022(2) 0.001(2)
C36 0.062(3) 0.047(3) 0.041(2) 0.0052(19) -0.009(2) 0.011(2)
C37 0.090(3) 0.029(2) 0.046(3) -0.0045(18) -0.019(2) 0.002(2)
C38 0.075(3) 0.037(2) 0.040(2) -0.0044(18) -0.025(2) -0.004(2)
C39 0.044(2) 0.035(2) 0.024(2) -0.0028(16) -0.0015(17) -0.0015(18)
C40 0.072(3) 0.036(2) 0.033(2) -0.0021(17) -0.007(2) -0.003(2)
C41 0.076(3) 0.043(2) 0.046(3) -0.017(2) -0.010(2) -0.006(2)
C42 0.097(4) 0.061(3) 0.031(2) -0.019(2) -0.013(2) 0.009(3)
C43 0.128(4) 0.055(3) 0.023(2) 0.0001(19) -0.013(3) 0.006(3)
C44 0.082(3) 0.034(2) 0.027(2) -0.0017(17) -0.004(2) -0.005(2)
C45 0.047(3) 0.051(3) 0.046(2) -0.004(2) -0.017(2) -0.006(2)
O1 0.0472(17) 0.0566(18) 0.0463(17) 0.0042(13) -0.0117(14) 0.0023(14)
C46 0.048(3) 0.055(3) 0.060(3) -0.007(2) -0.022(2) 0.007(2)
C47 0.061(3) 0.067(3) 0.066(3) 0.017(2) -0.011(3) 0.006(2)
Si1 0.0633(9) 0.0582(8) 0.0643(9) 0.0104(6) -0.0191(7) 0.0047(7)
C48 0.090(4) 0.064(3) 0.126(5) -0.007(3) -0.032(4) 0.002(3)
C49 0.095(4) 0.066(3) 0.076(3) 0.008(3) -0.033(3) -0.010(3)
C50 0.102(5) 0.133(5) 0.098(5) 0.058(4) -0.013(4) 0.002(4)

_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
C1 N1 1.341(4) . ?
C1 C2 1.414(5) . ?
C1 H68 0.9400 . ?
C2 C3 1.402(4) . ?
C2 C20 1.430(5) . ?
C3 C4 1.378(4) . ?
C3 H78 0.9400 . ?
C4 N1 1.429(4) . ?
C4 C5 1.435(5) . ?
C5 C6 1.391(4) . ?
C5 C21 1.504(5) . ?
C6 N2 1.383(4) . ?
C6 C7 1.448(5) . ?
C7 C8 1.351(5) . ?
C7 H45 0.9400 . ?
C8 C9 1.449(5) . ?
C8 H46 0.9400 . ?
C9 N2 1.347(4) . ?
C9 C10 1.429(5) . ?
C10 C11 1.387(5) . ?
C10 C27 1.496(5) . ?
C11 N3 1.371(4) . ?
C11 C12 1.439(5) . ?
C12 C13 1.348(5) . ?
C12 H69 0.9400 . ?
C13 C14 1.439(4) . ?
C13 H70 0.9400 . ?
C14 C15 1.384(5) . ?
C14 N3 1.384(4) . ?
C15 C16 1.435(4) . ?
C15 C33 1.499(5) . ?
C16 N4 1.361(4) . ?
C16 C17 1.443(5) . ?
C17 C18 1.348(5) . ?
C17 H71 0.9400 . ?
C18 C19 1.444(5) . ?
C18 H72 0.9400 . ?
C19 N4 1.388(4) . ?
C19 C20 1.397(4) . ?
C20 C39 1.496(4) . ?
N1 C45 1.436(4) . ?
N3 H79 0.8700 . ?
C21 C22 1.378(5) . ?
C21 C26 1.382(5) . ?
C22 C23 1.379(5) . ?
C22 H47 0.9400 . ?
C23 C24 1.372(6) . ?
C23 H48 0.9400 . ?
C24 C25 1.366(6) . ?
C24 H49 0.9400 . ?
C25 C26 1.381(5) . ?
C25 H50 0.9400 . ?
C26 H51 0.9400 . ?
C27 C28 1.382(6) . ?
C27 C32 1.385(5) . ?
C28 C29 1.408(6) . ?
C28 H52 0.9400 . ?
C29 C30 1.363(7) . ?
C29 H53 0.9400 . ?
C30 C31 1.360(7) . ?
C30 H54 0.9400 . ?
C31 C32 1.395(6) . ?
C31 H55 0.9400 . ?
C32 H56 0.9400 . ?
C33 C34 1.386(5) . ?
C33 C38 1.389(5) . ?
C34 C35 1.380(5) . ?
C34 H57 0.9400 . ?
C35 C36 1.368(5) . ?
C35 H58 0.9400 . ?
C36 C37 1.370(5) . ?
C36 H59 0.9400 . ?
C37 C38 1.381(5) . ?
C37 H60 0.9400 . ?
C38 H61 0.9400 . ?
C39 C40 1.379(5) . ?
C39 C44 1.390(5) . ?
C40 C41 1.380(5) . ?
C40 H73 0.9400 . ?
C41 C42 1.360(6) . ?
C41 H74 0.9400 . ?
C42 C43 1.376(5) . ?
C42 H75 0.9400 . ?
C43 C44 1.378(5) . ?
C43 H76 0.9400 . ?
C44 H77 0.9400 . ?
C45 O1 1.426(4) . ?
C45 H62 0.9800 . ?
C45 H63 0.9800 . ?
O1 C46 1.449(4) . ?
C46 C47 1.506(6) . ?
C46 H64 0.9800 . ?
C46 H65 0.9800 . ?
C47 Si1 1.878(4) . ?
C47 H66 0.9800 . ?
C47 H67 0.9800 . ?
Si1 C48 1.851(5) . ?
Si1 C50 1.862(5) . ?
Si1 C49 1.874(5) . ?
C48 H36 0.9700 . ?
C48 H37 0.9700 . ?
C48 H38 0.9700 . ?
C49 H39 0.9700 . ?
C49 H40 0.9700 . ?
C49 H41 0.9700 . ?
C50 H42 0.9700 . ?
C50 H43 0.9700 . ?
C50 H44 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
N1 C1 C2 110.5(3) . . ?
N1 C1 H68 124.8 . . ?
C2 C1 H68 124.8 . . ?
C3 C2 C1 104.7(3) . . ?
C3 C2 C20 130.1(3) . . ?
C1 C2 C20 125.1(3) . . ?
C4 C3 C2 110.5(3) . . ?
C4 C3 H78 124.7 . . ?
C2 C3 H78 124.7 . . ?
C3 C4 N1 106.0(3) . . ?
C3 C4 C5 129.2(3) . . ?
N1 C4 C5 124.8(3) . . ?
C6 C5 C4 121.5(3) . . ?
C6 C5 C21 115.6(3) . . ?
C4 C5 C21 122.9(3) . . ?
N2 C6 C5 126.2(3) . . ?
N2 C6 C7 109.4(3) . . ?
C5 C6 C7 124.4(3) . . ?
C8 C7 C6 107.0(3) . . ?
C8 C7 H45 126.5 . . ?
C6 C7 H45 126.5 . . ?
C7 C8 C9 106.5(3) . . ?
C7 C8 H46 126.8 . . ?
C9 C8 H46 126.8 . . ?
N2 C9 C10 124.1(3) . . ?
N2 C9 C8 110.8(3) . . ?
C10 C9 C8 125.1(3) . . ?
C11 C10 C9 125.2(3) . . ?
C11 C10 C27 117.2(3) . . ?
C9 C10 C27 117.6(3) . . ?
N3 C11 C10 129.3(3) . . ?
N3 C11 C12 105.6(3) . . ?
C10 C11 C12 125.0(3) . . ?
C13 C12 C11 108.5(3) . . ?
C13 C12 H69 125.7 . . ?
C11 C12 H69 125.7 . . ?
C12 C13 C14 109.3(3) . . ?
C12 C13 H70 125.4 . . ?
C14 C13 H70 125.4 . . ?
C15 C14 N3 129.0(3) . . ?
C15 C14 C13 126.2(3) . . ?
N3 C14 C13 104.8(3) . . ?
C14 C15 C16 125.2(3) . . ?
C14 C15 C33 116.9(3) . . ?
C16 C15 C33 117.9(3) . . ?
N4 C16 C15 123.4(3) . . ?
N4 C16 C17 111.2(3) . . ?
C15 C16 C17 125.3(3) . . ?
C18 C17 C16 106.5(3) . . ?
C18 C17 H71 126.8 . . ?
C16 C17 H71 126.8 . . ?
C17 C18 C19 107.2(3) . . ?
C17 C18 H72 126.4 . . ?
C19 C18 H72 126.4 . . ?
N4 C19 C20 123.2(3) . . ?
N4 C19 C18 109.9(3) . . ?
C20 C19 C18 126.7(3) . . ?
C19 C20 C2 123.4(3) . . ?
C19 C20 C39 120.0(3) . . ?
C2 C20 C39 116.6(3) . . ?
C1 N1 C4 108.3(3) . . ?
C1 N1 C45 121.8(3) . . ?
C4 N1 C45 129.8(3) . . ?
C9 N2 C6 106.3(3) . . ?
C11 N3 C14 111.8(3) . . ?
C11 N3 H79 124.1 . . ?
C14 N3 H79 124.1 . . ?
C16 N4 C19 105.2(3) . . ?
C22 C21 C26 118.4(3) . . ?
C22 C21 C5 120.1(3) . . ?
C26 C21 C5 121.4(3) . . ?
C21 C22 C23 119.9(4) . . ?
C21 C22 H47 120.1 . . ?
C23 C22 H47 120.1 . . ?
C24 C23 C22 121.0(4) . . ?
C24 C23 H48 119.5 . . ?
C22 C23 H48 119.5 . . ?
C25 C24 C23 119.7(4) . . ?
C25 C24 H49 120.1 . . ?
C23 C24 H49 120.1 . . ?
C24 C25 C26 119.4(4) . . ?
C24 C25 H50 120.3 . . ?
C26 C25 H50 120.3 . . ?
C25 C26 C21 121.5(4) . . ?
C25 C26 H51 119.2 . . ?
C21 C26 H51 119.2 . . ?
C28 C27 C32 118.3(4) . . ?
C28 C27 C10 121.0(4) . . ?
C32 C27 C10 120.7(4) . . ?
C27 C28 C29 121.4(4) . . ?
C27 C28 H52 119.3 . . ?
C29 C28 H52 119.3 . . ?
C30 C29 C28 119.1(5) . . ?
C30 C29 H53 120.5 . . ?
C28 C29 H53 120.5 . . ?
C31 C30 C29 120.1(5) . . ?
C31 C30 H54 120.0 . . ?
C29 C30 H54 120.0 . . ?
C30 C31 C32 121.5(5) . . ?
C30 C31 H55 119.2 . . ?
C32 C31 H55 119.2 . . ?
C27 C32 C31 119.6(5) . . ?
C27 C32 H56 120.2 . . ?
C31 C32 H56 120.2 . . ?
C34 C33 C38 117.5(3) . . ?
C34 C33 C15 122.5(3) . . ?
C38 C33 C15 119.9(3) . . ?
C35 C34 C33 121.1(4) . . ?
C35 C34 H57 119.5 . . ?
C33 C34 H57 119.5 . . ?
C36 C35 C34 120.5(4) . . ?
C36 C35 H58 119.7 . . ?
C34 C35 H58 119.7 . . ?
C35 C36 C37 119.3(4) . . ?
C35 C36 H59 120.3 . . ?
C37 C36 H59 120.3 . . ?
C36 C37 C38 120.5(4) . . ?
C36 C37 H60 119.7 . . ?
C38 C37 H60 119.7 . . ?
C37 C38 C33 121.0(4) . . ?
C37 C38 H61 119.5 . . ?
C33 C38 H61 119.5 . . ?
C40 C39 C44 116.6(3) . . ?
C40 C39 C20 122.3(3) . . ?
C44 C39 C20 121.0(3) . . ?
C39 C40 C41 122.1(4) . . ?
C39 C40 H73 118.9 . . ?
C41 C40 H73 118.9 . . ?
C42 C41 C40 120.3(4) . . ?
C42 C41 H74 119.8 . . ?
C40 C41 H74 119.8 . . ?
C41 C42 C43 119.1(4) . . ?
C41 C42 H75 120.5 . . ?
C43 C42 H75 120.5 . . ?
C42 C43 C44 120.5(4) . . ?
C42 C43 H76 119.7 . . ?
C44 C43 H76 119.7 . . ?
C43 C44 C39 121.4(4) . . ?
C43 C44 H77 119.3 . . ?
C39 C44 H77 119.3 . . ?
O1 C45 N1 106.6(3) . . ?
O1 C45 H62 110.4 . . ?
N1 C45 H62 110.4 . . ?
O1 C45 H63 110.4 . . ?
N1 C45 H63 110.4 . . ?
H62 C45 H63 108.6 . . ?
C45 O1 C46 112.4(3) . . ?
O1 C46 C47 108.2(3) . . ?
O1 C46 H64 110.0 . . ?
C47 C46 H64 110.0 . . ?
O1 C46 H65 110.0 . . ?
C47 C46 H65 110.0 . . ?
H64 C46 H65 108.4 . . ?
C46 C47 Si1 116.9(3) . . ?
C46 C47 H66 108.1 . . ?
Si1 C47 H66 108.1 . . ?
C46 C47 H67 108.1 . . ?
Si1 C47 H67 108.1 . . ?
H66 C47 H67 107.3 . . ?
C48 Si1 C50 112.1(3) . . ?
C48 Si1 C49 108.5(2) . . ?
C50 Si1 C49 108.6(2) . . ?
C48 Si1 C47 109.0(2) . . ?
C50 Si1 C47 107.0(2) . . ?
C49 Si1 C47 111.6(2) . . ?
Si1 C48 H36 109.5 . . ?
Si1 C48 H37 109.5 . . ?
H36 C48 H37 109.5 . . ?
Si1 C48 H38 109.5 . . ?
H36 C48 H38 109.5 . . ?
H37 C48 H38 109.5 . . ?
Si1 C49 H39 109.5 . . ?
Si1 C49 H40 109.5 . . ?
H39 C49 H40 109.5 . . ?
Si1 C49 H41 109.5 . . ?
H39 C49 H41 109.5 . . ?
H40 C49 H41 109.5 . . ?
Si1 C50 H42 109.5 . . ?
Si1 C50 H43 109.5 . . ?
H42 C50 H43 109.5 . . ?
Si1 C50 H44 109.5 . . ?
H42 C50 H44 109.5 . . ?
H43 C50 H44 109.5 . . ?

