 
data_2011ilk0020
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             
'1,3-bis(3,5-dinitro)phenyl urea TMACl'
_chemical_melting_point           ?
_chemical_formula_moiety        
'4(C13 H8 N6 O9), 4(C4 H12 N), 2(C2 H3 N), 4(Cl)'
_chemical_formula_sum
 'C72 H86 Cl4 N30 O36'
_chemical_formula_weight          2089.51
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting           'Monoclinic'
_symmetry_space_group_name_H-M    'C 2/m'
_symmetry_space_group_name_Hall	  '-C 2y'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    26.6631(6)
_cell_length_b                    24.0557(4)
_cell_length_c                    17.3853(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  120.9950(10)
_cell_angle_gamma                 90.00
_cell_volume                      9558.7(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     130198
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'brown'
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.452
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              4336
_exptl_absorpt_coefficient_mu     0.224
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.9359
_exptl_absorpt_correction_T_max   0.9566
_exptl_absorpt_process_details    
'SADABS 2007/2 (Sheldrick, G.M., 2007)' 

 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2) 
_diffrn_radiation_wavelength           0.71073 
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper CCD camera on κ-goniostat' 
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '9.091'
_diffrn_reflns_number             61826
_diffrn_reflns_av_R_equivalents   0.0587
_diffrn_reflns_av_sigmaI/netI     0.0392
_diffrn_reflns_limit_h_min        -31
_diffrn_reflns_limit_h_max        31
_diffrn_reflns_limit_k_min        -28
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          3.09
_diffrn_reflns_theta_max          25.03
_reflns_number_total              8664
_reflns_number_gt                 6567
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)' 
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   'WINGX (Farrugia, 1998)' 
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0807P)²+16.1544P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          8664
_refine_ls_number_parameters      687
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0839
_refine_ls_R_factor_gt            0.0614
_refine_ls_wR_factor_ref          0.1708
_refine_ls_wR_factor_gt           0.1580
_refine_ls_goodness_of_fit_ref    1.091
_refine_ls_restrained_S_all       1.097
_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
C30 C 0.2945(3) 0.05170(17) 0.1432(3) 0.0902(17) Uani 1 1 d . . .
H30A H 0.3077 0.0530 0.1001 0.135 Uiso 1 1 calc R . .
H30B H 0.3094 0.0843 0.1826 0.135 Uiso 1 1 calc R . .
H30C H 0.2516 0.0517 0.1109 0.135 Uiso 1 1 calc R . .
C31 C 0.2959(2) 0.0000 0.2626(3) 0.0471(12) Uani 1 2 d S . .
H31A H 0.3102 0.0334 0.3001 0.071 Uiso 0.50 1 calc PR . .
H31B H 0.3106 -0.0331 0.3007 0.071 Uiso 0.50 1 calc PR . .
H31C H 0.2530 -0.0003 0.2293 0.071 Uiso 1 2 calc SR . .
C32 C 0.3822(3) 0.0000 0.2491(4) 0.0602(15) Uani 1 2 d S . .
H32A H 0.3961 0.0000 0.2068 0.090 Uiso 1 2 calc SR . .
H32B H 0.3967 -0.0333 0.2869 0.090 Uiso 0.50 1 calc PR . .
H32C H 0.3967 0.0333 0.2869 0.090 Uiso 0.50 1 calc PR . .
C40 C 0.05785(19) 0.05104(14) 0.1299(2) 0.0558(10) Uani 1 1 d . . .
H40A H 0.0815 0.0507 0.1016 0.084 Uiso 1 1 calc R . .
H40B H 0.0673 0.0842 0.1677 0.084 Uiso 1 1 calc R . .
H40C H 0.0163 0.0516 0.0834 0.084 Uiso 1 1 calc R . .
C41 C 0.03466(19) 0.0000 0.2294(3) 0.0427(11) Uani 1 2 d S . .
H41A H 0.0432 -0.0335 0.2661 0.064 Uiso 0.50 1 calc PR . .
H41B H -0.0069 0.0006 0.1828 0.064 Uiso 1 2 calc SR . .
H41C H 0.0440 0.0330 0.2675 0.064 Uiso 0.50 1 calc PR . .
C42 C 0.13423(18) 0.0000 0.2576(3) 0.0342(10) Uani 1 2 d S . .
H42A H 0.1579 0.0000 0.2293 0.051 Uiso 1 2 calc SR . .
H42B H 0.1432 -0.0333 0.2950 0.051 Uiso 0.50 1 calc PR . .
