# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LIU4-fa_open
_database_code_depnum_ccdc_archive 'CCDC 1422814'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_LIU4-fa_open        
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.938 Note  
RESPONSE: Due to the geometry restraints of the beamline (only phi scans possible)
the complete dataset could not be measured for the given crystal symmetry and 
orientation.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        LIU-4_fa
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H14 N4 O12 Zn3'
_chemical_formula_weight         770.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.0350 2.0980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.320(2)
_cell_length_b                   15.320(2)
_cell_length_c                   23.240(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5454.5(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    354
_cell_measurement_theta_min      3.87
_cell_measurement_theta_max      24.65

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.938
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.429
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.829
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Scala (Diederichs, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            12822
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.585
_diffrn_reflns_theta_max         36.164
_diffrn_reflns_theta_full        32.098
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measured_fraction_theta_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_point_group_measured_fraction_full 0.951
_reflns_number_total             5847
_reflns_number_gt                5704
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_max     0.909
_reflns_Friedel_fraction_full    0.969

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX


_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0533P)²+1.6643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.511(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5847
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.21484(2) 0.21484(2) 0.2500 0.02188(11) Uani 1 2 d S T P . .
Zn2 Zn -0.16317(2) 0.26278(2) 0.11041(2) 0.02368(10) Uani 1 1 d . . . . .
C1 C -0.02645(17) 0.2142(2) 0.19301(13) 0.0319(6) Uani 1 1 d . . . . .
C2 C 0.06704(19) 0.2019(3) 0.21146(14) 0.0436(8) Uani 1 1 d . . . . .
C3 C 0.0866(2) 0.1752(5) 0.26702(18) 0.083(2) Uani 1 1 d . . . . .
H3 H 0.0417 0.1621 0.2925 0.100 Uiso 1 1 calc R U . . .
C4 C 0.1704(3) 0.1682(6) 0.28429(19) 0.097(2) Uani 1 1 d . . . . .
H4 H 0.1835 0.1489 0.3212 0.116 Uiso 1 1 calc R U . . .
C5 C 0.2372(2) 0.1904(4) 0.24597(15) 0.0575(11) Uani 1 1 d . . . . .
C6 C 0.13684(17) 0.2176(2) 0.17488(12) 0.0316(6) Uani 1 1 d . . . . .
H6 H 0.1252 0.2320 0.1368 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3303(2) 0.1907(4) 0.26231(14) 0.0656(15) Uani 1 1 d . . . . .
C8 C 0.3587(3) 0.1700(6) 0.31813(18) 0.110(3) Uani 1 1 d . . . . .
H8 H 0.3187 0.1546 0.3465 0.132 Uiso 1 1 calc R U . . .
C9 C 0.4466(2) 0.1730(5) 0.33030(17) 0.092(2) Uani 1 1 d . . . . .
H9 H 0.4661 0.1611 0.3674 0.111 Uiso 1 1 calc R U . . .
C10 C 0.50524(19) 0.1932(3) 0.28822(14) 0.0438(9) Uani 1 1 d . . . . .
C11 C 0.47371(18) 0.2116(2) 0.23317(13) 0.0342(6) Uani 1 1 d . . . . .
H11 H 0.5135 0.2249 0.2042 0.041 Uiso 1 1 calc R U . . .
C12 C 0.60210(19) 0.1940(2) 0.30076(13) 0.0337(6) Uani 1 1 d . . . . .
C13 C -0.2444(4) 0.1123(3) 0.1389(2) 0.0664(13) Uani 1 1 d . . . . .
H13 H -0.2767 0.0699 0.1580 0.080 Uiso 1 1 calc R U . . .
N1 N 0.22014(15) 0.21284(18) 0.19193(10) 0.0327(5) Uani 1 1 d . . . . .
N2 N 0.38872(15) 0.2108(2) 0.22046(10) 0.0343(6) Uani 1 1 d . . . . .
O1 O -0.08087(14) 0.2113(2) 0.23329(10) 0.0496(7) Uani 1 1 d . . . . .
O2 O -0.04139(13) 0.22798(17) 0.14139(9) 0.0379(5) Uani 1 1 d . . . . .
O3 O 0.62229(14) 0.1706(2) 0.35051(10) 0.0454(6) Uani 1 1 d . . . . .
O4 O 0.65164(14) 0.2176(2) 0.26103(11) 0.0455(6) Uani 1 1 d . . . . .
O5 O -0.23395(14) 0.18510(14) 0.16337(8) 0.0314(4) Uani 1 1 d . . . . .
O6 O -0.2150(5) 0.0945(3) 0.09269(19) 0.134(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 2.062(2) 1_455 ?
Zn1 O4 2.062(2) 8_565 ?
Zn1 O5 2.085(2) . ?
Zn1 O5 2.085(2) 8 ?
Zn1 O1 2.090(2) . ?
Zn1 O1 2.090(2) 8 ?
Zn2 O3 1.984(2) 8_565 ?
Zn2 O5 2.027(2) . ?
Zn2 O2 2.070(2) . ?
Zn2 N2 2.080(2) 5_455 ?
Zn2 N1 2.194(2) 5_455 ?
C1 O2 1.239(4) . ?
C1 O1 1.254(4) . ?
C1 C2 1.507(4) . ?
C2 C3 1.387(5) . ?
C2 C6 1.387(4) . ?
C3 C4 1.348(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(5) . ?
C4 H4 0.9300 . ?
C5 N1 1.328(4) . ?
C5 C7 1.477(5) . ?
C6 N1 1.338(3) . ?
C6 H6 0.9300 . ?
C7 N2 1.357(4) . ?
C7 C8 1.404(5) . ?
C8 C9 1.377(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.363(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(4) . ?
C10 C12 1.512(4) . ?
C11 N2 1.335(4) . ?
C11 H11 0.9300 . ?
C12 O4 1.248(4) . ?
C12 O3 1.250(4) . ?
C13 O6 1.197(7) . ?
C13 O5 1.262(4) . ?
C13 H13 0.9300 . ?
N1 Zn2 2.194(2) 5 ?
N2 Zn2 2.080(2) 5 ?
O3 Zn2 1.984(2) 8_655 ?
O4 Zn1 2.062(2) 1_655 ?

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
O4 Zn1 O4 88.57(17) 1_455 8_565 ?
O4 Zn1 O5 89.15(9) 1_455 . ?
O4 Zn1 O5 95.39(9) 8_565 . ?
O4 Zn1 O5 95.39(9) 1_455 8 ?
O4 Zn1 O5 89.15(9) 8_565 8 ?
O5 Zn1 O5 173.67(13) . 8 ?
O4 Zn1 O1 176.42(9) 1_455 . ?
O4 Zn1 O1 91.28(12) 8_565 . ?
O5 Zn1 O1 87.30(9) . . ?
O5 Zn1 O1 88.19(9) 8 . ?
O4 Zn1 O1 91.28(12) 1_455 8 ?
O4 Zn1 O1 176.42(9) 8_565 8 ?
O5 Zn1 O1 88.19(9) . 8 ?
O5 Zn1 O1 87.30(9) 8 8 ?
O1 Zn1 O1 89.09(19) . 8 ?
O3 Zn2 O5 102.27(10) 8_565 . ?
O3 Zn2 O2 96.95(11) 8_565 . ?
O5 Zn2 O2 96.88(9) . . ?
O3 Zn2 N2 105.24(11) 8_565 5_455 ?
O5 Zn2 N2 150.14(10) . 5_455 ?
O2 Zn2 N2 91.14(9) . 5_455 ?
O3 Zn2 N1 93.22(11) 8_565 5_455 ?
O5 Zn2 N1 90.03(9) . 5_455 ?
O2 Zn2 N1 166.19(9) . 5_455 ?
N2 Zn2 N1 77.14(9) 5_455 5_455 ?
O2 C1 O1 127.3(3) . . ?
O2 C1 C2 118.2(3) . . ?
O1 C1 C2 114.5(3) . . ?
C3 C2 C6 117.0(3) . . ?
C3 C2 C1 120.5(3) . . ?
C6 C2 C1 122.4(3) . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C7 115.6(3) . . ?
C4 C5 C7 123.0(3) . . ?
N1 C6 C2 123.0(3) . . ?
N1 C6 H6 118.5 . . ?
C2 C6 H6 118.5 . . ?
N2 C7 C8 120.6(3) . . ?
N2 C7 C5 117.0(3) . . ?
C8 C7 C5 122.4(3) . . ?
C9 C8 C7 119.0(4) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C10 C9 C8 120.3(3) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 118.4(3) . . ?
C9 C10 C12 120.7(3) . . ?
C11 C10 C12 121.0(3) . . ?
N2 C11 C10 122.6(3) . . ?
N2 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
O4 C12 O3 128.1(3) . . ?
O4 C12 C10 117.2(3) . . ?
O3 C12 C10 114.8(3) . . ?
O6 C13 O5 123.9(5) . . ?
O6 C13 H13 118.0 . . ?
O5 C13 H13 118.0 . . ?
C5 N1 C6 118.8(3) . . ?
C5 N1 Zn2 114.1(2) . 5 ?
C6 N1 Zn2 127.13(19) . 5 ?
C11 N2 C7 119.1(3) . . ?
C11 N2 Zn2 124.81(19) . 5 ?
C7 N2 Zn2 116.1(2) . 5 ?
C1 O1 Zn1 142.2(2) . . ?
C1 O2 Zn2 123.15(18) . . ?
C12 O3 Zn2 131.3(2) . 8_655 ?
C12 O4 Zn1 133.6(2) . 1_655 ?
C13 O5 Zn2 108.3(3) . . ?
C13 O5 Zn1 130.2(2) . . ?
Zn2 O5 Zn1 112.52(10) . . ?

