# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_ms050
_database_code_depnum_ccdc_archive 'CCDC 915396'
#TrackingRef 'ms050.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 N4 O, C4 F8 I2'
_chemical_formula_sum            'C16 H8 F8 I2 N4 O'
_chemical_formula_weight         678.06
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   8.0406(12)
_cell_length_b                   22.942(3)
_cell_length_c                   11.6153(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.400(12)
_cell_angle_gamma                90.00
_cell_volume                     2033.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9932
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      34.15
_exptl_crystal_description       table
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    3.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_absorpt_correction_T_min  0.3687
_exptl_absorpt_correction_T_max  0.5233
_exptl_special_details           
;
Bruker KRYOFLEX low temperature device.
;
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            29563
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         34.74
_reflns_number_total             7828
_reflns_number_gt                6584
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    
;
SIR2002 (Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L.,
Giacovazzo, C., Polidori, G. & Spagna, R. (2003).
J. Appl. Cryst. 36, 1103.)
;
_computing_structure_refinement  
'SHELXL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, L.J. (1997) Jour. Appl. Cryst. 30, 565)
Mercury (Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E.,
Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006).
J. Appl. Cryst. 39, 453-457
;
_computing_publication_material  SHELXTL
_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.
;
_iucr_refine_instructions_details 
;
TITL MS050 in P2(1)/n
CELL 0.71073 8.0406 22.942 11.6153 90.000 108.400 90.000
ZERR 4.00 0.0012 0.003 0.0015 0.000 0.012 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N O F I
UNIT 64 32 16 4 32 8
L.S. 4
ACTA
BOND $H
CONF
FMAP 2
PLAN 20
SIZE 0.04 0.22 0.35
TEMP -170.000
OMIT 0 1 1
WGHT 0.024000 1.198800
FVAR 0.05715 0.57917
MOLE 1
I1 6 0.705706 1.031042 0.897333 11.00000 0.02385 0.01542 =
0.02427 -0.00120 0.00869 0.00139
I2 6 0.444008 0.711580 0.764251 11.00000 0.02531 0.01628 =
0.02873 -0.00103 0.01150 -0.00219
C1 1 0.426904 0.804456 0.732497 11.00000 0.01970 0.01716 =
0.02854 0.00121 0.00773 -0.00016
F1 5 0.432274 0.815902 0.620552 11.00000 0.04333 0.02394 =
0.02151 0.00128 0.00281 -0.00497
F2 5 0.273929 0.825771 0.739483 11.00000 0.01781 0.02299 =
0.06153 -0.00328 0.01079 0.00152
C2 1 0.578122 0.837810 0.826153 11.00000 0.01868 0.01709 =
0.01923 0.00174 0.00792 0.00146
F3 5 0.579405 0.822122 0.938011 11.00000 0.04300 0.02305 =
0.02029 0.00367 0.01303 -0.00329
F4 5 0.729512 0.819909 0.810852 11.00000 0.01774 0.01801 =
0.03422 -0.00138 0.01001 0.00229
C3 1 0.568461 0.905305 0.818345 11.00000 0.01784 0.01820 =
0.01912 0.00087 0.00681 0.00381
F5 5 0.534613 0.921417 0.701208 11.00000 0.02979 0.01937 =
0.01942 0.00381 0.00234 0.00119
F6 5 0.432941 0.922604 0.854686 11.00000 0.02214 0.02374 =
0.04264 -0.00518 0.01708 0.00263
C4 1 0.734809 0.937683 0.893452 11.00000 0.02305 0.01620 =
0.01722 0.00093 0.00636 0.00205
F7 5 0.784428 0.916067 1.007596 11.00000 0.03745 0.02314 =
0.01889 0.00404 0.00217 -0.00182
F8 5 0.864521 0.925130 0.846628 11.00000 0.01908 0.01918 =
0.03245 -0.00117 0.01011 0.00179
MOLE 2
EADP O1A N2B
EXYZ O1A N2B
EADP O1B N2A
EXYZ O1B N2A
part 1
O1A 4 0.847699 0.419590 1.036332 21.00000 0.02339 0.01809 =
0.02630 -0.00269 0.00386 -0.00034
N2A 3 0.876920 0.358973 1.051467 21.00000 0.02473 0.02068 =
0.02377 -0.00095 0.00123 0.00421
part 2
O1B 4 0.876920 0.358973 1.051467 -21.00000 0.02473 0.02068 =
0.02377 -0.00095 0.00123 0.00421
N2B 3 0.847699 0.419590 1.036332 -21.00000 0.02339 0.01809 =
0.02630 -0.00269 0.00386 -0.00034
part 0
N1 3 0.625304 0.373298 0.901677 11.00000 0.01886 0.01508 =
0.01826 0.00053 0.00574 0.00039
N3 3 0.707431 0.151400 0.920340 11.00000 0.02557 0.01743 =
0.03076 -0.00036 0.00955 0.00334
N4 3 0.495915 0.592191 0.823519 11.00000 0.03239 0.01514 =
0.02788 -0.00044 0.01075 0.00124
C5 1 0.741377 0.335013 0.968686 11.00000 0.02145 0.01658 =
0.01996 0.00127 0.00803 0.00261
C6 1 0.697410 0.424169 0.946620 11.00000 0.02081 0.01659 =
0.02055 -0.00175 0.00963 -0.00110
C7 1 0.730939 0.271695 0.953942 11.00000 0.02127 0.01655 =
0.01897 0.00214 0.00859 0.00338
C8 1 0.859992 0.235065 1.025764 11.00000 0.02521 0.02061 =
0.02671 0.00133 0.00131 0.00424
H8 2 0.970789 0.252443 1.085628 11.00000 -1.20000
C9 1 0.841837 0.175636 1.006104 11.00000 0.02764 0.01977 =
0.03188 0.00240 0.00406 0.00617
H9 2 0.929825 0.148848 1.054232 11.00000 -1.20000
C10 1 0.584254 0.186937 0.851505 11.00000 0.02487 0.02061 =
0.02714 -0.00101 0.00622 0.00085
H10 2 0.492211 0.168676 0.794006 11.00000 -1.20000
C11 1 0.590020 0.246872 0.865260 11.00000 0.02137 0.01904 =
0.02386 0.00242 0.00455 0.00334
H11 2 0.506508 0.269567 0.820909 11.00000 -1.20000
C12 1 0.627551 0.481983 0.904455 11.00000 0.02231 0.01534 =
0.02017 -0.00104 0.01087 -0.00071
C13 1 0.460535 0.488288 0.821798 11.00000 0.02351 0.01711 =
0.02104 -0.00218 0.00867 -0.00163
H13 2 0.379834 0.451713 0.790228 11.00000 -1.20000
C14 1 0.400787 0.544155 0.784218 11.00000 0.02437 0.02045 =
0.02235 0.00014 0.00728 0.00110
H14 2 0.282714 0.550620 0.732440 11.00000 -1.20000
C15 1 0.656916 0.585355 0.901956 11.00000 0.03354 0.01599 =
0.03009 -0.00348 0.00993 -0.00456
H15 2 0.722498 0.620770 0.926715 11.00000 -1.20000
C16 1 0.728579 0.531624 0.945153 11.00000 0.02454 0.01672 =
0.02580 -0.00217 0.00605 -0.00224
H16 2 0.838681 0.529428 0.995678 11.00000 -1.20000
HKLF 4
END
;
_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^)+(0.0240P)^2^+1.1988P] 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    REFXYZ
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7828
_refine_ls_number_parameters     305
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0242
_refine_ls_wR_factor_ref         0.0573
_refine_ls_wR_factor_gt          0.0532
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.008
_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 0.705706(16) 1.031042(5) 0.897333(11) 0.02092(3) Uani 1 1 d . . .
