# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       akc30@cam.ac.uk
_publ_contact_author_name        'Wei Li'
loop_
_publ_author_name
'Wei Li'
P.Barton
R.Burwood
T.Cheetham

data_1
_database_code_depnum_ccdc_archive 'CCDC 802590'

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C18 H17 Mn N3 O9' 
_chemical_formula_sum 
 'C18 H17 Mn N3 O9' 
_chemical_formula_weight          474.29 
 
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' 
 'Mn'  'Mn'   0.3368   0.7283 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P21
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    10.8736(10) 
_cell_length_b                    8.4288(5) 
_cell_length_c                    11.5942(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  113.764(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      972.53(14) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     4996 
_cell_measurement_theta_min       3.0743
_cell_measurement_theta_max       29.1552
 
_exptl_crystal_description        sheet 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.620 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              486 
_exptl_absorpt_coefficient_mu     0.738 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.876
_exptl_absorpt_correction_T_max   0.964
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(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   'Xcalibur, Eos, Gemini ultra' 
_diffrn_measurement_method        '\w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0
_diffrn_standards_interval_count  0 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             6351 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0469 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.09 
_diffrn_reflns_theta_max          26.50 
_reflns_number_total              6351 
_reflns_number_gt                 5941 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
; 
_computing_cell_refinement        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;  
_computing_data_reduction         
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
; 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.428(16) 
_refine_ls_number_reflns          6351 
_refine_ls_number_parameters      305 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0407 
_refine_ls_R_factor_gt            0.0376 
_refine_ls_wR_factor_ref          0.0987 
_refine_ls_wR_factor_gt           0.0973 
_refine_ls_goodness_of_fit_ref    1.025 
_refine_ls_restrained_S_all       1.025 
_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 
Mn1 Mn -0.14788(4) 1.15111(4) -0.08570(3) 0.01277(10) Uani 1 1 d . . . 
O1 O -0.35931(19) 1.1054(2) -0.15708(18) 0.0171(4) Uani 1 1 d . . . 
O2 O -0.4684(2) 0.8849(3) -0.24885(19) 0.0221(5) Uani 1 1 d . . . 
O3 O -0.06592(17) 0.6658(3) 0.03361(16) 0.0160(4) Uani 1 1 d . . . 
O4 O -0.1205(2) 0.8948(2) -0.06891(18) 0.0167(4) Uani 1 1 d . . . 
O5 O -0.2240(3) 0.5905(3) 0.3666(2) 0.0376(6) Uani 1 1 d . . . 
O6 O -0.3682(3) 0.7552(4) 0.3843(2) 0.0433(7) Uani 1 1 d . . . 
O1W O -0.1967(2) 1.4007(2) -0.0994(2) 0.0210(5) Uani 1 1 d D . . 
O2W O 0.6268(3) 0.5813(3) 0.7222(3) 0.0446(7) Uani 1 1 d D . . 
O3W O 0.4808(3) 0.4669(3) 0.4872(2) 0.0372(6) Uani 1 1 d D . . 
N1 N -0.3054(3) 0.6990(3) 0.3269(2) 0.0251(6) Uani 1 1 d . . . 
N2 N -0.1247(2) 1.1635(4) 0.11863(19) 0.0165(5) Uani 1 1 d . . . 
N3 N -0.1622(2) 1.1328(3) 0.7146(2) 0.0168(5) Uani 1 1 d . . . 
C1 C -0.3685(3) 0.8932(3) -0.0273(3) 0.0165(6) Uani 1 1 d . . . 
C2 C -0.2535(3) 0.8029(3) 0.0380(3) 0.0157(6) Uani 1 1 d . . . 
C3 C -0.2357(3) 0.7353(4) 0.1528(3) 0.0184(6) Uani 1 1 d . . . 
H3 H -0.1601 0.6696 0.1965 0.022 Uiso 1 1 calc R . . 
C4 C -0.3295(3) 0.7652(4) 0.2027(3) 0.0190(6) Uani 1 1 d . . . 
C5 C -0.4419(3) 0.8588(4) 0.1426(3) 0.0215(6) Uani 1 1 d . . . 
H5 H -0.5031 0.8808 0.1802 0.026 Uiso 1 1 calc R . . 
C6 C -0.4614(3) 0.9189(4) 0.0256(3) 0.0200(6) Uani 1 1 d . . . 
H6 H -0.5400 0.9791 -0.0198 0.024 Uiso 1 1 calc R . . 
C7 C -0.3996(3) 0.9666(3) -0.1556(3) 0.0155(6) Uani 1 1 d . . . 