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
O2 C1 C2 C3 -171.6(5) . . . . ?
O1 C1 C2 C3 10.1(6) . . . . ?
O2 C1 C2 C6 9.5(6) . . . . ?
O1 C1 C2 C6 -168.9(4) . . . . ?
C6 C2 C3 C4 2.2(9) . . . . ?
C1 C2 C3 C4 -176.8(6) . . . . ?
C2 C3 C4 C5 1.6(12) . . . . ?
C3 C4 C5 N1 -4.2(11) . . . . ?
C3 C4 C5 C7 175.6(7) . . . . ?
C3 C2 C6 N1 -3.9(7) . . . . ?
C1 C2 C6 N1 175.1(3) . . . . ?
N1 C5 C7 N2 -2.2(8) . . . . ?
C4 C5 C7 N2 178.0(6) . . . . ?
N1 C5 C7 C8 178.8(7) . . . . ?
C4 C5 C7 C8 -1.0(11) . . . . ?
N2 C7 C8 C9 1.9(12) . . . . ?
C5 C7 C8 C9 -179.1(7) . . . . ?
C7 C8 C9 C10 -1.9(13) . . . . ?
C8 C9 C10 C11 0.7(10) . . . . ?
C8 C9 C10 C12 -178.2(7) . . . . ?
C9 C10 C11 N2 0.6(7) . . . . ?
C12 C10 C11 N2 179.5(3) . . . . ?
C9 C10 C12 O4 -176.4(5) . . . . ?
C11 C10 C12 O4 4.8(6) . . . . ?
C9 C10 C12 O3 3.7(7) . . . . ?
C11 C10 C12 O3 -175.2(4) . . . . ?
C4 C5 N1 C6 2.7(8) . . . . ?
C7 C5 N1 C6 -177.2(4) . . . . ?
C4 C5 N1 Zn2 -176.7(5) . . . 5 ?
C7 C5 N1 Zn2 3.4(6) . . . 5 ?
C2 C6 N1 C5 1.4(6) . . . . ?
C2 C6 N1 Zn2 -179.2(3) . . . 5 ?
C10 C11 N2 C7 -0.6(6) . . . . ?
C10 C11 N2 Zn2 -179.9(3) . . . 5 ?
C8 C7 N2 C11 -0.7(9) . . . . ?
C5 C7 N2 C11 -179.7(4) . . . . ?
C8 C7 N2 Zn2 178.7(6) . . . 5 ?
C5 C7 N2 Zn2 -0.4(6) . . . 5 ?
O2 C1 O1 Zn1 5.7(7) . . . . ?
C2 C1 O1 Zn1 -176.1(3) . . . . ?
O1 C1 O2 Zn2 6.6(6) . . . . ?
C2 C1 O2 Zn2 -171.5(3) . . . . ?
O4 C12 O3 Zn2 2.1(6) . . . 8_655 ?
C10 C12 O3 Zn2 -177.9(3) . . . 8_655 ?
O3 C12 O4 Zn1 10.1(6) . . . 1_655 ?
C10 C12 O4 Zn1 -169.9(3) . . . 1_655 ?
O6 C13 O5 Zn2 1.1(7) . . . . ?
O6 C13 O5 Zn1 -142.7(5) . . . . ?

_refine_diff_density_max         0.569
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'solvothermal reaction'
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c2221
_database_code_depnum_ccdc_archive 'CCDC 1422815'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-08-18
_audit_creation_method           'Materials Studio'
_symmetry_space_group_name_H-M   C2221
_symmetry_Int_Tables_number      20
_symmetry_cell_setting           orthorhombic



# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                'close sample cryostat with Be domes'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   block

_pd_char_particle_morphology     ?
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                0
_pd_prep_temperature             77

_pd_instr_location               
;
KMC-2 beamline HZB (Berlin)
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
Boron nitride powder was used as external standard
;

_diffrn_ambient_temperature      77
_diffrn_radiation_wavelength     1.5406
_diffrn_source                   Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_source_target            ?
_diffrn_radiation_monochromator  'silicium monochromator'
_diffrn_measurement_method       '2 Theta scan'
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'Area detector'
_diffrn_detector_type            'VANTEC 2000 detector (Bruker)'
_pd_meas_scan_method             step
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        2225
_pd_meas_2theta_range_min        5.50000
_pd_meas_2theta_range_max        50.00000
_pd_meas_2theta_range_inc        0.020000
_pd_proc_ls_prof_R_factor        12.20
_pd_proc_ls_prof_wR_factor       15.68
_refine_ls_number_parameters     56
_refine_ls_number_restraints     12
_pd_proc_2theta_range_min        5.5000
_pd_proc_2theta_range_max        50.0000
_pd_proc_2theta_range_inc        0.020000
_pd_proc_wavelength              1.5406


loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-x,y,-z+1/2
x,-y,-z
x+1/2,y+1/2,z
-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
_cell_length_a                   27.8213
_cell_length_b                   10.1840
_cell_length_c                   21.6261
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
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
H1 H 0.27523 0.29051 0.89014 0.05000 Uiso 1.00
H2 H 0.05855 0.11382 0.09791 0.05000 Uiso 1.00
H3 H 0.14385 0.15415 0.11106 0.05000 Uiso 1.00
H4 H 0.14505 0.36462 0.93819 0.05000 Uiso 1.00
H5 H 0.89570 0.10554 0.06976 0.05000 Uiso 1.00
H6 H -0.01928 0.11855 0.08979 0.05000 Uiso 1.00
H7 H 0.91804 0.29214 0.89322 0.05000 Uiso 1.00
H8 H 0.17003 0.55542 0.88705 0.05000 Uiso 1.00
H9 H 0.20393 0.57936 0.66327 0.05000 Uiso 1.00
H10 H 0.12523 0.50826 0.69659 0.05000 Uiso 1.00
H11 H 0.88467 0.17203 0.82147 0.05000 Uiso 1.00
H12 H 0.36539 0.62281 0.62597 0.05000 Uiso 1.00
H13 H 0.28045 0.58917 0.64226 0.05000 Uiso 1.00
H14 H 0.98498 0.55689 0.92838 0.05000 Uiso 1.00
C1 C 0.27798 0.38922 0.87168 0.05000 Uiso 1.00
C2 C 0.20481 0.28080 0.03703 0.05000 Uiso 1.00
C3 C 0.07689 0.16920 0.06250 0.05000 Uiso 1.00
C4 C 0.12643 0.19041 0.06968 0.05000 Uiso 1.00
C5 C 0.15247 0.26505 0.02667 0.05000 Uiso 1.00
C6 C 0.12622 0.30989 0.97348 0.05000 Uiso 1.00
C7 C 0.05211 0.22136 0.01112 0.05000 Uiso 1.00
C8 C 0.91829 0.15070 0.03495 0.05000 Uiso 1.00
C9 C -0.03227 0.15640 0.04628 0.05000 Uiso 1.00
C10 C -0.00098 0.21012 1.00199 0.05000 Uiso 1.00
C11 C 0.93137 0.25356 0.93625 0.05000 Uiso 1.00
C12 C 0.89826 0.19658 0.97922 0.05000 Uiso 1.00
C13 C 0.34463 0.68232 0.96561 0.05000 Uiso 1.00
C14 C 0.09349 0.48678 0.81336 0.05000 Uiso 1.00
C15 C 0.14174 0.51397 0.79444 0.05000 Uiso 1.00
C16 C 0.17851 0.54563 0.83729 0.05000 Uiso 1.00
C17 C 0.23271 0.59977 0.75644 0.05000 Uiso 1.00
C18 C 0.19703 0.57317 0.71227 0.05000 Uiso 1.00
C19 C 0.15156 0.53324 0.73152 0.05000 Uiso 1.00
C20 C 0.28320 0.62501 0.74152 0.05000 Uiso 1.00
C21 C 0.36152 0.66069 0.78219 0.05000 Uiso 1.00
C22 C 0.88236 0.15685 0.72246 0.05000 Uiso 1.00
C23 C 0.35170 0.62814 0.67274 0.05000 Uiso 1.00
C24 C 0.30254 0.61181 0.68190 0.05000 Uiso 1.00
C25 C 0.93539 0.18341 0.71087 0.05000 Uiso 1.00
C26 C 0.99145 0.55190 0.87904 0.05000 Uiso 1.00
N1 N -0.01956 0.25886 0.94843 0.05000 Uiso 1.00
N2 N 0.07725 0.28633 0.96672 0.05000 Uiso 1.00
N3 N 0.31256 0.64836 0.79047 0.05000 Uiso 1.00
N4 N 0.22219 0.59310 0.81752 0.05000 Uiso 1.00
O1 O 0.28990 0.40525 0.81803 0.05000 Uiso 1.00
O2 O 0.26821 0.49752 0.90920 0.05000 Uiso 1.00
O3 O 0.22250 0.37965 0.00901 0.05000 Uiso 1.00
O4 O 0.22860 0.22771 0.08182 0.05000 Uiso 1.00
O5 O 0.31714 0.62625 1.00509 0.05000 Uiso 1.00
O6 O 0.32771 0.71485 0.91250 0.05000 Uiso 1.00
O7 O 0.08641 0.44494 0.86848 0.05000 Uiso 1.00
O8 O 0.05919 0.48878 0.77312 0.05000 Uiso 1.00
O9 O 0.95147 0.17968 0.65554 0.05000 Uiso 1.00
O10 O 0.95890 0.24326 0.75348 0.05000 Uiso 1.00
O11 O 0.99210 0.43092 0.84809 0.05000 Uiso 1.00
O12 O 0.99745 0.65313 0.85000 0.05000 Uiso 1.00
ZN1 Zn 0.27155 0.65986 0.87220 0.05000 Uiso 1.00
ZN4 Zn 0.03648 0.33657 0.89850 0.05000 Uiso 1.00
ZN2 Zn 0.26820 0.50000 0.00000 0.05000 Uiso 0.50
ZN3 Zn 0.00000 0.39345 0.75000 0.05000 Uiso 0.50

_chemical_name_systematic        'JLU-LIU4 (close pore phase)'
_chemical_name_common            'Liu-4_formic (close pore phase)'
_exptl_crystal_colour            colorless
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LIU4-aa
_database_code_depnum_ccdc_archive 'CCDC 1422816'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT222_LIU4-aa             
;
PROBLEM: Large Non-Solvent  H     Uiso(max)/Uiso(min) ...       10.0 Ratio 
RESPONSE: The large difference is explained by disorder of the actate anion
coordinated to the Zn cluster.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        LIU-4_aa
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H18 N4 O12 Zn3'
_chemical_formula_weight         798.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.0350 2.0980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.300(2)
_cell_length_b                   15.300(2)
_cell_length_c                   23.280(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5449.6(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    534
_cell_measurement_theta_min      3.76
_cell_measurement_theta_max      23.34

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.434
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.868
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Scala (Diederichs, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            19800
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.985
_diffrn_reflns_theta_max         36.156
_diffrn_reflns_theta_full        32.098
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6337
_reflns_number_gt                6099
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_max     0.965
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX



_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0651P)²+1.4186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.508(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6337
_refine_ls_number_parameters     215
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.21615(2) 0.21615(2) 0.2500 0.01888(12) Uani 1 2 d S T P . .
Zn2 Zn -0.16393(2) 0.26297(2) 0.11049(2) 0.01969(11) Uani 1 1 d . . . . .
C1 C -0.0281(2) 0.2124(2) 0.19213(14) 0.0293(7) Uani 1 1 d . . . . .
C2 C 0.0662(2) 0.1985(3) 0.21071(16) 0.0375(8) Uani 1 1 d . U . . .
C3 C 0.0848(3) 0.1715(5) 0.2660(2) 0.083(2) Uani 1 1 d . U . . .
H3 H 0.0395 0.1595 0.2915 0.099 Uiso 1 1 calc R U . . .
C4 C 0.1695(3) 0.1622(6) 0.2833(2) 0.091(2) Uani 1 1 d . U . . .
H4 H 0.1827 0.1417 0.3199 0.109 Uiso 1 1 calc R U . . .
C5 C 0.2358(2) 0.1841(4) 0.24498(16) 0.0528(12) Uani 1 1 d . U . . .
C6 C 0.1359(2) 0.2144(2) 0.17440(14) 0.0299(7) Uani 1 1 d . . . . .
H6 H 0.1241 0.2292 0.1364 0.036 Uiso 1 1 calc R U . . .
C7 C 0.3296(2) 0.1851(4) 0.26177(15) 0.0586(15) Uani 1 1 d . U . . .
C8 C 0.3564(3) 0.1649(7) 0.3179(2) 0.109(3) Uani 1 1 d . U . . .
H8 H 0.3160 0.1496 0.3460 0.131 Uiso 1 1 calc R U . . .
C9 C 0.4452(3) 0.1686(6) 0.33000(18) 0.088(3) Uani 1 1 d . U . . .
H9 H 0.4647 0.1556 0.3668 0.105 Uiso 1 1 calc R U . . .
C10 C 0.5040(2) 0.1909(3) 0.28853(16) 0.0407(9) Uani 1 1 d . U . . .
C11 C 0.4725(2) 0.2106(2) 0.23382(14) 0.0305(7) Uani 1 1 d . . . . .
H11 H 0.5123 0.2256 0.2053 0.037 Uiso 1 1 calc R U . . .
C12 C -0.1925(2) 0.3987(2) 0.19902(14) 0.0308(7) Uani 1 1 d . . . . .
C13 C -0.2486(4) 0.1162(3) 0.1365(2) 0.0579(12) Uani 1 1 d . . . . .
C14 C -0.3166(13) 0.0541(11) 0.1568(8) 0.294(13) Uani 1 1 d . . . . .
H14A H -0.3303 0.0662 0.1962 0.441 Uiso 1 1 calc R U . . .
H14B H -0.2951 -0.0047 0.1534 0.441 Uiso 1 1 calc R U . . .
H14C H -0.3683 0.0606 0.1338 0.441 Uiso 1 1 calc R U . . .
N1 N 0.21907(17) 0.2093(2) 0.19107(11) 0.0305(6) Uani 1 1 d . . . . .
N2 N 0.38736(17) 0.2088(2) 0.22053(11) 0.0300(6) Uani 1 1 d . . . . .
O1 O -0.08256(15) 0.2101(2) 0.23234(11) 0.0451(8) Uani 1 1 d . . . . .
O2 O -0.04266(14) 0.22621(19) 0.14033(10) 0.0343(5) Uani 1 1 d . . . . .
O3 O -0.2185(2) 0.34982(15) 0.23788(11) 0.0401(6) Uani 1 1 d . . . . .
O4 O -0.1684(2) 0.37863(16) 0.14959(11) 0.0404(7) Uani 1 1 d . . . . .
O5 O -0.23716(16) 0.18683(16) 0.16308(10) 0.0296(5) Uani 1 1 d . . . . .
O6 O -0.2138(4) 0.1023(3) 0.09026(19) 0.1023(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 2.065(2) 8 ?
Zn1 O3 2.065(2) . ?
Zn1 O1 2.087(2) 8 ?
Zn1 O1 2.087(2) . ?
Zn1 O5 2.097(2) . ?
Zn1 O5 2.097(2) 8 ?
Zn2 O4 1.991(2) . ?
Zn2 O5 2.028(2) . ?
Zn2 O2 2.059(2) . ?
Zn2 N2 2.088(3) 5_455 ?
Zn2 N1 2.197(3) 5_455 ?
C1 O2 1.244(4) . ?
C1 O1 1.253(4) . ?
C1 C2 1.521(4) . ?
C2 C3 1.382(6) . ?
C2 C6 1.382(5) . ?
C3 C4 1.365(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.338(4) . ?
C5 C7 1.487(5) . ?
C6 N1 1.333(4) . ?
C6 H6 0.9300 . ?
C7 N2 1.355(5) . ?
C7 C8 1.403(5) . ?
C8 C9 1.389(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.363(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.395(5) . ?
C10 C12 1.517(4) 8_655 ?
C11 N2 1.339(4) . ?
C11 H11 0.9300 . ?
C12 O3 1.240(4) . ?
C12 O4 1.247(4) . ?
C12 C10 1.517(4) 8_565 ?
C13 O6 1.220(7) . ?
C13 O5 1.257(5) . ?
C13 C14 1.486(17) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
N1 Zn2 2.196(3) 5 ?
N2 Zn2 2.088(3) 5 ?

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
O3 Zn1 O3 89.05(18) 8 . ?
O3 Zn1 O1 91.98(13) 8 8 ?
O3 Zn1 O1 176.17(11) . 8 ?
O3 Zn1 O1 176.17(11) 8 . ?
O3 Zn1 O1 91.98(13) . . ?
O1 Zn1 O1 87.2(2) 8 . ?
O3 Zn1 O5 89.08(10) 8 . ?
O3 Zn1 O5 94.43(10) . . ?
O1 Zn1 O5 89.28(10) 8 . ?
O1 Zn1 O5 87.17(10) . . ?
O3 Zn1 O5 94.43(10) 8 8 ?
O3 Zn1 O5 89.08(10) . 8 ?
O1 Zn1 O5 87.16(10) 8 8 ?
O1 Zn1 O5 89.28(10) . 8 ?
O5 Zn1 O5 175.09(14) . 8 ?
O4 Zn2 O5 102.45(11) . . ?
O4 Zn2 O2 96.85(12) . . ?
O5 Zn2 O2 97.89(10) . . ?
O4 Zn2 N2 104.01(12) . 5_455 ?
O5 Zn2 N2 150.68(11) . 5_455 ?
O2 Zn2 N2 91.29(10) . 5_455 ?
O4 Zn2 N1 92.89(12) . 5_455 ?
O5 Zn2 N1 89.45(10) . 5_455 ?
O2 Zn2 N1 166.22(10) . 5_455 ?
N2 Zn2 N1 76.87(10) 5_455 5_455 ?
O2 C1 O1 127.6(3) . . ?
O2 C1 C2 117.9(3) . . ?
O1 C1 C2 114.4(3) . . ?
C3 C2 C6 117.6(3) . . ?
C3 C2 C1 120.2(3) . . ?
C6 C2 C1 122.2(3) . . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.5(4) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 122.2(4) . . ?
N1 C5 C7 115.3(3) . . ?
C4 C5 C7 122.5(4) . . ?
N1 C6 C2 123.3(3) . . ?
N1 C6 H6 118.4 . . ?
C2 C6 H6 118.4 . . ?
N2 C7 C8 121.8(4) . . ?
N2 C7 C5 116.5(3) . . ?
C8 C7 C5 121.6(4) . . ?
C9 C8 C7 117.8(4) . . ?
C9 C8 H8 121.1 . . ?
C7 C8 H8 121.1 . . ?
C10 C9 C8 120.8(4) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 118.2(3) . . ?
C9 C10 C12 121.1(3) . 8_655 ?
C11 C10 C12 120.7(3) . 8_655 ?
N2 C11 C10 122.9(3) . . ?
N2 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
O3 C12 O4 128.3(3) . . ?
O3 C12 C10 117.3(3) . 8_565 ?
O4 C12 C10 114.4(3) . 8_565 ?
O6 C13 O5 121.5(5) . . ?
O6 C13 C14 118.3(9) . . ?
O5 C13 C14 119.4(9) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 N1 C5 118.2(3) . . ?
C6 N1 Zn2 127.5(2) . 5 ?
C5 N1 Zn2 114.4(2) . 5 ?
C11 N2 C7 118.4(3) . . ?
C11 N2 Zn2 124.8(2) . 5 ?
C7 N2 Zn2 116.8(2) . 5 ?
C1 O1 Zn1 142.8(2) . . ?
C1 O2 Zn2 122.3(2) . . ?
C12 O3 Zn1 133.8(2) . . ?
C12 O4 Zn2 130.6(2) . . ?
C13 O5 Zn2 105.9(3) . . ?
C13 O5 Zn1 132.8(3) . . ?
Zn2 O5 Zn1 112.03(11) . . ?

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
O2 C1 C2 C3 -171.3(5) . . . . ?
O1 C1 C2 C3 10.1(7) . . . . ?
O2 C1 C2 C6 10.5(6) . . . . ?
O1 C1 C2 C6 -168.2(4) . . . . ?
C6 C2 C3 C4 0.8(11) . . . . ?
C1 C2 C3 C4 -177.5(7) . . . . ?
C2 C3 C4 C5 2.7(13) . . . . ?
C3 C4 C5 N1 -3.6(12) . . . . ?
C3 C4 C5 C7 173.5(7) . . . . ?
C3 C2 C6 N1 -3.8(7) . . . . ?
C1 C2 C6 N1 174.5(4) . . . . ?
N1 C5 C7 N2 -1.8(8) . . . . ?
C4 C5 C7 N2 -179.0(7) . . . . ?
N1 C5 C7 C8 176.4(7) . . . . ?
C4 C5 C7 C8 -0.8(11) . . . . ?
N2 C7 C8 C9 -1.1(13) . . . . ?
C5 C7 C8 C9 -179.2(7) . . . . ?
C7 C8 C9 C10 -0.1(14) . . . . ?
C8 C9 C10 C11 0.5(12) . . . . ?
C8 C9 C10 C12 -178.2(7) . . . 8_655 ?
C9 C10 C11 N2 0.3(8) . . . . ?
C12 C10 C11 N2 179.0(4) 8_655 . . . ?
C2 C6 N1 C5 3.0(7) . . . . ?
C2 C6 N1 Zn2 -177.6(3) . . . 5 ?
C4 C5 N1 C6 0.8(9) . . . . ?
C7 C5 N1 C6 -176.5(4) . . . . ?
C4 C5 N1 Zn2 -178.7(6) . . . 5 ?
C7 C5 N1 Zn2 4.1(6) . . . 5 ?
C10 C11 N2 C7 -1.4(7) . . . . ?
C10 C11 N2 Zn2 -179.7(3) . . . 5 ?
C8 C7 N2 C11 1.8(9) . . . . ?
C5 C7 N2 C11 180.0(5) . . . . ?
C8 C7 N2 Zn2 -179.8(6) . . . 5 ?
C5 C7 N2 Zn2 -1.6(7) . . . 5 ?
O2 C1 O1 Zn1 4.7(8) . . . . ?
C2 C1 O1 Zn1 -176.8(4) . . . . ?
O1 C1 O2 Zn2 7.1(6) . . . . ?
C2 C1 O2 Zn2 -171.3(3) . . . . ?
O4 C12 O3 Zn1 13.0(7) . . . . ?
C10 C12 O3 Zn1 -168.4(3) 8_565 . . . ?
O3 C12 O4 Zn2 2.1(6) . . . . ?
C10 C12 O4 Zn2 -176.5(3) 8_565 . . . ?
O6 C13 O5 Zn2 4.4(7) . . . . ?
C14 C13 O5 Zn2 -165.6(9) . . . . ?
O6 C13 O5 Zn1 -138.3(5) . . . . ?
C14 C13 O5 Zn1 51.7(11) . . . . ?