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
N1 C1 C2 C3 -2.1(4) . . . . ?
N1 C1 C2 C20 180.0(3) . . . . ?
C1 C2 C3 C4 1.8(4) . . . . ?
C20 C2 C3 C4 179.6(3) . . . . ?
C2 C3 C4 N1 -0.9(4) . . . . ?
C2 C3 C4 C5 -179.7(3) . . . . ?
C3 C4 C5 C6 19.7(6) . . . . ?
N1 C4 C5 C6 -158.8(3) . . . . ?
C3 C4 C5 C21 -157.9(4) . . . . ?
N1 C4 C5 C21 23.5(5) . . . . ?
C4 C5 C6 N2 3.2(6) . . . . ?
C21 C5 C6 N2 -179.0(3) . . . . ?
C4 C5 C6 C7 -175.8(3) . . . . ?
C21 C5 C6 C7 1.9(5) . . . . ?
N2 C6 C7 C8 1.4(4) . . . . ?
C5 C6 C7 C8 -179.4(3) . . . . ?
C6 C7 C8 C9 -0.6(4) . . . . ?
C7 C8 C9 N2 -0.3(4) . . . . ?
C7 C8 C9 C10 -179.5(4) . . . . ?
N2 C9 C10 C11 -7.6(6) . . . . ?
C8 C9 C10 C11 171.5(4) . . . . ?
N2 C9 C10 C27 172.3(3) . . . . ?
C8 C9 C10 C27 -8.6(6) . . . . ?
C9 C10 C11 N3 -5.5(6) . . . . ?
C27 C10 C11 N3 174.7(4) . . . . ?
C9 C10 C11 C12 171.3(4) . . . . ?
C27 C10 C11 C12 -8.6(6) . . . . ?
N3 C11 C12 C13 -0.4(4) . . . . ?
C10 C11 C12 C13 -177.9(4) . . . . ?
C11 C12 C13 C14 -0.9(4) . . . . ?
C12 C13 C14 C15 179.4(4) . . . . ?
C12 C13 C14 N3 1.9(4) . . . . ?
N3 C14 C15 C16 1.7(6) . . . . ?
C13 C14 C15 C16 -175.1(3) . . . . ?
N3 C14 C15 C33 179.9(3) . . . . ?
C13 C14 C15 C33 3.0(5) . . . . ?
C14 C15 C16 N4 12.2(5) . . . . ?
C33 C15 C16 N4 -165.9(3) . . . . ?
C14 C15 C16 C17 -170.3(4) . . . . ?
C33 C15 C16 C17 11.6(5) . . . . ?
N4 C16 C17 C18 1.5(4) . . . . ?
C15 C16 C17 C18 -176.3(3) . . . . ?
C16 C17 C18 C19 0.1(4) . . . . ?
C17 C18 C19 N4 -1.6(4) . . . . ?
C17 C18 C19 C20 173.6(3) . . . . ?
N4 C19 C20 C2 -11.5(5) . . . . ?
C18 C19 C20 C2 173.9(3) . . . . ?
N4 C19 C20 C39 165.8(3) . . . . ?
C18 C19 C20 C39 -8.8(5) . . . . ?
C3 C2 C20 C19 -12.9(6) . . . . ?
C1 C2 C20 C19 164.5(3) . . . . ?
C3 C2 C20 C39 169.8(3) . . . . ?
C1 C2 C20 C39 -12.9(5) . . . . ?
C2 C1 N1 C4 1.6(4) . . . . ?
C2 C1 N1 C45 179.0(3) . . . . ?
C3 C4 N1 C1 -0.4(4) . . . . ?
C5 C4 N1 C1 178.4(3) . . . . ?
C3 C4 N1 C45 -177.5(3) . . . . ?
C5 C4 N1 C45 1.3(6) . . . . ?
C10 C9 N2 C6 -179.7(3) . . . . ?
C8 C9 N2 C6 1.1(4) . . . . ?
C5 C6 N2 C9 179.3(3) . . . . ?
C7 C6 N2 C9 -1.5(4) . . . . ?
C10 C11 N3 C14 179.0(4) . . . . ?
C12 C11 N3 C14 1.7(4) . . . . ?
C15 C14 N3 C11 -179.6(3) . . . . ?
C13 C14 N3 C11 -2.2(4) . . . . ?
C15 C16 N4 C19 175.4(3) . . . . ?
C17 C16 N4 C19 -2.4(4) . . . . ?
C20 C19 N4 C16 -173.0(3) . . . . ?
C18 C19 N4 C16 2.4(4) . . . . ?
C6 C5 C21 C22 -102.3(4) . . . . ?
C4 C5 C21 C22 75.4(4) . . . . ?
C6 C5 C21 C26 74.4(4) . . . . ?
C4 C5 C21 C26 -107.8(4) . . . . ?
C26 C21 C22 C23 -2.3(5) . . . . ?
C5 C21 C22 C23 174.6(3) . . . . ?
C21 C22 C23 C24 2.1(6) . . . . ?
C22 C23 C24 C25 -1.4(6) . . . . ?
C23 C24 C25 C26 0.9(6) . . . . ?
C24 C25 C26 C21 -1.1(5) . . . . ?
C22 C21 C26 C25 1.8(5) . . . . ?
C5 C21 C26 C25 -175.0(3) . . . . ?
C11 C10 C27 C28 116.2(4) . . . . ?
C9 C10 C27 C28 -63.7(5) . . . . ?
C11 C10 C27 C32 -64.6(5) . . . . ?
C9 C10 C27 C32 115.5(4) . . . . ?
C32 C27 C28 C29 2.1(6) . . . . ?
C10 C27 C28 C29 -178.6(4) . . . . ?
C27 C28 C29 C30 -1.7(7) . . . . ?
C28 C29 C30 C31 0.6(7) . . . . ?
C29 C30 C31 C32 0.1(7) . . . . ?
C28 C27 C32 C31 -1.4(6) . . . . ?
C10 C27 C32 C31 179.4(3) . . . . ?
C30 C31 C32 C27 0.3(6) . . . . ?
C14 C15 C33 C34 58.3(5) . . . . ?
C16 C15 C33 C34 -123.4(4) . . . . ?
C14 C15 C33 C38 -118.3(4) . . . . ?
C16 C15 C33 C38 60.0(5) . . . . ?
C38 C33 C34 C35 2.8(6) . . . . ?
C15 C33 C34 C35 -173.9(4) . . . . ?
C33 C34 C35 C36 -1.1(6) . . . . ?
C34 C35 C36 C37 -1.3(6) . . . . ?
C35 C36 C37 C38 2.0(7) . . . . ?
C36 C37 C38 C33 -0.2(7) . . . . ?
C34 C33 C38 C37 -2.1(6) . . . . ?
C15 C33 C38 C37 174.6(4) . . . . ?
C19 C20 C39 C40 -53.1(5) . . . . ?
C2 C20 C39 C40 124.3(4) . . . . ?
C19 C20 C39 C44 130.8(4) . . . . ?
C2 C20 C39 C44 -51.7(5) . . . . ?
C44 C39 C40 C41 1.2(6) . . . . ?
C20 C39 C40 C41 -175.0(4) . . . . ?
C39 C40 C41 C42 -1.3(7) . . . . ?
C40 C41 C42 C43 0.6(7) . . . . ?
C41 C42 C43 C44 0.1(8) . . . . ?
C42 C43 C44 C39 -0.2(7) . . . . ?
C40 C39 C44 C43 -0.5(6) . . . . ?
C20 C39 C44 C43 175.8(4) . . . . ?
C1 N1 C45 O1 89.3(4) . . . . ?
C4 N1 C45 O1 -94.0(4) . . . . ?
N1 C45 O1 C46 171.6(3) . . . . ?
C45 O1 C46 C47 175.1(3) . . . . ?
O1 C46 C47 Si1 175.4(3) . . . . ?
C46 C47 Si1 C48 -79.4(4) . . . . ?
C46 C47 Si1 C50 159.1(4) . . . . ?
C46 C47 Si1 C49 40.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.057

