# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013


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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication 
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#  experimental, refinement, atomic coordinates, 
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#  as required by the journal to which it was submitted. 
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data_2011acc0563
_database_code_depnum_ccdc_archive 'CCDC 868429'
#TrackingRef '2011acc0563_revised.cif'



_chemical_compound_source        'Claudia Caltagirone'
_database_code_CSD               11AC0563
_database_code_depnum_ccdc_archive ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H14 N4 O, 3(CH3OH)'
_chemical_formula_sum            'C21 H26 N4 O4'
_chemical_formula_weight         398.46

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'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   32.989(7)
_cell_length_b                   32.989(7)
_cell_length_c                   7.098(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6689(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4013
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      31.3

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3816
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9826
_exptl_absorpt_correction_T_max  0.9982
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;


_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_source_current           24.00
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   RA
_diffrn_radiation_monochromator  'Varimax mirror'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 4 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2613
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2613
_reflns_number_gt                1922
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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^ > 2\s(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.

PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of 101 A**3
Electron density peaks centred around the 3-fold axes could not be
sensible modelled as solvent and the squeeze algorithm was applied
(Sluis, P. v.d. & Spek, A. L. (1990) Acta Cryst. A46, 194-201.) from
within the platon software (Spek, A. L. (1990) Acta Cryst. A46, C34).
From volume and electron count considerations this was assumed to be 3
molecules of MeOH.

;

_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^)+(0.0369P)^2^+8.9656P] 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         2613
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0712
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1314
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_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 0.76249(10) 0.06828(11) 0.3201(4) 0.0224(7) Uani 1 1 d . . .
C2 C 0.73792(11) 0.06763(11) 0.4837(4) 0.0263(7) Uani 1 1 d . . .
H2 H 0.7275 0.0896 0.4971 0.032 Uiso 1 1 calc R . .
C3 C 0.72901(11) 0.03563(11) 0.6232(4) 0.0289(8) Uani 1 1 d . . .
H3 H 0.7124 0.0354 0.7327 0.035 Uiso 1 1 calc R . .
C4 C 0.74442(11) 0.00296(11) 0.6053(4) 0.0300(8) Uani 1 1 d . . .
H4 H 0.7383 -0.0190 0.7031 0.036 Uiso 1 1 calc R . .
C5 C 0.76822(11) 0.00276(11) 0.4472(4) 0.0264(7) Uani 1 1 d . . .
H5 H 0.7786 -0.0193 0.4363 0.032 Uiso 1 1 calc R . .
C6 C 0.77748(10) 0.03522(11) 0.3002(4) 0.0227(7) Uani 1 1 d . . .
C7 C 0.80124(11) 0.03675(11) 0.1316(4) 0.0265(8) Uani 1 1 d . . .
H7 H 0.8119 0.0151 0.1126 0.032 Uiso 1 1 calc R . .
C8 C 0.80883(10) 0.06903(11) -0.0026(4) 0.0248(7) Uani 1 1 d . . .
H8 H 0.8243 0.0699 -0.1166 0.030 Uiso 1 1 calc R . .
C9 C 0.79324(10) 0.10144(10) 0.0300(4) 0.0211(7) Uani 1 1 d . . .
C10 C 0.79298(11) 0.17097(11) -0.1177(4) 0.0237(7) Uani 1 1 d . . .
C11 C 0.75824(10) 0.20925(10) 0.0832(4) 0.0207(7) Uani 1 1 d . . .
C12 C 0.73953(10) 0.20463(11) 0.2623(4) 0.0235(7) Uani 1 1 d . . .
H12 H 0.7346 0.1787 0.3376 0.028 Uiso 1 1 calc R . .
C13 C 0.72769(11) 0.23657(11) 0.3358(4) 0.0280(8) Uani 1 1 d . . .
H13 H 0.7147 0.2318 0.4587 0.034 Uiso 1 1 calc R . .
C14 C 0.73462(11) 0.27480(11) 0.2330(4) 0.0294(8) Uani 1 1 d . . .
H14 H 0.7270 0.2967 0.2844 0.035 Uiso 1 1 calc R . .
C15 C 0.75316(10) 0.28086(10) 0.0509(4) 0.0233(7) Uani 1 1 d . . .
C16 C 0.76560(12) 0.31601(11) -0.0908(4) 0.0302(8) Uani 1 1 d . . .
H16 H 0.7626 0.3431 -0.0817 0.036 Uiso 1 1 calc R . .
C17 C 0.78255(11) 0.30344(11) -0.2409(5) 0.0299(8) Uani 1 1 d . . .
H17 H 0.7935 0.3207 -0.3549 0.036 Uiso 1 1 calc R . .
C18 C 0.76431(10) 0.24760(11) -0.0245(4) 0.0223(7) Uani 1 1 d . . .
N1 N 0.77103(9) 0.10161(9) 0.1840(3) 0.0228(6) Uani 1 1 d . . .
N2 N 0.80290(9) 0.13502(9) -0.1094(3) 0.0248(6) Uani 1 1 d . . .
H2A H 0.8178 0.1329 -0.2084 0.030 Uiso 1 1 calc R . .
N3 N 0.77146(8) 0.17569(9) 0.0346(3) 0.0223(6) Uani 1 1 d . . .
H3A H 0.7642 0.1538 0.1204 0.027 Uiso 1 1 calc R . .
N4 N 0.78140(9) 0.26217(9) -0.2026(3) 0.0250(6) Uani 1 1 d . . .
H4A H 0.7903 0.2473 -0.2804 0.030 Uiso 1 1 calc R . .
O1 O 0.80414(8) 0.19558(8) -0.2619(3) 0.0308(6) Uani 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
C1 0.0184(16) 0.0221(17) 0.0212(16) 0.0006(14) -0.0034(13) 0.0059(14)
C2 0.0281(18) 0.0236(18) 0.0257(17) -0.0009(14) 0.0024(14) 0.0119(15)
C3 0.0305(19) 0.0310(19) 0.0228(17) -0.0012(15) 0.0028(15) 0.0136(16)
C4 0.034(2) 0.0254(18) 0.0273(18) 0.0028(15) -0.0034(15) 0.0129(16)
C5 0.0261(18) 0.0212(17) 0.0331(18) -0.0036(14) -0.0053(15) 0.0126(15)
C6 0.0228(17) 0.0229(17) 0.0237(17) -0.0027(14) -0.0032(14) 0.0123(14)
C7 0.0244(18) 0.0213(17) 0.0332(19) -0.0051(15) -0.0022(14) 0.0109(15)
C8 0.0193(16) 0.0279(18) 0.0253(16) -0.0046(14) -0.0007(14) 0.0103(15)
C9 0.0170(16) 0.0226(17) 0.0215(16) -0.0020(14) -0.0019(13) 0.0083(14)
C10 0.0237(17) 0.0269(18) 0.0195(16) -0.0012(14) 0.0011(14) 0.0118(15)
C11 0.0178(16) 0.0209(16) 0.0214(16) -0.0034(13) -0.0013(13) 0.0083(14)
C12 0.0222(17) 0.0253(17) 0.0196(16) 0.0021(14) 0.0023(13) 0.0093(14)
C13 0.0284(18) 0.0280(18) 0.0227(16) -0.0039(14) 0.0058(15) 0.0105(15)
C14 0.0325(19) 0.0256(18) 0.0321(19) -0.0058(15) 0.0034(16) 0.0161(16)
C15 0.0198(16) 0.0200(16) 0.0258(17) -0.0029(14) -0.0026(14) 0.0068(14)
C16 0.037(2) 0.0214(17) 0.0334(19) -0.0032(15) -0.0042(16) 0.0150(16)
C17 0.0320(19) 0.0232(18) 0.0296(18) 0.0024(15) -0.0040(15) 0.0100(16)
C18 0.0181(16) 0.0257(17) 0.0196(16) -0.0031(14) -0.0006(13) 0.0084(14)
N1 0.0231(14) 0.0236(15) 0.0228(14) -0.0007(11) 0.0004(11) 0.0125(12)
N2 0.0288(15) 0.0261(15) 0.0231(14) 0.0016(12) 0.0063(12) 0.0165(13)
N3 0.0246(14) 0.0222(14) 0.0200(13) 0.0037(11) 0.0052(11) 0.0115(12)
N4 0.0317(16) 0.0234(15) 0.0195(14) 0.0009(11) 0.0032(12) 0.0134(13)
O1 0.0396(14) 0.0319(13) 0.0249(12) 0.0086(11) 0.0118(11) 0.0209(12)

_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
C1 N1 1.383(4) . ?
C1 C2 1.410(4) . ?
C1 C6 1.412(4) . ?
C2 C3 1.368(4) . ?
C3 C4 1.409(4) . ?
C4 C5 1.371(4) . ?
C5 C6 1.415(4) . ?
C6 C7 1.418(4) . ?
C7 C8 1.355(4) . ?
C8 C9 1.418(4) . ?
C9 N1 1.317(4) . ?
C9 N2 1.398(4) . ?
C10 O1 1.243(3) . ?
C10 N3 1.344(4) . ?
C10 N2 1.380(4) . ?
C11 C12 1.387(4) . ?
C11 C18 1.404(4) . ?
C11 N3 1.421(4) . ?
C12 C13 1.395(4) . ?
C13 C14 1.374(4) . ?
C14 C15 1.401(4) . ?
C15 C18 1.425(4) . ?
C15 C16 1.431(4) . ?
C16 C17 1.361(4) . ?
C17 N4 1.370(4) . ?
C18 N4 1.370(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 118.3(3) . . ?
N1 C1 C6 122.2(3) . . ?
C2 C1 C6 119.4(3) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 120.3(3) . . ?
C5 C4 C3 120.3(3) . . ?
C4 C5 C6 120.5(3) . . ?
C1 C6 C5 119.0(3) . . ?
C1 C6 C7 117.3(3) . . ?
C5 C6 C7 123.8(3) . . ?
C8 C7 C6 120.2(3) . . ?
C7 C8 C9 118.9(3) . . ?
N1 C9 N2 119.4(3) . . ?
N1 C9 C8 123.4(3) . . ?
N2 C9 C8 117.2(3) . . ?
O1 C10 N3 126.0(3) . . ?
O1 C10 N2 118.5(3) . . ?
N3 C10 N2 115.5(3) . . ?
C12 C11 C18 116.9(3) . . ?
C12 C11 N3 115.5(3) . . ?
C18 C11 N3 127.5(3) . . ?
C11 C12 C13 122.5(3) . . ?
C14 C13 C12 120.9(3) . . ?
C13 C14 C15 118.8(3) . . ?
C14 C15 C18 119.9(3) . . ?
C14 C15 C16 133.8(3) . . ?
C18 C15 C16 106.3(3) . . ?
C17 C16 C15 107.4(3) . . ?
C16 C17 N4 109.6(3) . . ?
N4 C18 C11 131.8(3) . . ?
N4 C18 C15 107.2(3) . . ?
C11 C18 C15 120.9(3) . . ?
C9 N1 C1 118.0(3) . . ?
C10 N2 C9 130.8(3) . . ?
C10 N3 C11 132.2(3) . . ?
C18 N4 C17 109.5(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O1 0.88 1.98 2.845(3) 168.5 13_654
N3 H3A N1 0.88 1.90 2.657(3) 143.0 .
N4 H4A O1 0.88 1.98 2.686(3) 136.3 .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.052


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.002 101 16 ' '
2 0.333 0.667 1.003 101 16 ' '
3 0.667 0.333 0.670 101 16 ' '
_platon_squeeze_details          
;
>From consideration of the synthesis and crystallisation conditions the
most likely solvent molecule is methanol which has an electron count of
18; squeeze suggests an electron count of 47 per cell which would give
2.6 molecules of methanol. As the voids exist as channels, without any
obvious strong interaction possibilities, it is probable that the solvent
is disordered along these channels and maybe partially occupied.
Alternatively, there may be an integral number of molecules but with the
disorder giving a rather diffuse electron density distribution leading to
a low estimated electron count. The accessible volume of 304.4A3 could
accommodate up to ca. 6 molecules (assuming a molecular volume for
methanol of ca. 50A3).

