# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
J.Kahr ?
;
School of Chemistry,
University of St Andrews,
Purdie Building,
North Haugh,
St Andrews,
Fife,
KY16 9ST,
UK
;
A.M.Z.Slawin ?
;
School of Chemistry,
University of St Andrews,
Purdie Building,
North Haugh,
St Andrews,
Fife,
KY16 9ST,
UK
;
J.P.S.Mowat ?
;
School of Chemistry,
University of St Andrews,
Purdie Building,
North Haugh,
St Andrews,
Fife,
KY16 9ST,
UK
;
D.Fairen-Jimenez ?
;
Institute for Materials and Processes,
School of Engineering,
The University of Edinburgh,
United Kingdom
Current Address:
Dept. Chem. & Biochem. Eng. Northwestern Uni.,
Evanston, IL 60208, USA.
;
P.A.Wright ?
;
School of Chemistry,
University of St Andrews,
Purdie Building,
North Haugh,
St Andrews,
Fife,
KY16 9ST,
UK
;
_publ_contact_author_address     
;
School of Chemistry,
University of St Andrews,
Purdie Building,
North Haugh,
St Andrews,
KY16 9ST,
UK
;

_publ_contact_author_email       paw2@st-andrews.ac.uk
_publ_contact_author_fax         '+44 (0)1334 463808'
_publ_contact_author_phone       '+44 (0)1334 463791'

_publ_contact_author_name        'Prof. Paul A. Wright'
_publ_section_title              'A large pore mixed'

data_GME
_database_code_depnum_ccdc_archive 'CCDC 879004'
#TrackingRef '- crystallographic-files.cif'

_audit_creation_method           SHELXL-97
_audit_creation_date             2012-04-23
_audit_author_name               'Juergen Kahr'
_publ_section_abstract           
'A novel form of mixed-linker ZIF with the RHO topology.'

_vrf_RFACG01_GME                 
;
PROBLEM: The value of the R factor is > 0.20
RESPONSE: Low quality of collected data.
;
_vrf_RFACR01_GME                 
;
PROBLEM: The value of the weighted R factor is > 0.45
RESPONSE: Low quality of collected data.
;
_vrf_RINTA01_GME                 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Low quality of collected data.
;
_vrf_PLAT020_GME                 
;
PROBLEM: The value of Rint is greater than 0.12 ......... 0.310
RESPONSE: Low quality of collected data.
;
_vrf_PLAT082_GME                 
;
PROBLEM: High R1 Value .................................. 0.24
RESPONSE: Low quality of collected data.
;
_vrf_PLAT084_GME                 
;
PROBLEM: High wR2 Value ................................. 0.56
RESPONSE: Low quality of collected data.
;
_vrf_PLAT306_GME                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O21
RESPONSE: Disordered solvent.
;
_vrf_PLAT602_GME                 
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: Porous solid.
;
_vrf_PLAT213_GME                 
;
PROBLEM: Atom C3 has ADP max/min Ratio ..... 4.1 prola
RESPONSE: C/N positioning in purinate and high R values
;
_vrf_PLAT234_GME                 
;
PROBLEM: Large Hirshfeld Difference C9 -- C10 .. 0.26 Ang
RESPONSE: C/N positioning in purinate and high R values
;
_vrf_PLAT242_GME                 
;
PROBLEM: Check Low Ueq as Compared to Neighbors for C14
RESPONSE: C/N positioning in purinate and high R values
;
_vrf_PLAT334_GME                 
;
PROBLEM: Small Average Benzene C-C Dist. C2 -C2_s 1.34 Ang.
RESPONSE: C/N positioning in purinate and high R values
;
_vrf_PLAT341_GME                 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0350 Ang
RESPONSE: C/N positioning in purinate and high R values
;
_vrf_PLAT411_GME                 
;
PROBLEM: Short Inter H...H Contact H4A .. H4A .. 1.83 Ang.
RESPONSE: C/N positioning in purinate and high R values
;

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H5.5 N7 O2.25 Zn'
_chemical_formula_sum            'C8 H5.5 N7 O2.25 Zn'
_chemical_formula_weight         296.6

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'

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

_cell_length_a                   26.884(10)
_cell_length_b                   26.884(10)
_cell_length_c                   18.121(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     11342(9)
_cell_formula_units_Z            24
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      46.4

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3744
_exptl_absorpt_coefficient_mu    1.933
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Rigaku Saturn92 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_detector_area_resol_mean 22.2222
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            155295
_diffrn_reflns_av_R_equivalents  0.3100
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         68.25
_reflns_number_total             3828
_reflns_number_gt                3118
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^ > 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^)+(0.2000P)^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         3828
_refine_ls_number_parameters     175
_refine_ls_number_restraints     130
_refine_ls_R_factor_all          0.2721
_refine_ls_R_factor_gt           0.2365
_refine_ls_wR_factor_ref         0.5589
_refine_ls_wR_factor_gt          0.5451
_refine_ls_goodness_of_fit_ref   2.093
_refine_ls_restrained_S_all      2.067
_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 0.11057(7) 0.44222(9) 0.58395(11) 0.0692(9) Uani 1 1 d . . .
C1 C 0.2225(5) 0.4449(9) 0.5814(8) 0.067(5) Uani 1 2 d SU . .
H1A H 0.2249 0.4498 0.6335 0.081 Uiso 1 2 calc SR . .
N1 N 0.1790(5) 0.4413(5) 0.5417(6) 0.070(3) Uani 1 1 d U . .
C2 C 0.1912(6) 0.4356(7) 0.4722(8) 0.080(4) Uani 1 1 d U . .
CN1 C 0.1655(9) 0.4330(10) 0.4071(7) 0.111(7) Uani 1 1 d U . .
H3A H 0.1291 0.4307 0.4057 0.134 Uiso 0.50 1 calc PR . .
CN2 C 0.1918(10) 0.4338(14) 0.3458(11) 0.151(10) Uani 1 1 d U . .
H4A H 0.1749 0.4345 0.3000 0.181 Uiso 0.50 1 calc PR . .
C7 C 0.0000 0.3874(7) 0.5000 0.066(5) Uani 1 2 d SU . .
H7A H 0.0000 0.4228 0.5000 0.079 Uiso 1 2 calc SR . .
N7 N 0.0412(5) 0.3792(5) 0.5287(7) 0.079(4) Uani 1 1 d U . .
C8 C 0.0253(6) 0.3231(6) 0.5208(9) 0.080(5) Uani 1 1 d U . .
CN3 C 0.0519(9) 0.2939(9) 0.5344(11) 0.109(7) Uani 1 1 d U . .
H9A H 0.0898 0.3122 0.5539 0.131 Uiso 0.50 1 calc PR . .
CN4 C 0.0230(11) 0.2370(8) 0.5194(13) 0.123(8) Uani 1 1 d U . .
H10A H 0.0372 0.2134 0.5382 0.147 Uiso 0.50 1 calc PR . .
N11 N 0.0945(5) 0.4118(5) 0.6885(6) 0.068(3) Uani 1 1 d DU . .
C11 C 0.0513(7) 0.3632(7) 0.7126(8) 0.090(5) Uani 1 1 d DU . .
H11A H 0.0243 0.3329 0.6823 0.109 Uiso 1 1 calc R . .
C12 C 0.1209(8) 0.4402(8) 0.7500 0.057(5) Uani 1 2 d SDU . .
N12 N 0.1706(6) 0.4963(7) 0.7500 0.057(4) Uani 1 2 d SDU . .
O12 O 0.1888(4) 0.5181(4) 0.6897(5) 0.076(3) Uani 1 1 d U . .
N13 N 0.1225(6) 0.5198(5) 0.5541(8) 0.086(4) Uani 1 1 d DU . .
C13 C 0.1609(15) 0.5546(12) 0.5064(18) 0.223(18) Uani 1 1 d DU . .
H13A H 0.1848 0.5459 0.4768 0.267 Uiso 1 1 calc R . .
C14 C 0.0992(8) 0.5496(4) 0.5811(13) 0.091(8) Uani 1 2 d SDU . .
N14 N 0.0543(11) 0.5272(6) 0.635(2) 0.186(15) Uani 1 2 d SDU . .
O14 O 0.0387(11) 0.4768(10) 0.6537(19) 0.282(17) Uani 1 1 d U . .
O21 O 0.1956(5) 0.3912(11) 0.7500 0.100(7) Uani 1 4 d SU . .

