# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Sutter, Jean-Pascal'
_publ_contact_author_email       sutter@lcc-toulouse.fr

_publ_section_title              
;
Tubular crystals growth
for a nanoporous hydrogen-bonded metal-organic framework
;
loop_
_publ_author_name
G.Mouchaham
N.Roques
A.Kaiba
P.Guionneau
J.-P.Sutter

# Attachment '- Cmpd_1-250K.cif'

data_Compd-1
_database_code_depnum_ccdc_archive 'CCDC 768079'
#TrackingRef '- Cmpd_1-250K.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H13.50 N4 O8.75 Zr0.50'
_chemical_formula_weight         447.42

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnc2

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

_cell_length_a                   11.0239(10)
_cell_length_b                   17.0540(10)
_cell_length_c                   9.7540(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1833.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    18135
_cell_measurement_theta_min      0.41
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             910
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9620
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
?
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            14865
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         27.45
_reflns_number_total             4174
_reflns_number_gt                3062
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'

_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^)+(0.0479P)^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    noref
_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   -0.06(4)
_refine_ls_number_reflns         4174
_refine_ls_number_parameters     304
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.006
_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
Zr01 Zr 1.0000 1.0000 0.69784(6) 0.03526(11) Uani 1 2 d S . .
O4 O 0.7856(3) 1.06966(15) 1.0389(3) 0.0721(9) Uani 1 1 d . . .
O3 O 0.9067(2) 1.20148(14) 0.9365(3) 0.0555(6) Uani 1 1 d . . .
C2 C 0.8511(3) 1.0644(2) 0.9361(4) 0.0508(9) Uani 1 1 d . . .
N1 N 0.9602(3) 0.79774(18) 1.2684(3) 0.0541(8) Uani 1 1 d . . .
H1 H 1.0115 0.7732 1.3210 0.065 Uiso 1 1 calc R . .
N4 N 0.2903(3) 0.70658(17) 0.6501(3) 0.0579(8) Uani 1 1 d . . .
H4 H 0.2456 0.6692 0.6164 0.069 Uiso 1 1 calc R . .
O5 O 0.9132(2) 1.06777(12) 0.5381(2) 0.0474(5) Uani 1 1 d . . .
C21 C 0.3815(4) 0.6962(2) 0.7338(4) 0.0675(12) Uani 1 1 d . . .
H21 H 0.4095 0.6477 0.7668 0.081 Uiso 1 1 calc R . .
N3 N 0.4282(3) 0.76631(18) 0.7645(3) 0.0574(8) Uani 1 1 d . A .