For the refinement details 3 molecules of methanol have been included in
the CIF
;


_iucr_refine_instructions_details 
;
TITL 2011acc0563 in R-3
CELL 0.71073 32.9888 32.9888 7.0975 90.000 90.000 120.000
ZERR 18 0.0065 0.0065 0.0020 0.000 0.000 0.000
LATT 3
SYMM - Y, X - Y, Z
SYMM - X + Y, - X, Z
SFAC C H N O
UNIT 324 252 72 18
MERG 2
SHEL 7 0.84
HTAB
SIZE 0.2 0.03 0.02
HTAB N2 O1_$1
EQIV $1 [ -x+5/3, -y+1/3, -z-2/3 ]
HTAB N3 N1
HTAB N4 O1
FMAP 2
PLAN 20
ACTA 55.00
BOND
L.S. 4
TEMP -173.00
WGHT 0.036900 8.965600
FVAR 1.00753
C1 1 0.762489 0.068281 0.320129 11.00000 0.01836 0.02208 =
0.02125 0.00065 -0.00345 0.00593
C2 1 0.737920 0.067633 0.483658 11.00000 0.02810 0.02358 =
0.02572 -0.00092 0.00240 0.01186
AFIX 43
H2 2 0.727467 0.089592 0.497067 11.00000 -1.20000
AFIX 0
C3 1 0.729011 0.035633 0.623190 11.00000 0.03054 0.03095 =
0.02282 -0.00119 0.00275 0.01358
AFIX 43
H3 2 0.712353 0.035444 0.732680 11.00000 -1.20000
AFIX 0
C4 1 0.744421 0.002959 0.605295 11.00000 0.03449 0.02535 =
0.02732 0.00277 -0.00343 0.01293
AFIX 43
H4 2 0.738305 -0.019022 0.703139 11.00000 -1.20000
AFIX 0
C5 1 0.768217 0.002755 0.447185 11.00000 0.02607 0.02118 =
0.03305 -0.00355 -0.00530 0.01259
AFIX 43
H5 2 0.778558 -0.019344 0.436287 11.00000 -1.20000
AFIX 0
C6 1 0.777475 0.035222 0.300188 11.00000 0.02279 0.02286 =
0.02370 -0.00273 -0.00316 0.01230
C7 1 0.801241 0.036751 0.131601 11.00000 0.02442 0.02127 =
0.03316 -0.00508 -0.00221 0.01094
AFIX 43
H7 2 0.811880 0.015094 0.112628 11.00000 -1.20000
AFIX 0
C8 1 0.808829 0.069027 -0.002603 11.00000 0.01931 0.02792 =
0.02529 -0.00459 -0.00065 0.01035
AFIX 43
H8 2 0.824332 0.069923 -0.116646 11.00000 -1.20000
AFIX 0
C9 1 0.793239 0.101440 0.030048 11.00000 0.01701 0.02259 =
0.02148 -0.00197 -0.00186 0.00833
C10 1 0.792982 0.170967 -0.117678 11.00000 0.02367 0.02686 =
0.01948 -0.00116 0.00113 0.01181
C11 1 0.758243 0.209253 0.083245 11.00000 0.01779 0.02092 =
0.02143 -0.00339 -0.00126 0.00830
C12 1 0.739530 0.204628 0.262279 11.00000 0.02223 0.02527 =
0.01957 0.00206 0.00227 0.00929
AFIX 43
H12 2 0.734591 0.178744 0.337619 11.00000 -1.20000
AFIX 0
C13 1 0.727692 0.236570 0.335819 11.00000 0.02843 0.02802 =
0.02269 -0.00386 0.00580 0.01046
AFIX 43
H13 2 0.714663 0.231816 0.458695 11.00000 -1.20000
AFIX 0
C14 1 0.734617 0.274798 0.232989 11.00000 0.03246 0.02564 =
0.03208 -0.00578 0.00341 0.01610
AFIX 43
H14 2 0.726970 0.296722 0.284437 11.00000 -1.20000
AFIX 0
C15 1 0.753159 0.280864 0.050899 11.00000 0.01980 0.01995 =
0.02583 -0.00292 -0.00255 0.00676
C16 1 0.765596 0.316010 -0.090755 11.00000 0.03650 0.02139 =
0.03344 -0.00316 -0.00417 0.01497
AFIX 43
H16 2 0.762576 0.343112 -0.081667 11.00000 -1.20000
AFIX 0
C17 1 0.782546 0.303442 -0.240878 11.00000 0.03203 0.02321 =
0.02957 0.00239 -0.00403 0.01004
AFIX 43
H17 2 0.793505 0.320658 -0.354870 11.00000 -1.20000
AFIX 0
C18 1 0.764311 0.247599 -0.024457 11.00000 0.01806 0.02571 =
0.01956 -0.00309 -0.00061 0.00836
N1 3 0.771028 0.101608 0.184035 11.00000 0.02311 0.02356 =
0.02281 -0.00071 0.00043 0.01255
N2 3 0.802897 0.135017 -0.109400 11.00000 0.02883 0.02614 =
0.02307 0.00158 0.00635 0.01651
AFIX 43
H2A 2 0.817778 0.132869 -0.208387 11.00000 -1.20000
AFIX 0
N3 3 0.771460 0.175686 0.034600 11.00000 0.02456 0.02221 =
0.01997 0.00371 0.00515 0.01150
AFIX 43
H3A 2 0.764180 0.153850 0.120398 11.00000 -1.20000
AFIX 0
N4 3 0.781397 0.262175 -0.202573 11.00000 0.03167 0.02343 =
0.01947 0.00092 0.00323 0.01339
AFIX 43
H4A 2 0.790270 0.247322 -0.280413 11.00000 -1.20000
AFIX 0
O1 4 0.804139 0.195584 -0.261910 11.00000 0.03955 0.03194 =
0.02489 0.00865 0.01178 0.02091
HKLF 4

REM 2011acc0563 in R-3
REM R1 = 0.0712 for 1922 Fo > 4sig(Fo) and 0.0990 for all 2613 data
REM 208 parameters refined using 0 restraints

END

WGHT 0.0369 8.9582
REM Highest difference peak 0.256, deepest hole -0.227, 1-sigma level 0.052
Q1 1 0.6667 0.3333 0.0136 10.33333 0.05 0.26
Q2 1 0.6788 0.3244 0.4403 11.00000 0.05 0.21
Q3 1 0.6958 0.3469 -0.0773 11.00000 0.05 0.21
Q4 1 0.8119 0.1252 0.1798 11.00000 0.05 0.21
Q5 1 0.6703 0.3125 0.0270 11.00000 0.05 0.20
Q6 1 0.8306 0.0182 0.1202 11.00000 0.05 0.19
Q7 1 0.7372 0.1521 -0.1206 11.00000 0.05 0.19
Q8 1 0.8414 0.2156 -0.2794 11.00000 0.05 0.18
Q9 1 0.7561 0.0014 0.3298 11.00000 0.05 0.17
Q10 1 0.7520 0.1247 0.5252 11.00000 0.05 0.17
Q11 1 0.7661 0.1175 0.6729 11.00000 0.05 0.17
Q12 1 0.7718 0.2154 -0.2459 11.00000 0.05 0.17
Q13 1 0.7323 0.2355 0.5289 11.00000 0.05 0.16
Q14 1 0.7894 0.0659 0.3545 11.00000 0.05 0.16
Q15 1 0.8146 0.1315 -0.0125 11.00000 0.05 0.16
Q16 1 0.7411 0.2524 -0.0205 11.00000 0.05 0.16
Q17 1 0.8392 0.3153 -0.2492 11.00000 0.05 0.16
Q18 1 0.7624 0.1217 0.2109 11.00000 0.05 0.16
Q19 1 0.7017 0.1936 0.5994 11.00000 0.05 0.16
Q20 1 0.7773 -0.0085 0.2837 11.00000 0.05 0.16
;


data_2012acc0044
_database_code_depnum_ccdc_archive 'CCDC 887900'
#TrackingRef '2012acc0044.cif'

#MAR87_1AcO

_audit_creation_method           SHELXL-97

_chemical_compound_source        'Claudia Caltagirone'
_database_code_CSD               12AC0044
_database_code_depnum_ccdc_archive ?


