# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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 
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#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
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data_IRMOF-3-AM4XL
_database_code_depnum_ccdc_archive 'CCDC 906534'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 O13 Zn4'
_chemical_formula_sum            'C24 H0 N0 O13 Zn4'
_chemical_formula_weight         759.72
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'
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           Cubic
_symmetry_space_group_name_H-M   Fm-3m
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'
_cell_length_a                   25.543(2)
_cell_length_b                   25.543(2)
_cell_length_c                   25.543(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16666(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    622
_cell_measurement_theta_min      4.51
_cell_measurement_theta_max      19.51
_exptl_crystal_description       'square block'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    0.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8159
_exptl_absorpt_correction_T_max  0.9187
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_reflns_number            2430
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         19.72
_reflns_number_total             430
_reflns_number_gt                284
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Due to weak diffraction, CheckCif reported Alert_A on low theta_max/
wavelength. Due to the severe disorders, we cannot locate the
substituents on the ligands. SQUEEZE protocol has found 1304 electrons
that can be accounted for the disordered solvents and substituents.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         430
_refine_ls_number_parameters     25
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0900
_refine_ls_wR_factor_ref         0.2908
_refine_ls_wR_factor_gt          0.2624
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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
_platon_squeeze_void_content
1 -0.014 -0.007 -0.006 12993 1304 ' '
_platon_squeeze_details          
;
;
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 0.79368(5) 0.70632(5) 0.29368(5) 0.1452(19) Uani 1 6 d S . .
O13 O 0.7824(4) 0.6343(5) 0.2824(4) 0.229(6) Uani 1 2 d S . .
O1 O 0.7500 0.7500 0.2500 0.125(7) Uani 1 24 d S . .
C2 C 0.7500 0.6126(8) 0.2500 0.218(11) Uani 1 4 d S . .
C1 C 0.7223(8) 0.5238(7) 0.2223(8) 0.308(15) Uani 1 2 d S . .
C3 C 0.7500 0.5552(10) 0.2500 0.193(8) Uani 1 4 d S . .
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 0.1452(19) 0.1452(19) 0.1452(19) 0.0067(7) -0.0067(7) 0.0067(7)
O13 0.264(9) 0.159(10) 0.264(9) -0.020(6) -0.019(8) -0.020(6)
O1 0.125(7) 0.125(7) 0.125(7) 0.000 0.000 0.000
C2 0.28(2) 0.094(16) 0.28(2) 0.000 -0.02(3) 0.000
C1 0.39(2) 0.139(14) 0.39(2) -0.026(8) -0.10(3) -0.026(8)
C3 0.209(14) 0.16(2) 0.209(14) 0.000 -0.037(15) 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 O13 1.883(12) . ?
Zn1 O13 1.883(12) 86_566 ?
Zn1 O13 1.883(12) 61_664 ?
Zn1 O1 1.933(2) . ?
Zn1 Zn1 3.156(4) 122_565 ?
Zn1 Zn1 3.156(4) 75_665 ?
Zn1 Zn1 3.156(4) 148_655 ?
O13 C2 1.294(11) . ?
O1 Zn1 1.933(2) 122_565 ?
O1 Zn1 1.933(2) 148_655 ?
O1 Zn1 1.933(2) 75_665 ?
C2 O13 1.295(11) 57_655 ?
C2 C3 1.47(3) . ?
C1 C1 1.21(3) 105_565 ?
C1 C3 1.28(2) . ?
C1 C1 2.00(6) 57_655 ?
C3 C1 1.28(2) 57_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
O13 Zn1 O13 106.0(4) . 86_566 ?
O13 Zn1 O13 106.0(4) . 61_664 ?
O13 Zn1 O13 106.0(4) 86_566 61_664 ?
O13 Zn1 O1 112.7(4) . . ?
O13 Zn1 O1 112.7(4) 86_566 . ?
O13 Zn1 O1 112.7(4) 61_664 . ?
O13 Zn1 Zn1 77.5(4) . 122_565 ?
O13 Zn1 Zn1 125.6(3) 86_566 122_565 ?
O13 Zn1 Zn1 125.6(3) 61_664 122_565 ?
O1 Zn1 Zn1 35.3 . 122_565 ?
O13 Zn1 Zn1 125.6(3) . 75_665 ?
O13 Zn1 Zn1 77.5(4) 86_566 75_665 ?
O13 Zn1 Zn1 125.6(3) 61_664 75_665 ?
O1 Zn1 Zn1 35.3 . 75_665 ?
Zn1 Zn1 Zn1 60.0 122_565 75_665 ?
O13 Zn1 Zn1 125.6(3) . 148_655 ?