O1 O 0.98871(18) 1.12098(13) 0.7822(2) 0.0437(5) Uani 1 1 d . . .
C18 C 0.8573(3) 0.8920(2) 1.1698(4) 0.0609(11) Uani 1 1 d . . .
H18 H 0.8275 0.9415 1.1441 0.073 Uiso 1 1 calc R . .
C17 C 0.9467(4) 0.8772(2) 1.2599(4) 0.0655(10) Uani 1 1 d . . .
H17 H 0.9918 0.9149 1.3084 0.079 Uiso 1 1 calc R . .
C19 C 0.3618(3) 0.8223(2) 0.6972(5) 0.0661(10) Uani 1 1 d . . .
H19 H 0.3736 0.8768 0.7014 0.079 Uiso 1 1 calc R . .
C16 C 0.8830(3) 0.76450(19) 1.1842(4) 0.0495(8) Uani 1 1 d . . .
H16 H 0.8750 0.7102 1.1698 0.059 Uiso 1 1 calc R . .
N2 N 0.8176(2) 0.81980(17) 1.1223(3) 0.0475(7) Uani 1 1 d . . .
O2 O 0.8682(2) 1.00279(12) 0.8665(3) 0.0522(6) Uani 1 1 d . . .
C1 C 0.9202(3) 1.13609(18) 0.8834(3) 0.0415(7) Uani 1 1 d . . .
C12 C 0.5652(12) 0.7201(9) 0.9399(12) 0.047(3) Uani 0.50 1 d P A 1
H12 H 0.5238 0.6719 0.9367 0.056 Uiso 0.50 1 calc PR A 1
C20 C 0.2756(4) 0.7841(2) 0.6234(4) 0.0620(10) Uani 1 1 d . . .
H20 H 0.2174 0.8069 0.5653 0.074 Uiso 1 1 calc R . .
O6 O 0.8425(2) 0.93365(13) 0.6214(3) 0.0525(6) Uani 1 1 d . . .
C11 C 0.6602(10) 0.7297(7) 1.0283(13) 0.049(3) Uani 0.50 1 d P A 1
H11 H 0.6857 0.6890 1.0864 0.059 Uiso 0.50 1 calc PR A 1
O8 O 0.6689(3) 0.94154(15) 0.5052(4) 0.0828(10) Uani 1 1 d . . .
O7 O 0.7655(3) 1.07558(17) 0.3845(3) 0.0743(9) Uani 1 1 d . . .
C4 C 0.7692(3) 0.9663(2) 0.5379(4) 0.0523(9) Uani 1 1 d . . .
C3 C 0.8169(3) 1.0431(2) 0.4783(4) 0.0472(9) Uani 1 1 d . . .
C14B C 0.5410(8) 0.8592(4) 0.9225(10) 0.066(2) Uani 0.50 1 d P A 2
H14B H 0.4843 0.8990 0.9045 0.080 Uiso 0.50 1 calc PR A 2
C15B C 0.6371(8) 0.8719(4) 1.0120(10) 0.064(2) Uani 0.50 1 d P A 2
H15B H 0.6477 0.9196 1.0587 0.077 Uiso 0.50 1 calc PR A 2
C12B C 0.6026(13) 0.7259(9) 0.8908(13) 0.057(3) Uani 0.50 1 d P A 2
H12B H 0.5910 0.6750 0.8564 0.068 Uiso 0.50 1 calc PR A 2
C14 C 0.6084(8) 0.8365(5) 0.8231(9) 0.066(2) Uani 0.50 1 d P A 1
H14 H 0.6009 0.8646 0.7405 0.079 Uiso 0.50 1 calc PR A 1
C15 C 0.7016(8) 0.8526(4) 0.9135(9) 0.061(2) Uani 0.50 1 d P A 1
H15 H 0.7530 0.8955 0.8969 0.073 Uiso 0.50 1 calc PR A 1
C11B C 0.7001(9) 0.7407(7) 0.9808(11) 0.050(3) Uani 0.50 1 d P A 2
H11B H 0.7514 0.6989 1.0051 0.060 Uiso 0.50 1 calc PR A 2
C10 C 0.7206(3) 0.8061(2) 1.0287(4) 0.0500(9) Uani 1 1 d . . .
C13 C 0.5297(3) 0.7806(2) 0.8553(4) 0.0576(10) Uani 1 1 d . . .
O10 O 0.5000 1.0000 0.3034(6) 0.137(3) Uani 1 2 d S . .
O11 O 0.5000 1.0000 0.7016(17) 0.100(3) Uani 0.50 2 d SPD . .
H100 H 0.4306 1.0004 0.3678 0.100 Uiso 1 1 d . . .
H110 H 0.5544 1.0149 0.7785 0.100 Uiso 0.50 1 d PD . .