I2 I 0.444008(16) 0.711580(5) 0.764251(12) 0.02275(3) Uani 1 1 d . . .
C1 C 0.4269(2) 0.80446(8) 0.73250(18) 0.0218(3) Uani 1 1 d . . .
F1 F 0.43227(18) 0.81590(6) 0.62055(11) 0.0313(3) Uani 1 1 d . . .
F2 F 0.27393(16) 0.82577(6) 0.73948(14) 0.0345(3) Uani 1 1 d . . .
C2 C 0.5781(2) 0.83781(8) 0.82615(16) 0.0179(3) Uani 1 1 d . . .
F3 F 0.57941(18) 0.82212(5) 0.93801(10) 0.0281(3) Uani 1 1 d . . .
F4 F 0.72951(14) 0.81991(5) 0.81085(11) 0.0229(2) Uani 1 1 d . . .
C3 C 0.5685(2) 0.90530(8) 0.81834(16) 0.0182(3) Uani 1 1 d . . .
F5 F 0.53461(15) 0.92142(5) 0.70121(10) 0.0241(2) Uani 1 1 d . . .
F6 F 0.43294(15) 0.92260(5) 0.85469(12) 0.0279(3) Uani 1 1 d . . .
C4 C 0.7348(2) 0.93768(8) 0.89345(16) 0.0188(3) Uani 1 1 d . . .
F7 F 0.78443(17) 0.91607(5) 1.00760(10) 0.0281(3) Uani 1 1 d . . .
F8 F 0.86452(14) 0.92513(5) 0.84663(11) 0.0231(2) Uani 1 1 d . . .
O1A O 0.84770(19) 0.41959(7) 1.03633(14) 0.0235(3) Uani 0.579(19) 1 d P A 1
N2A N 0.8769(2) 0.35897(7) 1.05147(14) 0.0246(4) Uani 0.579(19) 1 d P A 1
O1B O 0.8769(2) 0.35897(7) 1.05147(14) 0.0246(4) Uani 0.421(19) 1 d P A 2
N2B N 0.84770(19) 0.41959(7) 1.03633(14) 0.0235(3) Uani 0.421(19) 1 d P A 2
N1 N 0.6253(2) 0.37330(7) 0.90168(14) 0.0174(3) Uani 1 1 d . A .
N3 N 0.7074(2) 0.15140(7) 0.92034(16) 0.0244(3) Uani 1 1 d . . .
N4 N 0.4959(2) 0.59219(7) 0.82352(16) 0.0248(3) Uani 1 1 d . . .
C5 C 0.7414(2) 0.33501(8) 0.96869(16) 0.0190(3) Uani 1 1 d . . .
C6 C 0.6974(2) 0.42417(8) 0.94662(16) 0.0186(3) Uani 1 1 d . . .
C7 C 0.7309(2) 0.27170(8) 0.95394(16) 0.0184(3) Uani 1 1 d . A .
C8 C 0.8600(3) 0.23507(9) 1.02576(19) 0.0258(4) Uani 1 1 d . . .
H8 H 0.971(3) 0.2524(12) 1.086(2) 0.031 Uiso 1 1 d . . .
C9 C 0.8418(3) 0.17564(9) 1.0061(2) 0.0277(4) Uani 1 1 d . A .
H9 H 0.930(3) 0.1488(12) 1.054(2) 0.033 Uiso 1 1 d . . .
C10 C 0.5843(3) 0.18694(9) 0.85150(19) 0.0247(4) Uani 1 1 d . A .
H10 H 0.492(3) 0.1687(12) 0.794(2) 0.030 Uiso 1 1 d . . .
C11 C 0.5900(3) 0.24687(9) 0.86526(18) 0.0220(4) Uani 1 1 d . . .
H11 H 0.507(3) 0.2696(11) 0.821(2) 0.026 Uiso 1 1 d . . .
C12 C 0.6276(2) 0.48198(8) 0.90446(16) 0.0183(3) Uani 1 1 d . A .
C13 C 0.4605(2) 0.48829(8) 0.82180(17) 0.0202(3) Uani 1 1 d . . .
H13 H 0.380(3) 0.4517(11) 0.790(2) 0.024 Uiso 1 1 d . . .
C14 C 0.4008(3) 0.54415(9) 0.78422(18) 0.0224(4) Uani 1 1 d . A .
H14 H 0.283(3) 0.5506(11) 0.732(2) 0.027 Uiso 1 1 d . . .
C15 C 0.6569(3) 0.58536(9) 0.90196(19) 0.0266(4) Uani 1 1 d . A .
H15 H 0.722(3) 0.6208(12) 0.927(2) 0.032 Uiso 1 1 d . . .
C16 C 0.7286(3) 0.53162(8) 0.94515(19) 0.0228(4) Uani 1 1 d . . .
H16 H 0.839(3) 0.5294(11) 0.996(2) 0.027 Uiso 1 1 d . . .
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 0.02385(6) 0.01542(6) 0.02427(6) -0.00120(4) 0.00869(4) 0.00139(4)
I2 0.02531(6) 0.01628(6) 0.02873(6) -0.00103(4) 0.01150(5) -0.00219(4)
C1 0.0197(8) 0.0172(8) 0.0285(9) 0.0012(7) 0.0077(7) -0.0002(6)
F1 0.0433(7) 0.0239(6) 0.0215(6) 0.0013(5) 0.0028(5) -0.0050(5)
F2 0.0178(5) 0.0230(6) 0.0615(9) -0.0033(6) 0.0108(6) 0.0015(5)
C2 0.0187(7) 0.0171(8) 0.0192(7) 0.0017(6) 0.0079(6) 0.0015(6)
F3 0.0430(7) 0.0230(6) 0.0203(5) 0.0037(4) 0.0130(5) -0.0033(5)
F4 0.0177(5) 0.0180(5) 0.0342(6) -0.0014(4) 0.0100(4) 0.0023(4)
C3 0.0178(7) 0.0182(8) 0.0191(7) 0.0009(6) 0.0068(6) 0.0038(6)
F5 0.0298(6) 0.0194(5) 0.0194(5) 0.0038(4) 0.0023(4) 0.0012(4)
F6 0.0221(5) 0.0237(6) 0.0426(7) -0.0052(5) 0.0171(5) 0.0026(4)
C4 0.0231(8) 0.0162(8) 0.0172(7) 0.0009(6) 0.0064(6) 0.0021(6)
F7 0.0374(7) 0.0231(6) 0.0189(5) 0.0040(4) 0.0022(5) -0.0018(5)
F8 0.0191(5) 0.0192(5) 0.0324(6) -0.0012(4) 0.0101(4) 0.0018(4)
O1A 0.0234(7) 0.0181(7) 0.0263(7) -0.0027(5) 0.0039(6) -0.0003(5)
N2A 0.0247(8) 0.0207(8) 0.0238(7) -0.0010(6) 0.0012(6) 0.0042(6)
O1B 0.0247(8) 0.0207(8) 0.0238(7) -0.0010(6) 0.0012(6) 0.0042(6)
N2B 0.0234(7) 0.0181(7) 0.0263(7) -0.0027(5) 0.0039(6) -0.0003(5)
N1 0.0189(7) 0.0151(7) 0.0183(6) 0.0005(5) 0.0057(5) 0.0004(5)
N3 0.0256(8) 0.0174(8) 0.0308(8) -0.0004(6) 0.0095(7) 0.0033(6)
N4 0.0324(9) 0.0151(7) 0.0279(8) -0.0004(6) 0.0108(7) 0.0012(6)
C5 0.0215(8) 0.0166(8) 0.0200(8) 0.0013(6) 0.0080(6) 0.0026(6)
C6 0.0208(8) 0.0166(8) 0.0205(8) -0.0017(6) 0.0096(6) -0.0011(6)
C7 0.0213(8) 0.0166(8) 0.0190(8) 0.0021(6) 0.0086(6) 0.0034(6)
C8 0.0252(9) 0.0206(9) 0.0267(9) 0.0013(7) 0.0013(7) 0.0042(7)
C9 0.0276(10) 0.0198(9) 0.0319(10) 0.0024(7) 0.0041(8) 0.0062(7)
C10 0.0249(9) 0.0206(9) 0.0271(9) -0.0010(7) 0.0062(7) 0.0009(7)
C11 0.0214(8) 0.0190(9) 0.0239(9) 0.0024(7) 0.0045(7) 0.0033(7)
C12 0.0223(8) 0.0153(8) 0.0202(8) -0.0010(6) 0.0109(7) -0.0007(6)
C13 0.0235(8) 0.0171(8) 0.0210(8) -0.0022(6) 0.0087(7) -0.0016(7)
C14 0.0244(9) 0.0204(9) 0.0224(8) 0.0001(7) 0.0073(7) 0.0011(7)
C15 0.0335(10) 0.0160(9) 0.0301(10) -0.0035(7) 0.0099(8) -0.0046(7)
C16 0.0245(9) 0.0167(8) 0.0258(9) -0.0022(7) 0.0060(7) -0.0022(7)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C4 2.1566(19) . ?