_refine_diff_density_max         0.629
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.088

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Liu4_2_cp
_database_code_depnum_ccdc_archive 'CCDC 1422817'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-08-31
_audit_creation_method           'Materials Studio'
_symmetry_space_group_name_H-M   C2221
_symmetry_Int_Tables_number      20
_symmetry_cell_setting           orthorhombic

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                capillary
_pd_spec_mount_mode              transmission
_pd_spec_shape                   block

_pd_char_particle_morphology     ?
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                101
_pd_prep_temperature             298

_pd_instr_location               
;
KMC-2 beamline HZB (Berlin)
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
Boron nitride powder was used as external standard
;

_diffrn_ambient_temperature      77
_diffrn_radiation_wavelength     1.5406
_diffrn_source                   'STOE P'
_diffrn_radiation_type           CuK\a
_diffrn_source_target            ?
_diffrn_radiation_monochromator  'germanium monochromator'
_diffrn_measurement_method       '2 Theta scan'
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'Area detector'
_diffrn_detector_type            Mythen
_pd_meas_scan_method             step
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        4533
_pd_meas_2theta_range_min        2.00000
_pd_meas_2theta_range_max        70.00000
_pd_meas_2theta_range_inc        0.015000
_pd_proc_ls_prof_R_factor        6.94
_pd_proc_ls_prof_wR_factor       9.06
_refine_ls_number_parameters     68
_refine_ls_number_restraints     14
_pd_proc_2theta_range_min        2.0000
_pd_proc_2theta_range_max        70.0000
_pd_proc_2theta_range_inc        0.015000
_pd_proc_wavelength              1.5406


loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-x,y,-z+1/2
x,-y,-z
x+1/2,y+1/2,z
-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
_cell_length_a                   27.7150
_cell_length_b                   10.5745
_cell_length_c                   21.6912
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
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
C1 C 0.28670 0.25359 0.90160 0.05000 Uiso 1.00
H2 H 0.05773 0.14113 0.09953 0.05000 Uiso 1.00
H3 H 0.14525 0.16015 0.10913 0.05000 Uiso 1.00
H4 H 0.15445 0.30300 0.92291 0.05000 Uiso 1.00
H5 H 0.89517 0.13422 0.06676 0.05000 Uiso 1.00
H6 H -0.01890 0.13901 0.08736 0.05000 Uiso 1.00
H7 H 0.92132 0.28788 0.88514 0.05000 Uiso 1.00
H8 H 0.16145 0.56699 0.88774 0.05000 Uiso 1.00
H9 H 0.20403 0.53652 0.66763 0.05000 Uiso 1.00
H10 H 0.12134 0.50132 0.69798 0.05000 Uiso 1.00
H11 H 0.87923 0.16990 0.83019 0.05000 Uiso 1.00
H12 H 0.36813 0.57042 0.63873 0.05000 Uiso 1.00
H13 H 0.28261 0.53577 0.65191 0.05000 Uiso 1.00
C14 C 0.99638 0.54899 0.92275 0.05000 Uiso 1.00
C15 C 0.28462 0.38778 0.87799 0.05000 Uiso 1.00
C16 C 0.20794 0.27910 0.03412 0.05000 Uiso 1.00
C17 C 0.07795 0.17572 0.06021 0.05000 Uiso 1.00
C18 C 0.12866 0.18467 0.06545 0.05000 Uiso 1.00
C19 C 0.15760 0.23300 0.01740 0.05000 Uiso 1.00
C20 C 0.13320 0.26832 0.96136 0.05000 Uiso 1.00
C21 C 0.05433 0.21928 0.00660 0.05000 Uiso 1.00
C22 C 0.91883 0.17024 0.03085 0.05000 Uiso 1.00
C23 C -0.03137 0.17095 0.04267 0.05000 Uiso 1.00
C24 C 0.00105 0.21216 0.99698 0.05000 Uiso 1.00
C25 C 0.93393 0.25450 0.92935 0.05000 Uiso 1.00
C26 C 0.89969 0.20920 0.97338 0.05000 Uiso 1.00
C27 C 0.34701 0.68007 0.96007 0.05000 Uiso 1.00
C28 C 0.08472 0.49146 0.81311 0.05000 Uiso 1.00
C29 C 0.13406 0.53417 0.79548 0.05000 Uiso 1.00
C30 C 0.16997 0.56840 0.83903 0.05000 Uiso 1.00
C31 C 0.22944 0.58284 0.76022 0.05000 Uiso 1.00
C32 C 0.19473 0.55163 0.71537 0.05000 Uiso 1.00
C33 C 0.14706 0.53092 0.73298 0.05000 Uiso 1.00
C34 C 0.28042 0.60917 0.74612 0.05000 Uiso 1.00
C35 C 0.35749 0.64985 0.79043 0.05000 Uiso 1.00
C36 C 0.88098 0.12872 0.73334 0.05000 Uiso 1.00
C37 C 0.35238 0.58764 0.68376 0.05000 Uiso 1.00
C38 C 0.30267 0.57390 0.69040 0.05000 Uiso 1.00
C39 C 0.92935 0.19040 0.71892 0.05000 Uiso 1.00
C40 C 0.98268 0.51440 0.85846 0.05000 Uiso 1.00
N41 N -0.01677 0.25412 0.94187 0.05000 Uiso 1.00
N42 N 0.08318 0.26219 0.95590 0.05000 Uiso 1.00
N43 N 0.30773 0.64457 0.79536 0.05000 Uiso 1.00
N44 N 0.21624 0.59682 0.82017 0.05000 Uiso 1.00
O45 O 0.29475 0.40519 0.82385 0.05000 Uiso 1.00
O46 O 0.27095 0.49259 0.91488 0.05000 Uiso 1.00
O47 O 0.22537 0.37052 0.00242 0.05000 Uiso 1.00
O48 O 0.22845 0.24749 0.08563 0.05000 Uiso 1.00
O49 O 0.32513 0.60645 0.99720 0.05000 Uiso 1.00
O50 O 0.32501 0.71461 0.91070 0.05000 Uiso 1.00
O51 O 0.07794 0.44128 0.86615 0.05000 Uiso 1.00
O52 O 0.05158 0.48830 0.77137 0.05000 Uiso 1.00
O53 O 0.94370 0.18473 0.66297 0.05000 Uiso 1.00
O54 O 0.95168 0.26013 0.75830 0.05000 Uiso 1.00
O55 O 0.99235 0.39157 0.83530 0.05000 Uiso 1.00
O56 O 0.96459 0.59588 0.82553 0.05000 Uiso 1.00
Zn57 Zn 0.27019 0.64123 0.87433 0.05000 Uiso 1.00
Zn58 Zn 0.03758 0.31205 0.88494 0.05000 Uiso 1.00
H59 H 1.02213 0.62920 0.92059 0.05000 Uiso 1.00
H60 H 1.01487 0.46969 0.94649 0.05000 Uiso 1.00
H61 H 0.96354 0.57641 0.94915 0.05000 Uiso 1.00
H62 H 0.76018 0.69568 0.87580 0.05000 Uiso 1.00
H63 H 0.77731 0.74287 0.95051 0.05000 Uiso 1.00
H64 H 0.82375 0.71476 0.89479 0.05000 Uiso 1.00
Zn65 Zn 0.27170 0.50000 0.00000 0.05000 Uiso 0.50
Zn66 Zn 0.00000 0.38455 0.75000 0.05000 Uiso 0.50
_chemical_name_systematic        'Liu-4_acetic (close pore phase)'
_chemical_name_common            'Liu-4_acetic (close pore phase)'
_exptl_crystal_colour            colorless
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LIU4-ba
_database_code_depnum_ccdc_archive 'CCDC 1422818'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        LIU-4_ba
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H22 N4 O12 Zn3'
_chemical_formula_weight         922.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.0350 2.0980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.160(2)
_cell_length_b                   15.160(2)
_cell_length_c                   23.030(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5292.9(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    365
_cell_measurement_theta_min      3.98
_cell_measurement_theta_max      24.36

_exptl_crystal_description       octrahedron
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.520
_shelx_estimated_absorpt_T_min   0.863
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Scala (Diederichs, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            40507
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.004
_diffrn_reflns_theta_max         35.689
_diffrn_reflns_theta_full        32.098
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6196
_reflns_number_gt                5442
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX


_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1163P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.252(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6196
_refine_ls_number_parameters     247
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1546
_refine_ls_wR_factor_gt          0.1480
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.079
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.21492(4) 0.21492(4) 0.0000 0.0301(2) Uani 1 2 d S T P . .
Zn2 Zn 0.16181(4) 0.25464(4) 0.14319(2) 0.03311(19) Uani 1 1 d . . . . .
C1 C 0.1921(4) 0.3948(3) 0.0557(2) 0.0452(13) Uani 1 1 d . . . . .
C2 C 0.1870(6) 0.4930(4) 0.0421(3) 0.0606(19) Uani 1 1 d . . . . .
C3 C 0.1559(11) 0.5538(5) 0.0821(4) 0.127(6) Uani 1 1 d . . . . .
H3 H 0.1380 0.5348 0.1186 0.152 Uiso 1 1 calc R U . . .
C4 C 0.1514(12) 0.6407(5) 0.0685(3) 0.139(7) Uani 1 1 d . . . . .
H4 H 0.1289 0.6811 0.0950 0.167 Uiso 1 1 calc R U . . .
C5 C 0.1812(8) 0.6684(4) 0.0142(3) 0.080(3) Uani 1 1 d . . . . .
C6 C 0.2130(4) 0.5253(4) -0.0110(2) 0.0450(12) Uani 1 1 d . . . . .
H6 H 0.2326 0.4855 -0.0389 0.054 Uiso 1 1 calc R U . . .
C7 C 0.1831(8) 0.7608(4) -0.0033(3) 0.083(3) Uani 1 1 d . . . . .
C8 C 0.1558(12) 0.8282(5) 0.0352(4) 0.148(7) Uani 1 1 d . . . . .
H8 H 0.1315 0.8148 0.0712 0.178 Uiso 1 1 calc R U . . .
C9 C 0.1668(10) 0.9162(4) 0.0171(3) 0.120(5) Uani 1 1 d . . . . .
H9 H 0.1540 0.9625 0.0422 0.143 Uiso 1 1 calc R U . . .
C10 C 0.1970(5) 0.9331(3) -0.0390(3) 0.0552(17) Uani 1 1 d . . . . .
C11 C 0.2162(5) 0.8618(3) -0.0739(2) 0.0441(13) Uani 1 1 d . . . . .
H11 H 0.2336 0.8727 -0.1119 0.053 Uiso 1 1 calc R U . . .
C12 C 0.0276(3) 0.2098(4) 0.0592(2) 0.0436(12) Uani 1 1 d . . . . .
C13 C 0.2445(5) 0.1100(5) 0.1205(3) 0.0654(18) Uani 1 1 d . . . . .
C14 C 0.3064(6) 0.0352(5) 0.1091(4) 0.113(4) Uani 1 1 d G U . . .
C15 C 0.3684(7) 0.0426(5) 0.0649(4) 0.145(6) Uani 1 1 d G U . . .
H15 H 0.3725 0.0946 0.0436 0.174 Uiso 1 1 calc R U . . .
C16 C 0.4243(7) -0.0276(7) 0.0526(4) 0.194(8) Uani 1 1 d G U . . .
H16 H 0.4658 -0.0226 0.0230 0.233 Uiso 1 1 calc R U . . .
C17 C 0.4183(9) -0.1052(6) 0.0845(5) 0.251(11) Uani 1 1 d G U . . .
H17 H 0.4557 -0.1522 0.0763 0.301 Uiso 1 1 calc R U . . .
C18 C 0.3563(9) -0.1126(5) 0.1287(6) 0.217(9) Uani 1 1 d G U . . .
H18 H 0.3522 -0.1645 0.1500 0.261 Uiso 1 1 calc R U . . .
C19 C 0.3004(7) -0.0424(6) 0.1410(5) 0.180(7) Uani 1 1 d G U . . .
H19 H 0.2589 -0.0473 0.1706 0.216 Uiso 1 1 calc R U . . .
N1 N 0.2116(4) 0.6104(3) -0.02450(18) 0.0464(11) Uani 1 1 d . . . . .
N2 N 0.2111(4) 0.7776(3) -0.0562(2) 0.0480(12) Uani 1 1 d . . . . .
O1 O 0.2218(3) 0.3475(2) 0.01774(18) 0.0528(10) Uani 1 1 d . . . . .
O2 O 0.1645(3) 0.3735(3) 0.10557(18) 0.0544(11) Uani 1 1 d . . . . .
O3 O 0.0828(3) 0.2085(4) 0.0200(2) 0.0652(14) Uani 1 1 d . . . . .
O4 O 0.0397(2) 0.2213(3) 0.11150(17) 0.0512(10) Uani 1 1 d . . . . .
O5 O 0.2448(3) 0.1789(3) 0.08816(17) 0.0457(9) Uani 1 1 d . . . . .
O6 O 0.1941(5) 0.1090(5) 0.1637(3) 0.092(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.053(4) 6 ?
Zn1 O1 2.053(4) . ?
Zn1 O3 2.057(4) . ?
Zn1 O3 2.058(4) 6 ?
Zn1 O5 2.151(4) . ?
Zn1 O5 2.151(4) 6 ?
Zn2 O2 2.000(4) . ?
Zn2 O4 2.053(4) . ?
Zn2 N1 2.112(4) 4_455 ?
Zn2 O5 2.123(4) . ?
Zn2 N2 2.170(4) 4_455 ?
Zn2 O6 2.310(7) . ?
Zn2 C13 2.579(8) . ?
C1 O1 1.217(7) . ?
C1 O2 1.264(7) . ?
C1 C2 1.524(8) . ?
C2 C6 1.376(8) . ?
C2 C3 1.384(10) . ?
C3 C4 1.355(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(9) . ?
C4 H4 0.9300 . ?
C5 N1 1.334(8) . ?
C5 C7 1.458(9) . ?
C6 N1 1.327(7) . ?
C6 H6 0.9300 . ?
C7 N2 1.316(8) . ?
C7 C8 1.415(10) . ?
C8 C9 1.409(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.394(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(8) . ?
C10 C12 1.518(7) 6_565 ?
C11 N2 1.341(7) . ?
C11 H11 0.9300 . ?
C12 O3 1.230(7) . ?
C12 O4 1.231(7) . ?
C12 C10 1.518(7) 6_455 ?
C13 O6 1.255(9) . ?
C13 O5 1.282(8) . ?
C13 C14 1.495(9) . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C15 C16 1.3900 . ?
C15 H15 0.9300 . ?
C16 C17 1.3900 . ?
C16 H16 0.9300 . ?
C17 C18 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
N1 Zn2 2.112(4) 2_554 ?
N2 Zn2 2.170(4) 2_554 ?

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 O1 86.6(3) 6 . ?
O1 Zn1 O3 178.50(17) 6 . ?
O1 Zn1 O3 92.9(2) . . ?
O1 Zn1 O3 92.9(2) 6 6 ?
O1 Zn1 O3 178.50(17) . 6 ?
O3 Zn1 O3 87.6(3) . 6 ?
O1 Zn1 O5 89.69(17) 6 . ?
O1 Zn1 O5 92.88(16) . . ?
O3 Zn1 O5 88.91(18) . . ?
O3 Zn1 O5 88.53(17) 6 . ?
O1 Zn1 O5 92.89(16) 6 6 ?
O1 Zn1 O5 89.70(17) . 6 ?
O3 Zn1 O5 88.53(17) . 6 ?
O3 Zn1 O5 88.91(18) 6 6 ?
O5 Zn1 O5 176.5(2) . 6 ?
O2 Zn2 O4 95.0(2) . . ?
O2 Zn2 N1 100.3(2) . 4_455 ?
O4 Zn2 N1 92.63(16) . 4_455 ?
O2 Zn2 O5 102.52(17) . . ?
O4 Zn2 O5 100.87(17) . . ?
N1 Zn2 O5 152.28(18) 4_455 . ?
O2 Zn2 N2 90.0(2) . 4_455 ?
O4 Zn2 N2 168.33(16) . 4_455 ?
N1 Zn2 N2 76.07(17) 4_455 4_455 ?
O5 Zn2 N2 88.30(17) . 4_455 ?
O2 Zn2 O6 161.0(2) . . ?
O4 Zn2 O6 91.6(2) . . ?
N1 Zn2 O6 97.2(2) 4_455 . ?
O5 Zn2 O6 58.64(19) . . ?
N2 Zn2 O6 87.0(2) 4_455 . ?
O2 Zn2 C13 131.9(2) . . ?
O4 Zn2 C13 99.0(2) . . ?
N1 Zn2 C13 124.5(2) 4_455 . ?
O5 Zn2 C13 29.68(19) . . ?
N2 Zn2 C13 85.3(2) 4_455 . ?
O6 Zn2 C13 29.1(2) . . ?
O1 C1 O2 128.6(5) . . ?
O1 C1 C2 116.6(5) . . ?
O2 C1 C2 114.8(5) . . ?
C6 C2 C3 116.9(6) . . ?
C6 C2 C1 121.0(6) . . ?
C3 C2 C1 122.1(6) . . ?
C4 C3 C2 120.7(7) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 118.9(8) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 120.8(6) . . ?
N1 C5 C7 116.2(5) . . ?
C4 C5 C7 122.9(6) . . ?
N1 C6 C2 123.3(6) . . ?
N1 C6 H6 118.3 . . ?
C2 C6 H6 118.3 . . ?
N2 C7 C8 122.4(6) . . ?
N2 C7 C5 116.7(6) . . ?
C8 C7 C5 120.9(6) . . ?
C9 C8 C7 117.6(7) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
C10 C9 C8 119.2(6) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C10 C9 117.7(5) . . ?
C11 C10 C12 122.3(5) . 6_565 ?
C9 C10 C12 119.9(5) . 6_565 ?
N2 C11 C10 123.9(5) . . ?
N2 C11 H11 118.1 . . ?
C10 C11 H11 118.1 . . ?
O3 C12 O4 128.1(5) . . ?
O3 C12 C10 114.5(5) . 6_455 ?
O4 C12 C10 117.3(5) . 6_455 ?
O6 C13 O5 118.2(7) . . ?
O6 C13 C14 120.8(7) . . ?
O5 C13 C14 120.8(6) . . ?
O6 C13 Zn2 63.5(4) . . ?
O5 C13 Zn2 55.1(3) . . ?
C14 C13 Zn2 170.2(7) . . ?
C15 C14 C19 120.0 . . ?
C15 C14 C13 119.5(6) . . ?
C19 C14 C13 120.5(6) . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C14 120.0 . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
C6 N1 C5 119.3(5) . . ?
C6 N1 Zn2 124.4(4) . 2_554 ?
C5 N1 Zn2 116.1(4) . 2_554 ?
C7 N2 C11 118.9(5) . . ?
C7 N2 Zn2 114.7(4) . 2_554 ?
C11 N2 Zn2 126.4(4) . 2_554 ?
C1 O1 Zn1 134.5(4) . . ?
C1 O2 Zn2 129.1(4) . . ?
C12 O3 Zn1 145.7(4) . . ?
C12 O4 Zn2 121.2(3) . . ?
C13 O5 Zn2 95.2(4) . . ?
C13 O5 Zn1 139.0(5) . . ?
Zn2 O5 Zn1 107.53(17) . . ?
C13 O6 Zn2 87.4(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 C1 C2 C6 1.3(11) . . . . ?
O2 C1 C2 C6 -178.6(7) . . . . ?
O1 C1 C2 C3 -178.9(10) . . . . ?
O2 C1 C2 C3 1.2(13) . . . . ?
C6 C2 C3 C4 0(2) . . . . ?
C1 C2 C3 C4 -179.4(13) . . . . ?
C2 C3 C4 C5 -2(3) . . . . ?
C3 C4 C5 N1 2(2) . . . . ?
C3 C4 C5 C7 -176.9(14) . . . . ?
C3 C2 C6 N1 1.7(13) . . . . ?
C1 C2 C6 N1 -178.5(7) . . . . ?
N1 C5 C7 N2 2.8(15) . . . . ?
C4 C5 C7 N2 -178.7(13) . . . . ?
N1 C5 C7 C8 -177.4(12) . . . . ?
C4 C5 C7 C8 1(2) . . . . ?
N2 C7 C8 C9 -6(2) . . . . ?
C5 C7 C8 C9 174.6(13) . . . . ?
C7 C8 C9 C10 5(2) . . . . ?
C8 C9 C10 C11 -1.0(19) . . . . ?
C8 C9 C10 C12 -179.7(12) . . . 6_565 ?
C9 C10 C11 N2 -3.1(13) . . . . ?
C12 C10 C11 N2 175.6(7) 6_565 . . . ?
O6 C13 C14 C15 -172.7(8) . . . . ?
O5 C13 C14 C15 3.7(13) . . . . ?
O6 C13 C14 C19 9.5(13) . . . . ?
O5 C13 C14 C19 -174.1(7) . . . . ?
C19 C14 C15 C16 0.0 . . . . ?
C13 C14 C15 C16 -177.8(11) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C14 0.0 . . . . ?
C15 C14 C19 C18 0.0 . . . . ?
C13 C14 C19 C18 177.8(11) . . . . ?
C2 C6 N1 C5 -2.1(12) . . . . ?
C2 C6 N1 Zn2 -177.0(6) . . . 2_554 ?
C4 C5 N1 C6 0.4(16) . . . . ?
C7 C5 N1 C6 178.9(8) . . . . ?
C4 C5 N1 Zn2 175.7(11) . . . 2_554 ?
C7 C5 N1 Zn2 -5.8(12) . . . 2_554 ?
C8 C7 N2 C11 1.8(16) . . . . ?
C5 C7 N2 C11 -178.4(8) . . . . ?
C8 C7 N2 Zn2 -178.3(11) . . . 2_554 ?
C5 C7 N2 Zn2 1.4(12) . . . 2_554 ?
C10 C11 N2 C7 2.7(12) . . . . ?
C10 C11 N2 Zn2 -177.1(6) . . . 2_554 ?
O2 C1 O1 Zn1 19.8(11) . . . . ?
C2 C1 O1 Zn1 -160.1(5) . . . . ?
O1 C1 O2 Zn2 2.2(11) . . . . ?
C2 C1 O2 Zn2 -177.9(5) . . . . ?
O4 C12 O3 Zn1 3.5(16) . . . . ?
C10 C12 O3 Zn1 -177.7(7) 6_455 . . . ?
O3 C12 O4 Zn2 6.5(11) . . . . ?
C10 C12 O4 Zn2 -172.3(5) 6_455 . . . ?
O6 C13 O5 Zn2 7.1(8) . . . . ?
C14 C13 O5 Zn2 -169.4(8) . . . . ?
O6 C13 O5 Zn1 -117.5(8) . . . . ?
C14 C13 O5 Zn1 66.1(12) . . . . ?
Zn2 C13 O5 Zn1 -124.5(7) . . . . ?
O5 C13 O6 Zn2 -6.5(8) . . . . ?
C14 C13 O6 Zn2 170.0(9) . . . . ?