_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 N4 O'
_chemical_formula_weight         302.33

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   22.003(4)
_cell_length_b                   7.1308(14)
_cell_length_c                   18.677(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2930.5(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5819
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Slab
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9806
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the
Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12023
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_sigmaI/netI    0.1068
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.03
_reflns_number_total             2677
_reflns_number_gt                2083
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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^ > 2\s(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^)+(0.0321P)^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         2677
_refine_ls_number_parameters     415
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1085
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
O101 O 0.39047(17) -0.0630(5) 0.13447(17) 0.0311(9) Uani 1 1 d . . .
N101 N 0.26439(18) -0.4639(6) 0.0654(2) 0.0226(10) Uani 1 1 d . . .
N102 N 0.31649(19) -0.1748(6) 0.0620(2) 0.0254(11) Uani 1 1 d . . .
H102 H 0.3198 -0.0673 0.0391 0.030 Uiso 1 1 calc R . .
N103 N 0.34901(19) -0.3559(5) 0.1578(2) 0.0235(10) Uani 1 1 d . . .
H103 H 0.3193 -0.4288 0.1430 0.028 Uiso 1 1 calc R . .
N104 N 0.4476(2) -0.1565(7) 0.2565(2) 0.0323(12) Uani 1 1 d . . .
H104 H 0.4362 -0.0708 0.2254 0.039 Uiso 1 1 calc R . .
C101 C 0.2221(2) -0.5848(7) 0.0353(3) 0.0245(12) Uani 1 1 d . . .
C102 C 0.2118(2) -0.7574(7) 0.0705(3) 0.0262(13) Uani 1 1 d . . .
H10A H 0.2337 -0.7874 0.1128 0.031 Uiso 1 1 calc R . .
C103 C 0.1699(2) -0.8817(8) 0.0435(3) 0.0317(14) Uani 1 1 d . . .
H10B H 0.1625 -0.9965 0.0679 0.038 Uiso 1 1 calc R . .
C104 C 0.1377(3) -0.8405(9) -0.0201(3) 0.0360(15) Uani 1 1 d . . .
H10C H 0.1091 -0.9277 -0.0388 0.043 Uiso 1 1 calc R . .
C105 C 0.1479(3) -0.6743(9) -0.0547(3) 0.0345(15) Uani 1 1 d . . .
H105 H 0.1267 -0.6482 -0.0979 0.041 Uiso 1 1 calc R . .
C106 C 0.1894(2) -0.5404(8) -0.0275(2) 0.0261(13) Uani 1 1 d . . .
C107 C 0.2005(2) -0.3612(8) -0.0586(3) 0.0297(14) Uani 1 1 d . . .
H107 H 0.1791 -0.3255 -0.1007 0.036 Uiso 1 1 calc R . .
C108 C 0.2410(2) -0.2408(8) -0.0290(3) 0.0274(13) Uani 1 1 d . . .
H108 H 0.2479 -0.1206 -0.0493 0.033 Uiso 1 1 calc R . .
C109 C 0.2730(2) -0.2998(7) 0.0336(3) 0.0245(13) Uani 1 1 d . . .
C110 C 0.3548(2) -0.1957(8) 0.1204(3) 0.0249(13) Uani 1 1 d . . .
C111 C 0.3820(2) -0.4292(7) 0.2170(3) 0.0234(12) Uani 1 1 d . . .
C112 C 0.3691(2) -0.6155(8) 0.2358(3) 0.0324(14) Uani 1 1 d . . .
H112 H 0.3394 -0.6826 0.2091 0.039 Uiso 1 1 calc R . .
C113 C 0.3988(3) -0.7060(8) 0.2930(3) 0.0324(14) Uani 1 1 d . . .
H113 H 0.3893 -0.8332 0.3033 0.039 Uiso 1 1 calc R . .
C114 C 0.4412(3) -0.6140(9) 0.3343(3) 0.0361(16) Uani 1 1 d . . .
H114 H 0.4605 -0.6762 0.3731 0.043 Uiso 1 1 calc R . .
C115 C 0.4554(2) -0.4287(8) 0.3183(3) 0.0273(13) Uani 1 1 d . . .
C116 C 0.4960(3) -0.2929(8) 0.3488(3) 0.0353(15) Uani 1 1 d . . .
H116 H 0.5220 -0.3121 0.3887 0.042 Uiso 1 1 calc R . .
C117 C 0.4904(3) -0.1306(9) 0.3100(3) 0.0399(16) Uani 1 1 d . . .
H117 H 0.5125 -0.0182 0.3184 0.048 Uiso 1 1 calc R . .
C118 C 0.4258(2) -0.3371(7) 0.2596(3) 0.0253(13) Uani 1 1 d . . .
O201 O 0.34548(15) 0.1737(5) -0.02097(18) 0.0267(9) Uani 1 1 d . . .
N201 N 0.47753(18) 0.5431(6) 0.0585(2) 0.0233(10) Uani 1 1 d . . .
N202 N 0.41969(19) 0.2657(6) 0.0550(2) 0.0265(11) Uani 1 1 d . . .
H202 H 0.4133 0.1582 0.0769 0.032 Uiso 1 1 calc R . .
N203 N 0.39091(19) 0.4624(6) -0.03772(19) 0.0244(11) Uani 1 1 d . . .
H203 H 0.4194 0.5326 -0.0183 0.029 Uiso 1 1 calc R . .
N204 N 0.2936(2) 0.2883(6) -0.1446(2) 0.0275(11) Uani 1 1 d . . .
H204 H 0.3029 0.1969 -0.1149 0.033 Uiso 1 1 calc R . .
C201 C 0.5227(2) 0.6491(7) 0.0919(3) 0.0238(12) Uani 1 1 d . . .
C202 C 0.5360(2) 0.8267(8) 0.0622(3) 0.0298(14) Uani 1 1 d . . .
H20A H 0.5147 0.8699 0.0212 0.036 Uiso 1 1 calc R . .
C203 C 0.5806(2) 0.9370(8) 0.0934(3) 0.0267(13) Uani 1 1 d . . .
H20B H 0.5894 1.0568 0.0737 0.032 Uiso 1 1 calc R . .
C204 C 0.6135(2) 0.8730(8) 0.1547(3) 0.0315(14) Uani 1 1 d . . .
H20C H 0.6446 0.9487 0.1749 0.038 Uiso 1 1 calc R . .
C205 C 0.5998(2) 0.7010(8) 0.1842(3) 0.0315(14) Uani 1 1 d . . .
H205 H 0.6210 0.6594 0.2256 0.038 Uiso 1 1 calc R . .
C206 C 0.5540(2) 0.5849(8) 0.1533(2) 0.0243(12) Uani 1 1 d . . .
C207 C 0.5400(2) 0.4021(8) 0.1792(3) 0.0283(13) Uani 1 1 d . . .
H207 H 0.5612 0.3521 0.2192 0.034 Uiso 1 1 calc R . .
C208 C 0.4963(2) 0.3007(7) 0.1465(3) 0.0231(12) Uani 1 1 d . . .
H208 H 0.4861 0.1795 0.1638 0.028 Uiso 1 1 calc R . .
C209 C 0.4656(2) 0.3763(8) 0.0858(3) 0.0254(13) Uani 1 1 d . . .
C210 C 0.3826(2) 0.2966(8) -0.0040(3) 0.0233(13) Uani 1 1 d . . .
C211 C 0.3627(2) 0.5455(8) -0.0985(3) 0.0256(13) Uani 1 1 d . . .
C212 C 0.3797(2) 0.7322(7) -0.1134(3) 0.0239(12) Uani 1 1 d . . .
H212 H 0.4095 0.7906 -0.0841 0.029 Uiso 1 1 calc R . .
C213 C 0.3541(2) 0.8349(8) -0.1702(3) 0.0280(13) Uani 1 1 d . . .
H213 H 0.3669 0.9602 -0.1786 0.034 Uiso 1 1 calc R . .
C214 C 0.3100(2) 0.7542(8) -0.2145(3) 0.0329(14) Uani 1 1 d . . .
H214 H 0.2924 0.8237 -0.2527 0.040 Uiso 1 1 calc R . .
C215 C 0.2922(2) 0.5687(8) -0.2013(2) 0.0261(13) Uani 1 1 d . . .
C216 C 0.2488(2) 0.4451(8) -0.2348(3) 0.0321(14) Uani 1 1 d . . .
H216 H 0.2234 0.4745 -0.2743 0.039 Uiso 1 1 calc R . .
C217 C 0.2512(3) 0.2763(8) -0.1987(3) 0.0322(14) Uani 1 1 d . . .
H217 H 0.2273 0.1689 -0.2095 0.039 Uiso 1 1 calc R . .
C218 C 0.3192(2) 0.4656(8) -0.1440(3) 0.0238(13) Uani 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
O101 0.036(2) 0.026(2) 0.0308(19) 0.0024(17) -0.0030(17) -0.008(2)
N101 0.020(2) 0.021(3) 0.026(2) -0.002(2) 0.0053(17) -0.002(2)
N102 0.025(2) 0.023(3) 0.029(2) 0.005(2) -0.0012(19) 0.002(2)
N103 0.017(2) 0.019(3) 0.034(2) 0.002(2) -0.0009(18) -0.006(2)
N104 0.026(3) 0.035(3) 0.036(3) 0.001(2) -0.002(2) 0.004(2)
C101 0.021(3) 0.022(3) 0.030(3) -0.001(3) 0.003(2) -0.001(3)
C102 0.020(3) 0.021(3) 0.037(3) -0.004(3) 0.007(2) 0.001(3)
C103 0.030(3) 0.023(3) 0.042(3) -0.004(3) 0.006(2) -0.006(3)
C104 0.031(3) 0.039(4) 0.038(3) -0.005(3) 0.002(3) -0.009(3)
C105 0.033(4) 0.047(4) 0.024(3) -0.009(3) 0.001(2) -0.012(3)
C106 0.020(3) 0.035(4) 0.024(3) -0.011(3) 0.001(2) -0.002(3)
C107 0.021(3) 0.042(4) 0.026(3) -0.001(3) 0.003(2) -0.004(3)
C108 0.027(3) 0.028(3) 0.028(3) 0.001(3) 0.003(2) 0.005(3)
C109 0.015(3) 0.026(4) 0.032(3) -0.002(3) 0.005(2) 0.005(3)
C110 0.019(3) 0.029(4) 0.027(3) -0.002(3) -0.001(2) 0.001(3)
C111 0.019(3) 0.027(3) 0.025(3) -0.004(3) 0.002(2) 0.002(3)
C112 0.025(3) 0.033(4) 0.039(3) 0.001(3) 0.010(2) -0.002(3)
C113 0.036(3) 0.022(4) 0.039(3) 0.013(3) 0.011(3) 0.007(3)
C114 0.036(4) 0.043(4) 0.029(3) 0.003(3) 0.008(2) 0.016(3)
C115 0.030(3) 0.025(3) 0.027(3) 0.006(3) 0.002(2) 0.013(3)
C116 0.034(3) 0.039(4) 0.033(3) 0.000(3) -0.010(3) 0.009(3)
C117 0.023(3) 0.047(4) 0.050(4) -0.006(3) -0.011(3) 0.002(3)
C118 0.022(3) 0.018(3) 0.036(3) 0.000(3) 0.007(2) 0.000(2)
O201 0.022(2) 0.023(2) 0.0350(19) 0.0038(17) -0.0027(17) -0.0062(18)
N201 0.025(3) 0.015(3) 0.030(2) 0.001(2) 0.0007(18) -0.003(2)
N202 0.028(3) 0.021(3) 0.030(2) 0.009(2) -0.003(2) -0.006(2)
N203 0.022(3) 0.022(3) 0.029(2) 0.002(2) 0.0000(18) -0.005(2)
N204 0.029(3) 0.018(3) 0.036(2) 0.001(2) -0.002(2) -0.004(2)
C201 0.018(3) 0.022(3) 0.032(3) -0.001(3) 0.003(2) -0.004(3)
C202 0.022(3) 0.032(4) 0.036(3) -0.001(3) 0.002(2) -0.005(3)
C203 0.019(3) 0.026(3) 0.035(3) -0.001(3) 0.003(2) -0.005(3)
C204 0.023(3) 0.037(4) 0.035(3) -0.003(3) -0.001(2) -0.005(3)
C205 0.024(3) 0.036(4) 0.034(3) -0.009(3) -0.004(2) -0.003(3)
C206 0.020(3) 0.028(3) 0.025(3) -0.002(3) 0.001(2) 0.001(3)
C207 0.019(3) 0.029(4) 0.037(3) 0.002(3) 0.003(2) 0.002(3)
C208 0.022(3) 0.020(3) 0.027(3) 0.000(2) 0.000(2) 0.003(2)
C209 0.012(3) 0.032(4) 0.032(3) -0.007(3) 0.004(2) 0.000(3)
C210 0.017(3) 0.024(3) 0.029(3) -0.003(3) 0.003(2) 0.004(3)
C211 0.018(3) 0.030(4) 0.029(3) 0.000(3) 0.004(2) 0.007(3)
C212 0.020(3) 0.022(3) 0.030(3) -0.001(3) 0.002(2) -0.002(3)
C213 0.027(3) 0.026(3) 0.030(3) 0.001(3) 0.002(2) -0.001(3)
C214 0.028(3) 0.036(4) 0.035(3) -0.004(3) 0.001(2) 0.000(3)
C215 0.029(3) 0.027(3) 0.022(2) -0.002(3) -0.001(2) 0.001(3)
C216 0.035(3) 0.032(4) 0.030(3) 0.005(3) -0.007(2) -0.009(3)
C217 0.027(3) 0.036(4) 0.034(3) -0.008(3) -0.008(3) -0.013(3)
C218 0.015(3) 0.027(4) 0.029(3) 0.000(3) 0.002(2) 0.001(2)

