Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Can-Zhong Lu'
_publ_contact_author_address     
;
Fujian Institute of Research on the Structure of Matter, Chinese Academy
of Scie
Fuzhou
350002
CHINA
;

_publ_contact_author_email       'CZLU@MS.FJIRSM.AC.CN, CZLU68@YAHOO.COM'

_publ_section_title              
;
(3,4)-Connected jph-type Porous Framework with Cu4I4
clusters as jointing points of helices
;
loop_
_publ_author_name
'Can-Zhong Lu'
'Li-Juan Chen'
'Shu-Mei Chen'
'Xiao-Yuan Wu'
;
Yi-Ming Xie
;
'Quan-Guo Zhai'
'Jian Zhan'
'Zhen-Guo Zhao'

data_1
_database_code_depnum_ccdc_archive 'CCDC 653270'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 Cu2 I N3 O2'
_chemical_formula_sum            'C4 H6 Cu2 I N3 O2'
_chemical_formula_weight         382.10

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.3064(8)
_cell_length_b                   17.3064(8)
_cell_length_c                   18.5975(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5570.2(6)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5027
_cell_measurement_theta_min      2.1898
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2848
_exptl_absorpt_coefficient_mu    5.246
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3538
_exptl_absorpt_correction_T_max  0.4201
_exptl_absorpt_process_details   'CrystalClear, Rigaku, 2005'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  Mercury70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21082
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         27.45
_reflns_number_total             3187
_reflns_number_gt                2756
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.1405P)^2^+19.4911P] 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         3187
_refine_ls_number_parameters     99
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.2166
_refine_ls_wR_factor_gt          0.2045
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
I1 I 0.62767(3) 0.70682(3) 0.54699(3) 0.0635(3) Uani 1 1 d . . .
Cu1 Cu 0.48392(7) 0.67574(7) 0.56850(6) 0.0777(4) Uani 1 1 d . . .
N1 N 0.4312(4) 0.6024(3) 0.5039(3) 0.0597(14) Uani 1 1 d . . .
N2 N 0.3560(4) 0.5818(4) 0.5207(4) 0.0659(16) Uani 1 1 d . . .
C4 C 0.5212(6) 0.5694(6) 0.4057(5) 0.083(3) Uani 1 1 d . . .
H4A H 0.5583 0.5969 0.4352 0.099 Uiso 1 1 calc R . .
H4B H 0.5420 0.5185 0.3956 0.099 Uiso 1 1 calc R . .
C2 C 0.2559(7) 0.4940(8) 0.4771(9) 0.112(4) Uani 1 1 d . . .
H2A H 0.2611 0.4385 0.4716 0.134 Uiso 1 1 calc R . .
H2B H 0.2321 0.5047 0.5233 0.134 Uiso 1 1 calc R . .
O2 O 0.5101(11) 0.6106(10) 0.3391(9) 0.207(7) Uiso 1 1 d . . .
H2C H 0.5515 0.6140 0.3178 0.310 Uiso 1 1 calc R . .
O1 O 0.2119(12) 0.5251(12) 0.4212(9) 0.227(7) Uiso 1 1 d . . .
H1A H 0.1686 0.5059 0.4217 0.340 Uiso 1 1 calc R . .
C3 C 0.4483(5) 0.5616(4) 0.4452(4) 0.0567(15) Uani 1 1 d . . .
C1 C 0.3325(5) 0.5328(5) 0.4713(5) 0.0677(19) Uani 1 1 d . . .
N3 N 0.3883(4) 0.5171(4) 0.4245(4) 0.0685(16) Uani 1 1 d . . .
Cu2 Cu 0.37569(8) 0.44646(8) 0.34880(7) 0.0903(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
I1 0.0629(3) 0.0633(3) 0.0643(4) -0.0039(2) 0.0034(2) 0.0003(2)
Cu1 0.0824(7) 0.0740(7) 0.0767(7) -0.0224(5) 0.0090(5) -0.0186(5)
N1 0.065(3) 0.058(3) 0.056(3) -0.010(3) 0.012(3) -0.008(3)
N2 0.070(4) 0.058(3) 0.069(4) -0.015(3) 0.013(3) -0.005(3)
C4 0.091(6) 0.090(6) 0.068(5) -0.012(5) 0.021(4) -0.007(5)
C2 0.081(7) 0.109(9) 0.146(11) -0.038(8) -0.011(7) -0.002(6)
C3 0.069(4) 0.049(3) 0.052(3) -0.011(3) 0.005(3) -0.002(3)
C1 0.060(4) 0.063(4) 0.079(5) -0.012(4) 0.002(4) -0.004(3)
N3 0.067(4) 0.065(4) 0.073(4) -0.017(3) -0.001(3) -0.004(3)
Cu2 0.1004(9) 0.0877(8) 0.0828(8) -0.0342(6) -0.0106(6) -0.0090(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.5765(13) . ?
I1 Cu1 2.7077(13) 12_767 ?
I1 Cu1 2.8321(14) 6_564 ?
Cu1 N1 1.971(6) . ?
Cu1 Cu1 2.630(2) 6_564 ?
Cu1 I1 2.7077(13) 15_566 ?
Cu1 Cu1 2.8060(19) 12_767 ?
Cu1 Cu1 2.8060(18) 15_566 ?
Cu1 I1 2.8321(14) 6_564 ?
N1 C3 1.334(9) . ?
N1 N2 1.386(9) . ?
N2 C1 1.315(10) . ?
N2 Cu2 1.873(6) 3 ?
C4 O2 1.442(18) . ?
C4 C3 1.466(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 O1 1.40(2) . ?
C2 C1 1.491(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O2 H2C 0.8200 . ?
O1 H1A 0.8200 . ?
C3 N3 1.349(10) . ?
C1 N3 1.329(11) . ?
N3 Cu2 1.877(6) . ?
Cu2 N2 1.873(6) 4_454 ?