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 0.0531(12) 0.0844(15) 0.0732(14) -0.0084(9) -0.0175(8) 0.0367(10)
C1 0.086(10) 0.100(15) 0.020(7) -0.025(9) -0.013(4) 0.050(8)
N1 0.075(7) 0.092(9) 0.048(6) -0.027(6) -0.030(6) 0.045(7)
C2 0.082(10) 0.107(12) 0.051(7) -0.022(8) -0.014(7) 0.048(9)
CN1 0.129(15) 0.22(2) 0.035(7) -0.053(10) -0.044(8) 0.122(16)
CN2 0.151(18) 0.28(3) 0.086(13) 0.000(16) -0.029(12) 0.16(2)
C7 0.051(10) 0.065(9) 0.076(12) -0.011(5) -0.023(9) 0.025(5)
N7 0.076(8) 0.057(7) 0.092(9) -0.010(6) -0.045(7) 0.024(6)
C8 0.076(10) 0.052(8) 0.100(11) -0.026(7) -0.050(9) 0.024(7)
CN3 0.118(14) 0.111(14) 0.127(15) -0.003(12) -0.063(12) 0.079(13)
CN4 0.19(2) 0.070(11) 0.134(17) -0.041(10) -0.090(15) 0.081(13)
N11 0.056(7) 0.070(8) 0.081(8) 0.000(7) -0.006(6) 0.033(6)
C11 0.102(12) 0.071(10) 0.072(9) -0.001(8) -0.012(8) 0.024(10)
C12 0.063(12) 0.069(12) 0.034(8) 0.000 0.000 0.029(10)
N12 0.063(10) 0.083(11) 0.044(8) 0.000 0.000 0.049(9)
O12 0.083(7) 0.084(7) 0.056(5) -0.007(5) -0.008(5) 0.039(6)
N13 0.084(9) 0.074(8) 0.103(9) -0.016(8) -0.036(8) 0.042(8)
C13 0.28(4) 0.18(2) 0.24(3) 0.11(2) 0.20(3) 0.13(2)
C14 0.061(13) 0.055(9) 0.16(2) -0.025(7) -0.049(14) 0.030(6)
N14 0.105(19) 0.111(16) 0.34(4) 0.073(12) 0.15(2) 0.052(9)
O14 0.22(2) 0.177(19) 0.50(4) 0.16(2) 0.24(3) 0.136(18)
O21 0.090(11) 0.117(18) 0.102(16) 0.000 0.000 0.058(9)

_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
Zn1 N1 2.006(12) . ?
Zn1 N13 2.019(13) . ?
Zn1 N11 2.023(12) . ?
Zn1 N7 2.047(11) . ?
C1 N1 1.332(13) . ?
C1 N1 1.332(13) 20 ?
C1 H1A 0.9500 . ?
N1 C2 1.329(17) . ?
C2 CN1 1.351(18) . ?
C2 C2 1.43(3) 20 ?
CN1 CN2 1.31(2) . ?
CN1 H3A 0.9500 . ?
CN2 CN2 1.35(4) 20 ?
CN2 H4A 0.9500 . ?
C7 N7 1.339(15) . ?
C7 N7 1.339(15) 9_556 ?
C7 H7A 0.9500 . ?
N7 C8 1.353(17) . ?
C8 CN3 1.32(2) . ?
C8 C8 1.40(3) 9_556 ?
CN3 CN4 1.35(2) . ?
CN3 H9A 0.9500 . ?
CN4 CN4 1.28(4) 9_556 ?
CN4 H10A 0.9500 . ?
N11 C11 1.314(17) . ?
N11 C12 1.336(13) . ?
C11 C11 1.35(3) 16_557 ?
C11 H11A 0.9500 . ?
C12 N11 1.336(13) 16_557 ?
C12 N12 1.43(2) . ?
N12 O12 1.220(12) 16_557 ?
N12 O12 1.220(12) . ?
N13 C13 1.312(18) . ?
N13 C14 1.332(15) . ?
C13 C13 1.39(5) 21_565 ?
C13 H13A 0.9500 . ?
C14 N13 1.332(15) 21_565 ?
C14 N14 1.43(2) . ?
N14 O14 1.25(2) 21_565 ?
N14 O14 1.25(2) . ?

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 Zn1 N13 103.8(5) . . ?
N1 Zn1 N11 111.4(4) . . ?
N13 Zn1 N11 124.0(6) . . ?
N1 Zn1 N7 105.3(5) . . ?
N13 Zn1 N7 109.4(5) . . ?
N11 Zn1 N7 101.6(5) . . ?
N1 C1 N1 114.1(14) . 20 ?
N1 C1 H1A 122.9 . . ?
N1 C1 H1A 122.9 20 . ?
C2 N1 C1 105.3(11) . . ?
C2 N1 Zn1 130.0(9) . . ?
C1 N1 Zn1 124.7(8) . . ?
N1 C2 CN1 133.2(15) . . ?
N1 C2 C2 107.6(8) . 20 ?
CN1 C2 C2 119.0(10) . 20 ?
CN2 CN1 C2 118.8(17) . . ?
CN2 CN1 H3A 120.6 . . ?
C2 CN1 H3A 120.6 . . ?
CN1 CN2 CN2 122.1(10) . 20 ?
CN1 CN2 H4A 119.0 . . ?
CN2 CN2 H4A 119.0 20 . ?
N7 C7 N7 109.2(17) . 9_556 ?
N7 C7 H7A 125.4 . . ?
N7 C7 H7A 125.4 9_556 . ?
C7 N7 C8 108.5(12) . . ?
C7 N7 Zn1 122.7(10) . . ?
C8 N7 Zn1 128.6(9) . . ?
CN3 C8 N7 132.7(14) . . ?
CN3 C8 C8 119.6(10) . 9_556 ?
N7 C8 C8 106.7(7) . 9_556 ?
C8 CN3 CN4 117.3(16) . . ?
C8 CN3 H9A 121.4 . . ?
CN4 CN3 H9A 121.4 . . ?
CN4 CN4 CN3 121.7(10) 9_556 . ?
CN4 CN4 H10A 119.1 9_556 . ?
CN3 CN4 H10A 119.1 . . ?
C11 N11 C12 104.1(12) . . ?
C11 N11 Zn1 128.1(10) . . ?
C12 N11 Zn1 127.3(10) . . ?
N11 C11 C11 109.4(8) . 16_557 ?
N11 C11 H11A 125.3 . . ?
C11 C11 H11A 125.3 16_557 . ?
N11 C12 N11 113.0(16) . 16_557 ?
N11 C12 N12 123.5(8) . . ?
N11 C12 N12 123.5(8) 16_557 . ?
O12 N12 O12 127.0(16) 16_557 . ?
O12 N12 C12 116.5(8) 16_557 . ?
O12 N12 C12 116.5(8) . . ?
C13 N13 C14 104.6(14) . . ?
C13 N13 Zn1 125.1(13) . . ?
C14 N13 Zn1 130.0(12) . . ?
N13 C13 C13 108.6(11) . 21_565 ?
N13 C13 H13A 125.7 . . ?
C13 C13 H13A 125.7 21_565 . ?
N13 C14 N13 113.4(19) 21_565 . ?
N13 C14 N14 123.3(10) 21_565 . ?
N13 C14 N14 123.3(10) . . ?
O14 N14 O14 133(3) 21_565 . ?
O14 N14 C14 113.4(13) 21_565 . ?
O14 N14 C14 113.4(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.053
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.326

data_structure2
_database_code_depnum_ccdc_archive 'CCDC 879005'
#TrackingRef '- crystallographic-files.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11.50 H9.50 Br2 N8.50 O0.50 Zn2'
_chemical_formula_sum            'C11.50 H9.50 Br2 N8.50 O0.50 Zn2'
_chemical_formula_weight         543.85

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.636(7)
_cell_length_b                   10.209(5)
_cell_length_c                   14.124(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.568(9)
_cell_angle_gamma                90.00
_cell_volume                     1965.5(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    5653
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      27.8