C8 C -0.1400(3) 0.7877(3) -0.0040(2) 0.0150(6) Uani 1 1 d . . . 
C9 C -0.0226(3) 1.1079(3) 0.2207(3) 0.0191(6) Uani 1 1 d . . . 
H9 H 0.0564 1.0737 0.2119 0.023 Uiso 1 1 calc R . . 
C10 C -0.0265(3) 1.0979(4) 0.3377(3) 0.0200(6) Uani 1 1 d . . . 
H10 H 0.0485 1.0574 0.4073 0.024 Uiso 1 1 calc R . . 
C11 C -0.1406(3) 1.1475(4) 0.3536(2) 0.0152(5) Uani 1 1 d . . . 
C12 C -0.2454(3) 1.2109(4) 0.2488(3) 0.0185(6) Uani 1 1 d . . . 
H12 H -0.3240 1.2507 0.2556 0.022 Uiso 1 1 calc R . . 
C13 C -0.2328(3) 1.2148(4) 0.1351(3) 0.0179(6) Uani 1 1 d . . . 
H13 H -0.3055 1.2567 0.0641 0.021 Uiso 1 1 calc R . . 
C14 C -0.2316(3) 1.2395(4) 0.6271(3) 0.0201(6) Uani 1 1 d . . . 
H14 H -0.2856 1.3140 0.6471 0.024 Uiso 1 1 calc R . . 
C15 C -0.2288(3) 1.2471(4) 0.5091(3) 0.0187(6) Uani 1 1 d . . . 
H15 H -0.2798 1.3251 0.4500 0.022 Uiso 1 1 calc R . . 
C16 C -0.1507(3) 1.1395(4) 0.4781(2) 0.0161(5) Uani 1 1 d . . . 
C17 C -0.0830(3) 1.0242(4) 0.5664(3) 0.0205(6) Uani 1 1 d . . . 
H17 H -0.0320 0.9449 0.5472 0.025 Uiso 1 1 calc R . . 
C18 C -0.0908(3) 1.0262(4) 0.6820(3) 0.0206(6) Uani 1 1 d . . . 
H18 H -0.0429 0.9475 0.7420 0.025 Uiso 1 1 calc R . . 
H1A H -0.253(3) 1.455(4) -0.159(3) 0.041(12) Uiso 1 1 d D . . 
H2A H 0.576(4) 0.543(6) 0.651(2) 0.064(15) Uiso 1 1 d D . . 
H3A H 0.481(4) 0.456(5) 0.4146(18) 0.036(11) Uiso 1 1 d D . . 
H1B H -0.141(3) 1.466(4) -0.048(3) 0.052(14) Uiso 1 1 d D . . 
H2B H 0.593(5) 0.669(3) 0.730(5) 0.076(17) Uiso 1 1 d D . . 
H3B H 0.425(6) 0.396(7) 0.488(8) 0.15(3) Uiso 1 1 d 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 
Mn1 0.01500(17) 0.01358(17) 0.01076(17) -0.00002(19) 0.00626(14) -0.00029(19) 
O1 0.0150(9) 0.0171(11) 0.0178(9) 0.0036(7) 0.0053(8) 0.0017(7) 
O2 0.0213(11) 0.0236(11) 0.0188(11) -0.0004(9) 0.0052(9) -0.0029(9) 
O3 0.0153(8) 0.0146(9) 0.0177(8) 0.0021(9) 0.0061(6) 0.0035(9) 
O4 0.0205(10) 0.0147(10) 0.0180(10) 0.0020(8) 0.0111(9) 0.0015(8) 
O5 0.0390(15) 0.0473(15) 0.0294(13) 0.0179(11) 0.0170(11) 0.0075(12) 
O6 0.0534(17) 0.0604(18) 0.0269(13) 0.0013(13) 0.0275(13) 0.0048(13) 
O1W 0.0223(11) 0.0154(11) 0.0190(11) -0.0011(9) 0.0016(9) 0.0001(10) 
O2W 0.0591(19) 0.0288(13) 0.0273(14) -0.0037(12) -0.0018(13) 0.0170(14) 
O3W 0.0454(16) 0.0469(16) 0.0191(12) -0.0045(11) 0.0128(12) -0.0035(13) 
N1 0.0252(13) 0.0341(16) 0.0195(12) 0.0008(11) 0.0125(11) -0.0081(12) 
N2 0.0172(11) 0.0183(12) 0.0149(10) -0.0018(12) 0.0074(8) 0.0003(12) 
N3 0.0173(11) 0.0190(13) 0.0140(10) 0.0004(11) 0.0063(9) 0.0011(11) 
C1 0.0155(14) 0.0153(14) 0.0199(15) -0.0032(11) 0.0082(12) -0.0046(11) 