#==============================================================================

# End of CIF

#==============================================================================

#==============================================================================

data_inner-Me_NCTPP
_database_code_depnum_ccdc_archive 'CCDC 856309'

#==============================================================================

# CHEMICAL DATA

_chemical_formula_sum            'C46 H34 Cl2 N4'

_chemical_formula_moiety         'C45 H32 N4, C H2 Cl2'

_chemical_formula_weight         713.71

_chemical_melting_point          ?

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic

_symmetry_space_group_name_H-M   P-1

_symmetry_space_group_name_Hall  '-P 1'

_symmetry_Int_Tables_number      2

loop_

_symmetry_equiv_pos_site_id

_symmetry_equiv_pos_as_xyz

1 +X,+Y,+Z
2 -X,-Y,-Z

#------------------------------------------------------------------------------

_cell_length_a                   10.881(4)

_cell_length_b                   12.396(5)

_cell_length_c                   14.261(6)

_cell_angle_alpha                84.614(14)

_cell_angle_beta                 73.106(11)

_cell_angle_gamma                74.751(13)

_cell_volume                     1775.4(13)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    4768

_cell_measurement_theta_min      1.49

_cell_measurement_theta_max      30.32

_cell_measurement_temperature    123

#------------------------------------------------------------------------------

_exptl_crystal_description       platelet

_exptl_crystal_colour            green

_exptl_crystal_size_max          0.400

_exptl_crystal_size_mid          0.070

_exptl_crystal_size_min          0.060

_exptl_crystal_density_diffrn    1.335

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             744.00

_exptl_absorpt_coefficient_mu    0.223

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

_exptl_absorpt_correction_T_min  0.839

_exptl_absorpt_correction_T_max  0.987

#==============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      123

_diffrn_radiation_type           'Mo K\a'

_diffrn_radiation_wavelength     0.71075

_diffrn_measurement_device_type  'Rigaku Saturn724'

_diffrn_measurement_method       \w

_diffrn_detector_area_resol_mean 7.111

_diffrn_reflns_number            17372

_diffrn_reflns_av_R_equivalents  0.0301

_diffrn_reflns_av_sigmaI/netI    0.0399

_diffrn_reflns_theta_max         27.50

_diffrn_reflns_theta_full        27.50

_diffrn_measured_fraction_theta_max 0.978

_diffrn_measured_fraction_theta_full 0.978

_diffrn_reflns_limit_h_min       -14

_diffrn_reflns_limit_h_max       14

_diffrn_reflns_limit_k_min       -16

_diffrn_reflns_limit_k_max       16

_diffrn_reflns_limit_l_min       -16

_diffrn_reflns_limit_l_max       18

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F^2^, conventional R-factors R are based

on F, with F set to zero for negative F^2^. The threshold expression of

F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F^2^ are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

;

_reflns_number_total             7964

_reflns_number_gt                6633

_reflns_threshold_expression     F^2^>2.0\s(F^2^)

_refine_ls_structure_factor_coef Fsqd

_refine_ls_R_factor_all          0.0806

_refine_ls_R_factor_gt           0.0696

_refine_ls_wR_factor_ref         0.1934

_refine_ls_wR_factor_gt          0.1837

_refine_ls_goodness_of_fit_ref   1.065

_refine_ls_restrained_S_all      1.065

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000

_refine_ls_number_restraints     0

_refine_ls_hydrogen_treatment    constr

_refine_ls_number_reflns         7962

_refine_ls_number_parameters     471

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'w = 1/[\s^2^(Fo^2^)+(0.0945P)^2^+1.3007P] where P=(Fo^2^+2Fc^2^)/3'

_atom_sites_solution_hydrogens   geom

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_refine_diff_density_max         0.340

_refine_diff_density_min         -0.620

_refine_ls_extinction_method     none

_iucr_refine_instructions_details 
;