H42C H 0.1432 0.0333 0.2950 0.051 Uiso 0.50 1 calc PR . .
C50 C 0.3363(2) 0.44923(16) 0.3836(3) 0.0734(13) Uani 1 1 d . . .
H50A H 0.3460 0.4162 0.4217 0.110 Uiso 1 1 calc R . .
H50B H 0.3588 0.4489 0.3534 0.110 Uiso 1 1 calc R . .
H50C H 0.2944 0.4491 0.3386 0.110 Uiso 1 1 calc R . .
C51 C 0.4140(2) 0.5000 0.5102(4) 0.0609(15) Uani 1 2 d S . .
H51A H 0.4231 0.5336 0.5470 0.091 Uiso 0.50 1 calc PR . .
H51B H 0.4375 0.4994 0.4817 0.091 Uiso 1 2 calc SR . .
H51C H 0.4229 0.4670 0.5482 0.091 Uiso 0.50 1 calc PR . .
C52 C 0.3150(2) 0.5000 0.4844(4) 0.0541(13) Uani 1 2 d S . .
H52A H 0.3241 0.5333 0.5218 0.081 Uiso 0.50 1 calc PR . .
H52B H 0.3242 0.4668 0.5219 0.081 Uiso 0.50 1 calc PR . .
H52C H 0.2733 0.4999 0.4383 0.081 Uiso 1 2 calc SR . .
C63 C 0.3389(3) 0.0000 0.7753(5) 0.0612(15) Uani 1 2 d S . .
C60 C 0.3548(3) 0.5000 0.1137(4) 0.0684(16) Uani 1 2 d S . .
H60A H 0.3148 0.5121 0.0936 0.103 Uiso 0.50 1 calc PR . .
H60B H 0.3827 0.5255 0.1599 0.103 Uiso 0.50 1 calc PR . .
H60C H 0.3608 0.4624 0.1386 0.103 Uiso 0.50 1 calc PR . .
C62 C 0.3623(3) 0.0000 0.8704(5) 0.084(2) Uani 1 2 d S . .
H62A H 0.3651 0.0383 0.8914 0.125 Uiso 0.50 1 calc PR . .
H62B H 0.4013 -0.0169 0.9009 0.125 Uiso 0.50 1 calc PR . .
H62C H 0.3364 -0.0214 0.8839 0.125 Uiso 0.50 1 calc PR . .
C61 C 0.3637(3) 0.5000 0.0380(5) 0.0628(15) Uani 1 2 d S . .
N100 N 0.3214(3) 0.0000 0.7002(4) 0.0897(18) Uani 1 2 d S . .
N102 N 0.3721(4) 0.5000 -0.0185(5) 0.112(3) Uani 1 2 d S . .
C1 C 0.37660(11) 0.22810(11) 0.63314(17) 0.0227(6) Uani 1 1 d . . .
C2 C 0.29996(11) 0.24468(11) 0.47450(17) 0.0214(6) Uani 1 1 d . . .
C3 C 0.26849(11) 0.28675(11) 0.41296(17) 0.0217(6) Uani 1 1 d . . .
H3 H 0.2764 0.3246 0.4305 0.026 Uiso 1 1 calc R . .
C4 C 0.22604(11) 0.27298(10) 0.32695(17) 0.0207(6) Uani 1 1 d . . .
C5 C 0.21268(11) 0.21873(11) 0.29652(17) 0.0213(6) Uani 1 1 d . . .
H5 H 0.1834 0.2099 0.2366 0.026 Uiso 1 1 calc R . .
C6 C 0.24470(11) 0.17842(11) 0.35891(17) 0.0212(6) Uani 1 1 d . . .
C7 C 0.28750(11) 0.18914(11) 0.44664(17) 0.0224(6) Uani 1 1 d . . .
H7 H 0.3080 0.1596 0.4872 0.027 Uiso 1 1 calc R . .
C8 C 0.45630(11) 0.24223(12) 0.79152(17) 0.0252(6) Uani 1 1 d . . .
C9 C 0.48956(11) 0.28366(12) 0.85317(18) 0.0272(6) Uani 1 1 d . . .
H9 H 0.4816 0.3218 0.8372 0.033 Uiso 1 1 calc R . .
C10 C 0.53401(12) 0.26849(13) 0.93736(18) 0.0300(7) Uani 1 1 d . . .
C11 C 0.54824(12) 0.21414(13) 0.96539(19) 0.0320(7) Uani 1 1 d . . .