O13 Zn1 Zn1 125.6(3) 86_566 148_655 ?
O13 Zn1 Zn1 77.5(4) 61_664 148_655 ?
O1 Zn1 Zn1 35.3 . 148_655 ?
Zn1 Zn1 Zn1 60.0 122_565 148_655 ?
Zn1 Zn1 Zn1 59.999(1) 75_665 148_655 ?
C2 O13 Zn1 127.9(13) . . ?
Zn1 O1 Zn1 109.475(1) . 122_565 ?
Zn1 O1 Zn1 109.474(1) . 148_655 ?
Zn1 O1 Zn1 109.5 122_565 148_655 ?
Zn1 O1 Zn1 109.5 . 75_665 ?
Zn1 O1 Zn1 109.468(1) 122_565 75_665 ?
Zn1 O1 Zn1 109.468(2) 148_655 75_665 ?
O13 C2 O13 129(2) . 57_655 ?
O13 C2 C3 115.4(10) . . ?
O13 C2 C3 115.4(10) 57_655 . ?
C1 C1 C3 128.8(15) 105_565 . ?
C1 C1 C1 90.000(3) 105_565 57_655 ?
C3 C1 C1 38.8(15) . 57_655 ?
C1 C3 C1 102(3) . 57_655 ?
C1 C3 C2 128.8(15) . . ?
C1 C3 C2 128.8(15) 57_655 . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        19.72
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.067


data_IRMOF-3-AM7XL
_database_code_depnum_ccdc_archive 'CCDC 906535'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H0 N0 O13 Zn4'
_chemical_formula_sum            'C24 H0 N0 O13 Zn4'
_chemical_formula_weight         757.72
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           Cubic
_symmetry_space_group_name_H-M   Fm-3m
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'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'
'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'
'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'
'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, 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, 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'
'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'
'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'
'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'
'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, 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, 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'
'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'
'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'
'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'
'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, 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, 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'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-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'
'-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'
'-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'
'-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, -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, -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'
'-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'
'-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'
'-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'
'-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, -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, -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'
'-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'
'-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'
'-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'
'-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, -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, -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'
_cell_length_a                   25.654(19)
_cell_length_b                   25.654(19)
_cell_length_c                   25.654(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16884(22)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    568
_cell_measurement_theta_min      4.49
_cell_measurement_theta_max      19.49
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_max          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8952
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1773
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         19.70
_reflns_number_total             418
_reflns_number_gt                227
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The structure of IRMOF_Az was collected at 250 K because at lower
temperature, the diffraction was weak and the resolution was low.
The organic linkers are severely disordered and distored, thus we cannot
locate the substituents and C1 and C2 have to be refined as isotropically
rather than anisotropically.Due to the low resolution and weak diffraction,
CheckCif reported Alert_A on low value of theta_max/wavelenght.
SQUEEZE protocol has found 2124 electrons that can be accounted for
the disordered solvent molecules and substituents.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         418
_refine_ls_number_parameters     21
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.1074
_refine_ls_wR_factor_ref         0.3421
_refine_ls_wR_factor_gt          0.2889
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.2146(4) 0.1334(5) 0.2146(4) 0.188(6) Uani 1 2 d S . .
O2 O 0.2500 0.2500 0.2500 0.133(12) Uani 1 24 d S . .
C3 C 0.2189(8) 0.0230(7) 0.2189(8) 0.243(14) Uani 1 2 d S . .
C1 C 0.2500 0.1152(18) 0.2500 0.187(14) Uiso 1 4 d SD . .
C2 C 0.2500 0.0562(19) 0.2500 0.239(18) Uiso 1 4 d SD . .
Zn1 Zn 0.20639(7) 0.20639(7) 0.20639(7) 0.124(2) Uani 1 6 d S . .
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 0.200(9) 0.162(12) 0.200(9) -0.015(7) 0.031(10) -0.015(7)
O2 0.133(12) 0.133(12) 0.133(12) 0.000 0.000 0.000
C3 0.30(2) 0.127(17) 0.30(2) 0.004(12) 0.00(2) 0.004(12)
Zn1 0.124(2) 0.124(2) 0.124(2) -0.0025(10) -0.0025(10) -0.0025(10)
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
_platon_squeeze_void_content
1 -0.014 -0.007 -0.006 13163 2124 ' '
_platon_squeeze_details          
;
;
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.367(16) . ?
O1 Zn1 1.895(14) . ?
O2 Zn1 1.938(4) 28 ?
O2 Zn1 1.938(4) 74 ?
O2 Zn1 1.938(4) . ?