C2 0.0182(14) 0.0147(13) 0.0142(13) -0.0028(11) 0.0066(11) -0.0052(11) 
C3 0.0190(15) 0.0177(14) 0.0178(14) 0.0005(12) 0.0068(11) -0.0028(12) 
C4 0.0227(16) 0.0218(15) 0.0159(14) 0.0004(11) 0.0113(12) -0.0061(12) 
C5 0.0210(15) 0.0232(16) 0.0255(16) -0.0033(13) 0.0148(13) -0.0042(13) 
C6 0.0194(15) 0.0190(15) 0.0246(16) 0.0001(13) 0.0119(13) -0.0005(13) 
C7 0.0099(12) 0.0195(14) 0.0169(14) 0.0001(11) 0.0050(11) 0.0023(11) 
C8 0.0142(14) 0.0167(14) 0.0128(13) -0.0046(10) 0.0041(11) -0.0029(11) 
C9 0.0193(13) 0.0235(16) 0.0168(13) -0.0005(11) 0.0098(11) 0.0033(11) 
C10 0.0206(14) 0.0232(15) 0.0156(14) 0.0019(11) 0.0066(11) 0.0026(12) 
C11 0.0200(12) 0.0145(11) 0.0126(11) 0.0011(15) 0.0079(10) -0.0002(14) 
C12 0.0159(14) 0.0237(14) 0.0186(14) -0.0034(11) 0.0100(12) 0.0009(11) 
C13 0.0186(14) 0.0219(14) 0.0125(12) 0.0008(11) 0.0056(10) 0.0033(12) 
C14 0.0232(16) 0.0211(16) 0.0171(14) 0.0029(12) 0.0094(12) 0.0067(13) 
C15 0.0205(15) 0.0214(15) 0.0141(13) 0.0023(12) 0.0067(12) 0.0039(12) 
C16 0.0182(11) 0.0194(14) 0.0117(12) -0.0026(13) 0.0070(10) -0.0030(13) 
C17 0.0233(15) 0.0218(15) 0.0171(14) 0.0010(12) 0.0088(12) 0.0069(13) 
C18 0.0269(16) 0.0209(14) 0.0142(14) 0.0031(12) 0.0084(12) 0.0053(14) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Mn1 O1 2.1413(19) . ? 
Mn1 O3 2.1571(18) 2 ? 
Mn1 O1W 2.160(2) . ? 
Mn1 O4 2.179(2) . ? 
Mn1 N3 2.263(2) 1_554 ? 
Mn1 N2 2.281(2) . ? 
O1 C7 1.252(3) . ? 
O2 C7 1.245(3) . ? 
O3 C8 1.269(4) . ? 
O3 Mn1 2.1571(18) 2_545 ? 
O4 C8 1.247(3) . ? 
O5 N1 1.226(4) . ? 
O6 N1 1.226(3) . ? 
O1W H1A 0.851(10) . ? 
O1W H1B 0.855(10) . ? 
O2W H2A 0.847(10) . ? 
O2W H2B 0.848(10) . ? 
O3W H3A 0.848(10) . ? 
O3W H3B 0.849(10) . ? 
N1 C4 1.467(4) . ? 
N2 C13 1.337(3) . ? 
N2 C9 1.339(4) . ? 
N3 C18 1.337(4) . ? 
N3 C14 1.338(4) . ? 
N3 Mn1 2.263(2) 1_556 ? 
C1 C6 1.395(4) . ? 
C1 C2 1.397(4) . ? 
C1 C7 1.518(4) . ? 
C2 C3 1.387(4) . ? 
C2 C8 1.504(4) . ? 
C3 C4 1.384(4) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.384(4) . ? 
C5 C6 1.382(4) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C9 C10 1.377(4) . ? 
C9 H9 0.9500 . ? 
C10 C11 1.390(4) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.394(4) . ? 
C11 C16 1.493(3) . ? 
C12 C13 1.380(4) . ? 
C12 H12 0.9500 . ? 
C13 H13 0.9500 . ? 
C14 C15 1.381(4) . ? 
C14 H14 0.9500 . ? 
C15 C16 1.385(4) . ? 
C15 H15 0.9500 . ? 
C16 C17 1.388(4) . ? 
C17 C18 1.378(4) . ? 
C17 H17 0.9500 . ? 
C18 H18 0.9500 . ? 
 
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 
O1 Mn1 O3 170.62(8) . 2 ? 