TITL General

CELL 0.71075 10.88100 12.39600 14.26100 84.614 73.106 74.751

ZERR 2 0.00400 0.00500 0.00600 0.014 0.011 0.013

LATT 1

SFAC C H CL N

UNIT 92 68 4 8

SHEL 99999.000000 0.769625

L.S. 5

FMAP 2

PLAN -25

WPDB -2

HTAB

TEMP -150.0

ACTA

BOND $H

CONF

EXYZ N1 C3A

EADP N1 C3A

EXYZ C1 C1A

EADP C1 C1A

EXYZ N1A C3

EADP N1A C3

EXYZ N3 C12A

EADP N3 C12A

EXYZ N3A C12

EADP N3A C12

EXYZ C13 C13A

EADP C13 C13A

EXYZ N4 N4A

EADP N4 N4A

SIZE 0.400 0.070 0.060

WGHT 0.094500 1.295300

FVAR 1.30862 0.55441

CL1 3 0.204838 0.652117 0.229004 11.00000 0.07894 0.05031 =

0.05337 0.00349 0.00108 -0.00603

CL2 3 0.192194 0.887348 0.250711 11.00000 0.06957 0.06959 =

0.05939 -0.01693 -0.00292 -0.02543

PART 1

N1 4 0.007957 0.265021 0.523421 21.00000 0.02872 0.02904 =

0.03018 0.00296 -0.00469 -0.00346

C1 1 0.078505 0.168543 0.548481 21.00000 0.02992 0.03066 =

0.03808 0.00378 -0.00684 -0.00649

AFIX 43

H1 2 0.066683 0.138488 0.613350 21.00000 -1.20000

AFIX 0

C3 1 0.163456 0.186205 0.383879 21.00000 0.02961 0.02567 =

0.03689 0.00533 -0.00101 -0.00349

AFIX 43

H3 2 0.215323 0.174997 0.317693 21.00000 -1.20000

AFIX 0

N3 4 0.442264 0.175953 0.127999 21.00000 0.04281 0.02908 =

0.02281 0.00335 0.00071 -0.00201

AFIX 43

H3N 2 0.376826 0.171912 0.180659 21.00000 -1.20000

AFIX 0

C12 1 0.568493 0.238330 -0.015979 21.00000 0.03445 0.03118 =

0.02820 -0.00036 -0.00610 -0.00572

AFIX 43

H12 2 0.594847 0.282911 -0.072488 21.00000 -1.20000

AFIX 0

C13 1 0.641179 0.142401 0.011091 21.00000 0.04126 0.03242 =

0.03071 0.00053 -0.01068 -0.00733

AFIX 43

H13 2 0.730035 0.107437 -0.022651 21.00000 -1.20000

AFIX 0

N4 4 0.421381 0.027474 0.299664 21.00000 0.03348 0.02580 =

0.03484 0.00314 -0.01418 -0.00183

PART 2

C3A 1 0.007957 0.265021 0.523421 -21.00000 0.02872 0.02904 =

0.03018 0.00296 -0.00469 -0.00346

AFIX 43

H3A 2 -0.062928 0.315758 0.565922 -21.00000 -1.20000

AFIX 0

C1A 1 0.078505 0.168543 0.548481 -21.00000 0.02992 0.03066 =

0.03808 0.00378 -0.00684 -0.00649

AFIX 43

H1A 2 0.066683 0.138488 0.613350 -21.00000 -1.20000

AFIX 0

N1A 4 0.163456 0.186205 0.383879 -21.00000 0.02961 0.02567 =

0.03689 0.00533 -0.00101 -0.00349

C12A 1 0.442264 0.175953 0.127999 -21.00000 0.04281 0.02908 =

0.02281 0.00335 0.00071 -0.00201

AFIX 43

H12A 2 0.371621 0.171590 0.184848 -21.00000 -1.20000

AFIX 0

N3A 4 0.568493 0.238330 -0.015979 -21.00000 0.03445 0.03118 =

0.02820 -0.00036 -0.00610 -0.00572

C13A 1 0.641179 0.142401 0.011091 -21.00000 0.04126 0.03242 =

0.03071 0.00053 -0.01068 -0.00733

AFIX 43

H13A 2 0.730035 0.107437 -0.022651 -21.00000 -1.20000

AFIX 0

N4A 4 0.421381 0.027474 0.299664 -21.00000 0.03348 0.02580 =

0.03484 0.00314 -0.01418 -0.00183

AFIX 43

H4N 2 0.378388 0.094207 0.284140 -21.00000 -1.20000

AFIX 0

PART 0

N2 4 0.200118 0.363446 0.222834 11.00000 0.02647 0.02915 =

0.02276 0.00276 -0.00626 -0.00079

C2 1 0.177345 0.114844 0.461853 11.00000 0.02631 0.02875 =

0.03898 0.00799 -0.00872 -0.00600

C4 1 0.059071 0.278182 0.419899 11.00000 0.02877 0.02608 =

0.02823 0.00156 -0.00293 -0.00352

C5 1 0.004700 0.371579 0.367595 11.00000 0.02921 0.02542 =

0.02668 -0.00032 -0.00502 -0.00533

C6 1 0.065479 0.396237 0.268779 11.00000 0.02849 0.02682 =

0.02492 0.00157 -0.00578 -0.00269

C7 1 0.002107 0.450259 0.197430 11.00000 0.02743 0.03311 =

0.03211 0.00236 -0.00986 0.00019

AFIX 43

H7 2 -0.090067 0.483363 0.208633 11.00000 -1.20000

AFIX 0

C8 1 0.096523 0.446588 0.109498 11.00000 0.03558 0.03386 =

0.02724 0.00387 -0.01123 -0.00167

AFIX 43

H8 2 0.081230 0.477004 0.049043 11.00000 -1.20000

AFIX 0

C9 1 0.220687 0.389894 0.123771 11.00000 0.02976 0.02912 =

0.02508 0.00287 -0.00692 -0.00426

C10 1 0.341313 0.354984 0.049888 11.00000 0.03286 0.03029 =

0.02519 0.00096 -0.00542 -0.00708

C11 1 0.443497 0.260671 0.056659 11.00000 0.03465 0.02983 =

0.02443 0.00019 -0.00387 -0.00599

C14 1 0.562322 0.100259 0.100455 11.00000 0.04217 0.02891 =

0.02798 -0.00256 -0.01145 -0.00080

C15 1 0.608001 -0.000492 0.149290 11.00000 0.03919 0.02911 =

0.02857 -0.00341 -0.01151 0.00111

C16 1 0.537774 -0.034330 0.241367 11.00000 0.03767 0.02621 =

0.03021 -0.00120 -0.01340 0.00001

C17 1 0.573182 -0.137122 0.293482 11.00000 0.04577 0.02490 =

0.03287 -0.00107 -0.01409 0.00118

AFIX 43

H17 2 0.649767 -0.196398 0.271357 11.00000 -1.20000

AFIX 0

C18 1 0.478288 -0.134928 0.379821 11.00000 0.04207 0.02387 =

0.03406 0.00090 -0.01495 -0.00060

AFIX 43

H18 2 0.476203 -0.193136 0.428159 11.00000 -1.20000

AFIX 0

C19 1 0.381368 -0.029793 0.385977 11.00000 0.03285 0.02568 =

0.03322 0.00221 -0.01420 -0.00517

C20 1 0.270336 0.010625 0.464255 11.00000 0.03029 0.02486 =

0.03529 0.00567 -0.01305 -0.00649

C21 1 -0.125795 0.445863 0.415032 11.00000 0.02880 0.02946 =

0.02504 0.00119 -0.00586 -0.00243

C22 1 -0.231015 0.401937 0.471397 11.00000 0.02997 0.03170 =

0.03391 0.00444 -0.00943 -0.00423

AFIX 43

H22 2 -0.220801 0.323292 0.476612 11.00000 -1.20000

AFIX 0

C23 1 -0.350187 0.473233 0.519635 11.00000 0.02758 0.04436 =

0.03604 0.00410 -0.00886 -0.00540

AFIX 43

H23 2 -0.420692 0.443077 0.558757 11.00000 -1.20000

AFIX 0

C24 1 -0.366885 0.588460 0.510996 11.00000 0.03058 0.03997 =

0.03335 -0.00526 -0.01129 0.00127

AFIX 43

H24 2 -0.448507 0.636817 0.544377 11.00000 -1.20000

AFIX 0

C25 1 -0.265515 0.632358 0.454275 11.00000 0.03784 0.02960 =

0.03438 -0.00249 -0.01214 0.00039

