# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

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

data_UOF_1A
_audit_block_doi                 10.5517/ccdc.csd.cc1pkgl9
_database_code_depnum_ccdc_archive 'CCDC 1565921'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_CHEMW03_UOF_1A              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The squeezed solvent molecules were included in the 
formula. See platon_squeeze_details
;
_vrf_RINTA01_UOF_1A              
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Owing to the disordered solvent and high ADPs, the data is of poor quality. 
;
_vrf_PLAT020_UOF_1A              
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.304 Report
RESPONSE: Owing to the disordered solvent and high ADPs, the data is of poor quality. 
;
_vrf_PLAT026_UOF_1A              
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         22 %     
RESPONSE: Owing to the disordered solvent and high ADPs, the data is of poor quality. 
;
_vrf_PLAT084_UOF_1A              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.50 Report
RESPONSE: Owing to the disordered solvent and high ADPs, the data is of poor quality. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C19 H14 Cu O4)(H2O)(C3 H7 N O)7'
_chemical_formula_sum            'C40 H64 Cu N7 O12'
_chemical_formula_weight         898.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_H-M_alt        'P 42/m m c'
_space_group_name_Hall           '-P 4c 2'

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

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

_cell_length_a                   14.686(5)
_cell_length_b                   14.686(5)
_cell_length_c                   26.103(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5630(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    407
_cell_measurement_theta_min      4.2600
_cell_measurement_theta_max      63.2950

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_F_000             788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2064
_exptl_crystal_size_mid          0.1329
_exptl_crystal_size_min          0.0883
_exptl_absorpt_coefficient_mu    0.992
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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           
;
 ?
;

_diffrn_ambient_temperature      100.0(2)
_diffrn_ambient_environment      N2
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.1725
_diffrn_reflns_number            22352
_diffrn_reflns_av_unetI/netI     0.1438
_diffrn_reflns_av_R_equivalents  0.3040
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.453
_diffrn_reflns_theta_max         67.952
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2826
_reflns_number_gt                625
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXL-T (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 > 2σ(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.
The structure was severely disordered.
The solvent molecules could not be adequately located and were SQUEEZEd
from the structure. The SQUEEZEd electron density can be attributed to 7
DMF molecules per Cu(II) cation.
H-atoms were not affixed to the axial H2O molecule.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1500P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2826
_refine_ls_number_parameters     35
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.3011
_refine_ls_R_factor_gt           0.1642
_refine_ls_wR_factor_ref         0.5026
_refine_ls_wR_factor_gt          0.4208
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002

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
C1 C 0.8854(8) 0.5000 0.4365(4) 0.094(3) Uiso 1 2 d DS . P . .
C2 C 0.8121(13) 0.5000 0.3967(7) 0.183(8) Uiso 1 2 d DS . P . .
C3 C 0.7859(13) 0.4253(12) 0.3741(7) 0.234(8) Uiso 1 1 d . . . . .
H3 H 0.8196 0.3727 0.3798 0.280 Uiso 1 1 calc R U . . .
C4 C 0.6993(12) 0.4186(11) 0.3372(6) 0.214(6) Uiso 1 1 d . . . . .
H4 H 0.6719 0.3635 0.3287 0.257 Uiso 1 1 calc R U . . .
C5 C 0.6692(12) 0.5000 0.3192(6) 0.152(6) Uiso 1 2 d S . P . .
C6 C 0.5861(8) 0.5000 0.2821(4) 0.091(3) Uiso 1 2 d S . P . .
C7 C 0.5828(6) 0.4172(6) 0.2500 0.104(3) Uiso 1 2 d S . P . .
H7A H 0.5844 0.3639 0.2719 0.125 Uiso 0.5 1 calc R U P . .
H7B H 0.6361 0.4156 0.2281 0.125 Uiso 0.5 1 calc R U P . .
C8 C 0.5000 0.5000 0.3148(6) 0.106(5) Uiso 1 4 d S . P . .
H8A H 0.5000 0.4466 0.3367 0.127 Uiso 0.5 2 calc R U P . .
H8B H 0.5000 0.5534 0.3367 0.127 Uiso 0.5 2 calc R U P . .
O1 O 0.9040(5) 0.5794(5) 0.4478(3) 0.135(2) Uiso 1 1 d . . . . .
O2 O 1.0000 0.7367(14) 0.5000 0.209(8) Uiso 1 4 d S . P . .
Cu1 Cu 1.0000 0.5878(3) 0.5000 0.1534(19) Uani 1 4 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
Cu1 0.140(3) 0.246(5) 0.0738(14) 0.000 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
C1 O1 1.234(7) . ?
C1 O1 1.234(7) 13_565 ?
C1 C2 1.496(15) . ?
C2 C3 1.304(18) 13_565 ?
C2 C3 1.304(18) . ?
C3 C4 1.60(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.358(15) . ?
C4 H4 0.9300 . ?
C5 C4 1.358(15) 13_565 ?
C5 C6 1.558(19) . ?
C6 C7 1.477(8) 12_656 ?
C6 C7 1.477(8) . ?
C6 C8 1.525(13) . ?
C7 C6 1.477(8) 11_566 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C6 1.525(13) 2_665 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O1 Cu1 1.965(7) . ?
O2 Cu1 2.19(2) . ?
Cu1 O1 1.965(7) 5_756 ?
Cu1 O1 1.965(7) 14_755 ?
Cu1 O1 1.965(7) 10_556 ?
Cu1 Cu1 2.578(9) 9_766 ?