I2 C1 2.159(2) . ?
C1 F1 1.341(2) . ?
C1 F2 1.350(2) . ?
C1 C2 1.553(3) . ?
C2 F3 1.345(2) . ?
C2 F4 1.349(2) . ?
C2 C3 1.552(3) . ?
C3 F6 1.347(2) . ?
C3 F5 1.352(2) . ?
C3 C4 1.538(3) . ?
C4 F8 1.351(2) . ?
C4 F7 1.352(2) . ?
O1A C6 1.327(2) . ?
O1A N2A 1.412(2) . ?
N2A C5 1.324(2) . ?
N1 C6 1.334(2) . ?
N1 C5 1.338(2) . ?
N3 C10 1.336(3) . ?
N3 C9 1.338(3) . ?
N4 C15 1.336(3) . ?
N4 C14 1.337(3) . ?
C5 C7 1.462(3) . ?
C6 C12 1.463(3) . ?
C7 C11 1.390(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.383(3) . ?
C8 H8 1.02(3) . ?
C9 H9 0.97(3) . ?
C10 C11 1.383(3) . ?
C10 H10 0.93(3) . ?
C11 H11 0.88(3) . ?
C12 C13 1.390(3) . ?
C12 C16 1.392(3) . ?
C13 C14 1.390(3) . ?
C13 H13 1.05(2) . ?
C14 H14 0.96(2) . ?
C15 C16 1.386(3) . ?
C15 H15 0.96(3) . ?
C16 H16 0.90(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
F1 C1 F2 107.24(16) . . ?
F1 C1 C2 108.97(15) . . ?
F2 C1 C2 107.83(16) . . ?
F1 C1 I2 109.83(13) . . ?
F2 C1 I2 110.94(12) . . ?
C2 C1 I2 111.90(12) . . ?
F3 C2 F4 108.29(14) . . ?
F3 C2 C3 107.97(15) . . ?
F4 C2 C3 109.08(14) . . ?
F3 C2 C1 108.08(15) . . ?
F4 C2 C1 107.30(15) . . ?
C3 C2 C1 115.92(15) . . ?
F6 C3 F5 108.00(14) . . ?
F6 C3 C4 108.95(15) . . ?
F5 C3 C4 107.55(15) . . ?
F6 C3 C2 107.84(15) . . ?
F5 C3 C2 108.79(14) . . ?
C4 C3 C2 115.49(14) . . ?
F8 C4 F7 106.87(14) . . ?
F8 C4 C3 108.20(14) . . ?
F7 C4 C3 108.28(15) . . ?
F8 C4 I1 108.83(12) . . ?
F7 C4 I1 110.13(12) . . ?
C3 C4 I1 114.26(12) . . ?
C6 O1A N2A 104.49(14) . . ?
C5 N2A O1A 104.60(14) . . ?
C6 N1 C5 102.09(15) . . ?
C10 N3 C9 117.65(18) . . ?
C15 N4 C14 117.56(17) . . ?
N2A C5 N1 114.40(16) . . ?
N2A C5 C7 120.08(16) . . ?
N1 C5 C7 125.49(17) . . ?
O1A C6 N1 114.42(16) . . ?
O1A C6 C12 119.51(16) . . ?
N1 C6 C12 126.05(17) . . ?
C11 C7 C8 118.45(18) . . ?
C11 C7 C5 119.81(16) . . ?
C8 C7 C5 121.73(17) . . ?
C9 C8 C7 118.50(19) . . ?
C9 C8 H8 121.4(15) . . ?
C7 C8 H8 119.8(15) . . ?
N3 C9 C8 123.45(18) . . ?
N3 C9 H9 115.9(16) . . ?
C8 C9 H9 120.7(16) . . ?
N3 C10 C11 123.09(19) . . ?
N3 C10 H10 115.4(17) . . ?
C11 C10 H10 121.5(17) . . ?
C10 C11 C7 118.85(17) . . ?
C10 C11 H11 122.1(17) . . ?
C7 C11 H11 119.1(17) . . ?
C13 C12 C16 118.84(18) . . ?
C13 C12 C6 120.71(17) . . ?
C16 C12 C6 120.45(17) . . ?
C14 C13 C12 118.40(17) . . ?
C14 C13 H13 120.8(13) . . ?
C12 C13 H13 120.8(13) . . ?
N4 C14 C13 123.31(18) . . ?
N4 C14 H14 115.6(15) . . ?
C13 C14 H14 120.9(16) . . ?
N4 C15 C16 123.63(19) . . ?
N4 C15 H15 115.2(16) . . ?
C16 C15 H15 121.1(16) . . ?
C15 C16 C12 118.25(19) . . ?
C15 C16 H16 119.9(16) . . ?
C12 C16 H16 121.8(16) . . ?
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
F1 C1 C2 F3 -175.09(15) . . . . ?
F2 C1 C2 F3 68.83(19) . . . . ?
I2 C1 C2 F3 -53.44(17) . . . . ?
F1 C1 C2 F4 -58.51(19) . . . . ?
F2 C1 C2 F4 -174.60(15) . . . . ?
I2 C1 C2 F4 63.13(16) . . . . ?
F1 C1 C2 C3 63.6(2) . . . . ?
F2 C1 C2 C3 -52.5(2) . . . . ?
I2 C1 C2 C3 -174.73(12) . . . . ?
F3 C2 C3 F6 -51.95(19) . . . . ?
F4 C2 C3 F6 -169.41(13) . . . . ?
C1 C2 C3 F6 69.41(19) . . . . ?
F3 C2 C3 F5 -168.85(14) . . . . ?
F4 C2 C3 F5 73.69(18) . . . . ?
C1 C2 C3 F5 -47.5(2) . . . . ?
F3 C2 C3 C4 70.15(19) . . . . ?
F4 C2 C3 C4 -47.3(2) . . . . ?
C1 C2 C3 C4 -168.50(15) . . . . ?
F6 C3 C4 F8 -172.92(14) . . . . ?
F5 C3 C4 F8 -56.09(18) . . . . ?
C2 C3 C4 F8 65.58(19) . . . . ?