AFIX 43

H25 2 -0.277562 0.711136 0.447444 11.00000 -1.20000

AFIX 0

C26 1 -0.144894 0.561572 0.406659 11.00000 0.03392 0.03080 =

0.03061 -0.00047 -0.00360 -0.00487

AFIX 43

H26 2 -0.074859 0.592596 0.368030 11.00000 -1.20000

AFIX 0

C27 1 0.352958 0.418959 -0.044666 11.00000 0.02646 0.02971 =

0.02750 0.00246 -0.00492 -0.00241

C28 1 0.347157 0.532380 -0.047861 11.00000 0.03540 0.03152 =

0.02755 -0.00107 -0.00452 -0.00585

AFIX 43

H28 2 0.335362 0.569367 0.010689 11.00000 -1.20000

AFIX 0

C29 1 0.358429 0.592022 -0.135715 11.00000 0.03725 0.02961 =

0.03312 0.00249 -0.00701 -0.00525

AFIX 43

H29 2 0.356292 0.669268 -0.137287 11.00000 -1.20000

AFIX 0

C30 1 0.372848 0.539671 -0.221629 11.00000 0.03177 0.03577 =

0.02849 0.00665 -0.00619 -0.00550

AFIX 43

H30 2 0.379867 0.580887 -0.281763 11.00000 -1.20000

AFIX 0

C31 1 0.376894 0.426733 -0.218750 11.00000 0.04285 0.03699 =

0.02770 0.00049 -0.01053 -0.00790

AFIX 43

H31 2 0.385961 0.390354 -0.277002 11.00000 -1.20000

AFIX 0

C32 1 0.367728 0.366911 -0.131033 11.00000 0.04115 0.02981 =

0.03023 0.00123 -0.00888 -0.00634

AFIX 43

H32 2 0.371567 0.289349 -0.129756 11.00000 -1.20000

AFIX 0

C33 1 0.740081 -0.073644 0.101001 11.00000 0.04022 0.02963 =

0.03464 -0.00008 -0.00812 0.00091

C34 1 0.764675 -0.113880 0.007322 11.00000 0.04742 0.03315 =

0.03426 0.00004 -0.00397 -0.00865

AFIX 43

H34 2 0.697098 -0.094536 -0.025448 11.00000 -1.20000

AFIX 0

C35 1 0.887746 -0.182118 -0.038009 11.00000 0.06000 0.03879 =

0.04553 -0.00579 0.00633 -0.00617

AFIX 43

H35 2 0.904319 -0.208896 -0.101892 11.00000 -1.20000

AFIX 0

C36 1 0.986015 -0.211108 0.009545 11.00000 0.05293 0.05718 =

0.06691 -0.00323 0.00122 0.01548

AFIX 43

H36 2 1.069520 -0.258915 -0.021122 11.00000 -1.20000

AFIX 0

C37 1 0.963129 -0.170927 0.101009 11.00000 0.04672 0.08014 =

0.07051 -0.00108 -0.01702 0.01266

AFIX 43

H37 2 1.031363 -0.190359 0.133158 11.00000 -1.20000

AFIX 0

C38 1 0.840490 -0.101774 0.147178 11.00000 0.04963 0.05380 =

0.05077 -0.00396 -0.01959 0.00717

AFIX 43

H38 2 0.825654 -0.073867 0.210371 11.00000 -1.20000

AFIX 0

C39 1 0.248464 -0.058028 0.556085 11.00000 0.03442 0.02383 =

0.03332 0.00280 -0.01215 -0.00516

C40 1 0.348361 -0.097149 0.603475 11.00000 0.03865 0.02798 =

0.03671 0.00108 -0.01500 -0.00600

AFIX 43

H40 2 0.432680 -0.081699 0.575643 11.00000 -1.20000

AFIX 0

C41 1 0.325410 -0.158083 0.690440 11.00000 0.04430 0.03175 =

0.03570 0.00226 -0.01625 -0.00189

AFIX 43

H41 2 0.394392 -0.185751 0.721275 11.00000 -1.20000

AFIX 0

C42 1 0.201131 -0.178803 0.732705 11.00000 0.05293 0.03183 =

0.03203 0.00496 -0.00911 -0.00502

AFIX 43

H42 2 0.184773 -0.219258 0.793135 11.00000 -1.20000

AFIX 0

C43 1 0.101728 -0.140683 0.686973 11.00000 0.04181 0.03267 =

0.04012 0.00193 -0.00686 -0.00911

AFIX 43

H43 2 0.016921 -0.154788 0.715939 11.00000 -1.20000

AFIX 0

C44 1 0.125560 -0.081832 0.598806 11.00000 0.03836 0.03034 =

0.03861 0.00452 -0.01389 -0.00703

AFIX 43

H44 2 0.057252 -0.057319 0.566960 11.00000 -1.20000

AFIX 0

C45 1 0.300393 0.362074 0.274190 11.00000 0.03118 0.03278 =

0.03003 0.00133 -0.01036 -0.00596

AFIX 137

H45A 2 0.339944 0.284707 0.290778 11.00000 -1.50000

H45B 2 0.258115 0.405135 0.334366 11.00000 -1.50000

H45C 2 0.369685 0.395469 0.231516 11.00000 -1.50000

AFIX 0

C46 1 0.261482 0.749869 0.276918 11.00000 0.09338 0.10077 =

0.15559 -0.02429 -0.08392 0.02116

AFIX 23

H46A 2 0.241327 0.739087 0.348957 11.00000 -1.20000

H46B 2 0.359006 0.734757 0.250228 11.00000 -1.20000

HKLF 4

REM General

REM R1 = 0.0696 for 6633 Fo > 4sig(Fo) and 0.0806 for all 7962 data

REM 471 parameters refined using 0 restraints

END

WGHT 0.0945 1.2953

REM Highest difference peak 0.337, deepest hole -0.618, 1-sigma level 0.058

Q1 1 0.3004 -0.2478 0.2265 11.00000 0.05 0.34

Q2 1 0.2542 -0.1777 0.2841 11.00000 0.05 0.33

Q3 1 0.2415 -0.2618 0.2978 11.00000 0.05 0.33

Q4 1 0.1381 -0.3629 0.3084 11.00000 0.05 0.32

Q5 1 0.2227 -0.2552 0.2153 11.00000 0.05 0.29

Q6 1 0.1278 0.1410 0.5045 11.00000 0.05 0.28

Q7 1 0.1125 -0.1039 0.2093 11.00000 0.05 0.28

Q8 1 0.5607 -0.0173 0.1960 11.00000 0.05 0.25

Q9 1 0.6082 0.1875 -0.0117 11.00000 0.05 0.24

Q10 1 0.2288 -0.2973 0.1466 11.00000 0.05 0.24

Q11 1 0.6010 0.1181 0.0559 11.00000 0.05 0.24

Q12 1 0.1885 0.1620 0.2951 11.00000 0.05 0.23

Q13 1 0.6007 0.0251 0.1425 11.00000 0.05 0.23

Q14 1 0.3404 0.1064 0.1214 11.00000 0.05 0.23

Q15 1 0.4740 0.2526 0.0304 11.00000 0.05 0.22

Q16 1 0.3970 0.5552 -0.1943 11.00000 0.05 0.22

Q17 1 0.1663 0.4227 0.1175 11.00000 0.05 0.21

Q18 1 0.0230 0.4327 0.2245 11.00000 0.05 0.21

Q19 1 0.0378 0.3345 0.3928 11.00000 0.05 0.21

Q20 1 0.3826 -0.2663 0.1720 11.00000 0.05 0.21

Q21 1 0.5729 -0.0766 0.2600 11.00000 0.05 0.21

Q22 1 0.0514 0.4641 0.1473 11.00000 0.05 0.21

Q23 1 0.0463 0.2169 0.5369 11.00000 0.05 0.21

Q24 1 0.4324 -0.0845 0.3884 11.00000 0.05 0.20

Q25 1 0.2218 0.0569 0.4619 11.00000 0.05 0.20

;

loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source

C C 0.0033 0.0016
;

International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)

;
H H 0.0000 0.0000
;

International Tables for Crystallography

(1992, Vol. C, Table 6.1.1.4)

;
Cl Cl 0.1484 0.1585
;

International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)

;
N N 0.0061 0.0033
;

International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)

;