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1098
_exptl_absorpt_coefficient_mu    6.521
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Rigaku Saturn70 (2x2 bin mode)
;

_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14892
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         6.34
_diffrn_reflns_theta_max         26.97
_reflns_number_total             3874
_reflns_number_gt                3527
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^ > 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^)+(0.0195P)^2^+16.5742P] 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    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3874
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1082
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_restrained_S_all      1.211
_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 0.66254(5) 0.08513(6) 0.67327(4) 0.01687(16) Uani 1 1 d . . .
Zn2 Zn 0.69209(5) 0.50397(6) 0.34538(4) 0.01667(16) Uani 1 1 d . . .
Br1 Br 0.50471(5) -0.00700(7) 0.67659(6) 0.03632(19) Uani 1 1 d . . .
Br2 Br 0.72864(6) 0.59107(7) 0.49590(5) 0.0380(2) Uani 1 1 d . . .
O21 O 0.5085(19) 0.430(3) 0.904(2) 0.135(8) Uiso 0.50 1 d P . .
N1 N 0.7072(4) 0.1003(5) 0.5360(4) 0.0230(11) Uani 1 1 d . . .
N3 N 0.7564(4) -0.0155(5) 0.3975(4) 0.0232(11) Uani 1 1 d . . .
N5 N 0.7639(4) 0.1210(4) 0.2579(3) 0.0166(10) Uani 1 1 d . . .
N7 N 0.7249(4) 0.3149(5) 0.3272(3) 0.0199(10) Uani 1 1 d . . .
N11 N 0.4579(4) 0.4894(5) 0.6771(4) 0.0226(11) Uani 1 1 d . . .
N13 N 0.5980(4) 0.6037(5) 0.7408(4) 0.0244(11) Uani 1 1 d . . .
N15 N 0.7397(3) 0.4651(4) 0.7657(3) 0.0177(10) Uani 1 1 d . . .
N17 N 0.6719(4) 0.2735(4) 0.7135(4) 0.0197(10) Uani 1 1 d . . .
N20 N 0.4821(10) 0.2442(15) 0.9853(10) 0.047(3) Uiso 0.50 1 d P . .
C2 C 0.7339(5) -0.0095(6) 0.4886(4) 0.0245(13) Uani 1 1 d . . .
H2 H 0.7368 -0.0889 0.5236 0.029 Uiso 1 1 calc R . .
C4 C 0.7499(4) 0.0988(5) 0.3524(4) 0.0174(11) Uani 1 1 d . . .
C6 C 0.7479(5) 0.2520(6) 0.2481(5) 0.0213(12) Uani 1 1 d . . .
H6 H 0.7528 0.2956 0.1890 0.026 Uiso 1 1 calc R . .
C8 C 0.7247(4) 0.2178(5) 0.3957(4) 0.0178(11) Uani 1 1 d . . .
C9 C 0.7029(5) 0.2154(6) 0.4898(4) 0.0221(12) Uani 1 1 d . . .
H9 H 0.6851 0.2934 0.5218 0.027 Uiso 1 1 calc R . .
C12 C 0.5054(5) 0.5982(6) 0.7091(5) 0.0267(13) Uani 1 1 d . . .
H12 H 0.4692 0.6777 0.7089 0.032 Uiso 1 1 calc R . .
C14 C 0.6446(4) 0.4889(6) 0.7375(4) 0.0188(11) Uani 1 1 d . . .
C16 C 0.7512(5) 0.3356(6) 0.7496(4) 0.0191(11) Uani 1 1 d . . .
H16 H 0.8113 0.2915 0.7628 0.023 Uiso 1 1 calc R . .
C18 C 0.6018(4) 0.3709(5) 0.7055(4) 0.0197(12) Uani 1 1 d . . .
C19 C 0.5058(4) 0.3747(6) 0.6736(4) 0.0208(12) Uani 1 1 d . . .
H19 H 0.4741 0.2982 0.6497 0.025 Uiso 1 1 calc R . .
C21 C 0.4915(19) 0.377(3) 0.985(2) 0.086(7) Uiso 0.50 1 d P . .
H21 H 0.4858 0.4281 1.0410 0.103 Uiso 0.50 1 calc PR . .
C22 C 0.4839(14) 0.1734(18) 0.9024(13) 0.052(4) Uiso 0.50 1 d P . .
H22A H 0.4647 0.2300 0.8491 0.078 Uiso 0.50 1 calc PR . .
H22B H 0.4380 0.0998 0.9060 0.078 Uiso 0.50 1 calc PR . .
H22C H 0.5504 0.1399 0.8933 0.078 Uiso 0.50 1 calc PR . .
C23 C 0.4664(14) 0.1848(19) 1.0754(13) 0.056(4) Uiso 0.50 1 d P . .
H23A H 0.4018 0.2104 1.0979 0.083 Uiso 0.50 1 calc PR . .
H23B H 0.5173 0.2141 1.1209 0.083 Uiso 0.50 1 calc PR . .
H23C H 0.4693 0.0893 1.0691 0.083 Uiso 0.50 1 calc PR . .