_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
O101 C110 1.257(6) . ?
N101 C109 1.325(6) . ?
N101 C101 1.387(6) . ?
N102 C110 1.388(6) . ?
N102 C109 1.411(6) . ?
N103 C110 1.345(6) . ?
N103 C111 1.422(6) . ?
N104 C118 1.375(6) . ?
N104 C117 1.385(7) . ?
C101 C106 1.413(7) . ?
C101 C102 1.414(7) . ?
C102 C103 1.374(7) . ?
C103 C104 1.415(7) . ?
C104 C105 1.368(8) . ?
C105 C106 1.416(7) . ?
C106 C107 1.425(7) . ?
C107 C108 1.356(7) . ?
C108 C109 1.429(7) . ?
C111 C112 1.404(7) . ?
C111 C118 1.411(7) . ?
C112 C113 1.409(7) . ?
C113 C114 1.378(8) . ?
C114 C115 1.390(7) . ?
C115 C118 1.433(7) . ?
C115 C116 1.436(8) . ?
C116 C117 1.372(8) . ?
O201 C210 1.239(6) . ?
N201 C209 1.321(6) . ?
N201 C201 1.396(6) . ?
N202 C210 1.389(6) . ?
N202 C209 1.404(6) . ?
N203 C210 1.352(6) . ?
N203 C211 1.423(6) . ?
N204 C217 1.378(6) . ?
N204 C218 1.385(6) . ?
C201 C202 1.413(7) . ?
C201 C206 1.413(7) . ?
C202 C203 1.385(7) . ?
C203 C204 1.429(7) . ?
C204 C205 1.379(7) . ?
C205 C206 1.426(7) . ?
C206 C207 1.424(7) . ?
C207 C208 1.348(7) . ?
C208 C209 1.426(7) . ?
C211 C218 1.401(7) . ?
C211 C212 1.411(7) . ?
C212 C213 1.407(7) . ?
C213 C214 1.400(7) . ?
C214 C215 1.401(7) . ?
C215 C218 1.428(7) . ?
C215 C216 1.442(7) . ?
C216 C217 1.380(7) . ?

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
C109 N101 C101 117.6(4) . . ?
C110 N102 C109 129.7(5) . . ?
C110 N103 C111 131.9(4) . . ?
C118 N104 C117 109.4(5) . . ?
N101 C101 C106 122.6(5) . . ?
N101 C101 C102 117.5(5) . . ?
C106 C101 C102 119.9(5) . . ?
C103 C102 C101 120.0(5) . . ?
C102 C103 C104 120.6(5) . . ?
C105 C104 C103 119.7(5) . . ?
C104 C105 C106 121.3(5) . . ?
C101 C106 C105 118.4(5) . . ?
C101 C106 C107 116.9(5) . . ?
C105 C106 C107 124.6(5) . . ?
C108 C107 C106 120.9(5) . . ?
C107 C108 C109 118.2(5) . . ?
N101 C109 N102 119.2(5) . . ?
N101 C109 C108 123.8(5) . . ?
N102 C109 C108 117.1(5) . . ?
O101 C110 N103 126.2(5) . . ?
O101 C110 N102 117.5(5) . . ?
N103 C110 N102 116.3(5) . . ?
C112 C111 C118 116.0(5) . . ?
C112 C111 N103 116.0(5) . . ?
C118 C111 N103 128.0(5) . . ?
C111 C112 C113 121.9(5) . . ?
C114 C113 C112 121.4(5) . . ?
C113 C114 C115 119.0(5) . . ?
C114 C115 C118 119.8(5) . . ?
C114 C115 C116 134.0(5) . . ?
C118 C115 C116 106.2(5) . . ?
C117 C116 C115 107.7(5) . . ?
C116 C117 N104 109.3(5) . . ?
N104 C118 C111 130.6(5) . . ?
N104 C118 C115 107.5(5) . . ?
C111 C118 C115 121.9(5) . . ?
C209 N201 C201 117.1(4) . . ?
C210 N202 C209 131.2(5) . . ?
C210 N203 C211 132.6(4) . . ?
C217 N204 C218 109.8(4) . . ?
N201 C201 C202 117.2(5) . . ?
N201 C201 C206 122.3(5) . . ?
C202 C201 C206 120.5(5) . . ?
C203 C202 C201 119.4(5) . . ?
C202 C203 C204 120.9(5) . . ?
C205 C204 C203 119.6(5) . . ?
C204 C205 C206 120.6(5) . . ?
C201 C206 C207 117.8(5) . . ?
C201 C206 C205 119.0(5) . . ?
C207 C206 C205 123.1(5) . . ?
C208 C207 C206 119.4(5) . . ?
C207 C208 C209 119.7(5) . . ?
N201 C209 N202 119.4(5) . . ?
N201 C209 C208 123.6(5) . . ?
N202 C209 C208 117.0(5) . . ?
O201 C210 N203 126.1(5) . . ?
O201 C210 N202 118.6(5) . . ?
N203 C210 N202 115.4(4) . . ?
C218 C211 C212 116.4(5) . . ?
C218 C211 N203 127.8(5) . . ?
C212 C211 N203 115.8(5) . . ?
C213 C212 C211 122.2(5) . . ?
C214 C213 C212 120.7(5) . . ?
C213 C214 C215 118.5(5) . . ?
C214 C215 C218 120.2(5) . . ?
C214 C215 C216 133.3(5) . . ?
C218 C215 C216 106.6(5) . . ?
C217 C216 C215 107.3(5) . . ?
N204 C217 C216 109.2(5) . . ?
N204 C218 C211 130.9(5) . . ?
N204 C218 C215 107.1(4) . . ?
C211 C218 C215 122.0(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N102 H102 O201 0.88 2.13 2.997(5) 168.7 .
N103 H103 N101 0.88 1.90 2.654(6) 142.1 .
N104 H104 O101 0.88 1.97 2.687(5) 137.1 .
N202 H202 O101 0.88 1.97 2.848(5) 171.8 .
N203 H203 N201 0.88 1.92 2.682(6) 143.4 .
N204 H204 O201 0.88 2.00 2.703(5) 136.5 .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.052