H11 H 0.5793 0.2045 1.0237 0.038 Uiso 1 1 calc R . .
C12 C 0.51414(13) 0.17502(13) 0.9028(2) 0.0349(7) Uani 1 1 d . . .
C13 C 0.46842(12) 0.18689(12) 0.81709(19) 0.0303(6) Uani 1 1 d . . .
H13 H 0.4459 0.1579 0.7768 0.036 Uiso 1 1 calc R . .
C14 C 0.37891(11) 0.27388(11) 0.38512(16) 0.0212(6) Uani 1 1 d . . .
C15 C 0.45754(10) 0.25409(11) 0.54214(17) 0.0215(6) Uani 1 1 d . . .
C16 C 0.48642(11) 0.21070(11) 0.60187(17) 0.0217(6) Uani 1 1 d . . .
H16 H 0.4755 0.1733 0.5833 0.026 Uiso 1 1 calc R . .
C17 C 0.53088(11) 0.22225(11) 0.68798(17) 0.0233(6) Uani 1 1 d . . .
C18 C 0.54870(12) 0.27578(11) 0.71911(18) 0.0260(6) Uani 1 1 d . . .
H18 H 0.5794 0.2833 0.7787 0.031 Uiso 1 1 calc R . .
C19 C 0.51905(12) 0.31723(11) 0.65829(19) 0.0271(6) Uani 1 1 d . . .
C20 C 0.47430(11) 0.30878(11) 0.57074(18) 0.0239(6) Uani 1 1 d . . .
H20 H 0.4556 0.3392 0.5313 0.029 Uiso 1 1 calc R . .
C21 C 0.30137(11) 0.26197(11) 0.22486(17) 0.0219(6) Uani 1 1 d . . .
C22 C 0.26919(11) 0.22140(11) 0.16010(17) 0.0229(6) Uani 1 1 d . . .
H22 H 0.2775 0.1831 0.1741 0.027 Uiso 1 1 calc R . .
C23 C 0.22555(11) 0.23754(12) 0.07611(17) 0.0249(6) Uani 1 1 d . . .
C24 C 0.21048(12) 0.29233(12) 0.05144(19) 0.0287(6) Uani 1 1 d . . .
H24 H 0.1794 0.3027 -0.0064 0.034 Uiso 1 1 calc R . .
C25 C 0.24361(12) 0.33089(12) 0.11654(18) 0.0274(6) Uani 1 1 d . . .
C26 C 0.28886(12) 0.31768(11) 0.20218(18) 0.0255(6) Uani 1 1 d . . .
H26 H 0.3108 0.3461 0.2443 0.031 Uiso 1 1 calc R . .
N1 N 0.34220(9) 0.26127(9) 0.56041(14) 0.0220(5) Uani 1 1 d . . .
H1A H 0.3476 0.2973 0.5693 0.026 Uiso 1 1 calc R . .
N2 N 0.41286(9) 0.26025(10) 0.70702(14) 0.0255(5) Uani 1 1 d . . .
H2A H 0.4079 0.2965 0.6998 0.031 Uiso 1 1 calc R . .
N3 N 0.19387(10) 0.31836(10) 0.26307(15) 0.0263(5) Uani 1 1 d . . .
N4 N 0.23422(10) 0.11981(9) 0.32950(16) 0.0263(5) Uani 1 1 d . . .
N5 N 0.56773(11) 0.31344(12) 1.00183(16) 0.0391(7) Uani 1 1 d . . .
N6 N 0.52674(14) 0.11582(12) 0.9289(2) 0.0515(8) Uani 1 1 d . . .
N7 N 0.41410(9) 0.23967(9) 0.45578(14) 0.0224(5) Uani 1 1 d . . .
H7A H 0.4084 0.2038 0.4449 0.027 Uiso 1 1 calc R . .
N8 N 0.34371(9) 0.24278(9) 0.30902(14) 0.0232(5) Uani 1 1 d . . .
H8A H 0.3487 0.2065 0.3146 0.028 Uiso 1 1 calc R . .
N9 N 0.56121(10) 0.17531(10) 0.74886(15) 0.0280(5) Uani 1 1 d . . .
N10 N 0.53641(11) 0.37515(11) 0.68747(19) 0.0432(7) Uani 1 1 d . . .
N11 N 0.19341(10) 0.19380(11) 0.00879(15) 0.0302(6) Uani 1 1 d . . .
N12 N 0.22998(12) 0.39022(11) 0.09402(18) 0.0380(6) Uani 1 1 d . . .