O2 Zn1 1.938(4) 51 ?
C3 C3 1.18(4) 99 ?
C3 C2 1.41(3) . ?
C1 O1 1.367(16) 51 ?
C1 C2 1.513(19) . ?
C2 C3 1.41(3) 51 ?
Zn1 O1 1.895(14) 9 ?
Zn1 O1 1.895(14) 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
C1 O1 Zn1 119(2) . . ?
Zn1 O2 Zn1 109.474(1) 28 74 ?
Zn1 O2 Zn1 109.5 28 . ?
Zn1 O2 Zn1 109.5 74 . ?
Zn1 O2 Zn1 109.5 28 51 ?
Zn1 O2 Zn1 109.472(1) 74 51 ?
Zn1 O2 Zn1 109.5 . 51 ?
C3 C3 C2 127(2) 99 . ?
O1 C1 O1 140(4) 51 . ?
O1 C1 C2 110(2) 51 . ?
O1 C1 C2 110(2) . . ?
C3 C2 C3 106(4) 51 . ?
C3 C2 C1 127(2) 51 . ?
C3 C2 C1 127(2) . . ?
O1 Zn1 O1 101.9(6) . 9 ?
O1 Zn1 O1 101.9(6) . 5 ?
O1 Zn1 O1 101.9(6) 9 5 ?
O1 Zn1 O2 116.2(5) . . ?
O1 Zn1 O2 116.2(5) 9 . ?
O1 Zn1 O2 116.2(5) 5 . ?
_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        19.70
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.089


data_IRMOF-3-AM3XL
_database_code_depnum_ccdc_archive 'CCDC 906536'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H9 N0 O13 Zn4'
_chemical_formula_weight         766.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Fm-3m
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -z, y'
'x, z, -y'
'z, y, -x'
'-z, y, x'
'-y, x, z'
'y, -x, z'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'x, -y, -z'
'-x, y, -z'
'-x, -y, z'
'y, x, -z'
'-y, -x, -z'
'z, -y, x'
'-z, -y, -x'
'-x, z, y'
'-x, -z, -y'
'x, y+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-z, y+1/2, x+1/2'
'-y, x+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+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'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+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, -z, y+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-z+1/2, y, x+1/2'
'-y+1/2, x, z+1/2'
'y+1/2, -x, z+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+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'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+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, -z+1/2, y'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-z+1/2, y+1/2, x'
'-y+1/2, x+1/2, z'
'y+1/2, -x+1/2, z'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'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'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'-x, -y, -z'
'-x, z, -y'
'-x, -z, y'
'-z, -y, x'
'z, -y, -x'
'y, -x, -z'
'-y, x, -z'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-x, y, z'
'x, -y, z'
'x, y, -z'
'-y, -x, z'
'y, x, z'
'-z, y, -x'
'z, y, x'
'x, -z, -y'
'x, z, y'
'-x, -y+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'z, -y+1/2, -x+1/2'
'y, -x+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+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'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+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, z, -y+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'z+1/2, -y, -x+1/2'
'y+1/2, -x, -z+1/2'
'-y+1/2, x, -z+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+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'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+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, z+1/2, -y'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'z+1/2, -y+1/2, -x'
'y+1/2, -x+1/2, -z'
'-y+1/2, x+1/2, -z'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-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'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
_cell_length_a                   25.5827(7)
_cell_length_b                   25.5827(7)
_cell_length_c                   25.5827(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16743.2(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    787
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      38.78
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_max          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    0.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3016
_exptl_absorpt_coefficient_mu    1.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8356
_exptl_absorpt_correction_T_max  0.9146
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            374
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         46.06
_reflns_number_total             374
_reflns_number_gt                231
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The resolution of the crystal was at ~1.0 Angstrom, but we collected and
integrated the data upto to 0.83 to ensure if we can locate any substituents
on the organic ligand. (CHECKCIF reported Alert A on low completeness and
value of sine (theta_max)/wavelength <0.550.
Electron density for nitrogen atoms that belong to the cross-linker was found.
However, it is severely disordered, and we tried to resolve the disorders but
it then unabled us to apply SQUEEZE protocol to the structure (the refinement
is unstable/ not convergent).
SQUEEZE protocol found 2159 electrons in the structure that can be accounted
for the disorders DMF molecules and the cross-linker group.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         374
_refine_ls_number_parameters     25
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.1085
_refine_ls_wR_factor_ref         0.3420
_refine_ls_wR_factor_gt          0.3319
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_restrained_S_all      1.329
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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
_platon_squeeze_void_content
1 -0.014 -0.007 -0.006 12763 2159 ' '
_platon_squeeze_details          
;
;
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
O2 O 0.2500 0.2500 0.2500 0.174(9) Uani 1 24 d S . .