_iucr_refine_instructions_details 
;
TITL 2012acc0044 in Pna2(1)
CELL 0.71073 22.0034 7.1308 18.6771 90.000 90.000 90.000
ZERR 8 0.0038 0.0014 0.0035 0.000 0.000 0.000
LATT -1
SYMM - X, - Y, 1/2 + Z
SYMM 1/2 + X, 1/2 - Y, Z
SYMM 1/2 - X, 1/2 + Y, 1/2 + Z
SFAC C H N O
UNIT 144 112 32 8
MERG 4
SHEL 7 0.84
FMAP 2
PLAN 10
HTAB
SIZE 0.03 0.10 0.22
ACTA 55.00
HTAB N102 O201
HTAB N103 N101
HTAB N104 O101
HTAB N202 O101
HTAB N203 N201
HTAB N204 O201
L.S. 4
TEMP -173.00
WGHT 0.032100
FVAR 0.35925
MOLE 1
O101 4 0.390472 -0.062990 0.134468 11.00000 0.03587 0.02647 =
0.03084 0.00235 -0.00301 -0.00811
N101 3 0.264395 -0.463873 0.065370 11.00000 0.02030 0.02123 =
0.02640 -0.00213 0.00531 -0.00241
N102 3 0.316489 -0.174759 0.061963 11.00000 0.02455 0.02278 =
0.02880 0.00518 -0.00121 0.00222
AFIX 43
H102 2 0.319812 -0.067318 0.039117 11.00000 -1.20000
AFIX 0
N103 3 0.349010 -0.355911 0.157844 11.00000 0.01702 0.01940 =
0.03403 0.00166 -0.00095 -0.00601
AFIX 43
H103 2 0.319314 -0.428800 0.142958 11.00000 -1.20000
AFIX 0
N104 3 0.447644 -0.156494 0.256476 11.00000 0.02618 0.03510 =
0.03554 0.00076 -0.00222 0.00367
AFIX 43
H104 2 0.436194 -0.070777 0.225379 11.00000 -1.20000
AFIX 0
C101 1 0.222127 -0.584762 0.035338 11.00000 0.02133 0.02245 =
0.02977 -0.00119 0.00343 -0.00075
C102 1 0.211757 -0.757367 0.070494 11.00000 0.02022 0.02141 =
0.03699 -0.00430 0.00710 0.00065
AFIX 43
H10A 2 0.233725 -0.787389 0.112755 11.00000 -1.20000
AFIX 0
C103 1 0.169893 -0.881744 0.043533 11.00000 0.03018 0.02257 =
0.04233 -0.00381 0.00628 -0.00571
AFIX 43
H10B 2 0.162502 -0.996492 0.067865 11.00000 -1.20000
AFIX 0
C104 1 0.137689 -0.840483 -0.020142 11.00000 0.03086 0.03936 =
0.03792 -0.00480 0.00192 -0.00919
AFIX 43
H10C 2 0.109139 -0.927714 -0.038765 11.00000 -1.20000
AFIX 0
C105 1 0.147888 -0.674293 -0.054743 11.00000 0.03270 0.04698 =
0.02384 -0.00949 0.00088 -0.01200
AFIX 43
H105 2 0.126684 -0.648211 -0.097917 11.00000 -1.20000
AFIX 0
C106 1 0.189412 -0.540388 -0.027496 11.00000 0.02007 0.03467 =
0.02370 -0.01069 0.00126 -0.00168
C107 1 0.200465 -0.361162 -0.058594 11.00000 0.02141 0.04221 =
0.02562 -0.00104 0.00327 -0.00403
AFIX 43
H107 2 0.179129 -0.325486 -0.100664 11.00000 -1.20000
AFIX 0
C108 1 0.241003 -0.240831 -0.028988 11.00000 0.02670 0.02763 =
0.02787 0.00103 0.00300 0.00476
AFIX 43
H108 2 0.247946 -0.120612 -0.049325 11.00000 -1.20000
AFIX 0
C109 1 0.272994 -0.299826 0.033647 11.00000 0.01533 0.02593 =
0.03234 -0.00162 0.00465 0.00467
C110 1 0.354812 -0.195731 0.120430 11.00000 0.01852 0.02889 =
0.02743 -0.00155 -0.00123 0.00101
C111 1 0.382020 -0.429157 0.217013 11.00000 0.01872 0.02676 =
0.02477 -0.00435 0.00172 0.00191
C112 1 0.369071 -0.615517 0.235770 11.00000 0.02534 0.03326 =
0.03863 0.00107 0.00956 -0.00191
AFIX 43
H112 2 0.339412 -0.682585 0.209112 11.00000 -1.20000
AFIX 0
C113 1 0.398760 -0.706040 0.292963 11.00000 0.03627 0.02204 =
0.03899 0.01253 0.01125 0.00727
AFIX 43
H113 2 0.389320 -0.833210 0.303267 11.00000 -1.20000
AFIX 0
C114 1 0.441213 -0.613953 0.334278 11.00000 0.03576 0.04329 =
0.02920 0.00315 0.00819 0.01631
AFIX 43
H114 2 0.460506 -0.676155 0.373093 11.00000 -1.20000
AFIX 0
C115 1 0.455363 -0.428721 0.318288 11.00000 0.03008 0.02512 =
0.02659 0.00556 0.00154 0.01251
C116 1 0.495977 -0.292930 0.348817 11.00000 0.03352 0.03926 =
0.03322 -0.00009 -0.00955 0.00873
AFIX 43
H116 2 0.522002 -0.312053 0.388739 11.00000 -1.20000
AFIX 0
C117 1 0.490430 -0.130617 0.309955 11.00000 0.02298 0.04677 =
0.05002 -0.00636 -0.01073 0.00240
AFIX 43
H117 2 0.512460 -0.018192 0.318392 11.00000 -1.20000
AFIX 0
C118 1 0.425843 -0.337082 0.259556 11.00000 0.02167 0.01836 =
0.03599 -0.00003 0.00726 -0.00012
MOLE 2
O201 4 0.345481 0.173675 -0.020967 11.00000 0.02221 0.02284 =
0.03497 0.00382 -0.00272 -0.00616
N201 3 0.477530 0.543117 0.058474 11.00000 0.02491 0.01535 =
0.02960 0.00145 0.00074 -0.00297
N202 3 0.419690 0.265724 0.055035 11.00000 0.02775 0.02150 =
0.03040 0.00904 -0.00275 -0.00598
AFIX 43
H202 2 0.413328 0.158247 0.076944 11.00000 -1.20000
AFIX 0
N203 3 0.390913 0.462375 -0.037715 11.00000 0.02198 0.02219 =
0.02909 0.00177 0.00002 -0.00516
AFIX 43
H203 2 0.419363 0.532618 -0.018289 11.00000 -1.20000
AFIX 0
N204 3 0.293560 0.288256 -0.144645 11.00000 0.02871 0.01787 =
0.03593 0.00117 -0.00152 -0.00369
AFIX 43
H204 2 0.302922 0.196902 -0.114949 11.00000 -1.20000
AFIX 0
C201 1 0.522695 0.649103 0.091943 11.00000 0.01829 0.02166 =
0.03158 -0.00108 0.00258 -0.00352
C202 1 0.536045 0.826658 0.062225 11.00000 0.02195 0.03176 =
0.03572 -0.00135 0.00174 -0.00471
AFIX 43
H20A 2 0.514653 0.869942 0.021250 11.00000 -1.20000
AFIX 0
C203 1 0.580580 0.936959 0.093361 11.00000 0.01913 0.02553 =
0.03544 -0.00077 0.00263 -0.00465
AFIX 43
H20B 2 0.589399 1.056777 0.073701 11.00000 -1.20000
AFIX 0
C204 1 0.613464 0.873036 0.154674 11.00000 0.02284 0.03679 =
0.03478 -0.00310 -0.00105 -0.00540
AFIX 43
H20C 2 0.644566 0.948669 0.174943 11.00000 -1.20000
AFIX 0
C205 1 0.599786 0.700969 0.184233 11.00000 0.02437 0.03602 =
0.03410 -0.00851 -0.00417 -0.00297
AFIX 43
H205 2 0.621033 0.659383 0.225567 11.00000 -1.20000
AFIX 0
C206 1 0.554025 0.584922 0.153292 11.00000 0.02025 0.02799 =
0.02466 -0.00166 0.00075 0.00080
C207 1 0.539992 0.402122 0.179209 11.00000 0.01896 0.02907 =
0.03700 0.00162 0.00251 0.00224
AFIX 43
H207 2 0.561202 0.352066 0.219179 11.00000 -1.20000
AFIX 0
C208 1 0.496338 0.300746 0.146513 11.00000 0.02246 0.01992 =
0.02700 -0.00008 0.00038 0.00288
AFIX 43
H208 2 0.486102 0.179545 0.163849 11.00000 -1.20000
AFIX 0
C209 1 0.465603 0.376289 0.085793 11.00000 0.01247 0.03190 =
0.03195 -0.00700 0.00407 -0.00009
C210 1 0.382568 0.296552 -0.003975 11.00000 0.01671 0.02385 =
0.02923 -0.00307 0.00331 0.00393
C211 1 0.362701 0.545484 -0.098467 11.00000 0.01802 0.03032 =
0.02852 0.00018 0.00387 0.00680
C212 1 0.379740 0.732186 -0.113387 11.00000 0.02000 0.02162 =
0.03004 -0.00141 0.00177 -0.00160
AFIX 43
H212 2 0.409520 0.790565 -0.084071 11.00000 -1.20000
AFIX 0
C213 1 0.354129 0.834869 -0.170207 11.00000 0.02742 0.02626 =
0.03029 0.00091 0.00222 -0.00092
AFIX 43
H213 2 0.366936 0.960194 -0.178579 11.00000 -1.20000
AFIX 0
C214 1 0.309969 0.754248 -0.214528 11.00000 0.02784 0.03626 =
0.03467 -0.00402 0.00139 -0.00030
AFIX 43
H214 2 0.292427 0.823735 -0.252690 11.00000 -1.20000
AFIX 0
C215 1 0.292233 0.568721 -0.201316 11.00000 0.02932 0.02660 =
0.02245 -0.00239 -0.00099 0.00057
C216 1 0.248847 0.445121 -0.234765 11.00000 0.03489 0.03178 =
0.02975 0.00482 -0.00715 -0.00911
AFIX 43
H216 2 0.223381 0.474466 -0.274282 11.00000 -1.20000
AFIX 0
C217 1 0.251157 0.276275 -0.198749 11.00000 0.02732 0.03562 =
0.03370 -0.00815 -0.00753 -0.01269
AFIX 43
H217 2 0.227309 0.168875 -0.209540 11.00000 -1.20000
AFIX 0
C218 1 0.319239 0.465561 -0.143991 11.00000 0.01549 0.02714 =
0.02886 0.00043 0.00156 0.00051
HKLF 4

REM 2012acc0044 in Pna2(1)
REM R1 = 0.0624 for 2083 Fo > 4sig(Fo) and 0.0859 for all 2677 data
REM 415 parameters refined using 1 restraints

END

WGHT 0.0355 0.0000
REM Highest difference peak 0.239, deepest hole -0.302, 1-sigma level 0.052
Q1 1 0.4322 0.1413 0.1333 11.00000 0.05 0.24
Q2 1 0.3810 -0.2237 0.0537 11.00000 0.05 0.19
Q3 1 0.3002 0.5311 -0.1693 11.00000 0.05 0.19
Q4 1 0.4487 -0.2752 0.1542 11.00000 0.05 0.19
Q5 1 0.3955 0.0391 0.1614 11.00000 0.05 0.19
Q6 1 0.4756 -0.3821 0.4336 11.00000 0.05 0.18
Q7 1 0.2304 -0.7165 -0.0531 11.00000 0.05 0.18
Q8 1 0.4064 0.0653 0.2192 11.00000 0.05 0.18
Q9 1 0.3669 0.0887 0.0812 11.00000 0.05 0.18
Q10 1 0.3023 0.0353 0.0376 11.00000 0.05 0.17

;


data_2012acc0061
_database_code_depnum_ccdc_archive 'CCDC 903911'
#TrackingRef '2012acc0061.cif'

#MAR85_DMSO

_audit_creation_method           SHELXL-97


_chemical_compound_source        'Claudia Caltagirone'
_database_code_CSD               12AC0061
_database_code_depnum_ccdc_archive ?

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H14 N4 O'
_chemical_formula_weight         314.34

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.0410(17)
_cell_length_b                   19.459(4)
_cell_length_c                   18.998(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.696(3)
_cell_angle_gamma                90.00
_cell_volume                     2962.6(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5609
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      31.3

