# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_MOF650_ccdc922543

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
; 4(C36 H18 O13 Zn4), 4(C3 H7 N O), 4(C5 H9 N O), 13(H2 O)
;
_chemical_formula_sum            'C320 H234 N8 O125 Zn32'
_chemical_formula_weight         8282.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'

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

_cell_length_a                   30.5557(17)
_cell_length_b                   30.5557(17)
_cell_length_c                   30.5557(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     28528(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    709
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.8

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.482
_exptl_crystal_F_000             4170
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Version 1.171.35.11 (Oxford Diffraction, 2010)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
   1 -0.004 -0.011 -0.005     23342     10106
;
_platon_squeeze_details          
;
The unit cell contains 4 DMF, 4 NMP and 13 water solvent molecules (3920
 electrons) which have been treated as a diffuse contribution to the overall
 scattering without specific atom positions by SQUEEZE/PLATON.
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            13859
_diffrn_reflns_av_R_equivalents  0.1979
_diffrn_reflns_av_sigmaI/netI    0.1335
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         25.35
_reflns_number_total             1353
_reflns_number_gt                744
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_cell_refinement       
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_data_reduction        
;
CrysAlisPro, Version 1.171.33.55 (Oxford Diffraction, 2010).
;
_computing_structure_solution    
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_computing_structure_refinement  
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
  SQUEEZE/PLATON -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_molecular_graphics    
; ORTEP-3 for Windows.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material  
; WinGX -- Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97 -- Sheldrick, G. M (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;

_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1353
_refine_ls_number_parameters     37
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.2245
_refine_ls_R_factor_gt           0.1443
_refine_ls_wR_factor_ref         0.3752
_refine_ls_wR_factor_gt          0.3390
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.147
_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
O1 O 0.2500 0.2500 0.2500 0.025(5) Uani 1 24 d S T P . .
O2 O 0.2763(2) 0.2763(2) 0.1519(3) 0.087(3) Uani 1 2 d S TU P . .
C1 C 0.2500 0.2500 0.1388(4) 0.088(4) Uani 1 4 d DS TU P . .
C2 C 0.2500 0.2500 0.0894(3) 0.089(4) Uani 1 4 d DS TU P . .
C3 C 0.2766(2) 0.2766(2) 0.0633(2) 0.094(4) Uani 1 2 d DS TU P . .
H3 H 0.2970 0.2970 0.0728 0.122 Uiso 1 2 calc R U P . .
C4 C 0.26619(11) 0.26619(11) 0.0193(3) 0.103(6) Uani 0.5 2 d DS TU P . .
C5 C 0.2819(4) 0.2819(4) -0.01932(19) 0.108(7) Uani 0.5 2 d DS TU P . .
H5 H 0.3030 0.3030 -0.0140 0.129 Uiso 0.5 2 calc R U P . .
Zn1 Zn 0.28659(4) 0.28659(4) 0.21341(4) 0.0423(9) Uani 1 6 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.025(5) 0.025(5) 0.025(5) 0.000 0.000 0.000
O2 0.101(4) 0.101(4) 0.059(5) -0.002(3) -0.002(3) -0.043(5)
C1 0.100(6) 0.100(6) 0.064(7) 0.000 0.000 -0.060(7)
C2 0.102(6) 0.102(6) 0.063(7) 0.000 0.000 -0.056(8)
C3 0.111(6) 0.111(6) 0.060(7) 0.006(4) 0.006(4) -0.051(7)
C4 0.119(8) 0.119(8) 0.070(8) 0.005(5) 0.005(5) -0.062(10)
C5 0.125(10) 0.125(10) 0.073(11) -0.001(6) -0.001(6) -0.060(12)
Zn1 0.0423(9) 0.0423(9) 0.0423(9) 0.0058(6) 0.0058(6) -0.0058(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 Zn1 1.936(2) . ?
O1 Zn1 1.937(2) 75 ?
O1 Zn1 1.937(2) 52 ?
O1 Zn1 1.937(2) 26 ?
O2 C1 1.206(9) . ?
O2 Zn1 1.931(9) . ?
C1 O2 1.206(9) 75 ?
C1 C2 1.510(9) . ?
C2 C3 1.399(8) . ?
C2 C3 1.399(8) 75 ?
C3 C4 1.416(8) . ?
C3 H3 0.9300 . ?
C4 C4 1.18(2) 99 ?
C4 C5 1.360(8) . ?
C4 C4 1.400(10) 75 ?
C4 C4 1.830(15) 169 ?
C5 C3 1.362(8) 99 ?
C5 H5 0.9300 . ?
Zn1 O2 1.931(9) 159 ?
Zn1 O2 1.931(9) 35 ?