_refine_diff_density_max         0.656
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.123

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LIU4_ba_cp
_database_code_depnum_ccdc_archive 'CCDC 1422819'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-08-18
_audit_creation_method           'Materials Studio'
_symmetry_space_group_name_H-M   P43212
_symmetry_Int_Tables_number      96
_symmetry_cell_setting           tetragonal

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                'close sample cryostat with Be domes'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   block

_pd_char_particle_morphology     ?
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                0
_pd_prep_temperature             77

_pd_instr_location               
;
KMC-2 beamline HZB (Berlin)
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
Boron nitride powder was used as external standard
;

_diffrn_ambient_temperature      77
_diffrn_radiation_wavelength     1.5406
_diffrn_source                   Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_source_target            ?
_diffrn_radiation_monochromator  'silicium monochromator'
_diffrn_measurement_method       '2 Theta scan'
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'Area detector'
_diffrn_detector_type            'VANTEC 2000 detector (Bruker)'
_pd_meas_scan_method             step
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        2400
_pd_meas_2theta_range_min        2.00000
_pd_meas_2theta_range_max        50.00000
_pd_meas_2theta_range_inc        0.020000
_pd_proc_ls_prof_R_factor        12.10
_pd_proc_ls_prof_wR_factor       17.99
_refine_ls_number_parameters     28
_refine_ls_number_restraints     6
_pd_proc_2theta_range_min        2.0000
_pd_proc_2theta_range_max        50.0000
_pd_proc_2theta_range_inc        0.020000
_pd_proc_wavelength              1.5406

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-y+1/2,x+1/2,z+3/4
y+1/2,-x+1/2,z+1/4
-x+1/2,y+1/2,-z+3/4
x+1/2,-y+1/2,-z+1/4
y,x,-z
-y,-x,-z+1/2
_cell_length_a                   15.0193
_cell_length_b                   15.0193
_cell_length_c                   21.9053
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
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
C14 C 0.29453 0.03064 0.11376 0.05000 Uiso 1.00
C15 C 0.28844 -0.04409 0.14897 0.05000 Uiso 1.00
H15 H 0.24875 -0.04540 0.17967 0.05000 Uiso 1.00
C16 C 0.34180 -0.11670 0.13832 0.05000 Uiso 1.00
H16 H 0.33772 -0.16665 0.16190 0.05000 Uiso 1.00
C17 C 0.40114 -0.11476 0.09248 0.05000 Uiso 1.00
H17 H 0.43685 -0.16331 0.08535 0.05000 Uiso 1.00
C18 C 0.40722 -0.04003 0.05728 0.05000 Uiso 1.00
H18 H 0.44692 -0.03872 0.02657 0.05000 Uiso 1.00
C19 C 0.35386 0.03258 0.06792 0.05000 Uiso 1.00
H19 H 0.35785 0.08252 0.04434 0.05000 Uiso 1.00
Zn2 Zn 0.15590 0.24036 0.15000 0.05000 Uiso 1.00
N1 N 0.21746 0.59879 -0.02220 0.05000 Uiso 1.00
N2 N 0.21894 0.77061 -0.05533 0.05000 Uiso 1.00
O1 O 0.23261 0.17448 0.08960 0.05000 Uiso 1.00
O2 O 0.21481 0.33884 0.01726 0.05000 Uiso 1.00
O3 O 0.15869 0.35801 0.10611 0.05000 Uiso 1.00
O4 O 0.07269 0.20134 0.02500 0.05000 Uiso 1.00
O5 O 0.03463 0.20274 0.11757 0.05000 Uiso 1.00
O8 O 0.18398 0.10907 0.16809 0.05000 Uiso 1.00
C1 C 0.18794 0.38295 0.05751 0.05000 Uiso 1.00
C2 C 0.18887 0.48173 0.04421 0.05000 Uiso 1.00
C3 C 0.21955 0.51453 -0.00819 0.05000 Uiso 1.00
H3 H 0.24284 0.47481 -0.03494 0.05000 Uiso 1.00
C4 C 0.18225 0.65683 0.01567 0.05000 Uiso 1.00
C5 C 0.15107 0.62944 0.06842 0.05000 Uiso 1.00
H5 H 0.12753 0.67004 0.09446 0.05000 Uiso 1.00
C6 C 0.15489 0.54240 0.08251 0.05000 Uiso 1.00
H6 H 0.13434 0.52371 0.11843 0.05000 Uiso 1.00
C7 C 0.17617 0.75184 -0.00724 0.05000 Uiso 1.00
C8 C 0.13579 0.81662 0.02593 0.05000 Uiso 1.00
H8 H 0.10838 0.80241 0.06050 0.05000 Uiso 1.00
C9 C -0.14600 0.21927 0.07456 0.05000 Uiso 1.00
H9 H -0.13396 0.24715 0.10934 0.05000 Uiso 1.00
C10 C -0.07704 0.18077 0.04556 0.05000 Uiso 1.00
C11 C -0.09653 0.13762 -0.00576 0.05000 Uiso 1.00
H11 H -0.05208 0.11004 -0.02646 0.05000 Uiso 1.00
C12 C 0.01941 0.19629 0.06559 0.05000 Uiso 1.00
C13 C 0.23353 0.10854 0.12428 0.05000 Uiso 1.00
Zn1 Zn 0.20931 0.20931 0.00000 0.05000 Uiso 0.50
_chemical_name_systematic        'Liu-4_benzoic (close pore phase)'
_chemical_name_common            'Liu-4_benzoic_cp (close pore phase)'
_exptl_crystal_colour            colorless
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LIU4-ca
_database_code_depnum_ccdc_archive 'CCDC 1422820'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT222_LIU4-ca             
;
PROBLEM: Large Non-Solvent  H     Uiso(max)/Uiso(min) ...       10.0 Ratio 
RESPONSE:  Large Non-Solvent  H     Uiso(max)/Uiso(min) ...       10.0 Ratio 
RESPONSE: The large difference is explained by disorder of the actate anion
coordinated to the Zn cluster.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        LIU-4_ca
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H26 N4 O12 Zn3'
_chemical_formula_weight         974.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.0350 2.0980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.270(2)
_cell_length_b                   15.270(2)
_cell_length_c                   23.050(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5374.6(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    453
_cell_measurement_theta_min      3.87
_cell_measurement_theta_max      24.76

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             1968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.487
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Scala (Diederichs, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number            20740
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.993
_diffrn_reflns_theta_max         35.651
_diffrn_reflns_theta_full        32.098
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             6207
_reflns_number_gt                5850
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_max     0.982
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'marCCD 1994-2002'
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_reduction        scala
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX