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9891
_exptl_absorpt_correction_T_max  0.9964
#_exptl_absorpt_correction_T_max 1.000
#_exptl_absorpt_correction_T_min 0.748
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the
Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16289
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         31.28
_reflns_number_total             8526
_reflns_number_gt                6132
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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^ > 2\s(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^)+(0.0550P)^2^+0.9799P] 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         8526
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0793
_refine_ls_wR_factor_ref         0.1788
_refine_ls_wR_factor_gt          0.1604
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.08073(18) 0.24986(8) 0.03353(8) 0.0296(4) Uani 1 1 d . . .
N1 N 0.6263(2) 0.36327(9) 0.02921(10) 0.0268(4) Uani 1 1 d . . .
N2 N 0.3466(2) 0.29385(9) 0.04651(9) 0.0240(4) Uani 1 1 d . . .
H902 H 0.4436 0.2893 0.0710 0.029 Uiso 1 1 calc R . .
N3 N 0.2640(2) 0.20507(9) 0.11776(9) 0.0237(4) Uani 1 1 d . . .
H903 H 0.1846 0.1756 0.1257 0.028 Uiso 1 1 calc R . .
N4 N 0.5415(2) 0.23369(9) 0.15120(9) 0.0233(4) Uani 1 1 d . . .
C1 C 0.4876(3) 0.38147(10) -0.01280(11) 0.0233(4) Uani 1 1 d . . .
C2 C 0.7667(3) 0.39511(12) 0.02007(12) 0.0314(5) Uani 1 1 d . . .
H2 H 0.8637 0.3820 0.0488 0.038 Uiso 1 1 calc R . .
C3 C 0.7815(3) 0.44755(11) -0.02995(12) 0.0309(5) Uani 1 1 d . . .
H3 H 0.8867 0.4683 -0.0352 0.037 Uiso 1 1 calc R . .
C4 C 0.6435(3) 0.46834(11) -0.07092(12) 0.0298(5) Uani 1 1 d . . .
H4 H 0.6511 0.5048 -0.1038 0.036 Uiso 1 1 calc R . .
C5 C 0.4888(3) 0.43523(11) -0.06412(11) 0.0261(4) Uani 1 1 d . . .
C6 C 0.3419(3) 0.45178(11) -0.10612(11) 0.0277(5) Uani 1 1 d . . .
H6 H 0.3418 0.4880 -0.1396 0.033 Uiso 1 1 calc R . .
C7 C 0.1993(3) 0.41513(11) -0.09824(12) 0.0284(5) Uani 1 1 d . . .
H7 H 0.1009 0.4259 -0.1273 0.034 Uiso 1 1 calc R . .
C8 C 0.1944(3) 0.36194(11) -0.04817(11) 0.0262(4) Uani 1 1 d . . .
H8 H 0.0935 0.3375 -0.0439 0.031 Uiso 1 1 calc R . .
C9 C 0.3353(2) 0.34514(10) -0.00534(11) 0.0233(4) Uani 1 1 d . . .
C10 C 0.2233(3) 0.25020(10) 0.06301(11) 0.0236(4) Uani 1 1 d . . .
C11 C 0.4081(2) 0.19810(10) 0.16244(11) 0.0238(4) Uani 1 1 d . . .
C12 C 0.3989(3) 0.15139(11) 0.22040(11) 0.0272(5) Uani 1 1 d . . .
H12 H 0.3001 0.1260 0.2262 0.033 Uiso 1 1 calc R . .
C13 C 0.5344(3) 0.14462(11) 0.26629(12) 0.0286(5) Uani 1 1 d . . .
H13 H 0.5308 0.1144 0.3054 0.034 Uiso 1 1 calc R . .
C14 C 0.6837(3) 0.18228(10) 0.25704(11) 0.0248(4) Uani 1 1 d . . .
C15 C 0.8283(3) 0.17706(11) 0.30274(12) 0.0293(5) Uani 1 1 d . . .
H15 H 0.8299 0.1478 0.3428 0.035 Uiso 1 1 calc R . .
C16 C 0.9686(3) 0.21422(11) 0.28995(12) 0.0300(5) Uani 1 1 d . . .
H16 H 1.0668 0.2103 0.3211 0.036 Uiso 1 1 calc R . .
C17 C 0.9669(3) 0.25771(11) 0.23122(12) 0.0282(5) Uani 1 1 d . . .
H17 H 1.0638 0.2834 0.2230 0.034 Uiso 1 1 calc R . .
C18 C 0.8259(3) 0.26351(10) 0.18528(12) 0.0258(4) Uani 1 1 d . . .
H18 H 0.8263 0.2928 0.1453 0.031 Uiso 1 1 calc R . .
C19 C 0.6812(2) 0.22597(10) 0.19755(11) 0.0213(4) Uani 1 1 d . . .
O2 O 0.02407(18) 0.10399(8) 0.14454(8) 0.0297(4) Uani 1 1 d . . .
N5 N -0.5199(2) -0.00693(9) 0.15862(10) 0.0271(4) Uani 1 1 d . . .
N6 N -0.2423(2) 0.06078(8) 0.13596(9) 0.0239(4) Uani 1 1 d . . .
H906 H -0.3398 0.0639 0.1115 0.029 Uiso 1 1 calc R . .
N7 N -0.1579(2) 0.14301(9) 0.05677(9) 0.0254(4) Uani 1 1 d . . .
H907 H -0.0769 0.1704 0.0458 0.030 Uiso 1 1 calc R . .
N8 N -0.4324(2) 0.11041(9) 0.02406(9) 0.0253(4) Uani 1 1 d . . .
C20 C -0.3823(2) -0.02189(10) 0.20247(11) 0.0228(4) Uani 1 1 d . . .
C21 C -0.6593(3) -0.03953(12) 0.16912(12) 0.0307(5) Uani 1 1 d . . .
H21 H -0.7560 -0.0291 0.1389 0.037 Uiso 1 1 calc R . .
C22 C -0.6737(3) -0.08900(11) 0.22261(12) 0.0313(5) Uani 1 1 d . . .
H22 H -0.7775 -0.1110 0.2278 0.038 Uiso 1 1 calc R . .
C23 C -0.5363(3) -0.10479(11) 0.26678(12) 0.0291(5) Uani 1 1 d . . .
H23 H -0.5435 -0.1378 0.3032 0.035 Uiso 1 1 calc R . .
C24 C -0.3833(3) -0.07144(10) 0.25776(11) 0.0250(4) Uani 1 1 d . . .
C25 C -0.2355(3) -0.08490(10) 0.30091(11) 0.0268(4) Uani 1 1 d . . .
H25 H -0.2346 -0.1186 0.3371 0.032 Uiso 1 1 calc R . .
C26 C -0.0928(3) -0.04882(11) 0.29000(12) 0.0284(5) Uani 1 1 d . . .
H26 H 0.0062 -0.0577 0.3194 0.034 Uiso 1 1 calc R . .
C27 C -0.0895(3) 0.00093(11) 0.23641(11) 0.0256(4) Uani 1 1 d . . .
H27 H 0.0106 0.0254 0.2306 0.031 Uiso 1 1 calc R . .
C28 C -0.2312(3) 0.01451(10) 0.19205(11) 0.0240(4) Uani 1 1 d . . .
C29 C -0.1182(2) 0.10178(10) 0.11488(11) 0.0230(4) Uani 1 1 d . . .
C30 C -0.3038(3) 0.14877(11) 0.01268(11) 0.0258(4) Uani 1 1 d . . .
C31 C -0.3013(3) 0.19760(11) -0.04377(11) 0.0284(5) Uani 1 1 d . . .
H31 H -0.2044 0.2241 -0.0500 0.034 Uiso 1 1 calc R . .
C32 C -0.4411(3) 0.20481(11) -0.08779(12) 0.0298(5) Uani 1 1 d . . .
H32 H -0.4427 0.2366 -0.1258 0.036 Uiso 1 1 calc R . .
C33 C -0.5855(3) 0.16512(11) -0.07755(12) 0.0281(5) Uani 1 1 d . . .
C34 C -0.7357(3) 0.17118(12) -0.12055(12) 0.0320(5) Uani 1 1 d . . .
H34 H -0.7428 0.2023 -0.1592 0.038 Uiso 1 1 calc R . .
C35 C -0.8726(3) 0.13218(12) -0.10695(13) 0.0339(5) Uani 1 1 d . . .
H35 H -0.9742 0.1370 -0.1357 0.041 Uiso 1 1 calc R . .
C36 C -0.8617(3) 0.08531(12) -0.05058(13) 0.0327(5) Uani 1 1 d . . .
H36 H -0.9564 0.0585 -0.0417 0.039 Uiso 1 1 calc R . .
C37 C -0.7153(3) 0.07766(11) -0.00788(12) 0.0303(5) Uani 1 1 d . . .
H37 H -0.7090 0.0453 0.0297 0.036 Uiso 1 1 calc R . .
C38 C -0.5757(3) 0.11810(10) -0.02052(11) 0.0242(4) Uani 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
O1 0.0207(7) 0.0364(8) 0.0310(8) 0.0059(7) -0.0026(6) -0.0069(6)
N1 0.0225(8) 0.0296(9) 0.0278(9) -0.0010(8) -0.0006(7) -0.0042(7)
N2 0.0206(8) 0.0262(9) 0.0247(9) 0.0035(7) -0.0011(7) -0.0034(7)
N3 0.0197(8) 0.0246(8) 0.0262(9) 0.0032(7) -0.0015(7) -0.0066(7)
N4 0.0230(8) 0.0232(8) 0.0239(9) 0.0006(7) 0.0024(7) -0.0016(7)
C1 0.0225(10) 0.0244(10) 0.0232(10) -0.0049(8) 0.0026(8) -0.0017(8)
C2 0.0275(11) 0.0355(12) 0.0313(12) -0.0031(10) 0.0020(9) -0.0075(10)
C3 0.0296(11) 0.0312(11) 0.0328(12) -0.0033(9) 0.0080(10) -0.0118(10)
C4 0.0338(12) 0.0289(11) 0.0279(11) -0.0017(9) 0.0095(9) -0.0084(9)
C5 0.0291(11) 0.0232(10) 0.0266(10) -0.0034(8) 0.0060(9) -0.0029(9)
C6 0.0312(11) 0.0264(10) 0.0261(11) 0.0014(9) 0.0055(9) 0.0014(9)
C7 0.0283(11) 0.0298(11) 0.0269(11) 0.0006(9) 0.0007(9) 0.0019(9)
C8 0.0236(10) 0.0267(10) 0.0282(11) -0.0009(9) 0.0016(9) -0.0028(8)
C9 0.0227(10) 0.0235(9) 0.0237(10) -0.0015(8) 0.0021(8) -0.0024(8)
C10 0.0222(9) 0.0251(10) 0.0231(10) -0.0007(8) -0.0004(8) -0.0029(8)
C11 0.0226(10) 0.0243(10) 0.0242(10) -0.0026(8) 0.0003(8) -0.0016(8)
C12 0.0272(10) 0.0267(10) 0.0278(11) 0.0021(8) 0.0028(9) -0.0068(9)
C13 0.0303(11) 0.0277(11) 0.0281(11) 0.0036(9) 0.0049(9) -0.0042(9)
C14 0.0234(10) 0.0240(10) 0.0268(10) -0.0011(8) 0.0014(8) -0.0002(8)
C15 0.0289(11) 0.0298(11) 0.0284(11) 0.0017(9) -0.0029(9) -0.0012(9)
C16 0.0244(10) 0.0305(11) 0.0339(12) 0.0007(9) -0.0048(9) 0.0012(9)
C17 0.0226(10) 0.0264(10) 0.0351(12) -0.0006(9) -0.0011(9) -0.0021(8)
C18 0.0243(10) 0.0230(10) 0.0304(11) -0.0002(8) 0.0041(9) -0.0017(8)
C19 0.0218(9) 0.0190(9) 0.0230(9) -0.0030(7) 0.0018(8) 0.0003(8)
O2 0.0224(7) 0.0342(8) 0.0318(8) 0.0051(7) -0.0031(6) -0.0068(6)
N5 0.0228(9) 0.0267(9) 0.0316(10) -0.0015(8) 0.0005(8) -0.0050(7)
N6 0.0214(8) 0.0246(9) 0.0252(9) 0.0016(7) -0.0007(7) -0.0029(7)
N7 0.0223(8) 0.0291(9) 0.0246(9) 0.0030(7) 0.0012(7) -0.0068(7)
N8 0.0224(8) 0.0262(9) 0.0270(9) -0.0004(7) 0.0009(7) -0.0024(7)
C20 0.0220(9) 0.0224(9) 0.0242(10) -0.0025(8) 0.0024(8) -0.0001(8)
C21 0.0228(10) 0.0338(12) 0.0354(12) 0.0001(10) 0.0017(9) -0.0033(9)
C22 0.0281(11) 0.0302(11) 0.0362(13) 0.0007(10) 0.0053(10) -0.0059(9)
C23 0.0329(12) 0.0240(10) 0.0314(11) -0.0018(9) 0.0079(9) -0.0030(9)
C24 0.0280(11) 0.0212(9) 0.0263(10) -0.0032(8) 0.0052(9) -0.0001(8)
C25 0.0323(11) 0.0217(10) 0.0265(11) 0.0005(8) 0.0038(9) 0.0026(9)
C26 0.0270(11) 0.0289(11) 0.0292(11) -0.0008(9) 0.0012(9) 0.0028(9)
C27 0.0219(10) 0.0261(10) 0.0289(11) -0.0043(9) 0.0021(8) -0.0011(8)
C28 0.0257(10) 0.0206(9) 0.0259(10) -0.0015(8) 0.0037(8) -0.0012(8)
C29 0.0206(9) 0.0238(10) 0.0245(10) -0.0004(8) 0.0017(8) -0.0028(8)
C30 0.0250(10) 0.0270(10) 0.0253(10) -0.0036(8) 0.0015(8) 0.0002(8)
C31 0.0274(11) 0.0296(11) 0.0284(11) 0.0024(9) 0.0035(9) -0.0046(9)
C32 0.0326(11) 0.0281(11) 0.0286(11) 0.0001(9) 0.0014(9) -0.0016(9)
C33 0.0278(11) 0.0277(10) 0.0285(11) -0.0059(9) 0.0001(9) 0.0037(9)
C34 0.0320(11) 0.0338(12) 0.0290(11) -0.0049(9) -0.0048(9) 0.0099(10)
C35 0.0261(11) 0.0400(13) 0.0341(12) -0.0077(10) -0.0059(9) 0.0081(10)
C36 0.0234(11) 0.0355(12) 0.0389(13) -0.0095(10) 0.0008(10) -0.0012(9)
C37 0.0275(11) 0.0291(11) 0.0340(12) -0.0039(9) 0.0006(9) -0.0012(9)
C38 0.0226(10) 0.0247(10) 0.0249(10) -0.0050(8) -0.0014(8) 0.0026(8)