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
Zr01 0.03294(18) 0.03358(18) 0.03927(18) 0.000 0.000 -0.00200(17)
O4 0.083(2) 0.0508(17) 0.0828(18) 0.0100(14) 0.0488(17) 0.0086(14)
O3 0.0625(16) 0.0424(14) 0.0617(14) -0.0011(11) 0.0275(13) -0.0002(11)
C2 0.048(2) 0.044(2) 0.060(2) 0.0134(18) 0.0161(18) 0.0113(17)
N1 0.0534(18) 0.0488(18) 0.0600(17) 0.0044(15) -0.0251(15) -0.0006(14)
N4 0.0527(18) 0.0506(18) 0.070(2) 0.0084(14) -0.0242(15) -0.0170(14)
O5 0.0461(14) 0.0432(13) 0.0530(13) 0.0091(11) -0.0030(11) -0.0004(10)
C21 0.059(2) 0.057(2) 0.087(3) 0.028(2) -0.034(2) -0.0223(18)
N3 0.0453(17) 0.0573(19) 0.0694(19) 0.0203(15) -0.0260(15) -0.0185(15)
O1 0.0504(14) 0.0342(11) 0.0465(12) -0.0016(10) 0.0143(11) -0.0054(10)
C18 0.064(2) 0.0426(18) 0.077(3) 0.0044(18) -0.028(2) -0.0060(16)
C17 0.067(2) 0.054(2) 0.076(2) -0.0048(19) -0.032(2) -0.004(2)
C19 0.062(2) 0.0519(19) 0.085(2) 0.011(2) -0.038(3) -0.0095(16)
C16 0.0509(17) 0.0421(16) 0.055(2) 0.0093(18) -0.0196(18) -0.0044(14)
N2 0.0418(16) 0.0471(16) 0.0537(16) 0.0142(14) -0.0156(14) -0.0073(13)
O2 0.0510(15) 0.0390(13) 0.0665(15) 0.0014(12) 0.0217(12) -0.0021(10)
C1 0.0389(18) 0.0398(19) 0.0459(17) 0.0032(15) 0.0101(14) 0.0021(14)
C12 0.051(7) 0.040(4) 0.050(7) -0.002(6) -0.010(5) -0.006(5)
C20 0.054(2) 0.058(2) 0.074(3) 0.006(2) -0.023(2) -0.0054(18)
O6 0.0446(13) 0.0484(14) 0.0644(14) 0.0157(12) -0.0151(12) -0.0094(11)
C11 0.054(7) 0.038(5) 0.057(6) 0.005(4) -0.006(5) -0.018(4)
O8 0.0550(17) 0.0636(18) 0.130(3) 0.0238(17) -0.0407(18) -0.0159(14)
O7 0.086(2) 0.0622(18) 0.0745(19) 0.0211(14) -0.0316(17) 0.0029(16)
C4 0.046(2) 0.0453(19) 0.066(2) 0.0040(19) -0.0144(19) -0.0027(18)
C3 0.050(2) 0.041(2) 0.0509(19) -0.0009(17) -0.0069(17) 0.0064(17)
C14B 0.061(5) 0.042(4) 0.097(7) -0.015(4) -0.048(5) 0.015(4)
C15B 0.065(5) 0.033(4) 0.095(6) -0.018(4) -0.047(5) 0.013(3)
C12B 0.071(9) 0.044(6) 0.055(8) -0.017(6) -0.019(6) 0.015(6)
C14 0.065(5) 0.060(5) 0.071(5) 0.029(5) -0.038(5) -0.020(4)
C15 0.062(5) 0.047(4) 0.074(5) 0.021(4) -0.025(4) -0.021(4)
C11B 0.041(5) 0.039(6) 0.071(9) 0.009(5) -0.025(5) 0.005(5)
C10 0.044(2) 0.054(2) 0.052(2) 0.0159(18) -0.0166(16) -0.0131(16)
C13 0.049(2) 0.058(2) 0.066(2) 0.0194(19) -0.0223(18) -0.0204(19)
O10 0.059(3) 0.267(10) 0.086(3) 0.000 0.000 0.046(4)
O11 0.087(6) 0.063(5) 0.149(8) 0.000 0.000 -0.018(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr01 O5 2.163(2) 2_775 ?
Zr01 O5 2.163(2) . ?
Zr01 O2 2.195(2) 2_775 ?
Zr01 O2 2.195(2) . ?
Zr01 O6 2.203(2) . ?
Zr01 O6 2.203(2) 2_775 ?
Zr01 O1 2.225(2) . ?
Zr01 O1 2.225(2) 2_775 ?
O4 C2 1.239(4) . ?
O3 C1 1.238(4) . ?
C2 O2 1.265(4) . ?
C2 C1 1.530(5) . ?
N1 C16 1.312(4) . ?
N1 C17 1.367(5) . ?
N4 C21 1.308(4) . ?
N4 C20 1.358(5) . ?
O5 C3 1.283(4) . ?
C21 N3 1.336(4) . ?
N3 C19 1.371(4) . ?
N3 C13 1.448(4) . ?
O1 C1 1.269(4) . ?
C18 C17 1.344(5) . ?
C18 N2 1.386(4) . ?
C19 C20 1.358(5) . ?
C16 N2 1.331(4) . ?
N2 C10 1.425(4) . ?
C12 C11 1.367(19) . ?
C12 C13 1.377(15) . ?
O6 C4 1.275(4) . ?
C11 C10 1.462(12) . ?
O8 C4 1.226(4) . ?
O7 C3 1.211(4) . ?
C4 C3 1.526(5) . ?
C14B C15B 1.390(10) . ?
C14B C13 1.496(9) . ?
C15B C10 1.460(8) . ?
C12B C13 1.279(16) . ?
C12B C11B 1.410(19) . ?
C14 C13 1.327(8) . ?
C14 C15 1.381(10) . ?
C15 C10 1.391(8) . ?
C11B C10 1.230(12) . ?