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 0.0223(3) 0.0103(3) 0.0179(3) 0.0001(3) -0.0015(2) 0.0000(3)
Zn2 0.0222(3) 0.0102(3) 0.0177(3) 0.0010(3) 0.0014(2) 0.0008(2)
Br1 0.0250(3) 0.0332(4) 0.0504(4) 0.0043(3) -0.0056(3) -0.0080(3)
Br2 0.0626(5) 0.0300(4) 0.0212(3) -0.0050(3) -0.0036(3) -0.0033(3)
N1 0.035(3) 0.011(2) 0.023(3) -0.001(2) -0.003(2) 0.001(2)
N3 0.037(3) 0.011(2) 0.021(2) -0.001(2) 0.002(2) 0.004(2)
N5 0.024(2) 0.011(2) 0.015(2) 0.0000(18) 0.0004(19) 0.0012(18)
N7 0.029(3) 0.013(2) 0.018(2) 0.0000(19) 0.002(2) 0.000(2)
N11 0.021(2) 0.015(2) 0.031(3) 0.001(2) -0.001(2) 0.001(2)
N13 0.023(3) 0.014(2) 0.036(3) -0.001(2) -0.002(2) 0.003(2)
N15 0.019(2) 0.015(2) 0.019(2) -0.0015(18) -0.0010(19) 0.0002(18)
N17 0.022(2) 0.010(2) 0.026(3) 0.0001(19) -0.002(2) 0.0027(19)
C2 0.038(4) 0.019(3) 0.016(3) 0.001(2) 0.003(2) 0.002(3)
C4 0.020(3) 0.014(3) 0.018(3) -0.002(2) 0.001(2) 0.003(2)
C6 0.026(3) 0.014(3) 0.024(3) 0.003(2) -0.001(2) 0.003(2)
C8 0.023(3) 0.013(3) 0.018(3) 0.003(2) 0.002(2) 0.001(2)
C9 0.033(3) 0.013(3) 0.021(3) -0.002(2) 0.000(3) 0.002(2)
C12 0.027(3) 0.012(3) 0.041(4) -0.002(3) 0.000(3) 0.004(2)
C14 0.024(3) 0.014(3) 0.018(3) -0.003(2) -0.001(2) 0.000(2)
C16 0.023(3) 0.013(2) 0.021(3) -0.002(2) -0.004(2) 0.001(2)
C18 0.027(3) 0.012(3) 0.020(3) 0.000(2) 0.001(2) 0.000(2)
C19 0.023(3) 0.015(3) 0.024(3) -0.004(2) 0.004(2) 0.000(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
Zn1 N15 1.989(5) 2_646 ?
Zn1 N17 2.008(5) . ?
Zn1 N1 2.054(5) . ?
Zn1 Br1 2.3505(14) . ?
Zn2 N5 1.992(5) 2_655 ?
Zn2 N7 1.999(5) . ?
Zn2 N11 2.062(5) 3_666 ?
Zn2 Br2 2.3453(13) . ?
O21 C21 1.29(3) . ?
N1 C9 1.344(7) . ?
N1 C2 1.360(8) . ?
N3 C4 1.332(7) . ?
N3 C2 1.332(8) . ?
N5 C6 1.361(7) . ?
N5 C4 1.372(7) . ?
N5 Zn2 1.992(5) 2_645 ?
N7 C6 1.334(8) . ?
N7 C8 1.384(7) . ?
N11 C19 1.342(8) . ?
N11 C12 1.357(8) . ?
N11 Zn2 2.062(5) 3_666 ?
N13 C12 1.328(8) . ?
N13 C14 1.334(7) . ?
N15 C16 1.352(7) . ?
N15 C14 1.367(7) . ?
N15 Zn1 1.989(5) 2_656 ?
N17 C16 1.342(8) . ?
N17 C18 1.381(7) . ?
N20 C21 1.37(3) . ?
N20 C22 1.38(2) . ?
N20 C23 1.43(2) . ?
C2 H2 0.9500 . ?
C4 C8 1.406(8) . ?
C6 H6 0.9500 . ?
C8 C9 1.371(8) . ?
C9 H9 0.9500 . ?
C12 H12 0.9500 . ?
C14 C18 1.409(8) . ?
C16 H16 0.9500 . ?
C18 C19 1.374(8) . ?
C19 H19 0.9500 . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
N15 Zn1 N17 115.5(2) 2_646 . ?
N15 Zn1 N1 104.1(2) 2_646 . ?
N17 Zn1 N1 100.2(2) . . ?
N15 Zn1 Br1 110.37(14) 2_646 . ?
N17 Zn1 Br1 115.37(15) . . ?
N1 Zn1 Br1 110.13(15) . . ?
N5 Zn2 N7 114.35(19) 2_655 . ?
N5 Zn2 N11 100.7(2) 2_655 3_666 ?
N7 Zn2 N11 103.7(2) . 3_666 ?
N5 Zn2 Br2 112.08(14) 2_655 . ?
N7 Zn2 Br2 116.07(14) . . ?
N11 Zn2 Br2 108.19(15) 3_666 . ?
C9 N1 C2 119.4(5) . . ?
C9 N1 Zn1 120.9(4) . . ?
C2 N1 Zn1 119.5(4) . . ?
C4 N3 C2 114.0(5) . . ?
C6 N5 C4 103.6(5) . . ?
C6 N5 Zn2 124.4(4) . 2_645 ?
C4 N5 Zn2 131.8(4) . 2_645 ?
C6 N7 C8 104.2(5) . . ?
C6 N7 Zn2 129.1(4) . . ?
C8 N7 Zn2 126.7(4) . . ?
C19 N11 C12 119.8(5) . . ?
C19 N11 Zn2 120.3(4) . 3_666 ?
C12 N11 Zn2 119.1(4) . 3_666 ?
C12 N13 C14 113.6(5) . . ?
C16 N15 C14 103.8(5) . . ?
C16 N15 Zn1 126.6(4) . 2_656 ?
C14 N15 Zn1 129.5(4) . 2_656 ?
C16 N17 C18 103.9(5) . . ?
C16 N17 Zn1 127.1(4) . . ?
C18 N17 Zn1 128.9(4) . . ?
C21 N20 C22 121.1(19) . . ?
C21 N20 C23 116.2(18) . . ?
C22 N20 C23 122.7(16) . . ?
N3 C2 N1 125.8(6) . . ?
N3 C2 H2 117.1 . . ?
N1 C2 H2 117.1 . . ?
N3 C4 N5 126.9(5) . . ?
N3 C4 C8 124.3(5) . . ?
N5 C4 C8 108.8(5) . . ?
N7 C6 N5 115.4(5) . . ?
N7 C6 H6 122.3 . . ?
N5 C6 H6 122.3 . . ?
C9 C8 N7 134.0(5) . . ?
C9 C8 C4 117.9(5) . . ?
N7 C8 C4 108.1(5) . . ?
N1 C9 C8 118.5(5) . . ?
N1 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
N13 C12 N11 126.0(5) . . ?
N13 C12 H12 117.0 . . ?
N11 C12 H12 117.0 . . ?
N13 C14 N15 126.5(5) . . ?
N13 C14 C18 124.6(5) . . ?
N15 C14 C18 108.8(5) . . ?
N17 C16 N15 115.5(5) . . ?
N17 C16 H16 122.3 . . ?
N15 C16 H16 122.3 . . ?
C19 C18 N17 134.3(5) . . ?
C19 C18 C14 117.6(5) . . ?
N17 C18 C14 108.0(5) . . ?
N11 C19 C18 118.3(5) . . ?
N11 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
O21 C21 N20 116(3) . . ?
O21 C21 H21 122.0 . . ?
N20 C21 H21 122.0 . . ?
N20 C22 H22A 109.5 . . ?
N20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N20 C23 H23A 109.5 . . ?
N20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

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
N15 Zn1 N1 C9 -140.6(5) 2_646 . . . ?
N17 Zn1 N1 C9 -20.9(5) . . . . ?
Br1 Zn1 N1 C9 101.1(5) . . . . ?
N15 Zn1 N1 C2 44.7(5) 2_646 . . . ?
N17 Zn1 N1 C2 164.5(5) . . . . ?
Br1 Zn1 N1 C2 -73.6(5) . . . . ?
N5 Zn2 N7 C6 -19.1(6) 2_655 . . . ?
N11 Zn2 N7 C6 89.5(6) 3_666 . . . ?
Br2 Zn2 N7 C6 -152.1(5) . . . . ?
N5 Zn2 N7 C8 163.6(5) 2_655 . . . ?
N11 Zn2 N7 C8 -87.8(5) 3_666 . . . ?
Br2 Zn2 N7 C8 30.7(5) . . . . ?
N15 Zn1 N17 C16 24.0(6) 2_646 . . . ?
N1 Zn1 N17 C16 -87.0(5) . . . . ?
Br1 Zn1 N17 C16 154.8(5) . . . . ?
N15 Zn1 N17 C18 -160.5(5) 2_646 . . . ?
N1 Zn1 N17 C18 88.5(5) . . . . ?
Br1 Zn1 N17 C18 -29.7(5) . . . . ?
C4 N3 C2 N1 -0.7(9) . . . . ?
C9 N1 C2 N3 -0.7(10) . . . . ?
Zn1 N1 C2 N3 174.1(5) . . . . ?
C2 N3 C4 N5 -176.5(6) . . . . ?
C2 N3 C4 C8 1.9(9) . . . . ?
C6 N5 C4 N3 179.4(6) . . . . ?
Zn2 N5 C4 N3 -5.6(9) 2_645 . . . ?
C6 N5 C4 C8 0.8(6) . . . . ?
Zn2 N5 C4 C8 175.8(4) 2_645 . . . ?
C8 N7 C6 N5 -0.4(7) . . . . ?
Zn2 N7 C6 N5 -178.1(4) . . . . ?
C4 N5 C6 N7 -0.2(7) . . . . ?
Zn2 N5 C6 N7 -175.8(4) 2_645 . . . ?
C6 N7 C8 C9 -176.5(7) . . . . ?
Zn2 N7 C8 C9 1.2(10) . . . . ?
C6 N7 C8 C4 0.9(6) . . . . ?
Zn2 N7 C8 C4 178.7(4) . . . . ?
N3 C4 C8 C9 -1.8(9) . . . . ?
N5 C4 C8 C9 176.8(5) . . . . ?
N3 C4 C8 N7 -179.7(5) . . . . ?
N5 C4 C8 N7 -1.1(6) . . . . ?
C2 N1 C9 C8 0.8(9) . . . . ?
Zn1 N1 C9 C8 -173.9(4) . . . . ?
N7 C8 C9 N1 177.6(6) . . . . ?
C4 C8 C9 N1 0.4(9) . . . . ?
C14 N13 C12 N11 1.1(9) . . . . ?
C19 N11 C12 N13 -1.5(10) . . . . ?
Zn2 N11 C12 N13 168.8(5) 3_666 . . . ?
C12 N13 C14 N15 -179.7(6) . . . . ?
C12 N13 C14 C18 -1.0(9) . . . . ?
C16 N15 C14 N13 179.2(6) . . . . ?
Zn1 N15 C14 N13 3.9(9) 2_656 . . . ?
C16 N15 C14 C18 0.4(6) . . . . ?
Zn1 N15 C14 C18 -174.9(4) 2_656 . . . ?
C18 N17 C16 N15 -0.2(7) . . . . ?
Zn1 N17 C16 N15 176.2(4) . . . . ?
C14 N15 C16 N17 -0.1(7) . . . . ?
Zn1 N15 C16 N17 175.3(4) 2_656 . . . ?
C16 N17 C18 C19 179.5(7) . . . . ?
Zn1 N17 C18 C19 3.2(10) . . . . ?
C16 N17 C18 C14 0.4(6) . . . . ?
Zn1 N17 C18 C14 -175.9(4) . . . . ?
N13 C14 C18 C19 1.4(9) . . . . ?
N15 C14 C18 C19 -179.8(5) . . . . ?
N13 C14 C18 N17 -179.4(6) . . . . ?
N15 C14 C18 N17 -0.5(7) . . . . ?
C12 N11 C19 C18 1.8(9) . . . . ?
Zn2 N11 C19 C18 -168.4(4) 3_666 . . . ?
N17 C18 C19 N11 179.3(6) . . . . ?
C14 C18 C19 N11 -1.7(8) . . . . ?
C22 N20 C21 O21 -4(3) . . . . ?
C23 N20 C21 O21 178(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.565
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.126