F6 C3 C4 F7 71.59(18) . . . . ?
F5 C3 C4 F7 -171.58(14) . . . . ?
C2 C3 C4 F7 -49.9(2) . . . . ?
F6 C3 C4 I1 -51.52(17) . . . . ?
F5 C3 C4 I1 65.31(16) . . . . ?
C2 C3 C4 I1 -173.02(12) . . . . ?
C6 O1A N2A C5 0.35(19) . . . . ?
O1A N2A C5 N1 -0.7(2) . . . . ?
O1A N2A C5 C7 177.35(16) . . . . ?
C6 N1 C5 N2A 0.7(2) . . . . ?
C6 N1 C5 C7 -177.20(18) . . . . ?
N2A O1A C6 N1 0.1(2) . . . . ?
N2A O1A C6 C12 -178.82(16) . . . . ?
C5 N1 C6 O1A -0.5(2) . . . . ?
C5 N1 C6 C12 178.35(17) . . . . ?
N2A C5 C7 C11 -178.74(18) . . . . ?
N1 C5 C7 C11 -0.9(3) . . . . ?
N2A C5 C7 C8 0.5(3) . . . . ?
N1 C5 C7 C8 178.34(19) . . . . ?
C11 C7 C8 C9 -0.3(3) . . . . ?
C5 C7 C8 C9 -179.60(19) . . . . ?
C10 N3 C9 C8 -0.7(3) . . . . ?
C7 C8 C9 N3 0.9(3) . . . . ?
C9 N3 C10 C11 -0.1(3) . . . . ?
N3 C10 C11 C7 0.6(3) . . . . ?
C8 C7 C11 C10 -0.4(3) . . . . ?
C5 C7 C11 C10 178.92(18) . . . . ?
O1A C6 C12 C13 -171.74(18) . . . . ?
N1 C6 C12 C13 9.5(3) . . . . ?
O1A C6 C12 C16 9.3(3) . . . . ?
N1 C6 C12 C16 -169.49(19) . . . . ?
C16 C12 C13 C14 -0.7(3) . . . . ?
C6 C12 C13 C14 -179.68(17) . . . . ?
C15 N4 C14 C13 0.7(3) . . . . ?
C12 C13 C14 N4 0.0(3) . . . . ?
C14 N4 C15 C16 -0.8(3) . . . . ?
N4 C15 C16 C12 0.1(3) . . . . ?
C13 C12 C16 C15 0.6(3) . . . . ?
C6 C12 C16 C15 179.60(18) . . . . ?
_diffrn_measured_fraction_theta_max 0.892
_diffrn_reflns_theta_full        31.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.106


data_ms051lt
_database_code_depnum_ccdc_archive 'CCDC 915397'
#TrackingRef 'ms051lt.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H8 N4 O, C6 F12 I2 '
_chemical_formula_sum            'C18 H8 F12 I2 N4 O'
_chemical_formula_weight         778.08
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   13.1606(12)
_cell_length_b                   5.5451(6)
_cell_length_c                   31.302(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.877(10)
_cell_angle_gamma                90.00
_cell_volume                     2283.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    2488
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      31.71
_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    2.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_absorpt_correction_T_min  0.4482
_exptl_absorpt_correction_T_max  0.7470
_exptl_special_details           
;
Bruker KRYOFLEX low temperature device.
;
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            139794
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         35.61
_reflns_number_total             9494
_reflns_number_gt                8615
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    
;
SIR2002 (Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L.,
Giacovazzo, C., Polidori, G. & Spagna, R. (2003).
J. Appl. Cryst. 36, 1103.)
;
_computing_structure_refinement  
'SHELXL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, L.J. (1997) Jour. Appl. Cryst. 30, 565)
Mercury (Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E.,
Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006).
J. Appl. Cryst. 39, 453-457
;
_computing_publication_material  SHELXTL
_iucr_refine_instructions_details 
;
TITL ms051 -170 C, in P2(1)/n
CELL 0.71073 13.1606 5.5451 31.302 90.000 91.877 90.000
ZERR 4.00 0.0012 0.0006 0.003 0.000 0.010 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N O F I
UNIT 72 32 16 4 48 8
L.S. 10
ACTA
BOND
FMAP 2
PLAN 20
SIZE 0.10 0.35 0.42
TEMP -170.000
WGHT 0.028800 4.459600
FVAR 0.18184
MOLE 1
simu 0.005 F1A F1B F2A F2B
simu 0.005 F3A F3B F4A F4B
simu 0.005 F5A F5B F6A F6B
simu 0.005 F7A F7B F8A F8B
simu 0.005 F9A F9B F10A F10B
ISOR 0.01 F1A F1B F2A F2B
ISOR 0.01 F3A F3B F4A F4B
ISOR 0.01 F5A F5B F6A F6B
ISOR 0.01 F7A F7B F8A F8B
simu 0.01 F9A F9B F10A F10B
simu 0.01 F11A F11B F12A F12B
SADI 0.005 I1 C13A I1 C13B
eadp C13A C13B
eadp C14A C14B
eadp C15A C15B
eadp C16A C16B
eadp C17A C17B
eadp C18A C18B
dfix 1.35 0.005 C13A F1A C13A F2A C14A F3A C14A F4A C15A F5A C15A F6A =
C16A F7A C16A F8A C17A F9A C17A F10A C18A F11A C18A F12A =
C13B F1B C13B F2B C14B F3B C14B F4B C15B F5B C15B F6B =
C16B F7B C16B F8B C17B F9B C17B F10B C18B F11B C18B F12B
sadi 0.005 C13A C14A C14A C15A C15A C16A C16A C17A C17A C18A =
C13B C14B C14B C15B C15B C16B C16B C17B C17B C18B
dfix 2.12 0.02 F1A F2A F3A F4A F5A F6A F7A F8A F9A F10A F11A F12A =
F1B F2B F3B F4B F5B F6B F7B F8B F9B F10B F11B F12B
I1 6 -0.195892 0.111925 0.161054 11.00000 0.01375 0.02215 =
0.01601 0.00338 0.00520 -0.00005
I2 6 0.386079 0.293604 -0.044044 11.00000 0.01601 0.02241 =
0.01879 0.00416 0.00798 0.00191
part 1
F1A 5 -0.150163 0.405145 0.086793 10.50000 0.02426 0.03242 =
0.02115 0.01257 0.00703 0.01387
F2A 5 -0.049010 0.490028 0.140735 10.50000 0.02770 0.01631 =
0.02353 -0.00395 0.01106 -0.00590
F3A 5 0.038760 0.033812 0.133810 10.50000 0.01741 0.01593 =
0.01637 0.00709 0.00182 0.00069
F4A 5 -0.060721 -0.034191 0.077721 10.50000 0.01792 0.02071 =
0.01855 -0.00301 0.00173 -0.00631
F5A 5 0.010476 0.388041 0.040556 10.50000 0.01963 0.01478 =
0.01599 0.00586 0.00180 0.00503
F6A 5 0.111266 0.433585 0.097123 10.50000 0.01934 0.02132 =
0.01351 -0.00358 0.00299 -0.00686
F7A 5 0.209804 0.041806 0.087034 10.50000 0.02113 0.02856 =