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
O5 Zr01 O5 87.84(12) 2_775 . ?
O5 Zr01 O2 103.61(9) 2_775 2_775 ?
O5 Zr01 O2 147.56(8) . 2_775 ?
O5 Zr01 O2 147.56(8) 2_775 . ?
O5 Zr01 O2 103.61(9) . . ?
O2 Zr01 O2 82.96(15) 2_775 . ?
O5 Zr01 O6 80.23(9) 2_775 . ?
O5 Zr01 O6 71.46(8) . . ?
O2 Zr01 O6 139.85(9) 2_775 . ?
O2 Zr01 O6 75.09(10) . . ?
O5 Zr01 O6 71.46(8) 2_775 2_775 ?
O5 Zr01 O6 80.23(9) . 2_775 ?
O2 Zr01 O6 75.09(10) 2_775 2_775 ?
O2 Zr01 O6 139.85(9) . 2_775 ?
O6 Zr01 O6 140.44(13) . 2_775 ?
O5 Zr01 O1 141.89(8) 2_775 . ?
O5 Zr01 O1 75.30(8) . . ?
O2 Zr01 O1 77.29(8) 2_775 . ?
O2 Zr01 O1 70.47(8) . . ?
O6 Zr01 O1 123.88(8) . . ?
O6 Zr01 O1 72.12(8) 2_775 . ?
O5 Zr01 O1 75.30(8) 2_775 2_775 ?
O5 Zr01 O1 141.89(8) . 2_775 ?
O2 Zr01 O1 70.47(8) 2_775 2_775 ?
O2 Zr01 O1 77.29(8) . 2_775 ?
O6 Zr01 O1 72.12(8) . 2_775 ?
O6 Zr01 O1 123.88(8) 2_775 2_775 ?
O1 Zr01 O1 136.57(12) . 2_775 ?
O4 C2 O2 125.6(3) . . ?
O4 C2 C1 120.3(3) . . ?
O2 C2 C1 114.2(3) . . ?
C16 N1 C17 108.6(3) . . ?
C21 N4 C20 110.1(3) . . ?
C3 O5 Zr01 121.2(2) . . ?
N4 C21 N3 108.3(3) . . ?
C21 N3 C19 108.1(3) . . ?
C21 N3 C13 125.8(3) . . ?
C19 N3 C13 126.0(3) . . ?
C1 O1 Zr01 120.62(19) . . ?
C17 C18 N2 106.5(3) . . ?
C18 C17 N1 107.8(3) . . ?
C20 C19 N3 107.1(3) . . ?
N1 C16 N2 109.2(3) . . ?
C16 N2 C18 107.9(3) . . ?
C16 N2 C10 125.4(3) . . ?
C18 N2 C10 126.6(3) . . ?
C2 O2 Zr01 121.2(2) . . ?
O3 C1 O1 125.4(3) . . ?
O3 C1 C2 121.3(3) . . ?
O1 C1 C2 113.3(3) . . ?
C11 C12 C13 120.3(12) . . ?
N4 C20 C19 106.4(3) . . ?
C4 O6 Zr01 119.4(2) . . ?
C12 C11 C10 117.3(11) . . ?
O8 C4 O6 126.0(3) . . ?
O8 C4 C3 120.5(3) . . ?
O6 C4 C3 113.6(3) . . ?
O7 C3 O5 125.6(4) . . ?
O7 C3 C4 121.3(3) . . ?
O5 C3 C4 113.2(3) . . ?
C15B C14B C13 118.5(6) . . ?
C14B C15B C10 115.5(6) . . ?
C13 C12B C11B 121.1(12) . . ?
C13 C14 C15 118.5(6) . . ?
C14 C15 C10 121.0(6) . . ?
C10 C11B C12B 122.6(10) . . ?
C11B C10 C15 100.5(6) . . ?
C11B C10 N2 122.0(5) . . ?
C15 C10 N2 122.5(4) . . ?
C11B C10 C15B 122.5(6) . . ?
C15 C10 C15B 51.5(5) . . ?
N2 C10 C15B 114.7(4) . . ?
C11B C10 C11 26.9(6) . . ?
C15 C10 C11 115.9(7) . . ?
N2 C10 C11 119.3(6) . . ?
C15B C10 C11 113.4(6) . . ?
C12B C13 C14 100.2(8) . . ?
C12B C13 C12 27.5(6) . . ?
C14 C13 C12 119.7(7) . . ?
C12B C13 N3 121.9(7) . . ?
C14 C13 N3 118.8(4) . . ?
C12 C13 N3 117.3(7) . . ?
C12B C13 C14B 118.8(8) . . ?
C14 C13 C14B 53.6(5) . . ?
C12 C13 C14B 112.7(7) . . ?
N3 C13 C14B 118.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.058