#==============================================================================

# ATOMIC COORDINATES AND THERMAL PARAMETERS

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

Cl1 Cl 0.20484(10) 0.65212(7) 0.22900(6) 0.0674(3) Uani 1 1 d . . .
Cl2 Cl 0.19219(9) 0.88735(8) 0.25071(7) 0.0668(3) Uani 1 1 d . . .
N1 N 0.0080(2) 0.26502(17) 0.52342(15) 0.0310(5) Uani 0.554(15) 1 d P A 1
C1 C 0.0785(2) 0.16854(19) 0.54848(18) 0.0339(5) Uani 0.554(15) 1 d P A 1
H1 H 0.0667 0.1385 0.6134 0.041 Uiso 0.554(15) 1 calc PR A 1
C3 C 0.1635(2) 0.18621(17) 0.38388(17) 0.0336(5) Uani 0.554(15) 1 d P A 1
H3 H 0.2153 0.1750 0.3177 0.040 Uiso 0.554(15) 1 calc PR A 1
N3 N 0.4423(2) 0.17595(17) 0.12800(15) 0.0353(5) Uani 0.554(15) 1 d P A 1
H3N H 0.3768 0.1719 0.1807 0.042 Uiso 0.554(15) 1 calc PR A 1
C12 C 0.5685(2) 0.23833(17) -0.01598(16) 0.0323(5) Uani 0.554(15) 1 d P A 1
H12 H 0.5948 0.2829 -0.0725 0.039 Uiso 0.554(15) 1 calc PR A 1
C13 C 0.6412(2) 0.1424(2) 0.01109(18) 0.0351(5) Uani 0.554(15) 1 d P A 1
H13 H 0.7300 0.1074 -0.0227 0.042 Uiso 0.554(15) 1 calc PR A 1
N4 N 0.42138(19) 0.02747(15) 0.29966(14) 0.0317(4) Uani 0.554(15) 1 d P A 1
C3A C 0.0080(2) 0.26502(17) 0.52342(15) 0.0310(5) Uani 0.446(15) 1 d P A 2
H3A H -0.0629 0.3158 0.5659 0.037 Uiso 0.446(15) 1 calc PR A 2
C1A C 0.0785(2) 0.16854(19) 0.54848(18) 0.0339(5) Uani 0.446(15) 1 d P A 2
H1A H 0.0667 0.1385 0.6134 0.041 Uiso 0.446(15) 1 calc PR A 2
N1A N 0.1635(2) 0.18621(17) 0.38388(17) 0.0336(5) Uani 0.446(15) 1 d P A 2
C12A C 0.4423(2) 0.17595(17) 0.12800(15) 0.0353(5) Uani 0.446(15) 1 d P A 2
H12A H 0.3716 0.1716 0.1848 0.042 Uiso 0.446(15) 1 calc PR A 2
N3A N 0.5685(2) 0.23833(17) -0.01598(16) 0.0323(5) Uani 0.446(15) 1 d P A 2
C13A C 0.6412(2) 0.1424(2) 0.01109(18) 0.0351(5) Uani 0.446(15) 1 d P A 2
H13A H 0.7300 0.1074 -0.0227 0.042 Uiso 0.446(15) 1 calc PR A 2
N4A N 0.42138(19) 0.02747(15) 0.29966(14) 0.0317(4) Uani 0.446(15) 1 d P A 2
H4N H 0.3784 0.0942 0.2841 0.038 Uiso 0.446(15) 1 calc PR A 2
N2 N 0.20012(17) 0.36345(15) 0.22283(13) 0.0277(4) Uani 1 1 d . A .
C2 C 0.1773(2) 0.11484(18) 0.46185(18) 0.0322(5) Uani 1 1 d . . .
C4 C 0.0591(2) 0.27818(18) 0.41990(16) 0.0296(5) Uani 1 1 d . . .
C5 C 0.0047(2) 0.37158(17) 0.36759(16) 0.0280(4) Uani 1 1 d . A .
C6 C 0.0655(2) 0.39624(17) 0.26878(16) 0.0280(4) Uani 1 1 d . . .
C7 C 0.0021(2) 0.45026(19) 0.19743(17) 0.0322(5) Uani 1 1 d . A .
H7 H -0.0901 0.4834 0.2086 0.039 Uiso 1 1 calc R . .
C8 C 0.0965(2) 0.44659(19) 0.10950(17) 0.0333(5) Uani 1 1 d . . .
H8 H 0.0812 0.4770 0.0490 0.040 Uiso 1 1 calc R A .
C9 C 0.2207(2) 0.38989(18) 0.12377(16) 0.0290(4) Uani 1 1 d . A .
C10 C 0.3413(2) 0.35498(18) 0.04989(16) 0.0303(5) Uani 1 1 d . . .
C11 C 0.4435(2) 0.26067(18) 0.05666(16) 0.0310(5) Uani 1 1 d . A .
C14 C 0.5623(2) 0.10026(19) 0.10045(17) 0.0341(5) Uani 1 1 d . . .
C15 C 0.6080(2) -0.00049(19) 0.14929(17) 0.0335(5) Uani 1 1 d . A .
C16 C 0.5378(2) -0.03433(18) 0.24137(17) 0.0320(5) Uani 1 1 d . . .
C17 C 0.5732(3) -0.13712(19) 0.29348(18) 0.0357(5) Uani 1 1 d . A .
H17 H 0.6498 -0.1964 0.2714 0.043 Uiso 1 1 calc R . .
C18 C 0.4783(2) -0.13493(18) 0.37982(18) 0.0340(5) Uani 1 1 d . . .
H18 H 0.4762 -0.1931 0.4282 0.041 Uiso 1 1 calc R A .
C19 C 0.3814(2) -0.02979(18) 0.38598(17) 0.0301(5) Uani 1 1 d . A .
C20 C 0.2703(2) 0.01063(18) 0.46426(17) 0.0298(5) Uani 1 1 d . A .
C21 C -0.1258(2) 0.44586(18) 0.41503(16) 0.0292(5) Uani 1 1 d . . .
C22 C -0.2310(2) 0.40194(19) 0.47140(17) 0.0327(5) Uani 1 1 d . A .
H22 H -0.2208 0.3233 0.4766 0.039 Uiso 1 1 calc R . .
C23 C -0.3502(2) 0.4732(2) 0.51963(18) 0.0370(5) Uani 1 1 d . . .
H23 H -0.4207 0.4431 0.5588 0.044 Uiso 1 1 calc R A .
C24 C -0.3669(2) 0.5885(2) 0.51100(18) 0.0358(5) Uani 1 1 d . A .
H24 H -0.4485 0.6368 0.5444 0.043 Uiso 1 1 calc R . .
C25 C -0.2655(2) 0.63236(19) 0.45427(18) 0.0351(5) Uani 1 1 d . . .
H25 H -0.2776 0.7111 0.4474 0.042 Uiso 1 1 calc R A .
C26 C -0.1449(2) 0.56157(19) 0.40666(17) 0.0336(5) Uani 1 1 d . A .
H26 H -0.0749 0.5926 0.3680 0.040 Uiso 1 1 calc R . .
C27 C 0.3530(2) 0.41896(18) -0.04467(16) 0.0295(5) Uani 1 1 d . A .
C28 C 0.3472(2) 0.53238(19) -0.04786(17) 0.0328(5) Uani 1 1 d . . .
H28 H 0.3354 0.5694 0.0107 0.039 Uiso 1 1 calc R A .
C29 C 0.3584(2) 0.59202(19) -0.13571(17) 0.0347(5) Uani 1 1 d . A .
H29 H 0.3563 0.6693 -0.1373 0.042 Uiso 1 1 calc R . .
C30 C 0.3728(2) 0.5397(2) -0.22163(17) 0.0335(5) Uani 1 1 d . . .
H30 H 0.3799 0.5809 -0.2818 0.040 Uiso 1 1 calc R A .
C31 C 0.3769(2) 0.4267(2) -0.21875(18) 0.0361(5) Uani 1 1 d . A .
H31 H 0.3860 0.3904 -0.2770 0.043 Uiso 1 1 calc R . .
C32 C 0.3677(2) 0.36691(19) -0.13103(17) 0.0345(5) Uani 1 1 d . . .
H32 H 0.3716 0.2893 -0.1298 0.041 Uiso 1 1 calc R A .
C33 C 0.7401(2) -0.0736(2) 0.10100(18) 0.0372(5) Uani 1 1 d . . .
C34 C 0.7647(3) -0.1139(2) 0.00732(19) 0.0402(6) Uani 1 1 d . A .
H34 H 0.6971 -0.0945 -0.0254 0.048 Uiso 1 1 calc R . .
C35 C 0.8877(3) -0.1821(2) -0.0380(2) 0.0535(8) Uani 1 1 d . . .
H35 H 0.9043 -0.2089 -0.1019 0.064 Uiso 1 1 calc R A .
C36 C 0.9860(3) -0.2111(3) 0.0095(3) 0.0685(10) Uani 1 1 d . A .
H36 H 1.0695 -0.2589 -0.0211 0.082 Uiso 1 1 calc R . .
C37 C 0.9631(3) -0.1709(3) 0.1010(3) 0.0712(10) Uani 1 1 d . . .
H37 H 1.0314 -0.1904 0.1332 0.085 Uiso 1 1 calc R A .
C38 C 0.8405(3) -0.1018(3) 0.1472(2) 0.0539(7) Uani 1 1 d . A .
H38 H 0.8257 -0.0739 0.2104 0.065 Uiso 1 1 calc R . .
C39 C 0.2485(2) -0.05803(18) 0.55609(17) 0.0305(5) Uani 1 1 d . . .
C40 C 0.3484(2) -0.09715(18) 0.60347(18) 0.0340(5) Uani 1 1 d . A .
H40 H 0.4327 -0.0817 0.5756 0.041 Uiso 1 1 calc R . .
C41 C 0.3254(3) -0.1581(2) 0.69044(18) 0.0378(5) Uani 1 1 d . . .
H41 H 0.3944 -0.1858 0.7213 0.045 Uiso 1 1 calc R A .
C42 C 0.2011(3) -0.1788(2) 0.73271(19) 0.0410(6) Uani 1 1 d . A .
H42 H 0.1848 -0.2193 0.7931 0.049 Uiso 1 1 calc R . .
C43 C 0.1017(3) -0.1407(2) 0.68697(19) 0.0394(5) Uani 1 1 d . . .
H43 H 0.0169 -0.1548 0.7159 0.047 Uiso 1 1 calc R A .
C44 C 0.1256(2) -0.08183(19) 0.59881(18) 0.0357(5) Uani 1 1 d . A .
H44 H 0.0573 -0.0573 0.5670 0.043 Uiso 1 1 calc R . .
C45 C 0.3004(2) 0.36207(19) 0.27419(17) 0.0314(5) Uani 1 1 d . . .
H45A H 0.3399 0.2847 0.2908 0.047 Uiso 1 1 calc R A .
H45B H 0.2581 0.4051 0.3344 0.047 Uiso 1 1 calc R . .
H45C H 0.3697 0.3955 0.2315 0.047 Uiso 1 1 calc R . .
C46 C 0.2615(5) 0.74987(4) 0.2769(5) 0.113(2) Uani 1 1 d . . .
H46A H 0.2413 0.7391 0.3490 0.136 Uiso 1 1 calc R . .
H46B H 0.3590 0.7348 0.2502 0.136 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