O1 O 0.2191(4) 0.1357(7) 0.2191(4) 0.242(6) Uani 1 2 d S . .
C1 C 0.2500 0.1142(16) 0.2500 0.225(12) Uani 1 4 d SD . .
C2 C 0.2500 0.0566(16) 0.2500 0.220(10) Uani 1 4 d SD . .
C3 C 0.2799(6) 0.0259(9) 0.2799(6) 0.268(11) Uani 1 2 d SD . .
H3 H 0.3028 0.0424 0.3028 0.321 Uiso 0.75 2 calc SPR . .
Zn1 Zn 0.20630(9) 0.20630(9) 0.20630(9) 0.197(3) Uani 1 6 d S . .
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
O2 0.174(9) 0.174(9) 0.174(9) 0.000 0.000 0.000
O1 0.262(10) 0.201(12) 0.262(10) -0.013(7) 0.003(9) -0.013(7)
C1 0.26(2) 0.16(3) 0.26(2) 0.000 -0.02(3) 0.000
C2 0.22(2) 0.22(5) 0.22(2) 0.000 0.00(2) 0.000
C3 0.304(16) 0.20(2) 0.304(16) -0.041(11) -0.049(16) -0.041(11)
Zn1 0.197(3) 0.197(3) 0.197(3) 0.0034(13) 0.0034(13) 0.0034(13)
_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
O2 Zn1 1.936(4) . ?
O2 Zn1 1.936(4) 125 ?
O2 Zn1 1.936(4) 171 ?
O2 Zn1 1.936(4) 146 ?
O1 C1 1.246(14) . ?
O1 Zn1 1.865(17) . ?
C1 O1 1.246(14) 65 ?
C1 C2 1.473(19) . ?
C2 C3 1.336(16) . ?
C2 C3 1.336(16) 65 ?
C3 C3 1.33(4) 113 ?
Zn1 O1 1.865(17) 9 ?
Zn1 O1 1.865(17) 8 ?
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 O2 Zn1 109.5 . 125 ?
Zn1 O2 Zn1 109.5 . 171 ?
Zn1 O2 Zn1 109.472(1) 125 171 ?
Zn1 O2 Zn1 109.5 . 146 ?
Zn1 O2 Zn1 109.5 125 146 ?
Zn1 O2 Zn1 109.471(1) 171 146 ?
C1 O1 Zn1 131(2) . . ?
O1 C1 O1 128(4) 65 . ?
O1 C1 C2 116.2(18) 65 . ?
O1 C1 C2 116.2(18) . . ?
C3 C2 C3 108(3) . 65 ?
C3 C2 C1 126.0(16) . . ?
C3 C2 C1 126.0(16) 65 . ?
C3 C3 C2 126.0(16) 113 . ?
O1 Zn1 O1 108.0(5) . 9 ?
O1 Zn1 O1 108.0(5) . 8 ?
O1 Zn1 O1 108.0(5) 9 8 ?
O1 Zn1 O2 110.9(5) . . ?
O1 Zn1 O2 110.9(5) 9 . ?
O1 Zn1 O2 110.9(5) 8 . ?
_diffrn_measured_fraction_theta_max 0.901
_diffrn_reflns_theta_full        46.06
_diffrn_measured_fraction_theta_full 0.901
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.071


data_IRMOF-3-AM5XL
_database_code_depnum_ccdc_archive 'CCDC 906537'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H6 N0 O13 Zn4'
_chemical_formula_sum            'C24 H6 N0 O13 Zn4'
_chemical_formula_weight         763.77
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'F-43m '
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'
_cell_length_a                   25.6341(6)
_cell_length_b                   25.6341(6)
_cell_length_c                   25.6341(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     16844.3(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    2571
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      67.74
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_max          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    0.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2992
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8458
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8625
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         68.33
_reflns_number_total             1489
_reflns_number_gt                1007
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The Alert A for high or low Ueq for C2, C3, and C4 are due to distortion
of the benzene ring. C2, C3, and C4 have to be carbon atoms due to the
structure of the ligand. We cannot locate the substituents of the ligand
because of the severe disorder. SQUEEZE protocol found 2071 electrons that
belong to the solvent molecules [eg. DMF, CHCl3] and the substituents. The
Shelx program suggest the space group as Fm-3m but the structure could not
be solved and refined using that space group so F-43m was used.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_number_reflns         1489
_refine_ls_number_parameters     49
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0995
_refine_ls_wR_factor_ref         0.3213
_refine_ls_wR_factor_gt          0.2994
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_restrained_S_all      1.226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.0000 0.5000 0.0000 0.086(4) Uani 1 24 d S . .