data_structure3
_database_code_depnum_ccdc_archive 'CCDC 879006'
#TrackingRef '- crystallographic-files.cif'

_vrf_PLAT241_structure3          
;
PROBLEM: Check High Ueq as Compared to Neighbors for O1, O2
RESPONSE: Loosely bound counter anion
;
_vrf_PLAT601_structure3          
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 897 A**3
RESPONSE: Frameworks with inaccessible pores.
;
_vrf_PLAT242_structure3          
;
PROBLEM: Check Low Ueq as Compared to Neighbors for Zn1
RESPONSE: Loosely bound counter anion
;
_vrf_PLAT201_structure3          
;
PROBLEM: Check Low Ueq as Compared to Neighbors for Zn1
RESPONSE: Loosely bound counter anion
;
_vrf_PLAT220_structure3          
;
PROBLEM: Check Low Ueq as Compared to Neighbors for Zn1
RESPONSE: Loosely bound counter anion
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H6 N4 O2 Zn1'
_chemical_formula_sum            'C7 H6 N4 O2 Zn1'
_chemical_formula_weight         243.5

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4'
_symmetry_space_group_name_Hall  'I -4'

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

_cell_length_a                   15.02(3)
_cell_length_b                   15.02(3)
_cell_length_c                   9.570(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2159(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    3341
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      27.7

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(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  
;
Rigaku Saturn70 (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11116
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.45
_reflns_number_total             2016
_reflns_number_gt                1981
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^ > 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^)+(0.1661P)^2^+8.6295P] 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   0.16(5)
_refine_ls_number_reflns         2016
_refine_ls_number_parameters     108
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.2174
_refine_ls_wR_factor_gt          0.2167
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.135
_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 -0.32137(6) -0.15392(5) -0.45684(9) 0.0259(3) Uani 1 1 d . . .
N1 N -0.3190(5) -0.2033(5) -0.2621(7) 0.0298(14) Uani 1 1 d . . .
C1 C -0.2485(5) -0.2429(6) -0.2010(10) 0.0271(15) Uani 1 1 d . . .
H1 H -0.1917 -0.2422 -0.2398 0.033 Uiso 1 1 calc R . .
N2 N -0.2669(4) -0.2830(4) -0.0806(7) 0.0276(14) Uani 1 1 d . . .
C2 C -0.3556(5) -0.2711(5) -0.0612(8) 0.0237(15) Uani 1 1 d . . .
N3 N -0.4038(4) -0.2992(4) 0.0467(8) 0.0307(14) Uani 1 1 d . . .
C3 C -0.4884(5) -0.2750(6) 0.0420(10) 0.0327(17) Uani 1 1 d . . .
H3 H -0.5255 -0.2947 0.1134 0.039 Uiso 1 1 calc R . .
N4 N -0.5252(4) -0.2236(5) -0.0594(8) 0.0332(15) Uani 1 1 d . . .
C4 C -0.4770(5) -0.1957(6) -0.1689(9) 0.0302(17) Uani 1 1 d . . .
H4 H -0.5022 -0.1615 -0.2396 0.036 Uiso 1 1 calc R . .
C5 C -0.3869(5) -0.2204(5) -0.1722(8) 0.0254(15) Uani 1 1 d . . .
O1 O -0.4267(12) -0.1892(12) -0.572(3) 0.161(5) Uiso 1 1 d DU . .
O2 O -0.4769(12) -0.0794(12) -0.444(2) 0.153(5) Uiso 1 1 d DU . .
C6 C -0.4797(13) -0.1287(17) -0.549(3) 0.158(5) Uiso 1 1 d DU . .
C7 C -0.5707(14) -0.133(2) -0.628(3) 0.152(6) Uiso 1 1 d DU . .
H7A H -0.6042 -0.0801 -0.6099 0.227 Uiso 1 1 calc R . .
H7B H -0.6037 -0.1842 -0.5964 0.227 Uiso 1 1 calc R . .
H7C H -0.5601 -0.1385 -0.7268 0.227 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
Zn1 0.0314(5) 0.0250(5) 0.0215(5) 0.0011(3) 0.0023(3) 0.0027(3)
N1 0.034(3) 0.030(3) 0.026(3) 0.004(3) 0.001(3) 0.000(3)
C1 0.022(3) 0.027(4) 0.033(4) 0.000(3) -0.005(3) 0.003(3)
N2 0.021(3) 0.031(3) 0.031(4) 0.003(3) -0.002(2) 0.001(2)
C2 0.023(3) 0.024(3) 0.024(4) 0.003(3) -0.001(3) 0.000(3)
N3 0.027(3) 0.036(3) 0.029(4) 0.015(3) -0.001(3) -0.004(2)
C3 0.030(4) 0.048(4) 0.020(4) 0.010(4) 0.004(3) 0.001(3)
N4 0.026(3) 0.043(4) 0.030(4) 0.012(3) -0.006(3) 0.002(3)
C4 0.026(4) 0.035(4) 0.029(4) 0.009(3) -0.003(3) 0.000(3)
C5 0.028(4) 0.026(4) 0.023(4) 0.005(3) 0.001(3) 0.004(3)

_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
Zn1 O1 2.00(2) . ?
Zn1 N1 2.006(8) . ?
Zn1 N2 2.014(7) 7_444 ?
Zn1 N4 2.054(8) 8_454 ?
Zn1 C6 2.566(18) . ?
N1 C1 1.348(11) . ?
N1 C5 1.359(11) . ?
C1 N2 1.329(12) . ?
C1 H1 0.9300 . ?
N2 C2 1.358(10) . ?
N2 Zn1 2.014(7) 7_445 ?
C2 N3 1.329(11) . ?
C2 C5 1.390(11) . ?
N3 C3 1.322(11) . ?
C3 N4 1.357(11) . ?
C3 H3 0.9300 . ?
N4 C4 1.341(11) . ?
N4 Zn1 2.054(8) 6_444 ?
C4 C5 1.403(11) . ?
C4 H4 0.9300 . ?
O1 C6 1.228(9) . ?
O2 C6 1.254(9) . ?
C6 C7 1.562(10) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