0.01257 0.00931 0.00033 0.00841
F8A 5 0.108246 -0.085135 0.035547 10.50000 0.02513 0.01671 =
0.02547 -0.00553 0.01096 -0.00575
F9A 5 0.156381 0.334526 -0.012574 10.50000 0.02085 0.03099 =
0.02132 0.01708 0.00687 0.00776
F10A 5 0.257852 0.418810 0.041197 10.50000 0.03893 0.04256 =
0.02834 -0.01465 0.01812 -0.02877
F11A 5 0.298105 -0.108170 0.000920 10.50000 0.02767 0.01318 =
0.03529 0.00079 0.01543 0.00124
F12A 5 0.376970 0.137152 0.044818 10.50000 0.01388 0.03560 =
0.01579 0.01115 0.00094 0.00446
C13A 1 -0.096817 0.309263 0.120024 10.50000 0.02237 0.02125 =
0.01442 0.00396 0.00774 0.00602
C14A 1 -0.015618 0.138585 0.101576 10.50000 0.01123 0.01699 =
0.00921 0.00114 0.00268 -0.00009
C15A 1 0.060005 0.272102 0.072704 10.50000 0.01578 0.01350 =
0.01134 0.00181 0.00452 0.00136
C16A 1 0.146146 0.113400 0.054764 10.50000 0.01680 0.01484 =
0.00539 0.00073 0.00446 0.00110
C17A 1 0.210406 0.237450 0.020180 10.50000 0.01290 0.01542 =
0.01130 0.00307 0.00245 -0.00042
C18A 1 0.315292 0.127236 0.009969 10.50000 0.01807 0.02028 =
0.01811 0.00417 0.00526 0.00467
part 2
F1B 5 -0.167740 0.291301 0.076430 10.50000 0.02179 0.07641 =
0.03443 0.03476 0.00676 0.01755
F2B 5 -0.080771 0.491140 0.124650 10.50000 0.04677 0.01531 =
0.06008 0.00095 0.03281 0.00025
F3B 5 0.041602 0.079491 0.136711 10.50000 0.01852 0.03148 =
0.01259 0.00684 -0.00439 -0.00334
F4B 5 -0.042947 -0.083352 0.083305 10.50000 0.02387 0.02127 =
0.02154 -0.00305 0.00427 -0.00947
F5B 5 0.003453 0.345833 0.037093 10.50000 0.02688 0.02511 =
0.01830 0.01206 0.00779 0.01020
F6B 5 0.103117 0.449489 0.090790 10.50000 0.02826 0.01981 =
0.03241 -0.00431 0.01342 -0.00687
F7B 5 0.198347 -0.002722 0.080773 10.50000 0.02155 0.03182 =
0.01754 0.01079 0.00607 0.00792
F8B 5 0.094878 -0.073740 0.026333 10.50000 0.02261 0.02271 =
0.02192 -0.00752 0.00686 -0.00825
F9B 5 0.155670 0.260602 -0.016041 10.50000 0.01625 0.04264 =
0.01196 0.00916 -0.00203 0.00340
F10B 5 0.233580 0.470040 0.034222 10.50000 0.02693 0.00958 =
0.03055 0.00212 0.01370 0.00056
F11B 5 0.252655 -0.104410 -0.021286 10.50000 0.06043 0.01845 =
0.07940 -0.00818 0.04944 -0.00657
F12B 5 0.358258 -0.002535 0.030416 10.50000 0.03533 0.11156 =
0.05610 0.05869 0.02249 0.04199
C13B 1 -0.106479 0.268984 0.111627 10.50000 0.02237 0.02125 =
0.01442 0.00396 0.00774 0.00602
C14B 1 -0.009714 0.127439 0.099574 10.50000 0.01123 0.01699 =
0.00921 0.00114 0.00268 -0.00009
C15B 1 0.063120 0.260159 0.069350 10.50000 0.01578 0.01350 =
0.01134 0.00181 0.00452 0.00136
C16B 1 0.144603 0.100671 0.048205 10.50000 0.01680 0.01484 =
0.00539 0.00073 0.00446 0.00110
C17B 1 0.216148 0.246783 0.019251 10.50000 0.01290 0.01542 =
0.01130 0.00307 0.00245 -0.00042
C18B 1 0.297665 0.084845 -0.001092 10.50000 0.01807 0.02028 =
0.01811 0.00417 0.00526 0.00467
part 0
mole 2
MOLE 2
EADP O1A N1B
EXYZ O1A N1B
EADP O1B N1A
EXYZ O1B N1A
part 1
O1A 4 0.163030 0.052706 0.229772 10.50000 0.01541 0.01722 =
0.01988 0.00305 0.00688 0.00284
N1A 3 0.251347 0.057515 0.205751 10.50000 0.01574 0.01811 =
0.02048 0.00448 0.00759 0.00306
part 1
O1B 4 0.251347 0.057515 0.205751 10.50000 0.01574 0.01811 =
0.02048 0.00448 0.00759 0.00306
N1B 3 0.163030 0.052706 0.229772 10.50000 0.01541 0.01722 =
0.01988 0.00305 0.00688 0.00284
part 0
N2 3 0.170166 0.411053 0.196618 11.00000 0.01158 0.01436 =
0.01421 -0.00066 0.00284 0.00020
N3 3 -0.158963 0.438082 0.280314 11.00000 0.01600 0.01760 =
0.02460 -0.00200 0.00771 -0.00003
N4 3 0.488208 0.494217 0.107611 11.00000 0.01769 0.02272 =
0.01999 -0.00052 0.00691 -0.00085
C1 1 0.120300 0.267070 0.222867 11.00000 0.01205 0.01621 =
0.01271 -0.00203 0.00101 0.00092
C2 1 0.250427 0.273360 0.187466 11.00000 0.01284 0.01637 =
0.01110 -0.00088 0.00131 -0.00197
C3 1 0.332846 0.345853 0.159893 11.00000 0.01251 0.01382 =
0.01166 -0.00096 0.00143 -0.00062
C4 1 0.419022 0.202828 0.155247 11.00000 0.01607 0.01718 =
0.01702 -0.00026 0.00384 0.00238
AFIX 43
H4 2 0.425875 0.053164 0.169829 11.00000 -1.20000
AFIX 0
C5 1 0.494204 0.283777 0.128952 11.00000 0.01603 0.02273 =
0.02241 -0.00043 0.00402 0.00371
AFIX 43
H5 2 0.552839 0.186275 0.125802 11.00000 -1.20000
AFIX 0
C6 1 0.404703 0.628724 0.112058 11.00000 0.01771 0.01792 =
0.01747 0.00231 0.00411 -0.00159
AFIX 43
H6 2 0.399372 0.776063 0.096660 11.00000 -1.20000
AFIX 0
C7 1 0.325656 0.564393 0.137927 11.00000 0.01506 0.01660 =
0.01601 0.00187 0.00279 -0.00016
AFIX 43
H7 2 0.268184 0.666261 0.140626 11.00000 -1.20000
AFIX 0
C8 1 0.024834 0.326524 0.243376 11.00000 0.01132 0.01330 =
0.01291 -0.00228 0.00187 0.00002
C9 1 -0.017890 0.169669 0.272319 11.00000 0.01503 0.01426 =
0.01895 0.00277 0.00220 0.00016
AFIX 43
H9 2 0.014866 0.022304 0.279851 11.00000 -1.20000
AFIX 0
C10 1 -0.109412 0.232692 0.290004 11.00000 0.01699 0.02053 =
0.02157 0.00407 0.00553 -0.00173
AFIX 43
H10 2 -0.138390 0.125489 0.309907 11.00000 -1.20000
AFIX 0
C11 1 -0.117241 0.587633 0.252501 11.00000 0.01525 0.01684 =
0.02807 -0.00037 0.00637 0.00066
AFIX 43
H11 2 -0.152103 0.732956 0.245407 11.00000 -1.20000
AFIX 0
C12 1 -0.025313 0.541876 0.233336 11.00000 0.01462 0.01542 =
0.02324 0.00142 0.00693 0.00118
AFIX 43
H12 2 0.002509 0.654008 0.213975 11.00000 -1.20000
HKLF 4
END
;
_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.