O2 O 0.0000 0.5000 0.5000 0.083(4) Uani 1 24 d S . .
O3 O 0.0304(4) 0.4696(4) 0.3855(3) 0.178(5) Uani 1 2 d S . .
O4 O 0.0302(3) 0.4698(3) 0.1167(4) 0.145(3) Uani 1 2 d SD . .
C2 C 0.0000 0.5000 0.3635(6) 0.215(15) Uani 1 4 d S . .
C3 C 0.0000 0.5000 0.2995(6) 0.132(6) Uani 1 4 d S . .
C4 C 0.0317(13) 0.4683(13) 0.2750(6) 0.39(3) Uani 1 2 d SD . .
C1 C 0.0000 0.5000 0.1416(6) 0.112(4) Uani 1 4 d SD . .
C5 C 0.0000 0.5000 0.1921(9) 0.142(6) Uani 1 4 d S . .
C6 C 0.0306(4) 0.4694(4) 0.2244(5) 0.169(6) Uani 1 2 d SD . .
H6 H 0.0534 0.4466 0.2077 0.203 Uiso 1 2 calc SR . .
Zn1 Zn 0.04333(5) 0.45667(5) 0.45667(5) 0.1041(8) Uani 1 6 d S . .
Zn2 Zn 0.04332(5) 0.45668(5) 0.04332(5) 0.1049(8) Uani 1 6 d S . .
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 0.086(4) 0.086(4) 0.086(4) 0.000 0.000 0.000
O2 0.083(4) 0.083(4) 0.083(4) 0.000 0.000 0.000
O3 0.239(8) 0.239(8) 0.056(3) 0.018(4) -0.018(4) -0.005(10)
O4 0.157(4) 0.157(4) 0.120(5) 0.005(3) -0.005(3) 0.040(7)
C2 0.30(2) 0.30(2) 0.040(6) 0.000 0.000 -0.12(3)
C3 0.159(10) 0.159(10) 0.077(8) 0.000 0.000 0.033(13)
C4 0.54(4) 0.54(4) 0.092(10) -0.030(13) 0.030(13) 0.09(5)
C1 0.105(5) 0.105(5) 0.127(11) 0.000 0.000 0.005(7)
C5 0.157(10) 0.157(10) 0.112(11) 0.000 0.000 -0.019(13)
C6 0.189(9) 0.189(9) 0.128(8) 0.001(5) -0.001(5) 0.082(11)
Zn1 0.1041(8) 0.1041(8) 0.1041(8) -0.0011(8) 0.0011(8) 0.0011(8)
Zn2 0.1049(8) 0.1049(8) 0.1049(8) 0.0041(9) -0.0041(9) 0.0041(9)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_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
_platon_squeeze_void_content
1 -0.006 0.100 0.115 11693 2071 ' '
_platon_squeeze_details          
;
;
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 Zn2 1.924(2) . ?
O1 Zn2 1.924(2) 3_565 ?
O1 Zn2 1.924(2) 2_565 ?
O1 Zn2 1.924(2) 4 ?
O2 Zn1 1.924(2) 2_566 ?
O2 Zn1 1.924(2) . ?
O2 Zn1 1.924(2) 4_556 ?
O2 Zn1 1.924(2) 3_565 ?
O3 C2 1.238(14) . ?
O3 Zn1 1.884(8) . ?
O4 C1 1.266(12) . ?
O4 Zn2 1.941(9) . ?
C2 O3 1.238(14) 3_565 ?
C2 C3 1.64(2) . ?
C3 C4 1.31(4) 3_565 ?
C3 C4 1.31(4) . ?
C4 C6 1.296(15) . ?
C1 O4 1.266(12) 3_565 ?
C1 C5 1.29(3) . ?
C5 C6 1.39(2) 3_565 ?
C5 C6 1.39(2) . ?
Zn1 O3 1.884(8) 63 ?
Zn1 O3 1.884(8) 60 ?
Zn1 Zn1 3.142(4) 2_566 ?
Zn1 Zn1 3.142(4) 4_556 ?
Zn1 Zn1 3.142(4) 3_565 ?
Zn2 O4 1.941(9) 14 ?
Zn2 O4 1.941(9) 82 ?
Zn2 Zn2 3.141(4) 3_565 ?
Zn2 Zn2 3.141(4) 2_565 ?
Zn2 Zn2 3.141(4) 4 ?
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
Zn2 O1 Zn2 109.5 . 3_565 ?