O1 Mn1 O1W 87.31(8) . . ? 
O3 Mn1 O1W 99.78(9) 2 . ? 
O1 Mn1 O4 86.74(8) . . ? 
O3 Mn1 O4 86.47(8) 2 . ? 
O1W Mn1 O4 173.27(9) . . ? 
O1 Mn1 N3 88.39(8) . 1_554 ? 
O3 Mn1 N3 84.97(8) 2 1_554 ? 
O1W Mn1 N3 94.45(9) . 1_554 ? 
O4 Mn1 N3 88.53(9) . 1_554 ? 
O1 Mn1 N2 93.55(8) . . ? 
O3 Mn1 N2 92.91(7) 2 . ? 
O1W Mn1 N2 87.30(9) . . ? 
O4 Mn1 N2 89.92(9) . . ? 
N3 Mn1 N2 177.45(9) 1_554 . ? 
C7 O1 Mn1 119.34(17) . . ? 
C8 O3 Mn1 127.25(19) . 2_545 ? 
C8 O4 Mn1 136.19(18) . . ? 
Mn1 O1W H1A 131(3) . . ? 
Mn1 O1W H1B 120(3) . . ? 
H1A O1W H1B 107(4) . . ? 
H2A O2W H2B 108(5) . . ? 
H3A O3W H3B 103(6) . . ? 
O6 N1 O5 124.1(3) . . ? 
O6 N1 C4 117.9(3) . . ? 
O5 N1 C4 118.0(2) . . ? 
C13 N2 C9 116.8(2) . . ? 
C13 N2 Mn1 115.29(17) . . ? 
C9 N2 Mn1 127.40(18) . . ? 
C18 N3 C14 116.9(2) . . ? 
C18 N3 Mn1 121.74(19) . 1_556 ? 
C14 N3 Mn1 121.0(2) . 1_556 ? 
C6 C1 C2 119.6(3) . . ? 
C6 C1 C7 116.9(3) . . ? 
C2 C1 C7 123.4(2) . . ? 
C3 C2 C1 119.5(3) . . ? 
C3 C2 C8 117.4(3) . . ? 
C1 C2 C8 122.9(2) . . ? 
C4 C3 C2 119.0(3) . . ? 
C4 C3 H3 120.5 . . ? 
C2 C3 H3 120.5 . . ? 
C5 C4 C3 122.9(3) . . ? 
C5 C4 N1 118.9(3) . . ? 
C3 C4 N1 118.1(3) . . ? 
C6 C5 C4 117.3(3) . . ? 
C6 C5 H5 121.4 . . ? 
C4 C5 H5 121.4 . . ? 
C5 C6 C1 121.5(3) . . ? 
C5 C6 H6 119.2 . . ? 
C1 C6 H6 119.2 . . ? 
O2 C7 O1 126.6(3) . . ? 
O2 C7 C1 116.4(3) . . ? 
O1 C7 C1 116.9(2) . . ? 
O4 C8 O3 123.7(3) . . ? 
O4 C8 C2 119.7(2) . . ? 
O3 C8 C2 116.6(2) . . ? 
N2 C9 C10 123.3(3) . . ? 
N2 C9 H9 118.4 . . ? 
C10 C9 H9 118.4 . . ? 
C9 C10 C11 119.7(3) . . ? 
C9 C10 H10 120.2 . . ? 
C11 C10 H10 120.2 . . ? 
C10 C11 C12 117.4(2) . . ? 
C10 C11 C16 122.1(2) . . ? 
C12 C11 C16 120.5(2) . . ? 
C13 C12 C11 118.7(3) . . ? 
C13 C12 H12 120.6 . . ? 
C11 C12 H12 120.6 . . ? 
N2 C13 C12 124.1(3) . . ? 
N2 C13 H13 118.0 . . ? 
C12 C13 H13 118.0 . . ? 
N3 C14 C15 123.5(3) . . ? 
N3 C14 H14 118.3 . . ? 
C15 C14 H14 118.3 . . ? 
C14 C15 C16 119.1(3) . . ? 
C14 C15 H15 120.4 . . ? 
C16 C15 H15 120.4 . . ? 
C15 C16 C17 117.8(2) . . ? 
C15 C16 C11 120.9(3) . . ? 
C17 C16 C11 121.4(3) . . ? 
C18 C17 C16 119.1(3) . . ? 
C18 C17 H17 120.5 . . ? 
C16 C17 H17 120.5 . . ? 
N3 C18 C17 123.6(3) . . ? 
N3 C18 H18 118.2 . . ? 