# Attachment '- Compd_2-373K.cif'

data_Compd-2
_database_code_depnum_ccdc_archive 'CCDC 768080'
#TrackingRef '- Compd_2-373K.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H12 N4 O8 Zr0.50'
_chemical_formula_weight         433.91

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnc2

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

_cell_length_a                   10.699(3)
_cell_length_b                   16.784(6)
_cell_length_c                   10.022(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1799.7(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    22943
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      21.97

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   scalepack

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      373(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_number            6798
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         21.95
_reflns_number_total             2186
_reflns_number_gt                1700
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'

_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^)+(0.0974P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(11)
_refine_ls_number_reflns         2186
_refine_ls_number_parameters     258
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1359
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Zr01 Zr 0.0000 1.0000 -0.00078(19) 0.0629(4) Uani 1 2 d S . .
O002 O -0.0157(6) 0.8767(3) 0.0808(6) 0.0762(16) Uani 1 1 d . . .
O003 O -0.1327(7) 0.9977(3) 0.1663(7) 0.091(2) Uani 1 1 d . . .
O004 O -0.0980(7) 0.7956(3) 0.2327(7) 0.097(2) Uani 1 1 d . . .
O005 O -0.0907(6) 0.9337(3) -0.1578(7) 0.0792(17) Uani 1 1 d . . .
O006 O -0.2182(8) 0.9300(4) 0.3317(9) 0.109(3) Uani 1 1 d . . .
N02 N 0.1834(7) 0.8245(4) 0.4299(7) 0.0731(19) Uani 1 1 d . . .
O008 O -0.1624(6) 1.0662(3) -0.0688(8) 0.0879(18) Uani 1 1 d . . .
O009 O -0.2403(9) 0.9262(5) -0.3103(9) 0.117(3) Uani 1 1 d . . .
N03 N 0.0396(9) 0.8023(5) 0.5738(9) 0.093(3) Uani 1 1 d . . .
H03 H -0.0122 0.7777 0.6248 0.112 Uiso 1 1 calc R . .
C01 C 0.6226(10) 0.6977(6) 0.0364(11) 0.090(3) Uani 1 1 d . . .
H01 H 0.6036 0.6498 0.0783 0.108 Uiso 1 1 calc R . .
O012 O -0.3505(8) 1.0550(5) -0.1618(13) 0.147(4) Uani 1 1 d . . .
N01 N 0.5664(7) 0.7689(4) 0.0597(8) 0.077(2) Uani 1 1 d . . .
N014 N 0.7061(8) 0.7082(5) -0.0530(8) 0.087(2) Uani 1 1 d . . .
H014 H 0.7519 0.6705 -0.0843 0.105 Uiso 1 1 calc R . .
C03 C -0.0848(9) 0.8623(5) 0.1792(10) 0.074(2) Uani 1 1 d . . .
C016 C 0.2807(8) 0.8114(5) 0.3326(9) 0.074(2) Uani 1 1 d . . .
C017 C 0.1485(10) 0.8961(6) 0.4848(14) 0.105(4) Uani 1 1 d . . .
H017 H 0.1832 0.9454 0.4645 0.126 Uiso 1 1 calc R . .
C018 C -0.1870(11) 0.9573(6) -0.2135(10) 0.076(3) Uani 1 1 d . . .
C019 C 0.0587(13) 0.8836(6) 0.5700(12) 0.107(3) Uani 1 1 d . . .
H019 H 0.0158 0.9219 0.6189 0.128 Uiso 1 1 calc R . .
C020 C 0.1138(8) 0.7694(5) 0.4868(12) 0.083(2) Uani 1 1 d . . .
H020 H 0.1171 0.7152 0.4677 0.099 Uiso 1 1 calc R . .
C021 C 0.4675(9) 0.7830(6) 0.1516(10) 0.079(3) Uani 1 1 d . . .
C022 C -0.2439(12) 1.0334(6) -0.1459(11) 0.090(3) Uani 1 1 d . . .
C023 C -0.1521(11) 0.9347(5) 0.2354(11) 0.084(3) Uani 1 1 d . . .
C024 C 0.6252(11) 0.8228(6) -0.0163(15) 0.123(5) Uani 1 1 d . . .
H024 H 0.6089 0.8772 -0.0174 0.148 Uiso 1 1 calc R . .