The disordered -C6F12- group was refined with restrants and constraints
both on geometry and displacement parameters
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+4.4596P] 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    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9494
_refine_ls_number_parameters     460
_refine_ls_number_restraints     262
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.002
_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 -0.195892(10) 0.11193(3) 0.161054(5) 0.01720(4) Uani 1 1 d D . .
I2 I 0.386079(11) 0.29360(3) -0.044044(5) 0.01891(4) Uani 1 1 d . . .
F1A F -0.1502(3) 0.4051(8) 0.08679(13) 0.0258(8) Uani 0.50 1 d PDU A 1
F2A F -0.0490(3) 0.4900(8) 0.14074(12) 0.0223(7) Uani 0.50 1 d PDU A 1
F3A F 0.0388(14) 0.034(2) 0.1338(5) 0.0165(14) Uani 0.50 1 d PDU A 1
F4A F -0.0607(6) -0.0342(14) 0.0777(3) 0.0190(11) Uani 0.50 1 d PDU A 1
F5A F 0.0105(14) 0.388(3) 0.0406(5) 0.0168(14) Uani 0.50 1 d PDU A 1
F6A F 0.1113(15) 0.434(3) 0.0971(4) 0.0180(14) Uani 0.50 1 d PDU A 1
F7A F 0.2098(10) 0.042(2) 0.0870(4) 0.0208(14) Uani 0.50 1 d PDU A 1
F8A F 0.1082(10) -0.085(2) 0.0355(3) 0.0222(14) Uani 0.50 1 d PDU A 1
F9A F 0.1564(8) 0.3345(12) -0.0126(3) 0.0243(15) Uani 0.50 1 d PDU A 1
F10A F 0.2579(5) 0.4188(12) 0.0412(2) 0.0362(15) Uani 0.50 1 d PDU A 1
F11A F 0.2981(3) -0.1082(6) 0.00092(13) 0.0251(7) Uani 0.50 1 d PDU A 1
F12A F 0.3770(2) 0.1372(7) 0.04482(10) 0.0217(7) Uani 0.50 1 d PDU A 1
C13A C -0.0968(4) 0.3093(11) 0.12002(14) 0.0192(10) Uani 0.50 1 d PD A 1
C14A C -0.0156(7) 0.1386(18) 0.1016(4) 0.0124(5) Uani 0.50 1 d PD A 1
C15A C 0.0600(11) 0.272(3) 0.0727(5) 0.0134(8) Uani 0.50 1 d PD A 1
C16A C 0.1461(10) 0.113(2) 0.0548(4) 0.0123(11) Uani 0.50 1 d PD A 1
C17A C 0.2104(6) 0.2375(15) 0.0202(3) 0.0132(5) Uani 0.50 1 d PD A 1
C18A C 0.3153(5) 0.1272(9) 0.00997(18) 0.0187(9) Uani 0.50 1 d PD A 1
F1B F -0.1677(3) 0.2913(11) 0.07643(15) 0.0441(13) Uani 0.50 1 d PDU A 2
F2B F -0.0808(4) 0.4911(8) 0.12465(18) 0.0400(11) Uani 0.50 1 d PDU A 2
F3B F 0.0416(15) 0.079(2) 0.1367(5) 0.021(2) Uani 0.50 1 d PDU A 2
F4B F -0.0429(6) -0.0834(14) 0.0833(3) 0.0221(12) Uani 0.50 1 d PDU A 2
F5B F 0.0035(15) 0.346(3) 0.0371(5) 0.023(2) Uani 0.50 1 d PDU A 2
F6B F 0.1031(16) 0.449(4) 0.0908(5) 0.027(2) Uani 0.50 1 d PDU A 2
F7B F 0.1983(10) -0.003(2) 0.0808(4) 0.0235(15) Uani 0.50 1 d PDU A 2
F8B F 0.0949(10) -0.074(3) 0.0263(3) 0.0223(15) Uani 0.50 1 d PDU A 2
F9B F 0.1557(7) 0.2606(13) -0.0160(3) 0.0237(14) Uani 0.50 1 d PDU A 2
F10B F 0.2336(5) 0.4700(10) 0.0342(2) 0.0221(10) Uani 0.50 1 d PDU A 2
F11B F 0.2527(4) -0.1044(7) -0.02129(18) 0.0517(14) Uani 0.50 1 d PDU A 2
F12B F 0.3583(4) -0.0025(14) 0.03042(17) 0.067(2) Uani 0.50 1 d PDU A 2
C13B C -0.1065(4) 0.2690(11) 0.11163(14) 0.0192(10) Uani 0.50 1 d PD A 2
C14B C -0.0097(7) 0.1274(17) 0.0996(4) 0.0124(5) Uani 0.50 1 d PD A 2
C15B C 0.0631(11) 0.260(3) 0.0694(5) 0.0134(8) Uani 0.50 1 d PD A 2
C16B C 0.1446(10) 0.101(2) 0.0482(4) 0.0123(11) Uani 0.50 1 d PD A 2
C17B C 0.2161(6) 0.2468(14) 0.0193(3) 0.0132(5) Uani 0.50 1 d PD A 2
C18B C 0.2977(5) 0.0848(10) -0.00109(18) 0.0187(9) Uani 0.50 1 d PD A 2
O1A O 0.16303(13) 0.0527(4) 0.22977(6) 0.0174(3) Uani 0.50 1 d P B 1
N1A N 0.25135(13) 0.0575(4) 0.20575(6) 0.0180(3) Uani 0.50 1 d P B 1
O1B O 0.25135(13) 0.0575(4) 0.20575(6) 0.0180(3) Uani 0.50 1 d P B 1
N1B N 0.16303(13) 0.0527(4) 0.22977(6) 0.0174(3) Uani 0.50 1 d P B 1
N2 N 0.17017(13) 0.4111(3) 0.19662(6) 0.0133(3) Uani 1 1 d . B .
N3 N -0.15896(15) 0.4381(4) 0.28031(7) 0.0192(4) Uani 1 1 d . . .
N4 N 0.48821(15) 0.4942(4) 0.10761(7) 0.0200(4) Uani 1 1 d . . .
C1 C 0.12030(15) 0.2671(4) 0.22287(7) 0.0136(3) Uani 1 1 d . . .
C2 C 0.25043(15) 0.2734(4) 0.18747(7) 0.0134(3) Uani 1 1 d . . .
C3 C 0.33285(15) 0.3459(4) 0.15989(7) 0.0126(3) Uani 1 1 d . B .
C4 C 0.41902(17) 0.2028(4) 0.15525(7) 0.0167(4) Uani 1 1 d . . .
H4 H 0.4259 0.0532 0.1698 0.020 Uiso 1 1 calc R B .
C5 C 0.49420(18) 0.2838(5) 0.12895(8) 0.0203(4) Uani 1 1 d . B .
H5 H 0.5528 0.1863 0.1258 0.024 Uiso 1 1 calc R . .
C6 C 0.40470(17) 0.6287(5) 0.11206(8) 0.0176(4) Uani 1 1 d . B .
H6 H 0.3994 0.7761 0.0967 0.021 Uiso 1 1 calc R . .
C7 C 0.32566(16) 0.5644(4) 0.13793(7) 0.0158(4) Uani 1 1 d . . .
H7 H 0.2682 0.6663 0.1406 0.019 Uiso 1 1 calc R B .
C8 C 0.02483(15) 0.3265(4) 0.24338(7) 0.0125(3) Uani 1 1 d . B .
C9 C -0.01789(16) 0.1697(4) 0.27232(7) 0.0160(4) Uani 1 1 d . . .