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
Zn1 O1 Zn1 109.471(1) . 75 ?
Zn1 O1 Zn1 109.5 . 52 ?
Zn1 O1 Zn1 109.5 75 52 ?
Zn1 O1 Zn1 109.5 . 26 ?
Zn1 O1 Zn1 109.5 75 26 ?
Zn1 O1 Zn1 109.5 52 26 ?
C1 O2 Zn1 122.6(9) . . ?
O2 C1 O2 141.3(14) . 75 ?
O2 C1 C2 109.4(7) . . ?
O2 C1 C2 109.3(7) 75 . ?
C3 C2 C3 110.3(9) . 75 ?
C3 C2 C1 124.8(4) . . ?
C3 C2 C1 124.8(4) 75 . ?
C2 C3 C4 106.4(7) . . ?
C2 C3 H3 126.8 . . ?
C4 C3 H3 126.8 . . ?
C4 C4 C5 29.8(8) 99 . ?
C4 C4 C4 90.000(1) 99 75 ?
C5 C4 C4 119.8(8) . 75 ?
C4 C4 C3 161.6(4) 99 . ?
C5 C4 C3 131.7(9) . . ?
C4 C4 C3 108.4(4) 75 . ?
C4 C4 C4 49.9(5) 99 169 ?
C5 C4 C4 79.7(12) . 169 ?
C4 C4 C4 40.1(5) 75 169 ?
C3 C4 C4 148.6(8) . 169 ?
C4 C5 C3 140.5(17) . 99 ?
C4 C5 H5 109.7 . . ?
C3 C5 H5 109.7 99 . ?
O2 Zn1 O2 106.8(3) . 159 ?
O2 Zn1 O2 106.8(3) . 35 ?
O2 Zn1 O2 106.8(3) 159 35 ?
O2 Zn1 O1 112.0(3) . . ?
O2 Zn1 O1 112.0(3) 159 . ?
O2 Zn1 O1 112.0(3) 35 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.139

_iucr_refine_instructions_details 
;
TITL MOF650
CELL  0.71073  30.5557  30.5557  30.5557   90.000   90.000   90.000
ZERR     1.00   0.0017   0.0017   0.0017    0.000    0.000    0.000
LATT   4
SYMM    X, - Y, - Z
SYMM  - X, - Y,   Z
SYMM  - X,   Y, - Z
SYMM  - Y,   X,   Z
SYMM    Y,   X, - Z
SYMM    Y, - X,   Z
SYMM  - Y, - X, - Z
SYMM    Y,   Z,   X
SYMM  - Y, - Z,   X
SYMM    Y, - Z, - X
SYMM  - Y,   Z, - X
SYMM  - Z,   Y,   X
SYMM  - Z, - Y, - X
SYMM    Z, - Y,   X
SYMM    Z,   Y, - X
SYMM    Z,   X,   Y
SYMM  - Z,   X, - Y
SYMM  - Z, - X,   Y
SYMM    Z, - X, - Y
SYMM  - X, - Z, - Y
SYMM  - X,   Z,   Y
SYMM    X, - Z,   Y
SYMM    X,   Z, - Y
SFAC  C    H    O    ZN   N
UNIT  320  234  125  32   8
MERG   2
SHEL 100 0.83
EQIV $1 0.5-x,0.5-y,z
EQIV $2 x,y,-z
DFIX 1.52 0.010 C1 C2
DFIX 1.40 0.010 C2 C3 C3 C4 C4 C4_$1 C4 C5 C3 C5_$2
DANG 2.30 0.010 C2 C4
DANG 2.50 0.010 C3 C5 C2 C5_$2
SIMU 0.010 O2 > C5
BIND C4 C5_$2 C5 C3
FREE C3 C5_$2 C4 C5_$2 C5 C5_$2 C5 C3 C5 C4_$2
FMAP   2
PLAN   20
ACTA
BOND   $H
L.S.   8
WGHT    0.200000
FVAR       7.98730
O1    3    0.250000    0.250000    0.250000    10.04167    0.02450    0.02450 =
         0.02450    0.00000    0.00000    0.00000
O2    3    0.276333    0.276333    0.151918    10.50000    0.10068    0.10068 =
         0.05889   -0.00211   -0.00211   -0.04301
C1    1    0.250000    0.250000    0.138838    10.25000    0.10031    0.10031 =
         0.06411    0.00000    0.00000   -0.05953
C2    1    0.250000    0.250000    0.089418    10.25000    0.10157    0.10157 =
         0.06299    0.00000    0.00000   -0.05592
C3    1    0.276565    0.276565    0.063263    10.50000    0.11117    0.11117 =
         0.06008    0.00574    0.00574   -0.05057
AFIX  43
H3    2    0.296992    0.296992    0.072846    10.50000   -1.30000
AFIX   0
C4    1    0.266195    0.266195    0.019295    10.25000    0.11904    0.11904 =
         0.07044    0.00471    0.00471   -0.06226
C5    1    0.281855    0.281855   -0.019323    10.25000    0.12492    0.12492 =
         0.07350   -0.00061   -0.00061   -0.05969
AFIX  43
H5    2    0.303044    0.303044   -0.013993    10.25000   -1.20000
AFIX   0
ZN1   4    0.286589    0.286589    0.213411    10.16667    0.04228    0.04228 =
         0.04228    0.00582    0.00582   -0.00582
HKLF    4