N13 N 0.3170(2) 0.0000 0.1984(3) 0.0467(10) Uani 1 2 d S . .
N14 N 0.07079(16) 0.0000 0.1865(2) 0.0323(8) Uani 1 2 d S . .
N15 N 0.35097(17) 0.5000 0.4400(3) 0.0407(9) Uani 1 2 d S . .
O1 O 0.37529(8) 0.17757(8) 0.63315(12) 0.0297(5) Uani 1 1 d . . .
O2 O 0.15237(8) 0.30583(9) 0.18943(13) 0.0343(5) Uani 1 1 d . . .
O3 O 0.21117(9) 0.36594(8) 0.28666(14) 0.0395(5) Uani 1 1 d . . .
O4 O 0.20764(9) 0.11086(8) 0.24864(14) 0.0379(5) Uani 1 1 d . . .
O5 O 0.25323(9) 0.08361(8) 0.38714(14) 0.0346(5) Uani 1 1 d . . .
O6 O 0.55239(12) 0.36109(12) 0.97886(18) 0.0825(11) Uani 1 1 d . . .
O7 O 0.60948(9) 0.30041(10) 1.07427(13) 0.0446(6) Uani 1 1 d . . .
O8 O 0.50135(14) 0.08070(11) 0.87083(18) 0.0685(8) Uani 1 1 d . . .
O9 O 0.56120(13) 0.10613(12) 1.00826(18) 0.0769(9) Uani 1 1 d . . .
O10 O 0.37864(8) 0.32450(8) 0.38809(12) 0.0283(4) Uani 1 1 d . . .
O11 O 0.60833(9) 0.18470(9) 0.81729(13) 0.0375(5) Uani 1 1 d . . .
O12 O 0.53800(9) 0.12973(8) 0.72872(14) 0.0377(5) Uani 1 1 d . . .
O13 O 0.56457(14) 0.38380(11) 0.76851(18) 0.0855(11) Uani 1 1 d . . .
O14 O 0.52236(10) 0.41124(9) 0.63039(16) 0.0477(6) Uani 1 1 d . . .
O15 O 0.21085(9) 0.14605(9) 0.02751(14) 0.0385(5) Uani 1 1 d . . .
O16 O 0.15150(9) 0.20824(9) -0.06343(13) 0.0385(5) Uani 1 1 d . . .
O17 O 0.26103(11) 0.42456(9) 0.15091(17) 0.0537(7) Uani 1 1 d . . .
O18 O 0.18834(12) 0.40168(10) 0.02039(16) 0.0572(7) Uani 1 1 d . . .
Cl1 Cl 0.38128(4) 0.12049(3) 0.37753(5) 0.0402(2) Uani 1 1 d . . .
Cl2 Cl 0.11385(3) 0.11904(3) 0.36546(5) 0.0365(2) Uani 1 1 d . . .
N16 N 0.4160(3) 0.0063(6) 0.5973(4) 0.069(3) Uani 0.50 1 d PD A -1
C160 C 0.3964(5) 0.0618(3) 0.6111(7) 0.090(3) Uani 0.50 1 d PD A -1
H16A H 0.3757 0.0818 0.5539 0.134 Uiso 0.50 1 calc PR A -1
H16B H 0.4305 0.0835 0.6544 0.134 Uiso 0.50 1 calc PR A -1
H16C H 0.3701 0.0565 0.6343 0.134 Uiso 0.50 1 calc PR A -1
C161 C 0.4589(4) 0.0062(11) 0.5609(6) 0.260(13) Uani 0.50 1 d PD A -1
H16D H 0.4402 0.0246 0.5023 0.390 Uiso 0.50 1 calc PR A -1
H16E H 0.4686 -0.0322 0.5548 0.390 Uiso 0.50 1 calc PR A -1
H16F H 0.4948 0.0262 0.6030 0.390 Uiso 0.50 1 calc PR A -1
C162 C 0.3613(4) -0.0223(4) 0.5289(7) 0.106(4) Uani 0.50 1 d PD A -1
H16G H 0.3434 -0.0015 0.4724 0.159 Uiso 1 2 calc SR A -1
H16H H 0.3339 -0.0242 0.5505 0.159 Uiso 0.50 1 calc PR A -1
H16I H 0.3707 -0.0600 0.5190 0.159 Uiso 0.50 1 calc PR A -1
C163 C 0.4460(4) -0.0229(4) 0.6846(6) 0.099(4) Uani 0.50 1 d PD A -1
H16J H 0.4815 -0.0025 0.7269 0.149 Uiso 0.50 1 calc PR A -1
H16K H 0.4565 -0.0606 0.6764 0.149 Uiso 0.50 1 calc PR A -1
H16L H 0.4197 -0.0251 0.7084 0.149 Uiso 0.50 1 calc PR A -1
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C30 N13 1.494(4) . ?