C17 C18 H18 118.2 . . ? 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              26.50 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.344 
_refine_diff_density_min   -0.203 
_refine_diff_density_rms    0.051 

# Attachment '- Zn.cif'

data_Zn
_database_code_depnum_ccdc_archive 'CCDC 802591'

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C18 H17 N3 O9 Zn' 
_chemical_formula_sum 
 'C18 H17 N3 O9 Zn' 
_chemical_formula_weight          484.72 
 
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' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P21
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    10.8701(9) 
_cell_length_b                    8.4038(5) 
_cell_length_c                    11.3838(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  112.816(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      958.54(13) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     6263 
_cell_measurement_theta_min       3.0187
_cell_measurement_theta_max       29.2325
 
_exptl_crystal_description        sheet 
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.679 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              496 
_exptl_absorpt_coefficient_mu     1.341 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.7752 
_exptl_absorpt_correction_T_max   0.9360 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(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   'Xcalibur, Eos, Gemini ultra' 
_diffrn_measurement_method        '\w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  0 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             5770 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0525 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          3.11 
_diffrn_reflns_theta_max          25.40 
_reflns_number_total              5770 
_reflns_number_gt                 5354 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;  
_computing_cell_refinement        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;  
_computing_data_reduction         
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34 (release 07-07-2010 CrysAlis171 .NET)
(compiled Jul  7 2010,16:04:54)
;     
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.2273P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.567(13) 
_refine_ls_number_reflns          5770 
_refine_ls_number_parameters      305 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0411 
_refine_ls_R_factor_gt            0.0380 
_refine_ls_wR_factor_ref          0.1033 
_refine_ls_wR_factor_gt           0.1023 
_refine_ls_goodness_of_fit_ref    1.065 
_refine_ls_restrained_S_all       1.065 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 
Zn1 Zn -0.14611(4) 1.15141(4) -0.08279(4) 0.00986(11) Uani 1 1 d . . . 
O1 O -0.3512(3) 1.1083(3) -0.1560(3) 0.0131(7) Uani 1 1 d . . . 
O2 O -0.4669(3) 0.8916(4) -0.2485(3) 0.0199(7) Uani 1 1 d . . . 
O3 O -0.0604(2) 0.6663(4) 0.0333(2) 0.0118(6) Uani 1 1 d . . . 
O4 O -0.1126(3) 0.8994(3) -0.0673(3) 0.0122(7) Uani 1 1 d . . . 
O5 O -0.2191(4) 0.5831(4) 0.3716(3) 0.0318(8) Uani 1 1 d . . . 
O6 O -0.3700(4) 0.7381(5) 0.3903(3) 0.0374(9) Uani 1 1 d . . . 
O1W O -0.1906(4) 1.3954(4) -0.0953(3) 0.0175(7) Uani 1 1 d D . . 
O2W O 0.6292(4) 0.5807(5) 0.7296(4) 0.0383(11) Uani 1 1 d D . . 
O3W O 0.4818(4) 0.4706(5) 0.4925(4) 0.0345(9) Uani 1 1 d D . . 
N1 N -0.3034(4) 0.6891(4) 0.3318(3) 0.0202(10) Uani 1 1 d . . . 
N2 N -0.1288(3) 1.1627(6) 0.1121(3) 0.0130(7) Uani 1 1 d . . . 
N3 N -0.1600(3) 1.1348(5) 0.7238(3) 0.0143(8) Uani 1 1 d . . . 
C1 C -0.3634(4) 0.8932(5) -0.0249(4) 0.0130(9) Uani 1 1 d . . . 
C2 C -0.2485(4) 0.8020(5) 0.0394(4) 0.0109(8) Uani 1 1 d . . . 
C3 C -0.2324(4) 0.7315(5) 0.1550(4) 0.0148(9) Uani 1 1 d . . . 
H3 H -0.1572 0.6659 0.1982 0.018 Uiso 1 1 calc R . . 
C4 C -0.3268(4) 0.7579(5) 0.2067(4) 0.0164(9) Uani 1 1 d . . . 
C5 C -0.4383(5) 0.8513(5) 0.1470(4) 0.0180(10) Uani 1 1 d . . . 
H5 H -0.5002 0.8711 0.1856 0.022 Uiso 1 1 calc R . . 
C6 C -0.4568(4) 0.9153(5) 0.0294(4) 0.0148(9) Uani 1 1 d . . . 
H6 H -0.5349 0.9756 -0.0152 0.018 Uiso 1 1 calc R . . 
C7 C -0.3941(4) 0.9696(5) -0.1545(4) 0.0123(9) Uani 1 1 d . . . 