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 N1 115.2(7) . . ?
O1 Zn1 N2 94.2(6) . 7_444 ?
N1 Zn1 N2 111.2(3) . 7_444 ?
O1 Zn1 N4 123.5(6) . 8_454 ?
N1 Zn1 N4 105.8(3) . 8_454 ?
N2 Zn1 N4 105.7(3) 7_444 8_454 ?
O1 Zn1 C6 27.8(3) . . ?
N1 Zn1 C6 113.0(8) . . ?
N2 Zn1 C6 118.5(5) 7_444 . ?
N4 Zn1 C6 101.1(6) 8_454 . ?
C1 N1 C5 103.4(7) . . ?
C1 N1 Zn1 125.5(6) . . ?
C5 N1 Zn1 130.1(6) . . ?
N2 C1 N1 114.4(8) . . ?
N2 C1 H1 122.8 . . ?
N1 C1 H1 122.8 . . ?
C1 N2 C2 105.2(7) . . ?
C1 N2 Zn1 125.9(6) . 7_445 ?
C2 N2 Zn1 128.8(6) . 7_445 ?
N3 C2 N2 126.8(7) . . ?
N3 C2 C5 125.7(7) . . ?
N2 C2 C5 107.4(7) . . ?
C3 N3 C2 114.2(7) . . ?
N3 C3 N4 124.9(8) . . ?
N3 C3 H3 117.6 . . ?
N4 C3 H3 117.6 . . ?
C4 N4 C3 121.1(7) . . ?
C4 N4 Zn1 117.6(5) . 6_444 ?
C3 N4 Zn1 121.1(6) . 6_444 ?
N4 C4 C5 117.1(7) . . ?
N4 C4 H4 121.5 . . ?
C5 C4 H4 121.5 . . ?
N1 C5 C2 109.5(7) . . ?
N1 C5 C4 133.5(7) . . ?
C2 C5 C4 117.0(7) . . ?
C6 O1 Zn1 102.8(10) . . ?
O1 C6 O2 123.8(12) . . ?
O1 C6 C7 116.8(10) . . ?
O2 C6 C7 116.4(10) . . ?
O1 C6 Zn1 49.4(8) . . ?
O2 C6 Zn1 77.2(9) . . ?
C7 C6 Zn1 166.1(10) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

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
O1 Zn1 N1 C1 132.3(8) . . . . ?
N2 Zn1 N1 C1 26.7(7) 7_444 . . . ?
N4 Zn1 N1 C1 -87.5(7) 8_454 . . . ?
C6 Zn1 N1 C1 162.8(8) . . . . ?
O1 Zn1 N1 C5 -34.2(9) . . . . ?
N2 Zn1 N1 C5 -139.8(7) 7_444 . . . ?
N4 Zn1 N1 C5 105.9(7) 8_454 . . . ?
C6 Zn1 N1 C5 -3.8(9) . . . . ?
C5 N1 C1 N2 -0.1(10) . . . . ?
Zn1 N1 C1 N2 -169.5(5) . . . . ?
N1 C1 N2 C2 1.3(9) . . . . ?
N1 C1 N2 Zn1 -178.2(5) . . . 7_445 ?
C1 N2 C2 N3 -179.2(8) . . . . ?
Zn1 N2 C2 N3 0.2(12) 7_445 . . . ?
C1 N2 C2 C5 -1.9(8) . . . . ?
Zn1 N2 C2 C5 177.6(5) 7_445 . . . ?
N2 C2 N3 C3 177.2(8) . . . . ?
C5 C2 N3 C3 0.3(12) . . . . ?
C2 N3 C3 N4 -2.2(13) . . . . ?
N3 C3 N4 C4 2.8(14) . . . . ?
N3 C3 N4 Zn1 -172.8(7) . . . 6_444 ?
C3 N4 C4 C5 -1.3(12) . . . . ?
Zn1 N4 C4 C5 174.4(6) 6_444 . . . ?
C1 N1 C5 C2 -1.2(9) . . . . ?
Zn1 N1 C5 C2 167.6(6) . . . . ?
C1 N1 C5 C4 176.9(9) . . . . ?
Zn1 N1 C5 C4 -14.3(14) . . . . ?
N3 C2 C5 N1 179.3(7) . . . . ?
N2 C2 C5 N1 2.0(9) . . . . ?
N3 C2 C5 C4 0.9(12) . . . . ?
N2 C2 C5 C4 -176.5(7) . . . . ?
N4 C4 C5 N1 -178.3(9) . . . . ?
N4 C4 C5 C2 -0.4(12) . . . . ?
N1 Zn1 O1 C6 92(2) . . . . ?
N2 Zn1 O1 C6 -152(2) 7_444 . . . ?
N4 Zn1 O1 C6 -40(2) 8_454 . . . ?
Zn1 O1 C6 O2 -22(4) . . . . ?
Zn1 O1 C6 C7 178(2) . . . . ?
N1 Zn1 C6 O1 -100.8(19) . . . . ?
N2 Zn1 C6 O1 32(2) 7_444 . . . ?
N4 Zn1 C6 O1 146.6(19) 8_454 . . . ?
O1 Zn1 C6 O2 161(3) . . . . ?
N1 Zn1 C6 O2 60.3(19) . . . . ?
N2 Zn1 C6 O2 -167.1(15) 7_444 . . . ?
N4 Zn1 C6 O2 -52.3(18) 8_454 . . . ?
O1 Zn1 C6 C7 -7(9) . . . . ?
N1 Zn1 C6 C7 -108(9) . . . . ?
N2 Zn1 C6 C7 25(10) 7_444 . . . ?
N4 Zn1 C6 C7 139(9) 8_454 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.45
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.906
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.362

data_RHO
_database_code_depnum_ccdc_archive 'CCDC 879007'
#TrackingRef '- crystallographic-files.cif'

_vrf_PLAT019_RHO                 
;
PROBLEM: Check _diffrn_measured_fraction_theta_full/_max 0.996
RESPONSE: ...
;
_vrf_PLAT075_RHO                 
;
PROBLEM: Occupancy 2. greater than 1.0 for ...... H3A
RESPONSE: ...
;
_vrf_PLAT430_RHO                 
;
PROBLEM: Short Inter D...A Contact OS1 .. OS3 .. 2.13 Ang.
RESPONSE: Disordered solvent.
;
_vrf_PLAT601_RHO                 
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 2483 A**3
RESPONSE: Porous material.
;
_vrf_CHEMW03_RHO                 
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.95 <> 1.05
From the CIF: _cell_formula_units_Z 48
From the CIF: _chemical_formula_weight 376.85
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 10.51 126.18
H 1.01 6.00 6.05
N 14.01 5.51 77.18
O 16.00 3.80 60.77
Zn 65.39 1.33 86.97
Calculated formula weight 357.14
RESPONSE: C/N positioning in purinate
;
_vrf_PLAT043_RHO                 
;
PROBLEM: Check Reported Molecular Weight ................ 376.85
RESPONSE: C/N positioning in purinate
;
_vrf_PLAT044_RHO                 
;
PROBLEM: Calculated and Reported Dx Differ .............. ?
RESPONSE: C/N positioning in purinate
;
_vrf_PLAT097_RHO                 
;
PROBLEM: Large Reported Max. (Positive) Residual Density 3.31 eA-3
RESPONSE: Unresolved disordered solvent.
;
_vrf_PLAT201_RHO                 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 1
RESPONSE: Unresolved disordered solvent.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8.50 H6.75 N7.50 O3.55 Zn1.33'
_chemical_formula_sum            'C8.50 H6.75 N7.50 O3.55 Zn1.33'
_chemical_formula_weight         357.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z'
'-x, -y, z'
'-x, y, -z'
'-y, x, z'
'y, x, -z'
'y, -x, z'
'-y, -x, -z'
'y, z, x'
'-y, -z, x'
'y, -z, -x'
'-y, z, -x'
'-z, y, x'
'-z, -y, -x'
'z, -y, x'
'z, y, -x'
'z, x, y'
'-z, x, -y'
'-z, -x, y'
'z, -x, -y'
'-x, -z, -y'
'-x, z, y'
'x, -z, y'
'x, z, -y'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x, -y, -z'
'-x, y, z'
'x, y, -z'
'x, -y, z'
'y, -x, -z'
'-y, -x, z'
'-y, x, -z'
'y, x, z'
'-y, -z, -x'
'y, z, -x'
'-y, z, x'
'y, -z, x'
'z, -y, -x'
'z, y, x'
'-z, y, -x'
'-z, -y, x'
'-z, -x, -y'
'z, -x, y'
'z, x, -y'
'-z, x, y'
'x, z, y'
'x, -z, -y'
'-x, z, -y'
'-x, -z, y'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, -z+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'x+1/2, z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'