Zn2 O1 Zn2 109.5 . 2_565 ?
Zn2 O1 Zn2 109.5 3_565 2_565 ?
Zn2 O1 Zn2 109.5 . 4 ?
Zn2 O1 Zn2 109.5 3_565 4 ?
Zn2 O1 Zn2 109.5 2_565 4 ?
Zn1 O2 Zn1 109.471(1) 2_566 . ?
Zn1 O2 Zn1 109.5 2_566 4_556 ?
Zn1 O2 Zn1 109.5 . 4_556 ?
Zn1 O2 Zn1 109.5 2_566 3_565 ?
Zn1 O2 Zn1 109.5 . 3_565 ?
Zn1 O2 Zn1 109.5 4_556 3_565 ?
C2 O3 Zn1 131.4(9) . . ?
C1 O4 Zn2 134.5(8) . . ?
O3 C2 O3 126.0(12) 3_565 . ?
O3 C2 C3 117.0(6) 3_565 . ?
O3 C2 C3 117.0(6) . . ?
C4 C3 C4 123(3) 3_565 . ?
C4 C3 C2 118.7(13) 3_565 . ?
C4 C3 C2 118.7(13) . . ?
C6 C4 C3 117(4) . . ?
O4 C1 O4 119.5(13) . 3_565 ?
O4 C1 C5 120.3(7) . . ?
O4 C1 C5 120.3(7) 3_565 . ?
C1 C5 C6 126.8(9) . 3_565 ?
C1 C5 C6 126.8(9) . . ?
C6 C5 C6 106.5(19) 3_565 . ?
C4 C6 C5 128(3) . . ?
O3 Zn1 O3 108.0(5) 63 . ?
O3 Zn1 O3 108.0(5) 63 60 ?
O3 Zn1 O3 108.0(5) . 60 ?
O3 Zn1 O2 110.9(4) 63 . ?
O3 Zn1 O2 110.9(4) . . ?
O3 Zn1 O2 110.9(4) 60 . ?
O3 Zn1 Zn1 75.6(4) 63 2_566 ?
O3 Zn1 Zn1 124.1(4) . 2_566 ?
O3 Zn1 Zn1 124.1(4) 60 2_566 ?
O2 Zn1 Zn1 35.3 . 2_566 ?
O3 Zn1 Zn1 124.1(4) 63 4_556 ?
O3 Zn1 Zn1 124.1(4) . 4_556 ?
O3 Zn1 Zn1 75.6(4) 60 4_556 ?
O2 Zn1 Zn1 35.3 . 4_556 ?
Zn1 Zn1 Zn1 60.0 2_566 4_556 ?
O3 Zn1 Zn1 124.1(4) 63 3_565 ?
O3 Zn1 Zn1 75.6(4) . 3_565 ?
O3 Zn1 Zn1 124.1(4) 60 3_565 ?
O2 Zn1 Zn1 35.3 . 3_565 ?
Zn1 Zn1 Zn1 60.0 2_566 3_565 ?
Zn1 Zn1 Zn1 60.0 4_556 3_565 ?
O1 Zn2 O4 111.0(3) . 14 ?
O1 Zn2 O4 111.0(3) . . ?
O4 Zn2 O4 107.9(3) 14 . ?
O1 Zn2 O4 111.0(3) . 82 ?
O4 Zn2 O4 107.9(3) 14 82 ?
O4 Zn2 O4 107.9(3) . 82 ?
O1 Zn2 Zn2 35.3 . 3_565 ?
O4 Zn2 Zn2 124.2(2) 14 3_565 ?
O4 Zn2 Zn2 75.8(3) . 3_565 ?
O4 Zn2 Zn2 124.2(2) 82 3_565 ?
O1 Zn2 Zn2 35.3 . 2_565 ?
O4 Zn2 Zn2 75.8(3) 14 2_565 ?
O4 Zn2 Zn2 124.2(2) . 2_565 ?
O4 Zn2 Zn2 124.2(2) 82 2_565 ?
Zn2 Zn2 Zn2 60.0 3_565 2_565 ?
O1 Zn2 Zn2 35.3 . 4 ?
O4 Zn2 Zn2 124.2(2) 14 4 ?
O4 Zn2 Zn2 124.2(2) . 4 ?
O4 Zn2 Zn2 75.8(3) 82 4 ?
Zn2 Zn2 Zn2 60.0 3_565 4 ?