C025 C 0.3178(11) 0.7360(6) 0.3057(13) 0.115(5) Uani 1 1 d . . .
H025 H 0.2789 0.6931 0.3474 0.138 Uiso 1 1 calc R . .
C026 C 0.3332(15) 0.8705(6) 0.2667(15) 0.164(8) Uani 1 1 d . . .
H026 H 0.3082 0.9226 0.2836 0.197 Uiso 1 1 calc R . .
C027 C 0.4244(15) 0.8560(7) 0.1734(19) 0.165(8) Uani 1 1 d . . .
H027 H 0.4567 0.8983 0.1244 0.198 Uiso 1 1 calc R . .
C028 C 0.7145(12) 0.7840(6) -0.0929(13) 0.114(4) Uani 1 1 d . . .
H028 H 0.7676 0.8056 -0.1568 0.136 Uiso 1 1 calc R . .
C029 C 0.4139(12) 0.7230(6) 0.2160(13) 0.117(5) Uani 1 1 d . . .
H029 H 0.4414 0.6712 0.2005 0.141 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr01 0.0750(6) 0.0382(5) 0.0753(6) 0.000 0.000 -0.0019(5)
O002 0.101(4) 0.046(3) 0.081(3) -0.005(3) 0.019(4) 0.000(3)
O003 0.122(6) 0.039(3) 0.114(5) 0.004(3) 0.054(4) 0.011(3)
O004 0.138(6) 0.042(3) 0.112(5) 0.013(3) 0.051(5) 0.009(3)
O005 0.094(5) 0.050(4) 0.094(4) -0.016(3) -0.007(4) -0.005(3)
O006 0.146(7) 0.055(4) 0.125(6) -0.004(4) 0.069(6) -0.001(4)
N02 0.082(5) 0.056(4) 0.081(4) 0.006(4) 0.014(4) 0.006(4)
O008 0.090(4) 0.063(4) 0.111(4) -0.024(3) -0.025(4) 0.010(3)
O009 0.142(7) 0.091(5) 0.118(6) -0.026(5) -0.045(6) -0.010(5)
N03 0.113(7) 0.064(5) 0.103(5) 0.007(5) 0.034(5) 0.001(4)
C01 0.098(7) 0.064(6) 0.107(8) 0.017(5) 0.038(7) 0.016(5)
O012 0.101(6) 0.089(5) 0.250(11) -0.040(6) -0.074(7) 0.015(4)
N01 0.076(5) 0.059(4) 0.096(5) 0.002(4) 0.018(4) 0.011(4)
N014 0.087(6) 0.070(5) 0.105(6) -0.003(4) 0.013(5) 0.014(4)
C03 0.085(7) 0.054(5) 0.083(6) -0.006(5) 0.023(5) 0.003(4)
C016 0.072(6) 0.063(5) 0.086(6) 0.018(5) 0.014(5) 0.011(4)
C017 0.107(7) 0.069(6) 0.138(10) -0.006(7) 0.056(9) -0.003(5)
C018 0.089(7) 0.057(6) 0.083(7) 0.018(5) -0.010(6) -0.012(6)
C019 0.139(9) 0.062(6) 0.120(8) -0.008(6) 0.044(8) 0.004(7)
C020 0.087(5) 0.059(5) 0.102(7) 0.003(6) 0.036(6) -0.010(4)
C021 0.083(7) 0.066(6) 0.088(6) 0.005(5) 0.004(5) 0.013(5)
C022 0.094(8) 0.069(6) 0.108(8) -0.003(6) -0.036(7) 0.002(6)
C023 0.098(8) 0.050(6) 0.105(8) -0.010(5) 0.036(7) -0.005(5)
C024 0.147(9) 0.051(5) 0.173(11) 0.008(7) 0.101(10) 0.002(6)
C025 0.145(10) 0.052(6) 0.149(11) -0.020(6) 0.068(9) -0.021(6)
C026 0.193(15) 0.067(7) 0.232(18) 0.060(9) 0.140(14) 0.058(8)
C027 0.171(14) 0.072(8) 0.252(18) 0.064(9) 0.136(15) 0.044(8)
C028 0.130(10) 0.067(7) 0.143(10) -0.008(6) 0.049(8) -0.015(6)
C029 0.138(10) 0.059(6) 0.154(11) -0.027(7) 0.073(9) -0.020(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr01 O005 2.158(6) . ?
Zr01 O005 2.158(6) 2_575 ?
Zr01 O008 2.172(6) . ?
Zr01 O008 2.172(6) 2_575 ?
Zr01 O003 2.196(6) 2_575 ?
Zr01 O003 2.196(6) . ?
Zr01 O002 2.231(6) 2_575 ?
Zr01 O002 2.231(6) . ?
O002 C03 1.256(10) . ?
O003 C023 1.281(11) . ?
O004 C03 1.249(10) . ?
O005 C018 1.237(11) . ?
O006 C023 1.199(12) . ?
N02 C020 1.318(11) . ?
N02 C017 1.374(12) . ?
N02 C016 1.444(11) . ?
O008 C022 1.289(12) . ?
O009 C018 1.240(12) . ?
N03 C020 1.303(12) . ?
N03 C019 1.379(12) . ?
C01 N014 1.278(12) . ?
C01 N01 1.357(11) . ?
O012 C022 1.206(13) . ?
N01 C024 1.340(12) . ?
N01 C021 1.423(12) . ?
N014 C028 1.337(12) . ?
C03 C023 1.521(13) . ?
C016 C026 1.316(14) . ?
C016 C025 1.354(13) . ?
C017 C019 1.303(15) . ?
C018 C022 1.570(16) . ?
C021 C029 1.327(14) . ?
C021 C027 1.327(14) . ?
C024 C028 1.388(15) . ?
C025 C029 1.383(15) . ?
C026 C027 1.373(16) . ?