H9 H 0.0149 0.0223 0.2799 0.019 Uiso 1 1 calc R B .
C10 C -0.10941(18) 0.2327(5) 0.29000(8) 0.0196(4) Uani 1 1 d . B .
H10 H -0.1384 0.1255 0.3099 0.024 Uiso 1 1 calc R . .
C11 C -0.11724(17) 0.5876(5) 0.25250(9) 0.0199(4) Uani 1 1 d . B .
H11 H -0.1521 0.7330 0.2454 0.024 Uiso 1 1 calc R . .
C12 C -0.02531(16) 0.5419(4) 0.23334(8) 0.0176(4) Uani 1 1 d . . .
H12 H 0.0025 0.6540 0.2140 0.021 Uiso 1 1 calc R B .
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 0.01375(6) 0.02215(8) 0.01601(6) 0.00338(5) 0.00520(5) -0.00005(5)
I2 0.01601(6) 0.02241(8) 0.01879(7) 0.00416(5) 0.00798(5) 0.00191(5)
F1A 0.0243(17) 0.032(2) 0.0211(16) 0.0126(15) 0.0070(13) 0.0139(15)
F2A 0.0277(18) 0.0163(15) 0.0235(17) -0.0039(14) 0.0111(13) -0.0059(13)
F3A 0.017(2) 0.016(3) 0.016(3) 0.007(2) 0.0018(18) 0.001(2)
F4A 0.018(2) 0.021(3) 0.019(2) -0.0030(19) 0.0017(16) -0.0063(17)
F5A 0.020(2) 0.015(3) 0.016(2) 0.006(2) 0.0018(15) 0.005(2)
F6A 0.019(2) 0.021(3) 0.014(2) -0.004(2) 0.0030(17) -0.007(2)
F7A 0.021(3) 0.029(4) 0.013(3) 0.009(2) 0.0003(17) 0.008(2)
F8A 0.025(3) 0.0167(19) 0.025(4) -0.006(3) 0.011(3) -0.006(2)
F9A 0.0208(18) 0.031(4) 0.021(3) 0.017(3) 0.0069(16) 0.008(3)
F10A 0.039(3) 0.043(4) 0.028(3) -0.015(3) 0.018(2) -0.029(3)
F11A 0.0277(16) 0.0132(14) 0.0353(19) 0.0008(13) 0.0154(14) 0.0012(12)
F12A 0.0139(12) 0.0356(19) 0.0158(13) 0.0112(13) 0.0009(10) 0.0045(12)
C13A 0.0224(14) 0.021(2) 0.014(2) 0.0040(18) 0.0077(15) 0.0060(13)
C14A 0.0112(11) 0.0170(12) 0.0092(11) 0.0011(8) 0.0027(9) -0.0001(8)
C15A 0.0158(10) 0.0135(14) 0.0113(19) 0.0018(12) 0.0045(11) 0.0014(9)
C16A 0.0168(9) 0.0148(14) 0.005(3) 0.0007(18) 0.0045(16) 0.0011(8)
C17A 0.0129(10) 0.0154(10) 0.0113(8) 0.0031(7) 0.0025(8) -0.0004(8)
C18A 0.018(2) 0.020(2) 0.018(3) 0.0042(17) 0.0053(17) 0.0047(16)
F1B 0.0218(18) 0.076(4) 0.034(2) 0.035(2) 0.0068(16) 0.018(2)
F2B 0.047(3) 0.0153(17) 0.060(3) 0.001(2) 0.033(2) 0.0002(18)
F3B 0.0185(19) 0.031(5) 0.013(2) 0.007(3) -0.0044(16) -0.003(4)
F4B 0.024(3) 0.021(3) 0.022(3) -0.003(2) 0.0043(19) -0.009(2)
F5B 0.027(4) 0.025(5) 0.018(3) 0.012(3) 0.008(2) 0.010(3)
F6B 0.028(4) 0.020(3) 0.032(5) -0.004(4) 0.013(4) -0.007(3)
F7B 0.022(3) 0.032(4) 0.018(3) 0.011(3) 0.006(2) 0.008(3)
F8B 0.023(3) 0.023(2) 0.022(3) -0.008(3) 0.007(2) -0.008(2)
F9B 0.0162(16) 0.043(4) 0.0120(16) 0.009(3) -0.0020(12) 0.003(3)
F10B 0.027(2) 0.0096(16) 0.031(3) 0.0021(14) 0.0137(18) 0.0006(13)
F11B 0.060(3) 0.018(2) 0.079(4) -0.008(2) 0.049(3) -0.0066(19)
F12B 0.035(2) 0.112(5) 0.056(3) 0.059(3) 0.022(2) 0.042(3)
C13B 0.0224(14) 0.021(2) 0.014(2) 0.0040(18) 0.0077(15) 0.0060(13)
C14B 0.0112(11) 0.0170(12) 0.0092(11) 0.0011(8) 0.0027(9) -0.0001(8)
C15B 0.0158(10) 0.0135(14) 0.0113(19) 0.0018(12) 0.0045(11) 0.0014(9)
C16B 0.0168(9) 0.0148(14) 0.005(3) 0.0007(18) 0.0045(16) 0.0011(8)
C17B 0.0129(10) 0.0154(10) 0.0113(8) 0.0031(7) 0.0025(8) -0.0004(8)
C18B 0.018(2) 0.020(2) 0.018(3) 0.0042(17) 0.0053(17) 0.0047(16)
O1A 0.0154(7) 0.0172(8) 0.0199(8) 0.0031(6) 0.0069(6) 0.0028(6)
N1A 0.0157(7) 0.0181(9) 0.0205(8) 0.0045(7) 0.0076(6) 0.0031(6)
O1B 0.0157(7) 0.0181(9) 0.0205(8) 0.0045(7) 0.0076(6) 0.0031(6)
N1B 0.0154(7) 0.0172(8) 0.0199(8) 0.0031(6) 0.0069(6) 0.0028(6)
N2 0.0116(6) 0.0144(8) 0.0142(7) -0.0007(6) 0.0028(6) 0.0002(6)
N3 0.0160(8) 0.0176(9) 0.0246(9) -0.0020(7) 0.0077(7) 0.0000(6)
N4 0.0177(8) 0.0227(10) 0.0200(9) -0.0005(8) 0.0069(7) -0.0009(7)
C1 0.0121(7) 0.0162(9) 0.0127(8) -0.0020(7) 0.0010(6) 0.0009(6)
C2 0.0128(7) 0.0164(9) 0.0111(7) -0.0009(7) 0.0013(6) -0.0020(6)
C3 0.0125(7) 0.0138(9) 0.0117(8) -0.0010(7) 0.0014(6) -0.0006(6)
C4 0.0161(8) 0.0172(10) 0.0170(9) -0.0003(8) 0.0038(7) 0.0024(7)
C5 0.0160(9) 0.0227(12) 0.0224(10) -0.0004(9) 0.0040(8) 0.0037(8)
C6 0.0177(9) 0.0179(10) 0.0175(9) 0.0023(8) 0.0041(7) -0.0016(7)
C7 0.0151(8) 0.0166(10) 0.0160(9) 0.0019(7) 0.0028(7) -0.0002(7)
C8 0.0113(7) 0.0133(9) 0.0129(8) -0.0023(7) 0.0019(6) 0.0000(6)
C9 0.0150(8) 0.0143(9) 0.0190(9) 0.0028(7) 0.0022(7) 0.0002(7)
C10 0.0170(9) 0.0205(11) 0.0216(10) 0.0041(8) 0.0055(8) -0.0017(7)
C11 0.0152(8) 0.0168(10) 0.0281(11) -0.0004(9) 0.0064(8) 0.0007(7)
C12 0.0146(8) 0.0154(10) 0.0232(10) 0.0014(8) 0.0069(7) 0.0012(7)
_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 C13B 2.158(4) . ?