C31 N13 1.487(6) . ?
C32 N13 1.489(7) . ?
C40 N14 1.498(4) . ?
C41 N14 1.492(6) . ?
C42 N14 1.495(5) . ?
C50 N15 1.486(4) . ?
C51 N15 1.483(6) . ?
C52 N15 1.509(6) . ?
C63 N100 1.138(8) . ?
C63 C62 1.436(9) . ?
C60 C61 1.452(9) . ?
C61 N102 1.115(8) . ?
C1 O1 1.216(3) . ?
C1 N1 1.372(3) . ?
C1 N2 1.380(3) . ?
C2 N1 1.388(3) . ?
C2 C3 1.396(4) . ?
C2 C7 1.402(4) . ?
C3 C4 1.372(4) . ?
C4 C5 1.384(4) . ?
C4 N3 1.476(3) . ?
C5 C6 1.376(4) . ?
C6 C7 1.379(4) . ?
C6 N4 1.477(3) . ?
C8 C13 1.388(4) . ?
C8 N2 1.391(3) . ?
C8 C9 1.396(4) . ?
C9 C10 1.376(4) . ?
C10 C11 1.379(4) . ?
C10 N5 1.482(4) . ?
C11 C12 1.370(4) . ?
C12 C13 1.384(4) . ?
C12 N6 1.480(4) . ?
C14 O10 1.219(3) . ?
C14 N7 1.371(3) . ?
C14 N8 1.383(3) . ?
C15 N7 1.387(3) . ?
C15 C16 1.392(4) . ?
C15 C20 1.396(4) . ?
C16 C17 1.377(4) . ?
C17 C18 1.383(4) . ?
C17 N9 1.472(3) . ?
C18 C19 1.370(4) . ?
C19 C20 1.382(4) . ?
C19 N10 1.473(4) . ?
C21 N8 1.388(3) . ?
C21 C26 1.388(4) . ?
C21 C22 1.400(4) . ?
C22 C23 1.374(4) . ?
C23 C24 1.380(4) . ?
C23 N11 1.476(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.387(4) . ?
C25 N12 1.475(4) . ?
N3 O2 1.223(3) . ?
N3 O3 1.223(3) . ?
N4 O5 1.223(3) . ?
N4 O4 1.224(3) . ?
N5 O6 1.213(4) . ?
N5 O7 1.216(3) . ?
N6 O8 1.219(4) . ?
N6 O9 1.224(4) . ?
N9 O12 1.219(3) . ?
N9 O11 1.227(3) . ?
N10 O14 1.223(3) . ?
N10 O13 1.226(4) . ?
N11 O15 1.219(3) . ?
N11 O16 1.225(3) . ?
N12 O18 1.218(3) . ?
N12 O17 1.226(4) . ?
N13 C30 1.494(4) 6 ?
N14 C40 1.498(4) 6 ?
N15 C50 1.486(4) 6_565 ?
N16 C163 1.480(9) . ?
N16 C162 1.493(10) . ?
N16 C160 1.498(12) . ?
N16 C161 1.565(10) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N100 C63 C62 178.8(7) . . ?
N102 C61 C60 178.1(8) . . ?
O1 C1 N1 125.2(2) . . ?
O1 C1 N2 124.5(2) . . ?
N1 C1 N2 110.3(2) . . ?
N1 C2 C3 116.8(2) . . ?
N1 C2 C7 124.2(2) . . ?
C3 C2 C7 119.0(2) . . ?
C4 C3 C2 119.6(2) . . ?
C3 C4 C5 123.3(2) . . ?
C3 C4 N3 118.4(2) . . ?
C5 C4 N3 118.3(2) . . ?
C6 C5 C4 115.5(2) . . ?
C5 C6 C7 124.4(2) . . ?
C5 C6 N4 118.1(2) . . ?
C7 C6 N4 117.6(2) . . ?
C6 C7 C2 118.3(2) . . ?
C13 C8 N2 124.5(3) . . ?
C13 C8 C9 119.2(3) . . ?
N2 C8 C9 116.3(3) . . ?
C10 C9 C8 119.1(3) . . ?
C9 C10 C11 123.9(3) . . ?