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
Cu1 I1 Cu1 64.09(4) . 12_767 ?
Cu1 I1 Cu1 57.95(4) . 6_564 ?
Cu1 I1 Cu1 60.81(4) 12_767 6_564 ?
N1 Cu1 I1 119.11(18) . . ?
N1 Cu1 Cu1 136.6(2) . 6_564 ?
I1 Cu1 Cu1 65.90(5) . 6_564 ?
N1 Cu1 I1 105.26(19) . 15_566 ?
I1 Cu1 I1 112.46(5) . 15_566 ?
Cu1 Cu1 I1 111.74(3) 6_564 15_566 ?
N1 Cu1 Cu1 161.0(2) . 12_767 ?
I1 Cu1 Cu1 60.23(3) . 12_767 ?
Cu1 Cu1 Cu1 62.06(3) 6_564 12_767 ?
I1 Cu1 Cu1 61.78(5) 15_566 12_767 ?
N1 Cu1 Cu1 130.47(19) . 15_566 ?
I1 Cu1 Cu1 110.27(4) . 15_566 ?
Cu1 Cu1 Cu1 62.06(3) 6_564 15_566 ?
I1 Cu1 Cu1 55.68(4) 15_566 15_566 ?
Cu1 Cu1 Cu1 55.89(5) 12_767 15_566 ?
N1 Cu1 I1 93.5(2) . 6_564 ?
I1 Cu1 I1 119.13(4) . 6_564 ?
Cu1 Cu1 I1 56.15(5) 6_564 6_564 ?
I1 Cu1 I1 104.91(4) 15_566 6_564 ?
Cu1 Cu1 I1 103.19(4) 12_767 6_564 ?
Cu1 Cu1 I1 57.40(3) 15_566 6_564 ?
C3 N1 N2 104.9(6) . . ?
C3 N1 Cu1 137.5(5) . . ?
N2 N1 Cu1 117.6(4) . . ?
C1 N2 N1 107.3(6) . . ?
C1 N2 Cu2 130.8(6) . 3 ?
N1 N2 Cu2 121.7(5) . 3 ?
O2 C4 C3 111.2(12) . . ?
O2 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
O2 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O1 C2 C1 104.9(15) . . ?
O1 C2 H2A 110.8 . . ?
C1 C2 H2A 110.8 . . ?
O1 C2 H2B 110.8 . . ?
C1 C2 H2B 110.8 . . ?
H2A C2 H2B 108.9 . . ?
C4 O2 H2C 109.5 . . ?
C2 O1 H1A 109.5 . . ?
N1 C3 N3 111.4(7) . . ?
N1 C3 C4 123.5(7) . . ?
N3 C3 C4 124.9(7) . . ?
N2 C1 N3 111.5(7) . . ?
N2 C1 C2 121.0(9) . . ?
N3 C1 C2 127.0(8) . . ?
C1 N3 C3 104.8(6) . . ?
C1 N3 Cu2 122.7(6) . . ?
C3 N3 Cu2 132.5(6) . . ?
N2 Cu2 N3 160.8(3) 4_454 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.201
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.157

# Attachment 'H2ahmt.CIF'

data_H2ahmt
_database_code_depnum_ccdc_archive 'CCDC 653271'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 N4 O2'
_chemical_formula_sum            'C4 H8 N4 O2'
_chemical_formula_weight         144.14