REM  sami2705 in Pm-3m
REM R1 =  0.1443 for     744 Fo > 4sig(Fo)  and  0.2245 for all    1353 data
REM     37 parameters refined using     39 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  1.888,  deepest hole -1.934,  1-sigma level  0.139
Q1    1   0.2873  0.2873  0.1821  10.50000  0.05    1.89
Q2    1   0.2843  0.2843  0.2433  10.50000  0.05    1.77
Q3    1   0.2381  0.2619  0.0000  10.25000  0.05    0.69
Q4    1   0.2587  0.2167  0.1438  11.00000  0.05    0.67
Q5    1   0.2374  0.2626  0.0682  10.50000  0.05    0.62
Q6    1   0.2302  0.2795  0.1587  11.00000  0.05    0.59
Q7    1   0.2836  0.2164  0.1145  10.50000  0.05    0.45
Q8    1   0.3089  0.3089  0.1541  10.50000  0.05    0.36
Q9    1   0.2851  0.3005  0.1327  11.00000  0.05    0.31
Q10   1   0.3289  0.2755  0.0000  10.50000  0.05    0.30
Q11   1   0.3104  0.2651  0.1555  11.00000  0.05    0.30
Q12   1   0.2883  0.2883  0.1313  10.50000  0.05    0.30
Q13   1   0.2869  0.2869  0.0526  10.50000  0.05    0.28
Q14   1   0.2491  0.3079  0.0635  11.00000  0.05    0.28
Q15   1   0.2655  0.2655  0.1558  10.50000  0.05    0.28
Q16   1   0.2715  0.2715  0.1170  10.50000  0.05    0.28
Q17   1   0.2500  0.2500  0.1219  10.25000  0.05    0.27
Q18   1   0.3204  0.2829 -0.0222  11.00000  0.05    0.27
Q19   1   0.3117  0.3117 -0.0428  10.50000  0.05    0.26
Q20   1   0.3091  0.2918  0.1355  11.00000  0.05    0.26
;

_database_code_depnum_ccdc_archive 'CCDC 922543'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_MOF649_ccdc922544

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_formula_moiety         'C15 H12 N O4 Zn'
_chemical_formula_sum            'C15 H12 N O4 Zn'
_chemical_formula_weight         335.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m m m'
_symmetry_space_group_name_Hall  '-C 2 2'

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

_cell_length_a                   16.052(5)
_cell_length_b                   21.172(5)
_cell_length_c                   9.625(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     3271(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    5646
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.0

_exptl_crystal_description       needle
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897).
;

_exptl_special_details           
;