C9 C10 N5 117.7(3) . . ?
C11 C10 N5 118.4(3) . . ?
C12 C11 C10 114.9(3) . . ?
C11 C12 C13 124.7(3) . . ?
C11 C12 N6 117.7(3) . . ?
C13 C12 N6 117.6(3) . . ?
C12 C13 C8 118.2(3) . . ?
O10 C14 N7 125.3(2) . . ?
O10 C14 N8 124.4(2) . . ?
N7 C14 N8 110.3(2) . . ?
N7 C15 C16 116.9(2) . . ?
N7 C15 C20 123.8(2) . . ?
C16 C15 C20 119.2(2) . . ?
C17 C16 C15 119.7(2) . . ?
C16 C17 C18 122.9(3) . . ?
C16 C17 N9 118.3(2) . . ?
C18 C17 N9 118.8(2) . . ?
C19 C18 C17 115.5(2) . . ?
C18 C19 C20 124.8(3) . . ?
C18 C19 N10 117.9(2) . . ?
C20 C19 N10 117.3(3) . . ?
C19 C20 C15 117.9(3) . . ?
N8 C21 C26 124.5(2) . . ?
N8 C21 C22 116.4(2) . . ?
C26 C21 C22 119.1(2) . . ?
C23 C22 C21 119.4(2) . . ?
C22 C23 C24 123.5(3) . . ?
C22 C23 N11 118.0(2) . . ?
C24 C23 N11 118.5(2) . . ?
C25 C24 C23 115.3(3) . . ?
C24 C25 C26 124.3(3) . . ?
C24 C25 N12 117.9(3) . . ?
C26 C25 N12 117.8(3) . . ?
C25 C26 C21 118.3(3) . . ?
C1 N1 C2 127.7(2) . . ?
C1 N2 C8 127.7(2) . . ?
O2 N3 O3 124.3(2) . . ?
O2 N3 C4 117.9(2) . . ?
O3 N3 C4 117.8(2) . . ?
O5 N4 O4 124.5(2) . . ?
O5 N4 C6 118.1(2) . . ?
O4 N4 C6 117.4(2) . . ?
O6 N5 O7 123.9(3) . . ?
O6 N5 C10 118.0(2) . . ?
O7 N5 C10 118.1(3) . . ?
O8 N6 O9 125.2(3) . . ?
O8 N6 C12 118.1(3) . . ?
O9 N6 C12 116.7(3) . . ?
C14 N7 C15 128.6(2) . . ?
C14 N8 C21 127.7(2) . . ?
O12 N9 O11 124.0(2) . . ?
O12 N9 C17 118.3(2) . . ?
O11 N9 C17 117.7(2) . . ?
O14 N10 O13 124.2(3) . . ?
O14 N10 C19 118.8(3) . . ?
O13 N10 C19 117.0(3) . . ?
O15 N11 O16 124.2(2) . . ?
O15 N11 C23 118.3(2) . . ?
O16 N11 C23 117.5(2) . . ?
O18 N12 O17 124.5(3) . . ?
O18 N12 C25 117.7(3) . . ?
O17 N12 C25 117.8(3) . . ?
C31 N13 C32 109.4(4) . . ?
C31 N13 C30 107.4(3) . 6 ?
C32 N13 C30 109.9(3) . 6 ?
C31 N13 C30 107.4(3) . . ?
C32 N13 C30 109.9(3) . . ?
C30 N13 C30 112.7(4) 6 . ?
C41 N14 C42 109.5(3) . . ?
C41 N14 C40 109.8(2) . 6 ?
C42 N14 C40 108.8(2) . 6 ?
C41 N14 C40 109.8(2) . . ?
C42 N14 C40 108.8(2) . . ?
C40 N14 C40 110.1(3) 6 . ?
C51 N15 C50 110.2(3) . 6_565 ?
C51 N15 C50 110.2(3) . . ?
C50 N15 C50 110.5(5) 6_565 . ?
C51 N15 C52 109.1(4) . . ?
C50 N15 C52 108.4(3) 6_565 . ?
C50 N15 C52 108.4(3) . . ?
C163 N16 C162 112.7(11) . . ?
C163 N16 C160 107.9(7) . . ?
C162 N16 C160 105.0(7) . . ?
C163 N16 C161 107.1(8) . . ?
C162 N16 C161 107.2(8) . . ?
C160 N16 C161 117.1(13) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.03
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.881
_refine_diff_density_min   -0.764
_refine_diff_density_rms    0.202