Cl1 0.0789(6) 0.0503(4) 0.0534(5) 0.0035(3) 0.0011(4) -0.0060(4)
Cl2 0.0696(5) 0.0696(5) 0.0594(5) -0.0169(4) -0.0029(4) -0.0254(4)
N1 0.0287(10) 0.0290(10) 0.0302(11) 0.0030(8) -0.0047(8) -0.0035(8)
C1 0.0299(11) 0.0307(11) 0.0381(13) 0.0038(9) -0.0068(10) -0.0065(9)
C3 0.0296(10) 0.0257(10) 0.0369(12) 0.0053(8) -0.0010(9) -0.0035(8)
N3 0.0428(12) 0.0291(10) 0.0228(10) 0.0033(8) 0.0007(9) -0.0020(9)
C12 0.0345(11) 0.0312(10) 0.0282(11) -0.0004(8) -0.0061(9) -0.0057(8)
C13 0.0413(12) 0.0324(11) 0.0307(12) 0.0005(9) -0.0107(10) -0.0073(10)
N4 0.0335(10) 0.0258(9) 0.0348(10) 0.0031(7) -0.0142(8) -0.0018(7)
C3A 0.0287(10) 0.0290(10) 0.0302(11) 0.0030(8) -0.0047(8) -0.0035(8)
C1A 0.0299(11) 0.0307(11) 0.0381(13) 0.0038(9) -0.0068(10) -0.0065(9)
N1A 0.0296(10) 0.0257(10) 0.0369(12) 0.0053(8) -0.0010(9) -0.0035(8)
C12A 0.0428(12) 0.0291(10) 0.0228(10) 0.0033(8) 0.0007(9) -0.0020(9)
N3A 0.0345(11) 0.0312(10) 0.0282(11) -0.0004(8) -0.0061(9) -0.0057(8)
C13A 0.0413(12) 0.0324(11) 0.0307(12) 0.0005(9) -0.0107(10) -0.0073(10)
N4A 0.0335(10) 0.0258(9) 0.0348(10) 0.0031(7) -0.0142(8) -0.0018(7)
N2 0.0265(9) 0.0292(9) 0.0228(9) 0.0028(7) -0.0063(7) -0.0008(7)
C2 0.0263(10) 0.0288(11) 0.0390(13) 0.0080(9) -0.0087(9) -0.0060(8)
C4 0.0288(10) 0.0261(10) 0.0282(11) 0.0016(8) -0.0029(9) -0.0035(8)
C5 0.0292(10) 0.0254(10) 0.0267(11) -0.0003(8) -0.0050(8) -0.0053(8)
C6 0.0285(10) 0.0268(10) 0.0249(11) 0.0016(8) -0.0058(8) -0.0027(8)
C7 0.0274(10) 0.0331(11) 0.0321(12) 0.0024(9) -0.0099(9) 0.0002(8)
C8 0.0356(12) 0.0339(11) 0.0272(11) 0.0039(9) -0.0112(9) -0.0017(9)
C9 0.0298(10) 0.0291(10) 0.0251(11) 0.0029(8) -0.0069(8) -0.0043(8)
C10 0.0329(11) 0.0303(11) 0.0252(11) 0.0010(8) -0.0054(9) -0.0071(9)
C11 0.0347(11) 0.0298(11) 0.0244(11) 0.0002(8) -0.0039(9) -0.0060(9)
C14 0.0422(12) 0.0289(11) 0.0280(11) -0.0026(9) -0.0115(10) -0.0008(9)
C15 0.0392(12) 0.0291(11) 0.0286(11) -0.0034(9) -0.0115(10) 0.0011(9)
C16 0.0377(12) 0.0262(10) 0.0302(11) -0.0012(9) -0.0134(9) 0.0000(9)
C17 0.0458(13) 0.0249(10) 0.0329(12) -0.0011(9) -0.0141(10) 0.0012(9)
C18 0.0421(12) 0.0239(10) 0.0341(12) 0.0009(9) -0.0150(10) -0.0006(9)
C19 0.0329(11) 0.0257(10) 0.0332(12) 0.0022(8) -0.0142(9) -0.0052(8)
C20 0.0303(10) 0.0249(10) 0.0353(12) 0.0057(8) -0.0131(9) -0.0065(8)
C21 0.0288(10) 0.0295(10) 0.0250(10) 0.0012(8) -0.0059(8) -0.0024(8)
C22 0.0300(11) 0.0317(11) 0.0339(12) 0.0044(9) -0.0094(9) -0.0042(9)
C23 0.0276(11) 0.0444(13) 0.0360(13) 0.0041(10) -0.0089(10) -0.0054(9)
C24 0.0306(11) 0.0400(12) 0.0333(12) -0.0053(10) -0.0113(9) 0.0013(9)
C25 0.0378(12) 0.0296(11) 0.0344(12) -0.0025(9) -0.0121(10) 0.0004(9)
C26 0.0339(11) 0.0308(11) 0.0306(12) -0.0005(9) -0.0036(9) -0.0049(9)
C27 0.0265(10) 0.0297(10) 0.0275(11) 0.0025(8) -0.0049(8) -0.0024(8)
C28 0.0354(11) 0.0315(11) 0.0275(11) -0.0011(9) -0.0045(9) -0.0059(9)
C29 0.0373(12) 0.0296(11) 0.0331(12) 0.0025(9) -0.0070(10) -0.0052(9)
C30 0.0318(11) 0.0358(12) 0.0285(11) 0.0067(9) -0.0062(9) -0.0055(9)
C31 0.0429(13) 0.0370(12) 0.0277(12) 0.0005(9) -0.0105(10) -0.0079(10)
C32 0.0412(12) 0.0298(11) 0.0302(12) 0.0012(9) -0.0089(10) -0.0063(9)
C33 0.0402(13) 0.0296(11) 0.0346(13) -0.0001(9) -0.0081(10) 0.0009(9)
C34 0.0474(14) 0.0332(12) 0.0343(13) 0.0000(10) -0.0040(11) -0.0086(10)
C35 0.0600(18) 0.0388(14) 0.0455(16) -0.0058(12) 0.0063(14) -0.0062(13)
C36 0.0529(18) 0.0572(19) 0.067(2) -0.0032(16) 0.0012(16) 0.0155(15)
C37 0.0467(17) 0.080(2) 0.071(2) -0.0011(19) -0.0170(16) 0.0127(16)
C38 0.0496(16) 0.0538(17) 0.0508(17) -0.0040(13) -0.0196(14) 0.0072(13)
C39 0.0344(11) 0.0238(10) 0.0333(12) 0.0028(8) -0.0121(9) -0.0052(8)
C40 0.0386(12) 0.0280(10) 0.0367(13) 0.0011(9) -0.0150(10) -0.0060(9)
C41 0.0443(13) 0.0317(11) 0.0357(13) 0.0023(10) -0.0163(11) -0.0019(10)
C42 0.0529(15) 0.0318(12) 0.0320(13) 0.0050(10) -0.0091(11) -0.0050(11)
C43 0.0418(13) 0.0327(12) 0.0401(14) 0.0019(10) -0.0069(11) -0.0091(10)
C44 0.0384(12) 0.0303(11) 0.0386(13) 0.0045(9) -0.0139(10) -0.0070(9)
C45 0.0312(11) 0.0328(11) 0.0300(11) 0.0013(9) -0.0104(9) -0.0060(9)
C46 0.093(3) 0.101(4) 0.156(5) -0.024(3) -0.084(4) 0.021(3)

_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell esds are taken

into account individually in the estimation of esds in distances, angles

and torsion angles; correlations between esds in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell esds is used for estimating esds involving l.s. planes.

;

loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

Cl1 C46 1.763(5) . ?
Cl2 C46 1.727(2) . ?
N1 C1 1.320(3) . ?
N1 C4 1.429(3) . ?
C1 C2 1.460(3) . ?
C1 H1 0.9500 . ?
C3 C2 1.373(3) . ?
C3 C4 1.394(3) . ?
C3 H3 0.9500 . ?
N3 C14 1.367(3) . ?
N3 C11 1.392(3) . ?
N3 H3N 0.8800 . ?
C12 C13 1.336(3) . ?
C12 C11 1.427(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.452(3) . ?
C13 H13 0.9500 . ?
N4 C16 1.371(3) . ?
N4 C19 1.377(3) . ?
N2 C6 1.386(3) . ?
N2 C9 1.386(3) . ?
N2 C45 1.476(3) . ?
C2 C20 1.421(3) . ?
C4 C5 1.407(3) . ?
C5 C6 1.414(3) . ?
C5 C21 1.481(3) . ?
C6 C7 1.413(3) . ?
C7 C8 1.367(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.412(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.415(3) . ?
C10 C11 1.403(3) . ?
C10 C27 1.489(3) . ?
C14 C15 1.415(3) . ?
C15 C16 1.402(3) . ?
C15 C33 1.489(3) . ?
C16 C17 1.433(3) . ?
C17 C18 1.355(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.436(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(3) . ?
C20 C39 1.487(3) . ?
C21 C26 1.393(3) . ?
C21 C22 1.402(3) . ?
C22 C23 1.389(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.372(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.388(3) . ?
C27 C32 1.392(3) . ?
C28 C29 1.384(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.385(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.387(4) . ?
C33 C34 1.397(4) . ?
C34 C35 1.389(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.381(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.371(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.394(4) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C44 1.395(3) . ?
C39 C40 1.401(3) . ?
C40 C41 1.384(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.392(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.379(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?

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

C1 N1 C4 106.58(19) . . ?
N1 C1 C2 110.0(2) . . ?
N1 C1 H1 125.0 . . ?
C2 C1 H1 125.0 . . ?
C2 C3 C4 107.3(2) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
C14 N3 C11 106.7(2) . . ?
C14 N3 H3N 126.6 . . ?
C11 N3 H3N 126.6 . . ?
C13 C12 C11 106.5(2) . . ?
C13 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
C12 C13 C14 108.9(2) . . ?
C12 C13 H13 125.5 . . ?
C14 C13 H13 125.5 . . ?
C16 N4 C19 110.29(18) . . ?
C6 N2 C9 108.59(17) . . ?
C6 N2 C45 121.85(18) . . ?
C9 N2 C45 121.81(18) . . ?
C3 C2 C20 129.4(2) . . ?
C3 C2 C1 106.60(19) . . ?
C20 C2 C1 124.0(2) . . ?
C3 C4 C5 128.4(2) . . ?
C3 C4 N1 109.53(19) . . ?
C5 C4 N1 122.03(19) . . ?
C4 C5 C6 123.27(19) . . ?
C4 C5 C21 119.50(19) . . ?
C6 C5 C21 117.15(19) . . ?
N2 C6 C7 107.49(19) . . ?
N2 C6 C5 125.00(19) . . ?
C7 C6 C5 127.4(2) . . ?
C8 C7 C6 108.1(2) . . ?
C8 C7 H7 126.0 . . ?
C6 C7 H7 126.0 . . ?
C7 C8 C9 108.4(2) . . ?
C7 C8 H8 125.8 . . ?
C9 C8 H8 125.8 . . ?
N2 C9 C8 107.31(19) . . ?
N2 C9 C10 125.73(19) . . ?
C8 C9 C10 126.6(2) . . ?
C11 C10 C9 125.1(2) . . ?
C11 C10 C27 118.61(19) . . ?
C9 C10 C27 116.09(19) . . ?
N3 C11 C10 128.5(2) . . ?
N3 C11 C12 109.84(19) . . ?
C10 C11 C12 121.7(2) . . ?
N3 C14 C15 127.9(2) . . ?
N3 C14 C13 107.9(2) . . ?
C15 C14 C13 124.2(2) . . ?
C16 C15 C14 124.0(2) . . ?
C16 C15 C33 118.0(2) . . ?
C14 C15 C33 118.0(2) . . ?
N4 C16 C15 125.6(2) . . ?
N4 C16 C17 106.9(2) . . ?
C15 C16 C17 127.6(2) . . ?
C18 C17 C16 108.0(2) . . ?
C18 C17 H17 126.0 . . ?
C16 C17 H17 126.0 . . ?
C17 C18 C19 108.5(2) . . ?
C17 C18 H18 125.7 . . ?
C19 C18 H18 125.7 . . ?
N4 C19 C20 125.63(19) . . ?
N4 C19 C18 106.3(2) . . ?
C20 C19 C18 128.1(2) . . ?
C19 C20 C2 123.8(2) . . ?
C19 C20 C39 118.63(19) . . ?
C2 C20 C39 117.6(2) . . ?
C26 C21 C22 118.6(2) . . ?
C26 C21 C5 120.2(2) . . ?
C22 C21 C5 121.1(2) . . ?
C23 C22 C21 120.1(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.4(2) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 120.0(2) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.1(2) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 120.8(2) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C27 C32 118.8(2) . . ?
C28 C27 C10 120.3(2) . . ?
C32 C27 C10 120.9(2) . . ?
C29 C28 C27 120.5(2) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.4(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C31 C30 C29 119.4(2) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C32 C31 C30 120.0(2) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C27 120.9(2) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
C38 C33 C34 119.1(2) . . ?
C38 C33 C15 121.0(2) . . ?
C34 C33 C15 119.9(2) . . ?
C35 C34 C33 120.1(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C34 120.2(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C37 C36 C35 120.0(3) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 120.5(3) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 120.1(3) . . ?
C33 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C44 C39 C40 118.4(2) . . ?
C44 C39 C20 120.4(2) . . ?
C40 C39 C20 121.2(2) . . ?
C41 C40 C39 120.6(2) . . ?
C41 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C40 C41 C42 119.9(2) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 120.1(2) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 120.0(2) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 120.9(2) . . ?
C43 C44 H44 119.5 . . ?
C39 C44 H44 119.5 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Cl2 C46 Cl1 113.9(2) . . ?
Cl2 C46 H46A 108.8 . . ?
Cl1 C46 H46A 108.8 . . ?
Cl2 C46 H46B 108.8 . . ?
Cl1 C46 H46B 108.8 . . ?
H46A C46 H46B 107.7 . . ?