_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
O1 C10 1.234(2) . ?
N1 C2 1.312(3) . ?
N1 C1 1.364(3) . ?
N2 C10 1.361(2) . ?
N2 C9 1.400(3) . ?
N3 C10 1.380(3) . ?
N3 C11 1.386(3) . ?
N4 C11 1.309(2) . ?
N4 C19 1.378(3) . ?
C1 C5 1.431(3) . ?
C1 C9 1.431(3) . ?
C2 C3 1.406(3) . ?
C3 C4 1.364(3) . ?
C4 C5 1.416(3) . ?
C5 C6 1.407(3) . ?
C6 C7 1.369(3) . ?
C7 C8 1.408(3) . ?
C8 C9 1.379(3) . ?
C11 C12 1.434(3) . ?
C12 C13 1.345(3) . ?
C13 C14 1.430(3) . ?
C14 C15 1.397(3) . ?
C14 C19 1.413(3) . ?
C15 C16 1.378(3) . ?
C16 C17 1.400(3) . ?
C17 C18 1.377(3) . ?
C18 C19 1.410(3) . ?
O2 C29 1.234(2) . ?
N5 C21 1.317(3) . ?
N5 C20 1.361(3) . ?
N6 C29 1.363(2) . ?
N6 C28 1.392(3) . ?
N7 C29 1.381(3) . ?
N7 C30 1.389(3) . ?
N8 C30 1.307(3) . ?
N8 C38 1.381(3) . ?
C20 C24 1.426(3) . ?
C20 C28 1.434(3) . ?
C21 C22 1.411(3) . ?
C22 C23 1.367(3) . ?
C23 C24 1.414(3) . ?
C24 C25 1.412(3) . ?
C25 C26 1.375(3) . ?
C26 C27 1.407(3) . ?
C27 C28 1.386(3) . ?
C30 C31 1.434(3) . ?
C31 C32 1.352(3) . ?
C32 C33 1.421(3) . ?
C33 C34 1.406(3) . ?
C33 C38 1.415(3) . ?
C34 C35 1.379(3) . ?
C35 C36 1.404(3) . ?
C36 C37 1.382(3) . ?
C37 C38 1.408(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
C2 N1 C1 118.11(19) . . ?
C10 N2 C9 126.91(18) . . ?
C10 N3 C11 131.18(17) . . ?
C11 N4 C19 118.31(17) . . ?
N1 C1 C5 122.55(18) . . ?
N1 C1 C9 118.63(19) . . ?
C5 C1 C9 118.82(19) . . ?
N1 C2 C3 123.6(2) . . ?
C4 C3 C2 119.4(2) . . ?
C3 C4 C5 119.5(2) . . ?
C6 C5 C4 123.1(2) . . ?
C6 C5 C1 120.12(19) . . ?
C4 C5 C1 116.7(2) . . ?
C7 C6 C5 119.4(2) . . ?
C6 C7 C8 121.8(2) . . ?
C9 C8 C7 120.39(19) . . ?
C8 C9 N2 125.93(18) . . ?
C8 C9 C1 119.53(19) . . ?
N2 C9 C1 114.54(18) . . ?
O1 C10 N2 124.46(19) . . ?
O1 C10 N3 119.49(18) . . ?
N2 C10 N3 116.03(18) . . ?
N4 C11 N3 120.24(18) . . ?
N4 C11 C12 123.70(19) . . ?
N3 C11 C12 116.05(18) . . ?
C13 C12 C11 118.02(19) . . ?
C12 C13 C14 120.9(2) . . ?
C15 C14 C19 119.87(19) . . ?
C15 C14 C13 123.4(2) . . ?
C19 C14 C13 116.69(19) . . ?
C16 C15 C14 120.3(2) . . ?
C15 C16 C17 120.2(2) . . ?
C18 C17 C16 120.6(2) . . ?
C17 C18 C19 120.0(2) . . ?
N4 C19 C18 118.61(18) . . ?
N4 C19 C14 122.33(18) . . ?
C18 C19 C14 119.06(19) . . ?
C21 N5 C20 117.61(19) . . ?
C29 N6 C28 126.94(18) . . ?
C29 N7 C30 131.12(18) . . ?
C30 N8 C38 117.90(18) . . ?
N5 C20 C24 122.85(18) . . ?
N5 C20 C28 117.75(18) . . ?
C24 C20 C28 119.40(19) . . ?
N5 C21 C22 124.0(2) . . ?
C23 C22 C21 119.0(2) . . ?
C22 C23 C24 119.4(2) . . ?
C25 C24 C23 123.0(2) . . ?
C25 C24 C20 119.88(19) . . ?
C23 C24 C20 117.2(2) . . ?
C26 C25 C24 119.4(2) . . ?
C25 C26 C27 121.7(2) . . ?
C28 C27 C26 120.54(19) . . ?
C27 C28 N6 125.91(19) . . ?
C27 C28 C20 119.05(19) . . ?
N6 C28 C20 115.03(18) . . ?
O2 C29 N6 124.05(19) . . ?
O2 C29 N7 119.34(18) . . ?
N6 C29 N7 116.61(18) . . ?
N8 C30 N7 119.63(19) . . ?
N8 C30 C31 124.2(2) . . ?
N7 C30 C31 116.20(18) . . ?
C32 C31 C30 118.0(2) . . ?
C31 C32 C33 120.4(2) . . ?
C34 C33 C38 119.4(2) . . ?
C34 C33 C32 123.2(2) . . ?
C38 C33 C32 117.4(2) . . ?
C35 C34 C33 120.4(2) . . ?
C34 C35 C36 120.0(2) . . ?
C37 C36 C35 121.0(2) . . ?
C36 C37 C38 119.5(2) . . ?
N8 C38 C37 118.16(19) . . ?
N8 C38 C33 122.08(19) . . ?
C37 C38 C33 119.8(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H902 N4 0.88 1.98 2.697(2) 137.9 .
N3 H903 O2 0.88 1.95 2.830(2) 174.9 .
N6 H906 N8 0.88 1.98 2.694(3) 137.0 .
N7 H907 O1 0.88 2.03 2.888(2) 166.4 .

_diffrn_measured_fraction_theta_max 0.881
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.055

_iucr_refine_instructions_details 
;
TITL 2012acc0061 in P21/c
CELL 0.71069 8.0410 19.4590 18.9980 90.000 94.696 90.000
ZERR 8.00 0.0017 0.0043 0.0044 0 0.0034 0
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H N O
UNIT 152 112 32 8
MERG 2
FMAP 2
PLAN 20
ACTA 55
HTAB
HTAB N2 N4