Zn2 Zn2 Zn2 60.0 2_565 4 ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        68.33
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.087


data_IRMOF-3-AM6XL
_database_code_depnum_ccdc_archive 'CCDC 906538'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H6 N0 O13 Zn4'
_chemical_formula_sum            'C24 H6 N0 O13 Zn4'
_chemical_formula_weight         763.77
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           Cubic
_symmetry_space_group_name_H-M   'F-43m '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'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'
'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'
'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'
'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, 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, 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'
'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'
'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'
'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'
'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, 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, 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'
'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'
'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'
'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'
'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, 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, 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'
_cell_length_a                   25.741(3)
_cell_length_b                   25.741(3)
_cell_length_c                   25.741(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17055(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    1264
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      21.17
_exptl_crystal_description       cubic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    0.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2992
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8952
_exptl_absorpt_correction_T_max  0.9149
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3726
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         21.68
_reflns_number_total             1018
_reflns_number_gt                739
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The alert A about the low value of sine(theta_max)/wavelength is caused by
weak diffraction of the crystal. We cannot locate the substituents of
the ligand because of the severe disorder. SQUEEZE protocol found 6271
electrons that belong to the solvent molecules [eg. DMF, CHCl3] and the
substituents. Shelx program suggest the space group as Fm-3m but the
structure could not be solved and refined using that space group so F-43m
was used.
;
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
_platon_squeeze_void_content
1 -0.003 0.108 0.350 13091 6271 ' '
_platon_squeeze_details          
;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(17)
_refine_ls_number_reflns         1018
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.2063
_refine_ls_wR_factor_gt          0.1999
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
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 0.95662(7) 0.45662(7) 0.04338(7) 0.0508(10) Uani 1 6 d S . .
Zn2 Zn 0.95657(7) 0.45657(7) 0.45657(7) 0.0514(10) Uani 1 6 d S . .
O1 O 0.9683(5) 0.4683(5) 0.3849(5) 0.105(5) Uani 1 2 d S . .
O2 O 1.0000 0.5000 0.5000 0.028(8) Uani 1 24 d S . .
O3 O 0.9708(4) 0.4708(4) 0.1169(4) 0.097(5) Uani 1 2 d S . .
O4 O 1.0000 0.5000 0.0000 0.056(11) Uani 1 24 d S . .
C1 C 1.0000 0.5000 0.1951(11) 0.079(9) Uani 1 4 d S . .
C2 C 0.9705(8) 0.4705(8) 0.2285(7) 0.138(12) Uani 1 2 d S . .
C3 C 1.0000 0.5000 0.2993(12) 0.089(10) Uani 1 4 d S . .
C4 C 0.9677(6) 0.4677(6) 0.2765(5) 0.107(9) Uani 1 2 d S . .
H4 H 0.9455 0.4455 0.2942 0.128 Uiso 1 2 calc SR . .
C5 C 1.0000 0.5000 0.3607(16) 0.098(12) Uani 1 4 d S . .
C6 C 1.0000 0.5000 0.1383(9) 0.063(8) Uani 1 4 d S . .
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 0.0508(10) 0.0508(10) 0.0508(10) 0.0017(13) 0.0017(13) -0.0017(13)
Zn2 0.0514(10) 0.0514(10) 0.0514(10) -0.0031(13) -0.0031(13) -0.0031(13)
O1 0.115(7) 0.115(7) 0.084(9) 0.017(7) 0.017(7) -0.016(12)
O2 0.028(8) 0.028(8) 0.028(8) 0.000 0.000 0.000
O3 0.127(8) 0.127(8) 0.035(7) 0.010(5) 0.010(5) -0.047(12)
O4 0.056(11) 0.056(11) 0.056(11) 0.000 0.000 0.000
C1 0.110(14) 0.110(14) 0.017(10) 0.000 0.000 -0.024(17)
C2 0.178(18) 0.178(18) 0.057(14) 0.012(9) 0.012(9) -0.04(2)
C3 0.095(14) 0.095(14) 0.08(2) 0.000 0.000 -0.003(19)
C4 0.145(14) 0.145(14) 0.031(11) 0.021(6) 0.021(6) -0.091(16)
C5 0.092(16) 0.092(16) 0.11(3) 0.000 0.000 0.00(3)
C6 0.084(13) 0.084(13) 0.021(14) 0.000 0.000 0.00(2)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 1.934(3) . ?
Zn1 O3 1.961(12) . ?
Zn1 O3 1.961(12) 83_556 ?
Zn1 O3 1.961(12) 32_645 ?
Zn1 Zn1 3.158(5) 2_765 ?
Zn1 Zn1 3.158(5) 3_755 ?
Zn1 Zn1 3.158(5) 4_565 ?
Zn2 O1 1.894(13) 57_554 ?
Zn2 O1 1.894(13) 77_545 ?