_cell_length_a                   29.044(6)
_cell_length_b                   29.044(6)
_cell_length_c                   29.044(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     24500(9)
_cell_formula_units_Z            48
_cell_measurement_temperature    173
_cell_measurement_reflns_used    8637
_cell_measurement_theta_min      41.0
_cell_measurement_theta_max      69.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9016.00
_exptl_absorpt_coefficient_mu    2.33
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Rigaku PILATUS conversion
;
_diffrn_measurement_method       'profile data from \f-scans'
_diffrn_detector_area_resol_mean 11.6279
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            99240
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0082
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         68.23
_reflns_number_total             2174
_reflns_number_gt                2108
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^ > 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^)+(0.1000P)^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         2174
_refine_ls_number_parameters     122
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.1343
_refine_ls_wR_factor_ref         0.3671
_refine_ls_wR_factor_gt          0.3664
_refine_ls_goodness_of_fit_ref   3.355
_refine_ls_restrained_S_all      3.352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.2500 0.39602(3) 0.10398(3) 0.0634(6) Uani 1 2 d S . .
Zn2 Zn 0.31112(8) 0.39628(11) 0.31112(8) 0.0627(9) Uani 0.33 2 d SP . .
O10 O 0.3624(7) 0.3624(7) 0.3624(7) 0.208(11) Uiso 1 6 d S . .
O1 O 0.32029(17) 0.4137(2) 0.03783(15) 0.0824(14) Uani 1 1 d . . .
C1 C 0.2551(3) 0.3919(3) 0.0000 0.0631(19) Uani 1 2 d S . .
C2 C 0.1894(2) 0.3692(3) 0.0237(3) 0.0841(19) Uani 1 1 d . . .
H2A H 0.1646 0.3611 0.0423 0.101 Uiso 1 1 calc R . .
N1 N 0.23212(19) 0.38329(19) 0.03901(18) 0.0695(13) Uani 1 1 d . . .
N2 N 0.3010(3) 0.4071(3) 0.0000 0.0663(17) Uani 1 2 d S . .
C3 C 0.3281(2) 0.3281(2) 0.1023(3) 0.0599(18) Uani 1 2 d S . .
H3A H 0.3259 0.3259 0.0704 0.072 Uiso 1 2 calc SR . .
C4 C 0.3196(3) 0.3532(3) 0.1704(2) 0.0791(19) Uani 1 1 d . . .
CN5 C 0.3077(3) 0.3749(3) 0.2095(2) 0.0823(18) Uani 1 1 d . . .
HN5A H 0.2852 0.3977 0.2096 0.099 Uiso 0.50 1 calc PR . .
CN6 C 0.3291(3) 0.3629(3) 0.2472(2) 0.087(2) Uani 1 1 d . . .
HN6A H 0.3214 0.3773 0.2748 0.104 Uiso 0.50 1 calc PR . .
N3 N 0.30193(18) 0.35762(18) 0.12689(15) 0.0664(13) Uani 1 1 d . . .
OS1 O 0.2653(5) 0.2653(5) 0.0341(7) 0.057(4) Uiso 0.25 2 d SP . .
OS2 O 0.2912(4) 0.2912(4) 0.0000 0.060(3) Uiso 0.50 4 d SP . .
OS3 O 0.0873(16) 0.337(2) 0.0873(16) 0.164(19) Uiso 0.25 2 d SP . .
OS4 O 0.400(4) 0.5000 0.0000 0.20(4) Uiso 0.25 4 d SP . .
C7 C 0.1891(9) 0.1891(9) 0.0000 0.067(8) Uiso 0.33 4 d SPD . .
O2 O 0.139(2) 0.237(2) 0.0373(3) 0.151(19) Uiso 0.17 1 d PD . 1
N4 N 0.1606(16) 0.2285(13) 0.0000 0.085(13) Uiso 0.17 2 d SPD . 1
C8 C 0.151(2) 0.2457(16) 0.0241(3) 0.106(16) Uiso 0.17 1 d PD . 2
N5 N 0.1755(11) 0.2056(11) 0.0377(3) 0.077(8) Uiso 0.17 1 d PD . 2

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 0.0711(8) 0.0595(6) 0.0595(6) 0.0003(4) 0.0110(3) 0.0110(3)
Zn2 0.0598(11) 0.0684(19) 0.0598(11) 0.0007(9) -0.0049(13) 0.0007(9)
O1 0.075(3) 0.113(4) 0.059(2) -0.003(2) -0.003(2) -0.007(2)
C1 0.070(5) 0.062(4) 0.057(4) 0.000 0.000 0.005(3)
C2 0.069(4) 0.102(5) 0.081(4) -0.003(4) 0.005(3) -0.007(3)
N1 0.073(3) 0.071(3) 0.064(3) 0.005(2) 0.009(2) 0.003(2)
N2 0.072(4) 0.081(4) 0.045(3) 0.000 0.000 0.005(3)
C3 0.064(3) 0.064(3) 0.051(4) 0.005(2) 0.005(2) 0.016(3)
C4 0.092(4) 0.091(5) 0.055(3) 0.005(3) 0.015(3) 0.011(3)
CN5 0.100(5) 0.092(5) 0.055(3) 0.001(3) 0.005(3) 0.005(4)
CN6 0.105(5) 0.100(5) 0.056(3) 0.008(3) 0.006(3) 0.013(4)
N3 0.080(3) 0.072(3) 0.048(2) -0.0056(19) 0.002(2) 0.016(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
Zn1 N3 1.990(5) 45 ?
Zn1 N3 1.990(5) . ?
Zn1 N1 1.992(6) 45 ?
Zn1 N1 1.992(6) . ?
Zn2 N5 2.015(14) 81 ?
Zn2 N5 2.015(14) 45 ?
Zn2 CN6 2.157(7) 62 ?
Zn2 CN6 2.157(7) . ?
Zn2 O10 2.325(18) . ?
O10 Zn2 2.325(18) 17 ?
O10 Zn2 2.325(18) 56 ?
O1 N2 1.249(6) . ?
C1 N1 1.339(7) 51 ?
C1 N1 1.339(7) . ?
C1 N2 1.402(11) . ?
C2 C2 1.376(15) 51 ?
C2 N1 1.381(9) . ?
C2 H2A 0.9300 . ?
N2 O1 1.249(6) 51 ?
C3 N3 1.350(6) . ?
C3 N3 1.350(6) 56 ?
C3 H3A 0.9300 . ?
C4 CN5 1.344(9) . ?
C4 N3 1.370(8) . ?
C4 C4 1.378(15) 56 ?
CN5 CN6 1.308(9) . ?
CN5 HN5A 0.9300 . ?
CN6 CN6 1.389(16) 56 ?
CN6 HN6A 0.9300 . ?
OS1 OS2 1.45(2) . ?
OS2 OS1 1.45(2) 51 ?
C7 N5 1.259(18) . ?
C7 N5 1.259(18) 51 ?
C7 N5 1.259(18) 56 ?
C7 N5 1.259(18) 6 ?
C7 N4 1.412(19) . ?
C7 N4 1.412(19) 6 ?
O2 N4 1.28(4) . ?
N4 O2 1.28(4) 51 ?
C8 C8 1.40(2) 51 ?
C8 N5 1.41(2) . ?
N5 N5 1.24(6) 56 ?
N5 Zn2 2.015(14) 89 ?