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

C4 N1 C1 C2 -0.6(3) . . . . ?
C11 C12 C13 C14 1.5(3) . . . . ?
C4 C3 C2 C20 -179.0(2) . . . . ?
C4 C3 C2 C1 -1.4(3) . . . . ?
N1 C1 C2 C3 1.3(3) . . . . ?
N1 C1 C2 C20 179.0(2) . . . . ?
C2 C3 C4 C5 -177.7(2) . . . . ?
C2 C3 C4 N1 1.1(3) . . . . ?
C1 N1 C4 C3 -0.3(3) . . . . ?
C1 N1 C4 C5 178.6(2) . . . . ?
C3 C4 C5 C6 -11.9(4) . . . . ?
N1 C4 C5 C6 169.4(2) . . . . ?
C3 C4 C5 C21 164.9(2) . . . . ?
N1 C4 C5 C21 -13.8(3) . . . . ?
C9 N2 C6 C7 -3.5(2) . . . . ?
C45 N2 C6 C7 146.2(2) . . . . ?
C9 N2 C6 C5 172.3(2) . . . . ?
C45 N2 C6 C5 -37.9(3) . . . . ?
C4 C5 C6 N2 -26.0(4) . . . . ?
C21 C5 C6 N2 157.2(2) . . . . ?
C4 C5 C6 C7 149.0(2) . . . . ?
C21 C5 C6 C7 -27.8(3) . . . . ?
N2 C6 C7 C8 2.0(3) . . . . ?
C5 C6 C7 C8 -173.7(2) . . . . ?
C6 C7 C8 C9 0.2(3) . . . . ?
C6 N2 C9 C8 3.6(3) . . . . ?
C45 N2 C9 C8 -146.1(2) . . . . ?
C6 N2 C9 C10 -169.9(2) . . . . ?
C45 N2 C9 C10 40.4(3) . . . . ?
C7 C8 C9 N2 -2.4(3) . . . . ?
C7 C8 C9 C10 171.0(2) . . . . ?
N2 C9 C10 C11 23.1(4) . . . . ?
C8 C9 C10 C11 -149.2(2) . . . . ?
N2 C9 C10 C27 -162.5(2) . . . . ?
C8 C9 C10 C27 25.2(3) . . . . ?
C14 N3 C11 C10 177.2(2) . . . . ?
C14 N3 C11 C12 -1.3(3) . . . . ?
C9 C10 C11 N3 9.3(4) . . . . ?
C27 C10 C11 N3 -165.0(2) . . . . ?
C9 C10 C11 C12 -172.4(2) . . . . ?
C27 C10 C11 C12 13.3(3) . . . . ?
C13 C12 C11 N3 -0.2(3) . . . . ?
C13 C12 C11 C10 -178.7(2) . . . . ?
C11 N3 C14 C15 -179.8(2) . . . . ?
C11 N3 C14 C13 2.1(3) . . . . ?
C12 C13 C14 N3 -2.3(3) . . . . ?
C12 C13 C14 C15 179.5(2) . . . . ?
N3 C14 C15 C16 -5.7(4) . . . . ?
C13 C14 C15 C16 172.1(2) . . . . ?
N3 C14 C15 C33 175.8(2) . . . . ?
C13 C14 C15 C33 -6.4(4) . . . . ?
C19 N4 C16 C15 -178.6(2) . . . . ?
C19 N4 C16 C17 0.4(3) . . . . ?
C14 C15 C16 N4 -4.8(4) . . . . ?
C33 C15 C16 N4 173.7(2) . . . . ?
C14 C15 C16 C17 176.4(2) . . . . ?
C33 C15 C16 C17 -5.1(4) . . . . ?
N4 C16 C17 C18 0.5(3) . . . . ?
C15 C16 C17 C18 179.5(2) . . . . ?
C16 C17 C18 C19 -1.2(3) . . . . ?
C16 N4 C19 C20 176.8(2) . . . . ?
C16 N4 C19 C18 -1.1(3) . . . . ?
C17 C18 C19 N4 1.4(3) . . . . ?
C17 C18 C19 C20 -176.4(2) . . . . ?
N4 C19 C20 C2 4.8(4) . . . . ?
C18 C19 C20 C2 -177.7(2) . . . . ?
N4 C19 C20 C39 -174.3(2) . . . . ?
C18 C19 C20 C39 3.1(4) . . . . ?
C3 C2 C20 C19 10.8(4) . . . . ?
C1 C2 C20 C19 -166.4(2) . . . . ?
C3 C2 C20 C39 -170.1(2) . . . . ?
C1 C2 C20 C39 12.8(3) . . . . ?
C4 C5 C21 C26 135.5(2) . . . . ?
C6 C5 C21 C26 -47.5(3) . . . . ?
C4 C5 C21 C22 -42.5(3) . . . . ?
C6 C5 C21 C22 134.4(2) . . . . ?
C26 C21 C22 C23 -1.7(3) . . . . ?
C5 C21 C22 C23 176.4(2) . . . . ?
C21 C22 C23 C24 1.2(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C23 C24 C25 C26 -1.2(4) . . . . ?
C22 C21 C26 C25 0.8(3) . . . . ?
C5 C21 C26 C25 -177.3(2) . . . . ?
C24 C25 C26 C21 0.6(4) . . . . ?
C11 C10 C27 C28 -123.5(2) . . . . ?
C9 C10 C27 C28 61.7(3) . . . . ?
C11 C10 C27 C32 57.5(3) . . . . ?
C9 C10 C27 C32 -117.3(2) . . . . ?
C32 C27 C28 C29 -1.2(3) . . . . ?
C10 C27 C28 C29 179.8(2) . . . . ?
C27 C28 C29 C30 1.4(4) . . . . ?
C28 C29 C30 C31 -0.5(4) . . . . ?
C29 C30 C31 C32 -0.5(4) . . . . ?
C30 C31 C32 C27 0.7(4) . . . . ?
C28 C27 C32 C31 0.2(4) . . . . ?
C10 C27 C32 C31 179.2(2) . . . . ?
C16 C15 C33 C38 -57.2(4) . . . . ?
C14 C15 C33 C38 121.4(3) . . . . ?
C16 C15 C33 C34 123.6(3) . . . . ?
C14 C15 C33 C34 -57.8(3) . . . . ?
C38 C33 C34 C35 0.7(4) . . . . ?
C15 C33 C34 C35 180.0(2) . . . . ?
C33 C34 C35 C36 0.4(4) . . . . ?
C34 C35 C36 C37 -1.2(5) . . . . ?
C35 C36 C37 C38 0.7(6) . . . . ?
C34 C33 C38 C37 -1.2(5) . . . . ?
C15 C33 C38 C37 179.6(3) . . . . ?
C36 C37 C38 C33 0.4(6) . . . . ?
C19 C20 C39 C44 -129.6(2) . . . . ?
C2 C20 C39 C44 51.3(3) . . . . ?
C19 C20 C39 C40 52.6(3) . . . . ?
C2 C20 C39 C40 -126.6(2) . . . . ?
C44 C39 C40 C41 0.1(3) . . . . ?
C20 C39 C40 C41 178.0(2) . . . . ?
C39 C40 C41 C42 -1.5(4) . . . . ?
C40 C41 C42 C43 1.4(4) . . . . ?
C41 C42 C43 C44 0.1(4) . . . . ?
C42 C43 C44 C39 -1.4(4) . . . . ?
C40 C39 C44 C43 1.3(3) . . . . ?
C20 C39 C44 C43 -176.6(2) . . . . ?

#==============================================================================

loop_

_geom_hbond_atom_site_label_D

_geom_hbond_atom_site_label_H

_geom_hbond_atom_site_label_A

_geom_hbond_site_symmetry_D

_geom_hbond_site_symmetry_H

_geom_hbond_site_symmetry_A

_geom_hbond_distance_DA

_geom_hbond_distance_DH

_geom_hbond_distance_HA

_geom_hbond_angle_DHA

_geom_hbond_publ_flag

#==============================================================================

# Additional structures and associated data_? identifiers

# should be added at this point if there is more than one

# structure analysis in the CIF.

#==============================================================================

# End of CIF

#==============================================================================

N3 H3N N2 . . . 3.077(3) 0.880 2.625 113.0 no
N3 H3N N4 . . . 2.913(3) 0.880 2.402 117.3 no
N3 H3N N4A . . . 2.913(3) 0.880 2.402 117.3 no
N4A H4N N1A . . . 2.961(3) 0.880 2.400 121.9 no
N4A H4N N3 . . . 2.913(3) 0.880 2.348 122.0 no
cell_length_a 10.881(4) cell_length_b 12.396(5) cell_length_c 14.261(6) '' ''
'' '' ''