All hydrogen positions were
calculated after each cycle of refinement using a riding model, with C-H =
0.93 Å and Uiso(H) = 1.2Ueq(C) for aromatic H atoms, and
with C-H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl H
atoms.
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            12121
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         25.05
_reflns_number_total             1650
_reflns_number_gt                1332
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_cell_refinement       
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_data_reduction        
;
CrysAlisPro, Version 1.171.33.55 (Agilent Technologies, 2012).
;
_computing_structure_solution    
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_computing_structure_refinement  
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
  PLATON for Windows -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_molecular_graphics    
; ORTEP-3 for Windows.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material  
; WinGX -- Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97 -- Sheldrick, G. M (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows -- Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1181P)²+16.8721P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1650
_refine_ls_number_parameters     73
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.2145
_refine_ls_wR_factor_gt          0.2116
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.0000 0.34666(10) 0.0267(4) Uani 1 4 d S . .
O1 O 0.5867(3) -0.06762(19) 0.3854(4) 0.0606(13) Uani 1 1 d . . .
C1 C 0.6087(5) -0.0890(3) 0.5000 0.0413(18) Uani 1 2 d S . .
C2 C 0.6619(5) -0.1462(4) 0.5000 0.047(2) Uani 1 2 d SD . .
C3 C 0.6862(5) -0.1742(3) 0.3763(5) 0.067(2) Uani 1 1 d D . .
H3 H 0.6648 -0.1525 0.3002 0.080 Uiso 1 1 calc R . .
C4 C 0.7330(9) -0.2252(5) 0.3350(12) 0.066(4) Uani 0.50 1 d PD . .
H4 H 0.7427 -0.2309 0.2405 0.079 Uiso 0.50 1 calc PR . .
C5 C 0.7665(9) -0.2684(5) 0.4273(5) 0.061(4) Uani 0.50 1 d PD . .
N1 N 0.5000 0.0000 0.1333(7) 0.0348(16) Uani 1 4 d SU . .
C8 C 0.5747(7) 0.0316(5) 0.0800(10) 0.050(2) Uani 0.50 1 d PU . .
H8A H 0.6240 0.0100 0.1137 0.059 Uiso 0.50 1 calc PR . .
H8B H 0.5763 0.0748 0.1137 0.059 Uiso 0.50 1 calc PR . .
C9 C 0.5000 -0.0637(7) 0.0802(13) 0.042(2) Uani 0.50 2 d SPU . .
H9A H 0.4511 -0.0858 0.1138 0.051 Uiso 0.25 1 calc PR . .
H9B H 0.5489 -0.0858 0.1138 0.051 Uiso 0.25 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0441(7) 0.0231(6) 0.0130(6) 0.000 0.000 0.000
O1 0.095(3) 0.059(2) 0.028(2) 0.0017(17) -0.006(2) 0.053(2)
C1 0.057(5) 0.035(4) 0.031(4) 0.000 0.000 0.014(4)
C2 0.065(5) 0.047(4) 0.028(4) 0.000 0.000 0.020(4)
C3 0.109(5) 0.063(4) 0.028(3) 0.003(3) 0.001(3) 0.048(4)
C4 0.093(10) 0.076(9) 0.028(6) 0.004(6) -0.005(7) 0.049(8)
C5 0.087(10) 0.055(8) 0.039(6) -0.005(6) 0.003(7) 0.049(7)
N1 0.058(4) 0.037(4) 0.010(3) 0.000 0.000 0.000
C8 0.068(5) 0.065(5) 0.016(4) 0.002(3) -0.001(3) -0.019(3)
C9 0.076(6) 0.036(4) 0.015(5) 0.001(4) 0.000 0.000

_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 2.032(4) 12 ?
Zn1 O1 2.032(4) 11_655 ?
Zn1 O1 2.032(4) . ?
Zn1 O1 2.032(4) 2_655 ?
Zn1 N1 2.054(7) . ?
Zn1 Zn1 2.952(2) 9_656 ?
O1 C1 1.243(5) . ?
C1 O1 1.243(5) 10_556 ?
C1 C2 1.484(10) . ?
C2 C3 1.385(5) . ?
C2 C3 1.385(5) 10_556 ?
C3 C4 1.374(7) . ?
C4 C5 1.385(7) . ?
C5 C4 0.899(10) 6_645 ?
C5 C5 0.944(19) 6_645 ?
C5 C5 1.399(9) 10_556 ?
C5 C3 1.514(11) 6_645 ?
C5 C5 1.687(14) 13_646 ?
N1 C9 1.442(14) . ?
N1 C9 1.442(14) 12 ?
N1 C8 1.465(11) 2_655 ?
N1 C8 1.465(11) 11_655 ?
N1 C8 1.465(11) . ?
N1 C8 1.465(11) 12 ?
C8 C8 1.540(18) 10 ?
C9 C9 1.54(3) 10 ?