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
N3 Zn1 N3 101.5(3) 45 . ?
N3 Zn1 N1 114.2(2) 45 45 ?
N3 Zn1 N1 105.7(2) . 45 ?
N3 Zn1 N1 105.7(2) 45 . ?
N3 Zn1 N1 114.2(2) . . ?
N1 Zn1 N1 114.8(3) 45 . ?
N5 Zn2 N5 35.7(17) 81 45 ?
N5 Zn2 CN6 100.0(9) 81 62 ?
N5 Zn2 CN6 130.7(10) 45 62 ?
N5 Zn2 CN6 130.7(10) 81 . ?
N5 Zn2 CN6 100.0(9) 45 . ?
CN6 Zn2 CN6 102.3(5) 62 . ?
N5 Zn2 O10 115.6(12) 81 . ?
N5 Zn2 O10 115.6(12) 45 . ?
CN6 Zn2 O10 101.9(5) 62 . ?
CN6 Zn2 O10 101.9(5) . . ?
Zn2 O10 Zn2 97.5(10) 17 . ?
Zn2 O10 Zn2 97.5(10) 17 56 ?
Zn2 O10 Zn2 97.5(10) . 56 ?
N1 C1 N1 115.6(8) 51 . ?
N1 C1 N2 122.2(4) 51 . ?
N1 C1 N2 122.2(4) . . ?
C2 C2 N1 108.8(4) 51 . ?
C2 C2 H2A 125.6 51 . ?
N1 C2 H2A 125.6 . . ?
C1 N1 C2 103.4(6) . . ?
C1 N1 Zn1 129.6(5) . . ?
C2 N1 Zn1 126.5(4) . . ?
O1 N2 O1 123.3(8) . 51 ?
O1 N2 C1 118.4(4) . . ?
O1 N2 C1 118.4(4) 51 . ?
N3 C3 N3 115.8(7) . 56 ?
N3 C3 H3A 122.1 . . ?
N3 C3 H3A 122.1 56 . ?
CN5 C4 N3 129.6(7) . . ?
CN5 C4 C4 120.9(4) . 56 ?
N3 C4 C4 109.4(4) . 56 ?
CN6 CN5 C4 117.5(7) . . ?
CN6 CN5 HN5A 121.3 . . ?
C4 CN5 HN5A 121.3 . . ?
CN5 CN6 CN6 121.6(5) . 56 ?
CN5 CN6 Zn2 119.1(6) . . ?
CN6 CN6 Zn2 119.3(2) 56 . ?
CN5 CN6 HN6A 119.2 . . ?
CN6 CN6 HN6A 119.2 56 . ?
Zn2 CN6 HN6A 0.2 . . ?
C3 N3 C4 102.5(5) . . ?
C3 N3 Zn1 127.3(4) . . ?
C4 N3 Zn1 130.2(4) . . ?
OS1 OS2 OS1 86.0(18) 51 . ?
N5 C7 N5 121(3) . 51 ?
N5 C7 N5 59(3) . 56 ?
N5 C7 N5 175(5) 51 56 ?
N5 C7 N5 175(5) . 6 ?
N5 C7 N5 59(3) 51 6 ?
N5 C7 N5 121(3) 56 6 ?
N5 C7 N4 60.5(13) . . ?
N5 C7 N4 60.5(13) 51 . ?
N5 C7 N4 118.5(14) 56 . ?
N5 C7 N4 118.5(14) 6 . ?
N5 C7 N4 118.5(14) . 6 ?
N5 C7 N4 118.5(14) 51 6 ?
N5 C7 N4 60.5(13) 56 6 ?
N5 C7 N4 60.5(13) 6 6 ?
N4 C7 N4 162(5) . 6 ?
O2 N4 O2 116(5) 51 . ?
O2 N4 C7 117(3) 51 . ?
O2 N4 C7 117(3) . . ?
C8 C8 N5 106.2(6) 51 . ?
N5 N5 C7 60.6(13) 56 . ?
N5 N5 C8 159(2) 56 . ?
C7 N5 C8 103.0(15) . . ?
N5 N5 Zn2 72.1(9) 56 89 ?
C7 N5 Zn2 132(2) . 89 ?
C8 N5 Zn2 124.0(11) . 89 ?

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
N5 Zn2 O10 Zn2 110.8(12) 81 . . 17 ?
N5 Zn2 O10 Zn2 150.5(11) 45 . . 17 ?
CN6 Zn2 O10 Zn2 3.4(8) 62 . . 17 ?
CN6 Zn2 O10 Zn2 -102.1(6) . . . 17 ?
N5 Zn2 O10 Zn2 -150.5(11) 81 . . 56 ?
N5 Zn2 O10 Zn2 -110.8(12) 45 . . 56 ?
CN6 Zn2 O10 Zn2 102.1(6) 62 . . 56 ?
CN6 Zn2 O10 Zn2 -3.4(8) . . . 56 ?
N1 C1 N1 C2 -2.2(10) 51 . . . ?
N2 C1 N1 C2 -179.8(8) . . . . ?
N1 C1 N1 Zn1 -173.8(3) 51 . . . ?
N2 C1 N1 Zn1 8.6(12) . . . . ?
C2 C2 N1 C1 1.2(6) 51 . . . ?
C2 C2 N1 Zn1 173.2(3) 51 . . . ?
N3 Zn1 N1 C1 -179.7(6) 45 . . . ?
N3 Zn1 N1 C1 -69.0(7) . . . . ?
N1 Zn1 N1 C1 53.4(6) 45 . . . ?
N3 Zn1 N1 C2 10.4(6) 45 . . . ?
N3 Zn1 N1 C2 121.2(6) . . . . ?
N1 Zn1 N1 C2 -116.4(6) 45 . . . ?
N1 C1 N2 O1 -179.0(7) 51 . . . ?
N1 C1 N2 O1 -1.6(12) . . . . ?
N1 C1 N2 O1 1.6(12) 51 . . 51 ?
N1 C1 N2 O1 179.0(7) . . . 51 ?
N3 C4 CN5 CN6 177.3(8) . . . . ?
C4 C4 CN5 CN6 -0.2(9) 56 . . . ?
C4 CN5 CN6 CN6 0.2(10) . . . 56 ?
C4 CN5 CN6 Zn2 -179.6(6) . . . . ?
N5 Zn2 CN6 CN5 -37.8(14) 81 . . . ?
N5 Zn2 CN6 CN5 -58.5(12) 45 . . . ?
CN6 Zn2 CN6 CN5 77.2(8) 62 . . . ?
O10 Zn2 CN6 CN5 -177.6(9) . . . . ?
N5 Zn2 CN6 CN6 142.4(12) 81 . . 56 ?
N5 Zn2 CN6 CN6 121.7(10) 45 . . 56 ?
CN6 Zn2 CN6 CN6 -102.6(3) 62 . . 56 ?
O10 Zn2 CN6 CN6 2.6(6) . . . 56 ?
N3 C3 N3 C4 6.3(10) 56 . . . ?
N3 C3 N3 Zn1 -172.3(3) 56 . . . ?
CN5 C4 N3 C3 178.6(8) . . . . ?
C4 C4 N3 C3 -3.6(6) 56 . . . ?
CN5 C4 N3 Zn1 -2.8(13) . . . . ?
C4 C4 N3 Zn1 175.0(4) 56 . . . ?
N3 Zn1 N3 C3 120.0(7) 45 . . . ?
N1 Zn1 N3 C3 -120.5(6) 45 . . . ?
N1 Zn1 N3 C3 6.7(7) . . . . ?
N3 Zn1 N3 C4 -58.3(6) 45 . . . ?
N1 Zn1 N3 C4 61.2(7) 45 . . . ?
N1 Zn1 N3 C4 -171.6(6) . . . . ?
N5 C7 N4 O2 -160(6) . . . 51 ?
N5 C7 N4 O2 16(5) 51 . . 51 ?
N5 C7 N4 O2 -170(5) 56 . . 51 ?
N5 C7 N4 O2 26(7) 6 . . 51 ?
N4 C7 N4 O2 108(5) 6 . . 51 ?
N5 C7 N4 O2 -16(5) . . . . ?
N5 C7 N4 O2 160(6) 51 . . . ?
N5 C7 N4 O2 -26(7) 56 . . . ?
N5 C7 N4 O2 170(5) 6 . . . ?
N4 C7 N4 O2 -108(5) 6 . . . ?
N5 C7 N5 N5 -174(5) 51 . . 56 ?
N5 C7 N5 N5 -88.5(13) 6 . . 56 ?
N4 C7 N5 N5 -170(3) . . . 56 ?
N4 C7 N5 N5 -10(3) 6 . . 56 ?
N5 C7 N5 C8 -9(6) 51 . . . ?
N5 C7 N5 C8 165(3) 56 . . . ?
N5 C7 N5 C8 77(3) 6 . . . ?
N4 C7 N5 C8 -4(5) . . . . ?
N4 C7 N5 C8 155(4) 6 . . . ?
N5 C7 N5 Zn2 179.6(14) 51 . . 89 ?
N5 C7 N5 Zn2 -6(4) 56 . . 89 ?
N5 C7 N5 Zn2 -95(3) 6 . . 89 ?
N4 C7 N5 Zn2 -176(4) . . . 89 ?
N4 C7 N5 Zn2 -17(6) 6 . . 89 ?
C8 C8 N5 N5 42(7) 51 . . 56 ?
C8 C8 N5 C7 4(3) 51 . . . ?
C8 C8 N5 Zn2 177(2) 51 . . 89 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.273
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.238