I1 C13A 2.158(4) . ?
I2 C18B 2.146(7) . ?
I2 C18A 2.163(7) . ?
F1A C13A 1.345(4) . ?
F2A C13A 1.339(4) . ?
F3A C14A 1.349(4) . ?
F4A C14A 1.341(4) . ?
F5A C15A 1.345(4) . ?
F6A C15A 1.344(4) . ?
F7A C16A 1.351(4) . ?
F8A C16A 1.343(4) . ?
F9A C17A 1.341(4) . ?
F10A C17A 1.344(4) . ?
F11A C18A 1.353(4) . ?
F12A C18A 1.339(4) . ?
C13A C14A 1.553(3) . ?
C14A C15A 1.554(3) . ?
C15A C16A 1.555(3) . ?
C16A C17A 1.556(3) . ?
C17A C18A 1.552(4) . ?
F1B C13B 1.349(4) . ?
F2B C13B 1.338(4) . ?
F3B C14B 1.352(4) . ?
F4B C14B 1.342(4) . ?
F5B C15B 1.345(4) . ?
F6B C15B 1.344(5) . ?
F7B C16B 1.349(4) . ?
F8B C16B 1.343(4) . ?
F9B C17B 1.342(4) . ?
F10B C17B 1.341(4) . ?
F11B C18B 1.352(4) . ?
F12B C18B 1.339(4) . ?
C13B C14B 1.553(4) . ?
C14B C15B 1.554(3) . ?
C15B C16B 1.555(3) . ?
C16B C17B 1.556(3) . ?
C17B C18B 1.552(3) . ?
O1A C1 1.330(3) . ?
O1A N1A 1.405(2) . ?
N1A C2 1.327(3) . ?
N2 C1 1.334(3) . ?
N2 C2 1.342(3) . ?
N3 C11 1.334(3) . ?
N3 C10 1.342(3) . ?
N4 C6 1.339(3) . ?
N4 C5 1.346(3) . ?
C1 C8 1.467(3) . ?
C2 C3 1.464(3) . ?
C3 C7 1.395(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.383(3) . ?
C6 C7 1.386(3) . ?
C8 C9 1.388(3) . ?
C8 C12 1.395(3) . ?
C9 C10 1.387(3) . ?
C11 C12 1.391(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
C13B I1 C13A 9.7(2) . . ?
C18B I2 C18A 12.59(14) . . ?
F2A C13A F1A 107.7(4) . . ?
F2A C13A C14A 108.5(5) . . ?
F1A C13A C14A 107.5(6) . . ?
F2A C13A I1 112.0(3) . . ?
F1A C13A I1 110.5(3) . . ?
C14A C13A I1 110.4(6) . . ?
F4A C14A F3A 108.8(8) . . ?
F4A C14A C13A 110.2(7) . . ?
F3A C14A C13A 109.8(11) . . ?
F4A C14A C15A 107.3(10) . . ?
F3A C14A C15A 107.8(12) . . ?
C13A C14A C15A 112.8(9) . . ?
F6A C15A F5A 109.2(9) . . ?
F6A C15A C14A 107.8(14) . . ?
F5A C15A C14A 111.0(14) . . ?
F6A C15A C16A 103.0(13) . . ?
F5A C15A C16A 110.0(14) . . ?
C14A C15A C16A 115.4(9) . . ?
F8A C16A F7A 107.8(8) . . ?
F8A C16A C15A 111.2(12) . . ?
F7A C16A C15A 109.8(11) . . ?
F8A C16A C17A 104.7(10) . . ?
F7A C16A C17A 108.2(11) . . ?
C15A C16A C17A 114.9(9) . . ?
F9A C17A F10A 107.5(7) . . ?
F9A C17A C18A 117.0(8) . . ?
F10A C17A C18A 89.6(5) . . ?
F9A C17A C16A 115.0(8) . . ?
F10A C17A C16A 104.2(8) . . ?
C18A C17A C16A 118.5(8) . . ?
F12A C18A F11A 107.6(4) . . ?
F12A C18A C17A 109.6(5) . . ?
F11A C18A C17A 106.2(5) . . ?
F12A C18A I2 110.7(4) . . ?
F11A C18A I2 108.7(4) . . ?
C17A C18A I2 113.7(5) . . ?
F2B C13B F1B 107.6(6) . . ?
F2B C13B C14B 109.8(5) . . ?
F1B C13B C14B 108.7(6) . . ?
F2B C13B I1 107.0(3) . . ?
F1B C13B I1 107.3(3) . . ?
C14B C13B I1 116.2(6) . . ?
F4B C14B F3B 107.6(8) . . ?
F4B C14B C13B 105.8(7) . . ?
F3B C14B C13B 106.3(11) . . ?
F4B C14B C15B 112.4(10) . . ?
F3B C14B C15B 108.4(12) . . ?
C13B C14B C15B 115.8(9) . . ?
F6B C15B F5B 108.0(9) . . ?
F6B C15B C14B 107.8(14) . . ?
F5B C15B C14B 105.5(14) . . ?
F6B C15B C16B 113.1(14) . . ?
F5B C15B C16B 106.0(14) . . ?
C14B C15B C16B 116.0(9) . . ?
F8B C16B F7B 108.3(7) . . ?
F8B C16B C15B 107.2(12) . . ?
F7B C16B C15B 105.8(11) . . ?
F8B C16B C17B 111.9(10) . . ?
F7B C16B C17B 110.4(11) . . ?
C15B C16B C17B 113.0(9) . . ?
F10B C17B F9B 109.0(7) . . ?
F10B C17B C18B 124.4(7) . . ?
F9B C17B C18B 95.4(6) . . ?
F10B C17B C16B 112.2(8) . . ?
F9B C17B C16B 98.9(8) . . ?
C18B C17B C16B 112.2(8) . . ?
F12B C18B F11B 107.8(6) . . ?
F12B C18B C17B 108.1(5) . . ?
F11B C18B C17B 110.1(5) . . ?
F12B C18B I2 109.6(5) . . ?
F11B C18B I2 111.4(4) . . ?
C17B C18B I2 110.0(5) . . ?
C1 O1A N1A 104.41(18) . . ?
C2 N1A O1A 104.60(17) . . ?
C1 N2 C2 101.40(18) . . ?
C11 N3 C10 117.9(2) . . ?
C6 N4 C5 117.8(2) . . ?
O1A C1 N2 114.92(19) . . ?
O1A C1 C8 119.6(2) . . ?
N2 C1 C8 125.5(2) . . ?
N1A C2 N2 114.67(19) . . ?
N1A C2 C3 120.4(2) . . ?
N2 C2 C3 125.0(2) . . ?
C7 C3 C4 119.0(2) . . ?
C7 C3 C2 119.30(19) . . ?
C4 C3 C2 121.7(2) . . ?
C5 C4 C3 118.5(2) . . ?
N4 C5 C4 123.1(2) . . ?
N4 C6 C7 123.5(2) . . ?
C6 C7 C3 118.1(2) . . ?
C9 C8 C12 119.0(2) . . ?
C9 C8 C1 121.1(2) . . ?
C12 C8 C1 120.0(2) . . ?
C10 C9 C8 118.6(2) . . ?
N3 C10 C9 123.1(2) . . ?
N3 C11 C12 123.4(2) . . ?
C11 C12 C8 118.1(2) . . ?
_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.040
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.159