C8 C -0.1333(4) 0.7899(5) -0.0038(4) 0.0111(9) Uani 1 1 d . . . 
C9 C -0.0267(4) 1.1057(5) 0.2139(4) 0.0152(10) Uani 1 1 d . . . 
H9 H 0.0512 1.0706 0.2030 0.018 Uiso 1 1 calc R . . 
C10 C -0.0303(4) 1.0959(5) 0.3340(4) 0.0160(10) Uani 1 1 d . . . 
H10 H 0.0439 1.0543 0.4033 0.019 Uiso 1 1 calc R . . 
C11 C -0.1432(4) 1.1476(7) 0.3525(3) 0.0134(7) Uani 1 1 d . . . 
C12 C -0.2473(4) 1.2120(5) 0.2476(4) 0.0147(9) Uani 1 1 d . . . 
H12 H -0.3247 1.2530 0.2566 0.018 Uiso 1 1 calc R . . 
C13 C -0.2366(4) 1.2156(5) 0.1312(4) 0.0151(9) Uani 1 1 d . . . 
H13 H -0.3091 1.2576 0.0604 0.018 Uiso 1 1 calc R . . 
C14 C -0.2318(5) 1.2390(5) 0.6350(4) 0.0166(10) Uani 1 1 d . . . 
H14 H -0.2866 1.3122 0.6561 0.020 Uiso 1 1 calc R . . 
C15 C -0.2307(5) 1.2460(5) 0.5141(4) 0.0157(10) Uani 1 1 d . . . 
H15 H -0.2827 1.3236 0.4549 0.019 Uiso 1 1 calc R . . 
C16 C -0.1534(4) 1.1393(7) 0.4795(4) 0.0139(8) Uani 1 1 d . . . 
C17 C -0.0837(4) 1.0245(5) 0.5698(4) 0.0164(9) Uani 1 1 d . . . 
H17 H -0.0331 0.9452 0.5490 0.020 Uiso 1 1 calc R . . 
C18 C -0.0885(4) 1.0265(5) 0.6888(4) 0.0161(9) Uani 1 1 d . . . 
H18 H -0.0394 0.9484 0.7491 0.019 Uiso 1 1 calc R . . 
H1A H -0.251(4) 1.447(6) -0.154(4) 0.031(16) Uiso 1 1 d D . . 
H2A H 0.584(6) 0.546(8) 0.655(3) 0.06(2) Uiso 1 1 d D . . 
H3A H 0.475(5) 0.457(6) 0.417(2) 0.031(15) Uiso 1 1 d D . . 
H1B H -0.140(6) 1.453(7) -0.034(5) 0.07(2) Uiso 1 1 d D . . 
H2B H 0.597(6) 0.673(3) 0.727(6) 0.05(2) Uiso 1 1 d D . . 
H3B H 0.436(8) 0.400(8) 0.510(10) 0.13(4) Uiso 1 1 d 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 
Zn1 0.0135(2) 0.01035(18) 0.0069(2) 0.0002(3) 0.00521(17) -0.0003(2) 
O1 0.0156(14) 0.0103(17) 0.0119(14) 0.0020(10) 0.0037(12) -0.0002(10) 
O2 0.0226(18) 0.0199(16) 0.0136(17) -0.0007(13) 0.0030(14) -0.0028(13) 
O3 0.0131(12) 0.0105(14) 0.0119(12) 0.0010(14) 0.0050(10) 0.0031(15) 
O4 0.0183(17) 0.0105(14) 0.0118(17) 0.0017(13) 0.0100(15) 0.0012(13) 
O5 0.033(2) 0.0395(19) 0.024(2) 0.0168(16) 0.0123(17) 0.0071(16) 
O6 0.051(3) 0.049(2) 0.024(2) 0.0033(18) 0.029(2) 0.0020(19) 
O1W 0.0219(18) 0.0142(16) 0.0118(18) -0.0016(14) 0.0016(15) -0.0009(15) 
O2W 0.051(3) 0.0237(18) 0.021(2) -0.0026(17) -0.007(2) 0.0145(19) 
O3W 0.046(2) 0.044(2) 0.0134(19) -0.0028(17) 0.0111(18) -0.0075(19) 
N1 0.0192(19) 0.029(3) 0.0156(19) 0.0004(15) 0.0106(17) -0.0074(16) 
N2 0.0149(16) 0.0115(17) 0.0129(16) 0.002(2) 0.0058(14) -0.0007(19) 
N3 0.0153(16) 0.018(2) 0.0091(15) 0.0000(19) 0.0041(14) 0.0027(18) 
C1 0.016(2) 0.0094(19) 0.014(2) -0.0033(16) 0.0050(18) -0.0050(17) 