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
O005 Zr01 O005 86.3(4) . 2_575 ?
O005 Zr01 O008 71.1(2) . . ?
O005 Zr01 O008 82.3(3) 2_575 . ?
O005 Zr01 O008 82.3(3) . 2_575 ?
O005 Zr01 O008 71.1(2) 2_575 2_575 ?
O008 Zr01 O008 143.4(4) . 2_575 ?
O005 Zr01 O003 148.9(2) . 2_575 ?
O005 Zr01 O003 104.9(3) 2_575 2_575 ?
O008 Zr01 O003 138.4(2) . 2_575 ?
O008 Zr01 O003 74.4(3) 2_575 2_575 ?
O005 Zr01 O003 104.9(3) . . ?
O005 Zr01 O003 148.9(2) 2_575 . ?
O008 Zr01 O003 74.4(3) . . ?
O008 Zr01 O003 138.4(2) 2_575 . ?
O003 Zr01 O003 80.6(5) 2_575 . ?
O005 Zr01 O002 141.2(2) . 2_575 ?
O005 Zr01 O002 75.9(2) 2_575 2_575 ?
O008 Zr01 O002 72.6(2) . 2_575 ?
O008 Zr01 O002 122.0(2) 2_575 2_575 ?
O003 Zr01 O002 69.8(2) 2_575 2_575 ?
O003 Zr01 O002 77.6(2) . 2_575 ?
O005 Zr01 O002 75.9(2) . . ?
O005 Zr01 O002 141.2(2) 2_575 . ?
O008 Zr01 O002 122.0(2) . . ?
O008 Zr01 O002 72.6(2) 2_575 . ?
O003 Zr01 O002 77.6(2) 2_575 . ?
O003 Zr01 O002 69.8(2) . . ?
O002 Zr01 O002 137.0(3) 2_575 . ?
C03 O002 Zr01 120.8(5) . . ?
C023 O003 Zr01 122.1(6) . . ?
C018 O005 Zr01 122.6(6) . . ?
C020 N02 C017 106.7(8) . . ?
C020 N02 C016 126.4(7) . . ?
C017 N02 C016 126.9(8) . . ?
C022 O008 Zr01 120.7(6) . . ?
C020 N03 C019 108.2(9) . . ?
N014 C01 N01 108.0(8) . . ?
C024 N01 C01 106.8(8) . . ?
C024 N01 C021 127.2(7) . . ?
C01 N01 C021 126.0(8) . . ?
C01 N014 C028 112.8(9) . . ?
O004 C03 O002 125.2(7) . . ?
O004 C03 C023 120.3(9) . . ?
O002 C03 C023 114.5(8) . . ?
C026 C016 C025 118.6(9) . . ?
C026 C016 N02 122.1(8) . . ?
C025 C016 N02 119.2(8) . . ?
C019 C017 N02 108.8(9) . . ?
O005 C018 O009 127.0(10) . . ?
O005 C018 C022 112.9(9) . . ?
O009 C018 C022 120.1(10) . . ?
C017 C019 N03 106.7(10) . . ?
N03 C020 N02 109.6(8) . . ?
C029 C021 C027 118.1(10) . . ?
C029 C021 N01 120.6(9) . . ?
C027 C021 N01 121.2(9) . . ?
O012 C022 O008 126.2(10) . . ?
O012 C022 C018 123.7(10) . . ?
O008 C022 C018 110.1(9) . . ?
O006 C023 O003 125.8(9) . . ?
O006 C023 C03 121.6(9) . . ?
O003 C023 C03 112.5(9) . . ?
N01 C024 C028 108.7(9) . . ?
C016 C025 C029 119.6(9) . . ?
C016 C026 C027 120.8(10) . . ?
C021 C027 C026 121.4(10) . . ?
N014 C028 C024 103.6(10) . . ?
C021 C029 C025 121.2(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O005 Zr01 O002 C03 -113.6(7) . . . . ?
O005 Zr01 O002 C03 -178.8(6) 2_575 . . . ?
O008 Zr01 O002 C03 -57.1(7) . . . . ?
O008 Zr01 O002 C03 160.1(7) 2_575 . . . ?
O003 Zr01 O002 C03 82.8(7) 2_575 . . . ?
O003 Zr01 O002 C03 -1.6(7) . . . . ?
O002 Zr01 O002 C03 41.6(6) 2_575 . . . ?
O005 Zr01 O003 C023 72.9(9) . . . . ?
O005 Zr01 O003 C023 -179.0(7) 2_575 . . . ?
O008 Zr01 O003 C023 137.9(9) . . . . ?
O008 Zr01 O003 C023 -22.3(11) 2_575 . . . ?