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           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   8.7902(4)
_cell_length_b                   8.8646(4)
_cell_length_c                   16.0524(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1250.83(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3133
_cell_measurement_theta_min      2.2986
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9291
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_process_details   'CrystalClear, Rigaku, 2005'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  Mercury70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8562
_diffrn_reflns_av_R_equivalents  0.0126
_diffrn_reflns_av_sigmaI/netI    0.0079
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.44
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1421
_reflns_number_gt                1360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.1544P)^2^+1.3566P] 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         1421
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1939
_refine_ls_wR_factor_gt          0.1916
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_restrained_S_all      0.859
_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
O1 O -0.16335(18) 0.38788(15) 0.11467(8) 0.0348(4) Uani 1 1 d . . .
H1A H -0.2330 0.3317 0.1007 0.052 Uiso 1 1 calc R . .
O2 O 0.1337(2) 1.04604(16) 0.10307(9) 0.0386(4) Uani 1 1 d . . .
H2A H 0.1986 1.1031 0.0843 0.058 Uiso 1 1 calc R . .
N1 N -0.0335(2) 0.7158(2) 0.02322(10) 0.0384(5) Uani 1 1 d . . .
H1B H 0.0329 0.6694 -0.0109 0.046 Uiso 1 1 d R . .
H1C H -0.0759 0.7927 -0.0050 0.046 Uiso 1 1 d R . .
N2 N -0.01251(18) 0.71678(15) 0.10949(9) 0.0255(4) Uani 1 1 d . . .
N3 N -0.05786(18) 0.66547(17) 0.24003(9) 0.0290(4) Uani 1 1 d . . .
N4 N 0.06208(18) 0.76749(18) 0.23593(10) 0.0294(4) Uani 1 1 d . . .
C1 C -0.2235(2) 0.5307(2) 0.13719(12) 0.0321(5) Uani 1 1 d . . .
H1D H -0.2952 0.5181 0.1826 0.038 Uiso 1 1 calc R . .
H1E H -0.2780 0.5730 0.0901 0.038 Uiso 1 1 calc R . .
C2 C -0.1012(2) 0.63714(19) 0.16326(11) 0.0255(4) Uani 1 1 d . . .
C3 C 0.0878(2) 0.79729(19) 0.15710(11) 0.0253(4) Uani 1 1 d . . .
C4 C 0.2015(2) 0.9058(2) 0.12358(13) 0.0320(5) Uani 1 1 d . . .
H4B H 0.2806 0.9219 0.1647 0.038 Uiso 1 1 calc R . .
H4A H 0.2485 0.8633 0.0742 0.038 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
O1 0.0467(9) 0.0283(7) 0.0294(7) -0.0051(5) -0.0030(6) -0.0043(6)
O2 0.0558(10) 0.0304(7) 0.0297(7) 0.0067(5) 0.0065(6) -0.0015(6)
N1 0.0525(11) 0.0433(10) 0.0195(8) -0.0006(6) -0.0030(7) -0.0024(8)
N2 0.0315(8) 0.0250(8) 0.0201(8) -0.0007(5) 0.0000(5) 0.0014(6)
N3 0.0350(9) 0.0276(8) 0.0244(8) 0.0014(6) 0.0000(6) -0.0049(6)
N4 0.0341(9) 0.0283(8) 0.0257(8) 0.0001(6) -0.0020(6) -0.0048(6)
C1 0.0311(9) 0.0305(9) 0.0346(9) 0.0005(7) -0.0048(7) -0.0018(7)
C2 0.0279(8) 0.0226(8) 0.0260(8) 0.0004(6) -0.0001(7) 0.0028(6)
C3 0.0266(9) 0.0242(8) 0.0251(8) -0.0004(6) 0.0003(6) 0.0018(6)
C4 0.0332(10) 0.0313(9) 0.0314(9) -0.0001(7) 0.0068(7) -0.0030(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
O1 C1 1.419(2) . ?
O1 H1A 0.8200 . ?
O2 C4 1.417(2) . ?
O2 H2A 0.8200 . ?
N1 N2 1.397(2) . ?
N1 H1B 0.8999 . ?
N1 H1C 0.9000 . ?
N2 C2 1.361(2) . ?
N2 C3 1.368(2) . ?
N3 C2 1.314(2) . ?
N3 N4 1.391(2) . ?
N4 C3 1.312(2) . ?
C1 C2 1.490(2) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C3 C4 1.488(2) . ?
C4 H4B 0.9700 . ?
C4 H4A 0.9700 . ?

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
C1 O1 H1A 109.5 . . ?
C4 O2 H2A 109.5 . . ?
N2 N1 H1B 121.4 . . ?
N2 N1 H1C 123.3 . . ?
H1B N1 H1C 107.9 . . ?
C2 N2 C3 106.60(15) . . ?
C2 N2 N1 123.36(16) . . ?
C3 N2 N1 129.96(16) . . ?
C2 N3 N4 107.45(14) . . ?
C3 N4 N3 107.88(14) . . ?
O1 C1 C2 111.58(16) . . ?
O1 C1 H1D 109.3 . . ?
C2 C1 H1D 109.3 . . ?
O1 C1 H1E 109.3 . . ?
C2 C1 H1E 109.3 . . ?
H1D C1 H1E 108.0 . . ?
N3 C2 N2 109.23(16) . . ?
N3 C2 C1 126.42(16) . . ?
N2 C2 C1 124.31(16) . . ?
N4 C3 N2 108.84(16) . . ?
N4 C3 C4 126.48(17) . . ?
N2 C3 C4 124.63(16) . . ?
O2 C4 C3 111.63(16) . . ?
O2 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
O2 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
H4B C4 H4A 108.0 . . ?

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
O1 H1A N2 0.82 2.46 3.229(2) 156.0 8
O1 H1A N1 0.82 2.61 3.404(3) 162.9 8
N1 H1B O1 0.90 2.08 2.956(2) 162.6 5_565
N1 H1C O2 0.90 2.19 3.057(2) 162.7 5_575

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.069