_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0809P)²+2.0165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.560(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6207
_refine_ls_number_parameters     265
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1195
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.001
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.78577(3) 1.21423(3) 0.2500 0.02210(16) Uani 1 2 d S T P . .
Zn2 Zn 0.83875(3) 1.25780(3) 0.10834(2) 0.02352(14) Uani 1 1 d . . . . .
C1 C 0.9735(3) 1.2121(3) 0.19254(18) 0.0307(8) Uani 1 1 d . . . . .
C2 C 1.0681(3) 1.2018(4) 0.2122(2) 0.0404(11) Uani 1 1 d . . . . .
C3 C 1.0862(3) 1.1728(7) 0.2676(3) 0.078(3) Uani 1 1 d . . . . .
H3 H 1.0407 1.1585 0.2927 0.094 Uiso 1 1 calc R U . . .
C4 C 1.1711(4) 1.1651(7) 0.2855(3) 0.087(3) Uani 1 1 d . . . . .
H4 H 1.1836 1.1453 0.3228 0.105 Uiso 1 1 calc R U . . .
C5 C 1.2382(3) 1.1867(5) 0.2481(2) 0.0582(16) Uani 1 1 d . . . . .
C6 C 1.1389(3) 1.2209(3) 0.17602(18) 0.0356(10) Uani 1 1 d . . . . .
H6 H 1.1277 1.2387 0.1381 0.043 Uiso 1 1 calc R U . . .
C7 C 1.3319(3) 1.1862(6) 0.2649(2) 0.067(2) Uani 1 1 d . . . . .
C8 C 1.3596(4) 1.1586(10) 0.3193(3) 0.131(6) Uani 1 1 d . . . . .
H8 H 1.3196 1.1376 0.3463 0.157 Uiso 1 1 calc R U . . .
C9 C 1.4468(4) 1.1630(8) 0.3323(3) 0.105(4) Uani 1 1 d . . . . .
H9 H 1.4658 1.1482 0.3694 0.126 Uiso 1 1 calc R U . . .
C10 C 1.5067(3) 1.1891(4) 0.2914(2) 0.0460(13) Uani 1 1 d . . . . .
C11 C 1.4743(3) 1.2114(3) 0.23722(17) 0.0345(9) Uani 1 1 d . . . . .
H11 H 1.5140 1.2282 0.2087 0.041 Uiso 1 1 calc R U . . .
C12 C 1.6035(3) 1.1923(3) 0.30428(19) 0.0352(10) Uani 1 1 d . . . . .
C13 C 0.7575(5) 1.1123(4) 0.1332(3) 0.0575(15) Uani 1 1 d D U . . .
C14 C 0.7017(11) 1.0403(8) 0.1464(6) 0.170(6) Uani 1 1 d D U . . .
H14 H 0.7228 0.9898 0.1286 0.204 Uiso 1 1 calc R U . . .
C15 C 0.6380(12) 1.0243(14) 0.1723(11) 0.301(11) Uani 1 1 d D U . . .
H15 H 0.6108 1.0707 0.1911 0.361 Uiso 1 1 calc R U . . .
C16 C 0.5945(11) 0.9331(13) 0.1783(9) 0.342(12) Uani 1 1 d DG U . . .
C17 C 0.5332(13) 0.9558(9) 0.2203(8) 0.334(13) Uani 1 1 d G U . . .
H17 H 0.5345 1.0112 0.2370 0.401 Uiso 1 1 calc R U . . .
C18 C 0.4701(11) 0.8956(13) 0.2375(6) 0.304(12) Uani 1 1 d G U . . .
H18 H 0.4291 0.9107 0.2656 0.365 Uiso 1 1 calc R U . . .
C19 C 0.4681(12) 0.8126(11) 0.2126(9) 0.315(13) Uani 1 1 d G U . . .
H19 H 0.4258 0.7724 0.2241 0.378 Uiso 1 1 calc R U . . .
C20 C 0.5293(16) 0.7899(10) 0.1706(9) 0.371(14) Uani 1 1 d G U . . .
H20 H 0.5280 0.7345 0.1540 0.445 Uiso 1 1 calc R U . . .
C21 C 0.5925(13) 0.8501(15) 0.1535(8) 0.375(13) Uani 1 1 d G U . . .
H21 H 0.6335 0.8350 0.1253 0.450 Uiso 1 1 calc R U . . .
N1 N 1.2214(2) 1.2145(3) 0.19362(15) 0.0377(9) Uani 1 1 d . . . . .
N2 N 1.3898(2) 1.2102(3) 0.22379(14) 0.0331(8) Uani 1 1 d . . . . .
O1 O 0.9183(2) 1.2085(3) 0.23152(14) 0.0456(9) Uani 1 1 d . . . . .
O2 O 0.9602(2) 1.2267(3) 0.13985(14) 0.0397(8) Uani 1 1 d . . . . .
O3 O 1.6238(2) 1.1672(3) 0.35393(14) 0.0464(9) Uani 1 1 d . . . . .
O4 O 1.6520(2) 1.2183(3) 0.26505(14) 0.0424(8) Uani 1 1 d . . . . .
O5 O 0.7600(2) 1.1832(2) 0.16234(12) 0.0327(6) Uani 1 1 d . . . . .
O6 O 0.8030(5) 1.1048(5) 0.0895(2) 0.107(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.069(3) 8_775 ?
Zn1 O1 2.069(3) . ?
Zn1 O4 2.073(3) 8_785 ?
Zn1 O4 2.073(3) 1_455 ?
Zn1 O5 2.112(3) . ?
Zn1 O5 2.112(3) 8_775 ?
Zn2 O3 2.009(3) 8_785 ?
Zn2 O2 2.047(3) . ?
Zn2 O5 2.072(3) . ?
Zn2 N2 2.105(3) 5_475 ?
Zn2 N1 2.196(3) 5_475 ?
Zn2 O6 2.438(7) . ?
C1 O1 1.234(5) . ?
C1 O2 1.252(5) . ?
C1 C2 1.523(6) . ?
C2 C3 1.379(7) . ?
C2 C6 1.396(6) . ?
C3 C4 1.366(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.380(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.350(6) . ?
C5 C7 1.482(7) . ?
C6 N1 1.328(5) . ?
C6 H6 0.9300 . ?
C7 N2 1.347(6) . ?
C7 C8 1.388(7) . ?
C8 C9 1.367(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.372(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.386(6) . ?
C10 C12 1.509(6) . ?
C11 N2 1.327(5) . ?
C11 H11 0.9300 . ?
C12 O4 1.234(6) . ?
C12 O3 1.246(6) . ?
C13 O6 1.229(9) . ?
C13 O5 1.275(6) . ?
C13 C14 1.424(11) . ?
C14 C15 1.168(19) . ?
C14 H14 0.9300 . ?
C15 C16 1.549(18) . ?
C15 H15 0.9300 . ?
C16 C17 1.3900 . ?
C16 C21 1.3900 . ?
C17 C18 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 C21 1.3900 . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
N1 Zn2 2.196(3) 5_575 ?
N2 Zn2 2.105(3) 5_575 ?
O3 Zn2 2.009(3) 8_875 ?
O4 Zn1 2.073(3) 1_655 ?

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 O1 87.7(3) 8_775 . ?
O1 Zn1 O4 177.63(14) 8_775 8_785 ?
O1 Zn1 O4 92.10(17) . 8_785 ?
O1 Zn1 O4 92.10(17) 8_775 1_455 ?
O1 Zn1 O4 177.63(14) . 1_455 ?
O4 Zn1 O4 88.2(2) 8_785 1_455 ?
O1 Zn1 O5 89.18(13) 8_775 . ?
O1 Zn1 O5 88.62(13) . . ?
O4 Zn1 O5 93.17(12) 8_785 . ?
O4 Zn1 O5 89.03(13) 1_455 . ?
O1 Zn1 O5 88.61(13) 8_775 8_775 ?
O1 Zn1 O5 89.18(13) . 8_775 ?
O4 Zn1 O5 89.03(13) 8_785 8_775 ?
O4 Zn1 O5 93.17(12) 1_455 8_775 ?
O5 Zn1 O5 176.94(19) . 8_775 ?
O3 Zn2 O2 95.50(17) 8_785 . ?
O3 Zn2 O5 102.04(14) 8_785 . ?
O2 Zn2 O5 100.67(13) . . ?
O3 Zn2 N2 101.38(16) 8_785 5_475 ?
O2 Zn2 N2 92.14(13) . 5_475 ?
O5 Zn2 N2 151.99(14) . 5_475 ?
O3 Zn2 N1 91.51(17) 8_785 5_475 ?
O2 Zn2 N1 167.70(13) . 5_475 ?
O5 Zn2 N1 87.69(13) . 5_475 ?
N2 Zn2 N1 76.54(13) 5_475 5_475 ?
O3 Zn2 O6 158.4(2) 8_785 . ?
O2 Zn2 O6 92.5(2) . . ?
O5 Zn2 O6 56.64(18) . . ?
N2 Zn2 O6 98.36(19) 5_475 . ?
N1 Zn2 O6 84.5(2) 5_475 . ?
O1 C1 O2 127.1(4) . . ?
O1 C1 C2 115.3(4) . . ?
O2 C1 C2 117.5(4) . . ?
C3 C2 C6 117.8(4) . . ?
C3 C2 C1 120.0(4) . . ?
C6 C2 C1 122.3(4) . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.0(4) . . ?
N1 C5 C7 115.4(4) . . ?
C4 C5 C7 123.5(5) . . ?
N1 C6 C2 122.5(4) . . ?
N1 C6 H6 118.8 . . ?
C2 C6 H6 118.8 . . ?
N2 C7 C8 121.2(5) . . ?
N2 C7 C5 116.6(4) . . ?
C8 C7 C5 122.1(5) . . ?
C9 C8 C7 118.7(6) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C8 C9 C10 120.9(5) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C9 C10 C11 116.9(4) . . ?
C9 C10 C12 121.8(4) . . ?
C11 C10 C12 121.3(4) . . ?
N2 C11 C10 123.6(4) . . ?
N2 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
O4 C12 O3 128.6(4) . . ?
O4 C12 C10 117.0(4) . . ?
O3 C12 C10 114.4(4) . . ?
O6 C13 O5 119.6(6) . . ?
O6 C13 C14 116.1(9) . . ?
O5 C13 C14 124.2(9) . . ?
C15 C14 C13 140(2) . . ?
C15 C14 H14 109.9 . . ?
C13 C14 H14 109.9 . . ?
C14 C15 C16 126(2) . . ?
C14 C15 H15 116.9 . . ?
C16 C15 H15 116.9 . . ?
C17 C16 C21 120.0 . . ?
C17 C16 C15 97.3(16) . . ?
C21 C16 C15 142.3(17) . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C16 120.0 . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
C6 N1 C5 119.2(4) . . ?
C6 N1 Zn2 126.4(3) . 5_575 ?
C5 N1 Zn2 114.4(3) . 5_575 ?
C11 N2 C7 118.5(4) . . ?
C11 N2 Zn2 124.5(3) . 5_575 ?
C7 N2 Zn2 116.9(3) . 5_575 ?
C1 O1 Zn1 144.7(3) . . ?
C1 O2 Zn2 122.2(3) . . ?
C12 O3 Zn2 129.4(3) . 8_875 ?
C12 O4 Zn1 134.8(3) . 1_655 ?
C13 O5 Zn2 99.7(4) . . ?
C13 O5 Zn1 134.4(3) . . ?
Zn2 O5 Zn1 110.07(13) . . ?
C13 O6 Zn2 83.8(4) . . ?

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 C1 C2 C3 12.5(9) . . . . ?
O2 C1 C2 C3 -170.2(7) . . . . ?
O1 C1 C2 C6 -167.4(5) . . . . ?
O2 C1 C2 C6 9.8(8) . . . . ?
C6 C2 C3 C4 1.1(13) . . . . ?
C1 C2 C3 C4 -178.8(8) . . . . ?
C2 C3 C4 C5 0.3(16) . . . . ?
C3 C4 C5 N1 -0.8(15) . . . . ?
C3 C4 C5 C7 175.7(9) . . . . ?
C3 C2 C6 N1 -2.1(9) . . . . ?
C1 C2 C6 N1 177.9(5) . . . . ?
N1 C5 C7 N2 -2.3(11) . . . . ?
C4 C5 C7 N2 -179.0(8) . . . . ?
N1 C5 C7 C8 -179.5(10) . . . . ?
C4 C5 C7 C8 3.8(15) . . . . ?
N2 C7 C8 C9 5.3(19) . . . . ?
C5 C7 C8 C9 -177.6(11) . . . . ?
C7 C8 C9 C10 -4(2) . . . . ?
C8 C9 C10 C11 0.8(16) . . . . ?
C8 C9 C10 C12 -178.4(11) . . . . ?
C9 C10 C11 N2 1.2(11) . . . . ?
C12 C10 C11 N2 -179.6(5) . . . . ?
C9 C10 C12 O4 -178.6(8) . . . . ?
C11 C10 C12 O4 2.2(8) . . . . ?
C9 C10 C12 O3 2.0(10) . . . . ?
C11 C10 C12 O3 -177.2(5) . . . . ?
O6 C13 C14 C15 -158(2) . . . . ?
O5 C13 C14 C15 19(3) . . . . ?
C13 C14 C15 C16 -178.7(16) . . . . ?
C14 C15 C16 C17 171(2) . . . . ?
C14 C15 C16 C21 -18(4) . . . . ?
C21 C16 C17 C18 0.0 . . . . ?
C15 C16 C17 C18 174.0(16) . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C16 0.0 . . . . ?
C17 C16 C21 C20 0.0 . . . . ?
C15 C16 C21 C20 -170(3) . . . . ?
C2 C6 N1 C5 1.6(9) . . . . ?
C2 C6 N1 Zn2 180.0(4) . . . 5_575 ?
C4 C5 N1 C6 -0.1(11) . . . . ?
C7 C5 N1 C6 -176.9(6) . . . . ?
C4 C5 N1 Zn2 -178.7(7) . . . 5_575 ?
C7 C5 N1 Zn2 4.5(8) . . . 5_575 ?
C10 C11 N2 C7 0.1(9) . . . . ?
C10 C11 N2 Zn2 -179.2(4) . . . 5_575 ?
C8 C7 N2 C11 -3.4(13) . . . . ?
C5 C7 N2 C11 179.4(6) . . . . ?
C8 C7 N2 Zn2 175.9(9) . . . 5_575 ?
C5 C7 N2 Zn2 -1.3(9) . . . 5_575 ?
O2 C1 O1 Zn1 2.9(11) . . . . ?
C2 C1 O1 Zn1 179.9(5) . . . . ?
O1 C1 O2 Zn2 5.0(8) . . . . ?
C2 C1 O2 Zn2 -171.9(4) . . . . ?
O4 C12 O3 Zn2 1.8(9) . . . 8_875 ?
C10 C12 O3 Zn2 -178.8(4) . . . 8_875 ?
O3 C12 O4 Zn1 14.0(9) . . . 1_655 ?
C10 C12 O4 Zn1 -165.3(4) . . . 1_655 ?
O6 C13 O5 Zn2 6.2(7) . . . . ?
C14 C13 O5 Zn2 -171.1(8) . . . . ?
O6 C13 O5 Zn1 -124.7(6) . . . . ?
C14 C13 O5 Zn1 58.1(11) . . . . ?
O5 C13 O6 Zn2 -5.2(6) . . . . ?
C14 C13 O6 Zn2 172.2(8) . . . . ?