C2 0.014(2) 0.0089(19) 0.012(2) -0.0035(16) 0.0068(17) -0.0049(16) 
C3 0.014(2) 0.013(2) 0.017(2) 0.0011(18) 0.0059(19) -0.0010(18) 
C4 0.021(2) 0.017(2) 0.011(2) -0.0004(18) 0.0063(19) -0.0051(18) 
C5 0.021(2) 0.018(2) 0.020(3) -0.0043(19) 0.013(2) -0.0076(19) 
C6 0.015(2) 0.013(2) 0.017(2) -0.0004(18) 0.0071(18) -0.0009(19) 
C7 0.0053(19) 0.016(2) 0.016(2) -0.0015(17) 0.0046(18) -0.0003(17) 
C8 0.013(2) 0.013(2) 0.006(2) -0.0052(16) 0.0019(17) -0.0037(17) 
C9 0.014(2) 0.018(2) 0.015(2) -0.0012(16) 0.0078(17) 0.0036(16) 
C10 0.019(2) 0.018(2) 0.008(2) 0.0000(16) 0.0025(18) 0.0012(17) 
C11 0.0201(18) 0.0098(16) 0.0111(18) -0.001(3) 0.0068(16) -0.002(2) 
C12 0.015(2) 0.020(2) 0.011(2) -0.0021(17) 0.0071(19) 0.0009(17) 
C13 0.018(2) 0.018(2) 0.010(2) 0.0055(17) 0.0056(18) 0.0052(17) 
C14 0.023(3) 0.015(2) 0.013(2) 0.0001(18) 0.009(2) 0.0076(19) 
C15 0.021(2) 0.016(2) 0.011(2) 0.0030(18) 0.007(2) 0.0055(18) 
C16 0.0166(18) 0.016(2) 0.0082(18) -0.002(2) 0.0036(17) -0.002(2) 
C17 0.020(2) 0.016(2) 0.014(2) 0.0005(19) 0.0088(19) 0.0045(19) 
C18 0.019(2) 0.016(2) 0.013(2) 0.0014(19) 0.0057(19) 0.0010(19) 
 
_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 
Zn1 O1 2.087(3) . ? 
Zn1 O3 2.095(3) 2 ? 
Zn1 O1W 2.098(3) . ? 
Zn1 O4 2.145(3) . ? 
Zn1 N3 2.152(3) 1_554 ? 
Zn1 N2 2.155(3) . ? 
O1 C7 1.258(5) . ? 
O2 C7 1.242(5) . ? 
O3 C8 1.275(5) . ? 
O3 Zn1 2.095(3) 2_545 ? 
O4 C8 1.243(5) . ? 
O5 N1 1.231(5) . ? 
O6 N1 1.229(5) . ? 
O1W H1A 0.851(10) . ? 
O1W H1B 0.851(10) . ? 
O2W H2A 0.847(10) . ? 
O2W H2B 0.845(10) . ? 
O3W H3A 0.848(10) . ? 
O3W H3B 0.848(10) . ? 
N1 C4 1.465(6) . ? 
N2 C9 1.344(5) . ? 
N2 C13 1.347(5) . ? 
N3 C14 1.336(6) . ? 
N3 C18 1.354(6) . ? 
N3 Zn1 2.152(3) 1_556 ? 
C1 C6 1.391(6) . ? 
C1 C2 1.405(6) . ? 
C1 C7 1.522(6) . ? 
C2 C3 1.391(6) . ? 
C2 C8 1.516(6) . ? 
C3 C4 1.385(6) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.381(6) . ? 
C5 C6 1.383(6) . ? 
C5 H5 0.9500 . ? 
C6 H6 0.9500 . ? 
C9 C10 1.385(6) . ? 
C9 H9 0.9500 . ? 
C10 C11 1.393(6) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.398(6) . ? 
C11 C16 1.494(4) . ? 
C12 C13 1.374(6) . ? 
C12 H12 0.9500 . ? 
C13 H13 0.9500 . ? 
C14 C15 1.383(6) . ? 
C14 H14 0.9500 . ? 
C15 C16 1.386(7) . ? 
C15 H15 0.9500 . ? 
C16 C17 1.399(7) . ? 
C17 C18 1.376(6) . ? 
C17 H17 0.9500 . ? 
C18 H18 0.9500 . ? 
 
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 
O1 Zn1 O3 170.00(11) . 2 ? 
O1 Zn1 O1W 87.70(12) . . ? 
O3 Zn1 O1W 98.91(14) 2 . ? 