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 158.8(2) 12 11_655 ?
O1 Zn1 O1 89.6(3) 12 . ?
O1 Zn1 O1 86.5(3) 11_655 . ?
O1 Zn1 O1 86.5(3) 12 2_655 ?
O1 Zn1 O1 89.6(3) 11_655 2_655 ?
O1 Zn1 O1 158.8(2) . 2_655 ?
O1 Zn1 N1 100.58(11) 12 . ?
O1 Zn1 N1 100.58(11) 11_655 . ?
O1 Zn1 N1 100.58(11) . . ?
O1 Zn1 N1 100.58(11) 2_655 . ?
O1 Zn1 Zn1 79.42(11) 12 9_656 ?
O1 Zn1 Zn1 79.42(11) 11_655 9_656 ?
O1 Zn1 Zn1 79.42(11) . 9_656 ?
O1 Zn1 Zn1 79.42(11) 2_655 9_656 ?
N1 Zn1 Zn1 180.0 . 9_656 ?
C1 O1 Zn1 127.8(4) . . ?
O1 C1 O1 125.1(7) 10_556 . ?
O1 C1 C2 117.4(3) 10_556 . ?
O1 C1 C2 117.4(3) . . ?
C3 C2 C3 118.5(7) . 10_556 ?
C3 C2 C1 120.7(3) . . ?
C3 C2 C1 120.7(3) 10_556 . ?
C4 C3 C2 137.6(7) . . ?
C3 C4 C5 123.1(9) . . ?
C4 C5 C5 97.4(9) 6_645 6_645 ?
C4 C5 C4 57.9(10) 6_645 . ?
C5 C5 C4 40.1(5) 6_645 . ?
C4 C5 C5 171.3(11) 6_645 10_556 ?
C5 C5 C5 90.000(5) 6_645 10_556 ?
C4 C5 C5 129.9(5) . 10_556 ?
C4 C5 C3 63.6(8) 6_645 6_645 ?
C5 C5 C3 161.0(4) 6_645 6_645 ?
C4 C5 C3 121.1(5) . 6_645 ?
C5 C5 C3 108.9(2) 10_556 6_645 ?
C4 C5 C5 153.1(14) 6_645 13_646 ?
C5 C5 C5 56.0(5) 6_645 13_646 ?
C4 C5 C5 96.0(8) . 13_646 ?
C5 C5 C5 34.0(5) 10_556 13_646 ?
C3 C5 C5 142.9(7) 6_645 13_646 ?
C9 N1 C9 138.5(12) . 12 ?
C9 N1 C8 56.6(5) . 2_655 ?
C9 N1 C8 107.6(6) 12 2_655 ?
C9 N1 C8 107.6(6) . 11_655 ?
C9 N1 C8 56.6(5) 12 11_655 ?
C8 N1 C8 54.4(10) 2_655 11_655 ?
C9 N1 C8 107.6(6) . . ?
C9 N1 C8 56.6(5) 12 . ?
C8 N1 C8 139.0(9) 2_655 . ?
C8 N1 C8 109.8(10) 11_655 . ?
C9 N1 C8 56.6(5) . 12 ?
C9 N1 C8 107.6(6) 12 12 ?
C8 N1 C8 109.8(10) 2_655 12 ?
C8 N1 C8 139.0(9) 11_655 12 ?
C8 N1 C8 54.4(10) . 12 ?
C9 N1 Zn1 110.7(6) . . ?
C9 N1 Zn1 110.7(6) 12 . ?
C8 N1 Zn1 110.5(5) 2_655 . ?
C8 N1 Zn1 110.5(5) 11_655 . ?
C8 N1 Zn1 110.5(5) . . ?
C8 N1 Zn1 110.5(5) 12 . ?
N1 C8 C8 110.5(5) . 10 ?
N1 C9 C9 110.7(6) . 10 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.108

_iucr_refine_instructions_details 
;

;

_database_code_depnum_ccdc_archive 'CCDC 922544'