_refine_diff_density_max         0.500
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.126

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_LIU4_cinnamic_cp
_database_code_depnum_ccdc_archive 'CCDC 1422821'
_audit_update_record             
;
2015-09-07 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-08-25
_audit_creation_method           'Materials Studio'
_symmetry_space_group_name_H-M   C2221
_symmetry_Int_Tables_number      20
_symmetry_cell_setting           orthorhombic

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                'close sample cryostat with Be domes'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   block

_pd_char_particle_morphology     ?
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        

_pd_prep_cool_rate               ?
_pd_prep_pressure                0
_pd_prep_temperature             77

_pd_instr_location               
;
KMC-2 beamline HZB (Berlin)
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
Boron nitride powder was used as external standard
;

_diffrn_ambient_temperature      77
_diffrn_radiation_wavelength     1.5406
_diffrn_source                   Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_source_target            ?
_diffrn_radiation_monochromator  'silicium monochromator'
_diffrn_measurement_method       '2 Theta scan'
_diffrn_detector_area_resol_mean ? # Not in version 2.0.1
_diffrn_detector                 'Area detector'
_diffrn_detector_type            'VANTEC 2000 detector (Bruker)'
_pd_meas_scan_method             step
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        3400
_pd_meas_2theta_range_min        2.00000
_pd_meas_2theta_range_max        70.00000
_pd_meas_2theta_range_inc        0.020000
_pd_proc_ls_prof_R_factor        8.98
_pd_proc_ls_prof_wR_factor       11.65
_refine_ls_number_parameters     92
_refine_ls_number_restraints     18
_pd_proc_2theta_range_min        5.5000
_pd_proc_2theta_range_max        70.0000
_pd_proc_2theta_range_inc        0.020000
_pd_proc_wavelength              1.5406


loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-x,y,-z+1/2
x,-y,-z
x+1/2,y+1/2,z
-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
_cell_length_a                   17.3128
_cell_length_b                   24.5942
_cell_length_c                   22.1389
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
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
H1 H 0.95456 0.79965 0.83273 0.05000 Uiso 1.00
H2 H 0.98006 0.70130 0.82919 0.05000 Uiso 1.00
H3 H 0.92381 0.64017 0.90640 0.05000 Uiso 1.00
H4 H 0.84076 0.67787 -0.01266 0.05000 Uiso 1.00
H5 H 0.31585 0.27639 0.99270 0.05000 Uiso 1.00
H6 H 0.31273 0.36776 0.93818 0.05000 Uiso 1.00
H7 H 0.96575 0.88266 0.87341 0.05000 Uiso 1.00
H8 H 0.14253 0.38816 0.94301 0.05000 Uiso 1.00
H9 H 0.16954 0.33798 0.12650 0.05000 Uiso 1.00
H10 H 0.10138 0.25418 0.10277 0.05000 Uiso 1.00
H11 H 0.97453 0.17369 0.86260 0.05000 Uiso 1.00
H12 H 0.08514 0.17011 0.06714 0.05000 Uiso 1.00
H13 H 1.02381 0.08891 0.02832 0.05000 Uiso 1.00
H14 H 0.06127 0.43973 0.72092 0.05000 Uiso 1.00
H15 H 0.12274 0.52106 0.68825 0.05000 Uiso 1.00
H16 H 0.22944 0.42254 0.86197 0.05000 Uiso 1.00
H17 H 0.19666 0.58403 0.65453 0.05000 Uiso 1.00
H18 H 0.26153 0.66886 0.63812 0.05000 Uiso 1.00
H19 H 0.87845 0.15075 0.80879 0.05000 Uiso 1.00
H20 H 0.83613 0.31676 0.81638 0.05000 Uiso 1.00
H21 H 0.83856 0.39471 0.92296 0.05000 Uiso 1.00
H22 H 0.70275 0.31416 0.82349 0.05000 Uiso 1.00
H23 H 0.08418 0.85071 0.77739 0.05000 Uiso 1.00
H24 H 0.04822 0.94715 0.79319 0.05000 Uiso 1.00
H25 H 0.63736 0.50951 0.84560 0.05000 Uiso 1.00
H26 H 0.75658 0.47530 0.89016 0.05000 Uiso 1.00
C1 C 0.93083 0.77391 0.86760 0.05000 Uiso 1.00
C2 C 0.94483 0.71797 0.86505 0.05000 Uiso 1.00
C3 C 0.91290 0.68345 0.90846 0.05000 Uiso 1.00
C4 C 0.86613 0.70470 0.95410 0.05000 Uiso 1.00
C5 C 0.85201 0.76058 0.95684 0.05000 Uiso 1.00
C6 C 0.88504 0.79584 0.91409 0.05000 Uiso 1.00
C7 C 0.36482 0.35583 0.91600 0.05000 Uiso 1.00
C8 C 0.40996 0.39397 0.89147 0.05000 Uiso 1.00
C9 C 0.39037 0.45260 0.88108 0.05000 Uiso 1.00
C10 C 0.21963 0.41574 0.04665 0.05000 Uiso 1.00
C11 C 0.13793 0.35751 0.97677 0.05000 Uiso 1.00
C12 C 0.16751 0.36880 0.03455 0.05000 Uiso 1.00
C13 C 0.15160 0.33082 0.08034 0.05000 Uiso 1.00
C14 C 0.11508 0.28191 0.06685 0.05000 Uiso 1.00
C15 C 0.09714 0.26949 0.00692 0.05000 Uiso 1.00
C16 C 0.99745 0.17245 0.90786 0.05000 Uiso 1.00
C17 C 0.06218 0.21835 0.98750 0.05000 Uiso 1.00
C18 C 0.05991 0.17134 0.02283 0.05000 Uiso 1.00
C19 C 1.02403 0.12499 0.00065 0.05000 Uiso 1.00
C20 C 0.98462 0.12615 0.94550 0.05000 Uiso 1.00
C21 C 0.42539 0.58186 0.93236 0.05000 Uiso 1.00
C22 C 0.10960 0.36578 0.80289 0.05000 Uiso 1.00
C23 C 0.14557 0.41940 0.78943 0.05000 Uiso 1.00
C24 C 0.11428 0.45093 0.74290 0.05000 Uiso 1.00
C25 C 0.14892 0.49867 0.72485 0.05000 Uiso 1.00
C26 C 0.21272 0.51811 0.75677 0.05000 Uiso 1.00
C27 C 0.20733 0.44259 0.82290 0.05000 Uiso 1.00
C28 C 0.25162 0.56840 0.74130 0.05000 Uiso 1.00
C29 C 0.23598 0.59824 0.68893 0.05000 Uiso 1.00
C30 C 0.27313 0.64716 0.67971 0.05000 Uiso 1.00
C31 C 0.82558 0.16718 0.72241 0.05000 Uiso 1.00
C32 C 0.34016 0.63550 0.77438 0.05000 Uiso 1.00
C33 C 0.87097 0.21720 0.70818 0.05000 Uiso 1.00
C34 C 0.93729 0.32483 0.87518 0.05000 Uiso 1.00
C35 C 0.85714 0.33609 0.85701 0.05000 Uiso 1.00
C36 C 0.81354 0.37231 0.88615 0.05000 Uiso 1.00
C37 C 0.73788 0.39094 0.86281 0.05000 Uiso 1.00
C38 C 0.68938 0.35688 0.82880 0.05000 Uiso 1.00
C39 C 0.12227 0.87746 0.80227 0.05000 Uiso 1.00
C40 C 0.10255 0.93202 0.81006 0.05000 Uiso 1.00
C41 C 0.65213 0.46696 0.84085 0.05000 Uiso 1.00
C42 C 0.71957 0.44677 0.86705 0.05000 Uiso 1.00
N1 N 0.10473 0.30797 0.96370 0.05000 Uiso 1.00
N2 N 0.03849 0.21653 0.92929 0.05000 Uiso 1.00
N3 N 0.23763 0.49226 0.80715 0.05000 Uiso 1.00
N4 N 0.30519 0.58570 0.78149 0.05000 Uiso 1.00
O1 O 0.42563 0.47425 0.84004 0.05000 Uiso 1.00
O2 O 0.33195 0.48204 0.91099 0.05000 Uiso 1.00
O3 O 0.25032 0.44507 0.00474 0.05000 Uiso 1.00
O4 O 0.23774 0.42212 0.10177 0.05000 Uiso 1.00
O5 O 0.39621 0.57572 0.88002 0.05000 Uiso 1.00
O6 O 0.40087 0.55322 0.97699 0.05000 Uiso 1.00
O7 O 0.06799 0.34387 0.76229 0.05000 Uiso 1.00
O8 O 0.11620 0.34327 0.85415 0.05000 Uiso 1.00
O9 O 0.86103 0.23841 0.65637 0.05000 Uiso 1.00
O10 O 0.92213 0.23516 0.74505 0.05000 Uiso 1.00
O11 O 0.98505 0.29099 0.84078 0.05000 Uiso 1.00
O12 O 0.96188 0.34361 0.92223 0.05000 Uiso 1.00
Zn1 Zn 0.30422 0.54135 0.85720 0.05000 Uiso 1.00
Zn4 Zn 0.07482 0.28077 0.88471 0.05000 Uiso 1.00
Zn2 Zn 0.32899 0.50000 0.00000 0.05000 Uiso 0.50
Zn3 Zn 0.00000 0.28875 0.75000 0.05000 Uiso 0.50
_chemical_name_systematic        'Liu-4_cinnamic (close pore phase)'
_chemical_name_common            'Liu-4_cinnamic (close pore phase)'
_exptl_crystal_colour            colorless
_chemical_properties_physical    'Moisture-sensitive, Hygroscopic'