O003 Zr01 O003 C023 -75.7(9) 2_575 . . . ?
O002 Zr01 O003 C023 -147.0(9) 2_575 . . . ?
O002 Zr01 O003 C023 4.4(8) . . . . ?
O005 Zr01 O005 C018 -84.2(7) 2_575 . . . ?
O008 Zr01 O005 C018 -1.0(7) . . . . ?
O008 Zr01 O005 C018 -155.6(7) 2_575 . . . ?
O003 Zr01 O005 C018 162.8(7) 2_575 . . . ?
O003 Zr01 O005 C018 66.3(8) . . . . ?
O002 Zr01 O005 C018 -22.3(9) 2_575 . . . ?
O002 Zr01 O005 C018 130.5(8) . . . . ?
O005 Zr01 O008 C022 11.8(8) . . . . ?
O005 Zr01 O008 C022 100.5(8) 2_575 . . . ?
O008 Zr01 O008 C022 57.4(8) 2_575 . . . ?
O003 Zr01 O008 C022 -155.7(8) 2_575 . . . ?
O003 Zr01 O008 C022 -100.4(8) . . . . ?
O002 Zr01 O008 C022 178.0(9) 2_575 . . . ?
O002 Zr01 O008 C022 -47.0(9) . . . . ?
N014 C01 N01 C024 -2.9(13) . . . . ?
N014 C01 N01 C021 179.5(9) . . . . ?
N01 C01 N014 C028 1.5(13) . . . . ?
Zr01 O002 C03 O004 -179.0(8) . . . . ?
Zr01 O002 C03 C023 -0.8(11) . . . . ?
C020 N02 C016 C026 169.9(14) . . . . ?
C017 N02 C016 C026 -12.7(17) . . . . ?
C020 N02 C016 C025 -8.7(15) . . . . ?
C017 N02 C016 C025 168.7(12) . . . . ?
C020 N02 C017 C019 -1.2(14) . . . . ?
C016 N02 C017 C019 -179.0(10) . . . . ?
Zr01 O005 C018 O009 174.6(8) . . . . ?
Zr01 O005 C018 C022 -7.3(11) . . . . ?
N02 C017 C019 N03 2.5(15) . . . . ?
C020 N03 C019 C017 -3.0(15) . . . . ?
C019 N03 C020 N02 2.2(14) . . . . ?
C017 N02 C020 N03 -0.7(13) . . . . ?
C016 N02 C020 N03 177.1(8) . . . . ?
C024 N01 C021 C029 176.9(13) . . . . ?
C01 N01 C021 C029 -6.0(18) . . . . ?
C024 N01 C021 C027 -2(2) . . . . ?
C01 N01 C021 C027 175.5(15) . . . . ?
Zr01 O008 C022 O012 159.3(11) . . . . ?
Zr01 O008 C022 C018 -18.1(12) . . . . ?
O005 C018 C022 O012 -161.4(12) . . . . ?
O009 C018 C022 O012 16.9(18) . . . . ?
O005 C018 C022 O008 16.0(13) . . . . ?
O009 C018 C022 O008 -165.7(9) . . . . ?
Zr01 O003 C023 O006 176.1(10) . . . . ?
Zr01 O003 C023 C03 -6.1(13) . . . . ?
O004 C03 C023 O006 0.5(17) . . . . ?
O002 C03 C023 O006 -177.8(11) . . . . ?
O004 C03 C023 O003 -177.4(10) . . . . ?
O002 C03 C023 O003 4.3(13) . . . . ?
C01 N01 C024 C028 3.2(15) . . . . ?
C021 N01 C024 C028 -179.2(11) . . . . ?
C026 C016 C025 C029 4(2) . . . . ?
N02 C016 C025 C029 -177.8(11) . . . . ?
C025 C016 C026 C027 0(2) . . . . ?
N02 C016 C026 C027 -179.1(14) . . . . ?
C029 C021 C027 C026 5(3) . . . . ?
N01 C021 C027 C026 -176.8(15) . . . . ?
C016 C026 C027 C021 -4(3) . . . . ?
C01 N014 C028 C024 0.5(15) . . . . ?
N01 C024 C028 N014 -2.3(16) . . . . ?
C027 C021 C029 C025 -1(2) . . . . ?
N01 C021 C029 C025 179.9(11) . . . . ?
C016 C025 C029 C021 -3(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        21.95
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.076