HTAB N3 O2

HTAB N6 N8

HTAB N7 O1
TEMP -173
SIZE 0.12 0.1 0.04
L.S. 5
WGHT 0.055000 0.979900
FVAR 0.22713
MOLE 1
O1 4 0.080733 0.249857 0.033535 11.00000 0.02069 0.03635 =
0.03100 0.00590 -0.00261 -0.00690
N1 3 0.626316 0.363266 0.029210 11.00000 0.02249 0.02959 =
0.02779 -0.00104 -0.00056 -0.00424
N2 3 0.346576 0.293849 0.046506 11.00000 0.02060 0.02623 =
0.02473 0.00353 -0.00112 -0.00341
AFIX 43
H902 2 0.443642 0.289347 0.071031 11.00000 -1.20000
AFIX 0
N3 3 0.263955 0.205073 0.117761 11.00000 0.01968 0.02461 =
0.02619 0.00318 -0.00147 -0.00664
AFIX 43
H903 2 0.184581 0.175612 0.125685 11.00000 -1.20000
AFIX 0
N4 3 0.541462 0.233691 0.151204 11.00000 0.02297 0.02318 =
0.02387 0.00056 0.00238 -0.00164
C1 1 0.487613 0.381466 -0.012801 11.00000 0.02250 0.02439 =
0.02319 -0.00486 0.00256 -0.00167
C2 1 0.766674 0.395115 0.020073 11.00000 0.02748 0.03552 =
0.03128 -0.00315 0.00200 -0.00748
AFIX 43
H2 2 0.863703 0.382029 0.048844 11.00000 -1.20000
AFIX 0
C3 1 0.781502 0.447552 -0.029946 11.00000 0.02958 0.03116 =
0.03278 -0.00329 0.00796 -0.01180
AFIX 43
H3 2 0.886719 0.468313 -0.035151 11.00000 -1.20000
AFIX 0
C4 1 0.643489 0.468340 -0.070923 11.00000 0.03377 0.02886 =
0.02790 -0.00167 0.00950 -0.00842
AFIX 43
H4 2 0.651072 0.504772 -0.103793 11.00000 -1.20000
AFIX 0
C5 1 0.488767 0.435227 -0.064123 11.00000 0.02910 0.02319 =
0.02658 -0.00338 0.00604 -0.00294
C6 1 0.341933 0.451782 -0.106116 11.00000 0.03125 0.02643 =
0.02608 0.00144 0.00551 0.00141
AFIX 43
H6 2 0.341776 0.488039 -0.139608 11.00000 -1.20000
AFIX 0
C7 1 0.199265 0.415128 -0.098240 11.00000 0.02833 0.02983 =
0.02686 0.00061 0.00073 0.00187
AFIX 43
H7 2 0.100942 0.425861 -0.127325 11.00000 -1.20000
AFIX 0
C8 1 0.194415 0.361941 -0.048169 11.00000 0.02355 0.02674 =
0.02818 -0.00091 0.00165 -0.00279
AFIX 43
H8 2 0.093483 0.337494 -0.043874 11.00000 -1.20000
AFIX 0
C9 1 0.335325 0.345144 -0.005339 11.00000 0.02268 0.02355 =
0.02374 -0.00152 0.00214 -0.00239
C10 1 0.223336 0.250203 0.063007 11.00000 0.02217 0.02505 =
0.02310 -0.00074 -0.00038 -0.00290
C11 1 0.408088 0.198101 0.162437 11.00000 0.02259 0.02429 =
0.02424 -0.00262 0.00029 -0.00165
C12 1 0.398901 0.151388 0.220400 11.00000 0.02716 0.02666 =
0.02779 0.00210 0.00282 -0.00676
AFIX 43
H12 2 0.300054 0.125989 0.226199 11.00000 -1.20000
AFIX 0
C13 1 0.534393 0.144616 0.266294 11.00000 0.03028 0.02770 =
0.02808 0.00358 0.00485 -0.00421
AFIX 43
H13 2 0.530826 0.114387 0.305408 11.00000 -1.20000
AFIX 0
C14 1 0.683744 0.182282 0.257038 11.00000 0.02344 0.02401 =
0.02684 -0.00108 0.00135 -0.00021
C15 1 0.828309 0.177064 0.302744 11.00000 0.02894 0.02978 =
0.02836 0.00166 -0.00294 -0.00123
AFIX 43
H15 2 0.829947 0.147790 0.342813 11.00000 -1.20000
AFIX 0
C16 1 0.968608 0.214218 0.289948 11.00000 0.02437 0.03051 =
0.03386 0.00069 -0.00483 0.00121
AFIX 43
H16 2 1.066785 0.210299 0.321086 11.00000 -1.20000
AFIX 0
C17 1 0.966872 0.257705 0.231216 11.00000 0.02262 0.02639 =
0.03514 -0.00062 -0.00107 -0.00214
AFIX 43
H17 2 1.063763 0.283447 0.222961 11.00000 -1.20000
AFIX 0
C18 1 0.825923 0.263508 0.185279 11.00000 0.02431 0.02296 =
0.03044 -0.00018 0.00408 -0.00167
AFIX 43
H18 2 0.826257 0.292823 0.145304 11.00000 -1.20000
AFIX 0
C19 1 0.681153 0.225968 0.197551 11.00000 0.02177 0.01904 =
0.02302 -0.00298 0.00178 0.00029
MOLE 2
O2 4 0.024073 0.103987 0.144541 11.00000 0.02239 0.03418 =
0.03179 0.00507 -0.00312 -0.00677
N5 3 -0.519943 -0.006930 0.158623 11.00000 0.02278 0.02673 =
0.03160 -0.00148 0.00048 -0.00500
N6 3 -0.242260 0.060783 0.135959 11.00000 0.02136 0.02457 =
0.02521 0.00164 -0.00066 -0.00288
AFIX 43
H906 2 -0.339764 0.063892 0.111515 11.00000 -1.20000
AFIX 0
N7 3 -0.157948 0.143009 0.056766 11.00000 0.02229 0.02908 =
0.02464 0.00299 0.00118 -0.00676
AFIX 43
H907 2 -0.076852 0.170356 0.045765 11.00000 -1.20000
AFIX 0
N8 3 -0.432354 0.110411 0.024063 11.00000 0.02243 0.02618 =
0.02701 -0.00041 0.00092 -0.00244
C20 1 -0.382339 -0.021894 0.202465 11.00000 0.02197 0.02244 =
0.02415 -0.00254 0.00240 -0.00015
C21 1 -0.659302 -0.039527 0.169122 11.00000 0.02278 0.03382 =
0.03537 0.00014 0.00167 -0.00334
AFIX 43
H21 2 -0.755963 -0.029113 0.138863 11.00000 -1.20000
AFIX 0
C22 1 -0.673732 -0.088996 0.222609 11.00000 0.02807 0.03024 =
0.03616 0.00065 0.00527 -0.00590
AFIX 43
H22 2 -0.777465 -0.111000 0.227835 11.00000 -1.20000
AFIX 0
C23 1 -0.536275 -0.104785 0.266781 11.00000 0.03290 0.02398 =
0.03139 -0.00179 0.00790 -0.00302
AFIX 43
H23 2 -0.543496 -0.137848 0.303197 11.00000 -1.20000
AFIX 0
C24 1 -0.383257 -0.071443 0.257761 11.00000 0.02795 0.02119 =
0.02631 -0.00319 0.00522 -0.00015
C25 1 -0.235472 -0.084899 0.300906 11.00000 0.03225 0.02172 =
0.02655 0.00050 0.00377 0.00263
AFIX 43
H25 2 -0.234602 -0.118569 0.337144 11.00000 -1.20000
AFIX 0
C26 1 -0.092768 -0.048816 0.289996 11.00000 0.02697 0.02892 =
0.02925 -0.00077 0.00121 0.00281
AFIX 43
H26 2 0.006168 -0.057723 0.319415 11.00000 -1.20000
AFIX 0
C27 1 -0.089505 0.000932 0.236413 11.00000 0.02193 0.02609 =
0.02886 -0.00429 0.00207 -0.00106
AFIX 43
H27 2 0.010637 0.025429 0.230586 11.00000 -1.20000
AFIX 0
C28 1 -0.231185 0.014506 0.192046 11.00000 0.02566 0.02064 =
0.02592 -0.00147 0.00371 -0.00124
C29 1 -0.118198 0.101776 0.114883 11.00000 0.02062 0.02382 =
0.02446 -0.00043 0.00165 -0.00276
C30 1 -0.303838 0.148765 0.012681 11.00000 0.02495 0.02700 =
0.02529 -0.00356 0.00150 0.00016
C31 1 -0.301341 0.197603 -0.043772 11.00000 0.02742 0.02960 =
0.02840 0.00235 0.00352 -0.00458
AFIX 43
H31 2 -0.204409 0.224088 -0.050041 11.00000 -1.20000
AFIX 0
C32 1 -0.441067 0.204812 -0.087787 11.00000 0.03257 0.02811 =
0.02860 0.00006 0.00139 -0.00156
AFIX 43
H32 2 -0.442731 0.236599 -0.125792 11.00000 -1.20000
AFIX 0
C33 1 -0.585513 0.165119 -0.077551 11.00000 0.02782 0.02767 =
0.02852 -0.00590 0.00012 0.00368
C34 1 -0.735666 0.171177 -0.120553 11.00000 0.03203 0.03377 =
0.02896 -0.00487 -0.00475 0.00990
AFIX 43
H34 2 -0.742815 0.202314 -0.159197 11.00000 -1.20000
AFIX 0
C35 1 -0.872559 0.132184 -0.106948 11.00000 0.02608 0.04003 =
0.03413 -0.00772 -0.00590 0.00807
AFIX 43
H35 2 -0.974217 0.137032 -0.135708 11.00000 -1.20000
AFIX 0
C36 1 -0.861685 0.085313 -0.050583 11.00000 0.02338 0.03551 =
0.03893 -0.00954 0.00079 -0.00121
AFIX 43
H36 2 -0.956368 0.058458 -0.041670 11.00000 -1.20000
AFIX 0
C37 1 -0.715332 0.077658 -0.007879 11.00000 0.02753 0.02913 =
0.03403 -0.00390 0.00056 -0.00122
AFIX 43
H37 2 -0.708986 0.045345 0.029730 11.00000 -1.20000
AFIX 0
C38 1 -0.575655 0.118104 -0.020516 11.00000 0.02257 0.02467 =
0.02494 -0.00502 -0.00142 0.00256
HKLF 4

REM 2012acc0061 in P21/c
REM R1 = 0.0793 for 6132 Fo > 4sig(Fo) and 0.1121 for all 8526 data
REM 433 parameters refined using 0 restraints

END

WGHT 0.0511 1.0661
REM Highest difference peak 0.294, deepest hole -0.243, 1-sigma level 0.055
Q1 1 0.2030 0.1587 0.1455 11.00000 0.05 0.29
Q2 1 -0.9303 0.0494 -0.0236 11.00000 0.05 0.27
Q3 1 0.5394 0.2004 0.2027 11.00000 0.05 0.27
Q4 1 0.9814 0.2253 0.2548 11.00000 0.05 0.26
Q5 1 0.7493 0.2786 0.1490 11.00000 0.05 0.25
Q6 1 -0.3161 -0.0029 0.1970 11.00000 0.05 0.24
Q7 1 -0.3839 -0.0443 0.2295 11.00000 0.05 0.24
Q8 1 0.0298 0.0892 0.2068 11.00000 0.05 0.24
Q9 1 0.3485 0.4015 -0.0577 11.00000 0.05 0.24
Q10 1 0.0300 0.3094 0.0487 11.00000 0.05 0.24
Q11 1 0.2001 0.3841 -0.0672 11.00000 0.05 0.23
Q12 1 -0.6513 0.1171 -0.0106 11.00000 0.05 0.23
Q13 1 -0.1084 0.1893 0.0168 11.00000 0.05 0.23
Q14 1 0.7402 0.2489 0.2034 11.00000 0.05 0.22
Q15 1 0.6845 0.4450 -0.0454 11.00000 0.05 0.22
Q16 1 -0.5867 0.1412 -0.0466 11.00000 0.05 0.22
Q17 1 -0.5531 0.2089 -0.1150 11.00000 0.05 0.22
Q18 1 0.2256 0.2612 0.1249 11.00000 0.05 0.22
Q19 1 1.0622 0.2677 0.2057 11.00000 0.05 0.21
Q20 1 0.1138 0.2514 0.1001 11.00000 0.05 0.21

;