O1 Zn1 O4 89.01(11) . . ? 
O3 Zn1 O4 84.64(13) 2 . ? 
O1W Zn1 O4 176.09(15) . . ? 
O1 Zn1 N3 86.56(12) . 1_554 ? 
O3 Zn1 N3 85.51(12) 2 1_554 ? 
O1W Zn1 N3 94.06(15) . 1_554 ? 
O4 Zn1 N3 87.85(14) . 1_554 ? 
O1 Zn1 N2 94.12(12) . . ? 
O3 Zn1 N2 93.68(11) 2 . ? 
O1W Zn1 N2 87.29(15) . . ? 
O4 Zn1 N2 90.84(15) . . ? 
N3 Zn1 N2 178.52(18) 1_554 . ? 
C7 O1 Zn1 120.0(3) . . ? 
C8 O3 Zn1 126.9(3) . 2_545 ? 
C8 O4 Zn1 135.7(3) . . ? 
Zn1 O1W H1A 129(4) . . ? 
Zn1 O1W H1B 116(5) . . ? 
H1A O1W H1B 114(6) . . ? 
H2A O2W H2B 102(6) . . ? 
H3A O3W H3B 109(8) . . ? 
O6 N1 O5 123.6(4) . . ? 
O6 N1 C4 118.5(4) . . ? 
O5 N1 C4 117.8(4) . . ? 
C9 N2 C13 117.2(3) . . ? 
C9 N2 Zn1 125.8(3) . . ? 
C13 N2 Zn1 116.6(3) . . ? 
C14 N3 C18 116.8(3) . . ? 
C14 N3 Zn1 121.4(3) . 1_556 ? 
C18 N3 Zn1 121.6(3) . 1_556 ? 
C6 C1 C2 119.7(4) . . ? 
C6 C1 C7 116.8(4) . . ? 
C2 C1 C7 123.5(4) . . ? 
C3 C2 C1 119.0(4) . . ? 
C3 C2 C8 117.5(4) . . ? 
C1 C2 C8 123.1(4) . . ? 
C4 C3 C2 119.5(4) . . ? 
C4 C3 H3 120.3 . . ? 
C2 C3 H3 120.3 . . ? 
C5 C4 C3 122.4(4) . . ? 
C5 C4 N1 119.4(4) . . ? 
C3 C4 N1 118.2(4) . . ? 
C4 C5 C6 117.9(4) . . ? 
C4 C5 H5 121.1 . . ? 
C6 C5 H5 121.1 . . ? 
C5 C6 C1 121.4(4) . . ? 
C5 C6 H6 119.3 . . ? 
C1 C6 H6 119.3 . . ? 
O2 C7 O1 126.3(4) . . ? 
O2 C7 C1 116.1(4) . . ? 
O1 C7 C1 117.4(4) . . ? 
O4 C8 O3 124.5(4) . . ? 
O4 C8 C2 119.8(4) . . ? 
O3 C8 C2 115.6(4) . . ? 
N2 C9 C10 122.8(4) . . ? 
N2 C9 H9 118.6 . . ? 
C10 C9 H9 118.6 . . ? 
C9 C10 C11 119.6(4) . . ? 
C9 C10 H10 120.2 . . ? 
C11 C10 H10 120.2 . . ? 
C10 C11 C12 117.4(4) . . ? 
C10 C11 C16 122.2(4) . . ? 
C12 C11 C16 120.4(4) . . ? 
C13 C12 C11 119.3(4) . . ? 
C13 C12 H12 120.4 . . ? 
C11 C12 H12 120.4 . . ? 
N2 C13 C12 123.6(4) . . ? 
N2 C13 H13 118.2 . . ? 
C12 C13 H13 118.2 . . ? 
N3 C14 C15 123.6(4) . . ? 
N3 C14 H14 118.2 . . ? 
C15 C14 H14 118.2 . . ? 
C14 C15 C16 119.7(4) . . ? 
C14 C15 H15 120.2 . . ? 
C16 C15 H15 120.2 . . ? 
C15 C16 C17 117.0(4) . . ? 
C15 C16 C11 121.7(4) . . ? 
C17 C16 C11 121.4(4) . . ? 
C18 C17 C16 119.9(4) . . ? 
C18 C17 H17 120.1 . . ? 
C16 C17 H17 120.1 . . ? 
N3 C18 C17 122.9(4) . . ? 
N3 C18 H18 118.5 . . ? 
C17 C18 H18 118.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              25.40 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.506 
_refine_diff_density_min   -0.273 
_refine_diff_density_rms    0.058