Zn2 O1 1.894(13) . ?
Zn2 O2 1.936(3) . ?
O1 C5 1.31(2) . ?
O2 Zn2 1.936(3) 4_566 ?
O2 Zn2 1.936(3) 2_765 ?
O2 Zn2 1.936(3) 3_756 ?
O3 C6 1.197(15) . ?
O4 Zn1 1.934(3) 2_765 ?
O4 Zn1 1.934(3) 3_755 ?
O4 Zn1 1.934(3) 4_565 ?
C1 C2 1.37(3) 2_765 ?
C1 C2 1.37(3) . ?
C1 C6 1.46(4) . ?
C2 C4 1.240(15) . ?
C3 C4 1.31(2) . ?
C3 C4 1.31(2) 2_765 ?
C3 C5 1.58(5) . ?
C4 H4 0.9300 . ?
C5 O1 1.31(2) 2_765 ?
C6 O3 1.197(15) 2_765 ?
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 O3 110.0(5) . . ?
O4 Zn1 O3 110.0(5) . 83_556 ?
O3 Zn1 O3 108.9(5) . 83_556 ?
O4 Zn1 O3 110.0(5) . 32_645 ?
O3 Zn1 O3 108.9(5) . 32_645 ?
O3 Zn1 O3 108.9(5) 83_556 32_645 ?
O4 Zn1 Zn1 35.3 . 2_765 ?
O3 Zn1 Zn1 74.7(5) . 2_765 ?
O3 Zn1 Zn1 123.4(4) 83_556 2_765 ?
O3 Zn1 Zn1 123.4(4) 32_645 2_765 ?
O4 Zn1 Zn1 35.3 . 3_755 ?
O3 Zn1 Zn1 123.4(4) . 3_755 ?
O3 Zn1 Zn1 74.7(5) 83_556 3_755 ?
O3 Zn1 Zn1 123.4(4) 32_645 3_755 ?
Zn1 Zn1 Zn1 60.0 2_765 3_755 ?
O4 Zn1 Zn1 35.3 . 4_565 ?
O3 Zn1 Zn1 123.4(4) . 4_565 ?
O3 Zn1 Zn1 123.4(4) 83_556 4_565 ?
O3 Zn1 Zn1 74.7(5) 32_645 4_565 ?
Zn1 Zn1 Zn1 60.0 2_765 4_565 ?
Zn1 Zn1 Zn1 60.0 3_755 4_565 ?
O1 Zn2 O1 106.6(6) 57_554 77_545 ?
O1 Zn2 O1 106.6(6) 57_554 . ?
O1 Zn2 O1 106.6(6) 77_545 . ?
O1 Zn2 O2 112.2(6) 57_554 . ?
O1 Zn2 O2 112.2(6) 77_545 . ?
O1 Zn2 O2 112.2(6) . . ?
C5 O1 Zn2 131(2) . . ?
Zn2 O2 Zn2 109.5 . 4_566 ?
Zn2 O2 Zn2 109.5 . 2_765 ?
Zn2 O2 Zn2 109.471(1) 4_566 2_765 ?
Zn2 O2 Zn2 109.5 . 3_756 ?
Zn2 O2 Zn2 109.471(1) 4_566 3_756 ?
Zn2 O2 Zn2 109.471(1) 2_765 3_756 ?
C6 O3 Zn1 132.7(14) . . ?
Zn1 O4 Zn1 109.471(1) 2_765 3_755 ?
Zn1 O4 Zn1 109.5 2_765 . ?
Zn1 O4 Zn1 109.5 3_755 . ?
Zn1 O4 Zn1 109.5 2_765 4_565 ?
Zn1 O4 Zn1 109.5 3_755 4_565 ?
Zn1 O4 Zn1 109.5 . 4_565 ?
C2 C1 C2 103(3) 2_765 . ?
C2 C1 C6 128.7(13) 2_765 . ?
C2 C1 C6 128.7(13) . . ?
C4 C2 C1 133(3) . . ?
C4 C3 C4 127(3) . 2_765 ?
C4 C3 C5 116.5(13) . . ?
C4 C3 C5 116.5(13) 2_765 . ?
C2 C4 C3 112(3) . . ?
C2 C4 H4 124.1 . . ?
C3 C4 H4 124.1 . . ?
O1 C5 O1 123(3) . 2_765 ?
O1 C5 C3 118.4(16) . . ?
O1 C5 C3 118.4(16) 2_765 . ?
O3 C6 O3 125(2) . 2_765 ?
O3 C6 C1 117.4(11) . . ?
O3 C6 C1 117.4(11) 2_765 . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        21.68
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.179