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 C1 O1 141.9(13) . 13_565 ?
O1 C1 C2 109.0(6) . . ?
O1 C1 C2 109.0(6) 13_565 . ?
C3 C2 C3 115(2) 13_565 . ?
C3 C2 C1 121.8(12) 13_565 . ?
C3 C2 C1 121.8(12) . . ?
C2 C3 C4 124.0(18) . . ?
C2 C3 H3 118.0 . . ?
C4 C3 H3 118.0 . . ?
C5 C4 C3 114.4(17) . . ?
C5 C4 H4 122.8 . . ?
C3 C4 H4 122.8 . . ?
C4 C5 C4 123(2) . 13_565 ?
C4 C5 C6 118.0(12) . . ?
C4 C5 C6 118.0(12) 13_565 . ?
C7 C6 C7 110.7(8) 12_656 . ?
C7 C6 C8 106.9(7) 12_656 . ?
C7 C6 C8 106.9(7) . . ?
C7 C6 C5 112.3(7) 12_656 . ?
C7 C6 C5 112.3(7) . . ?
C8 C6 C5 107.5(9) . . ?
C6 C7 C6 112.1(12) . 11_566 ?
C6 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 11_566 . ?
C6 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 11_566 . ?
H7A C7 H7B 107.9 . . ?
C6 C8 C6 111.9(13) 2_665 . ?
C6 C8 H8A 109.2 2_665 . ?
C6 C8 H8A 109.2 . . ?
C6 C8 H8B 109.2 2_665 . ?
C6 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C1 O1 Cu1 112.6(8) . . ?
O1 Cu1 O1 87.9(4) 5_756 14_755 ?
O1 Cu1 O1 91.7(4) 5_756 10_556 ?
O1 Cu1 O1 172.9(5) 14_755 10_556 ?
O1 Cu1 O1 172.8(5) 5_756 . ?
O1 Cu1 O1 91.7(4) 14_755 . ?
O1 Cu1 O1 87.9(4) 10_556 . ?
O1 Cu1 O2 93.6(2) 5_756 . ?
O1 Cu1 O2 93.6(2) 14_755 . ?
O1 Cu1 O2 93.6(2) 10_556 . ?
O1 Cu1 O2 93.6(2) . . ?
O1 Cu1 Cu1 86.4(2) 5_756 9_766 ?
O1 Cu1 Cu1 86.4(2) 14_755 9_766 ?
O1 Cu1 Cu1 86.4(2) 10_556 9_766 ?
O1 Cu1 Cu1 86.4(2) . 9_766 ?
O2 Cu1 Cu1 180.0 . 9_766 ?
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 -0.018 -0.006 -0.006 4486 1905 ' '
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat regions of diffuse
solvent which could not be sensibly modelled in terms of atomic
sites. Their contribution to the diffraction pattern was removed
and modified F(obs)**2 written to a new HKL file. 
Total electron count is 1905 electrons in a total void volume of 4486 Å³.
The number of electrons thus located are included in the
formula, formula weight, calculated density, mu and F(000).
This residual electron density was assigned to 7 molecules of DMF per Cu(II)
cation
[1905/4 = 291.25 e per asymmetric unit; DMF = 56 e]
;
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.082

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL shelxt_a.res in P4(2)/mmc
CELL  1.54184  14.6861  14.6861  26.1026   90.000   90.000   90.000
ZERR     8.00   0.0053   0.0053   0.0090    0.000    0.000    0.000
LATT   1
SYMM  - X, - Y,   Z
SYMM  - Y,   X, 1/2 + Z
SYMM    Y, - X, 1/2 + Z
SYMM  - X,   Y, - Z
SYMM    X, - Y, - Z
SYMM    Y,   X, 1/2 - Z
SYMM  - Y, - X, 1/2 - Z
SFAC  C    H    O    CU
UNIT  76 56 20 4
MERG   2
OMIT    -2 136
OMIT     0   4   1
OMIT     0   3   2
OMIT     1   3   2
OMIT     0   1   4
OMIT     0   2   5
OMIT     1   3   3
OMIT     0   4   5
OMIT     0   4   0
OMIT     1   3   6
OMIT     2   4   0
OMIT     1   4   0
OMIT     1   3   4
OMIT     1   2   6
OMIT     1   2   5
OMIT     1   4   2
DFIX 1.35 0.02 C1 C2
FMAP   2
PLAN   20
BOND   $H
BOND
ACTA
LIST   6
L.S.  10
WGHT    0.150000
FVAR      27.39723
C1    1    0.885352    0.500000    0.436474    10.50000    0.09391
C2    1    0.812087    0.500000    0.396680    10.50000    0.18292
C3    1    0.785865    0.425324    0.374075    11.00000    0.23361
AFIX  43
H3    2    0.819623    0.372714    0.379773    11.00000   -1.20000
AFIX   0
C4    1    0.699345    0.418594    0.337199    11.00000    0.21397
AFIX  43
H4    2    0.671909    0.363544    0.328726    11.00000   -1.20000
AFIX   0
C5    1    0.669184    0.500000    0.319245    10.50000    0.15199
C6    1    0.586073    0.500000    0.282124    10.50000    0.09055
C7    1    0.582763    0.417237    0.250000    10.50000    0.10396
AFIX  23
H7A   2    0.584415    0.363917    0.271911    10.50000   -1.20000
H7B   2    0.636085    0.415582    0.228090    10.50000   -1.20000
AFIX   0
C8    1    0.500000    0.500000    0.314833    10.25000    0.10588
AFIX  23
H8A   2    0.500001    0.446594    0.336698    10.25000   -1.20000
H8B   2    0.500001    0.553406    0.336698    10.25000   -1.20000
AFIX   0
O1    3    0.904026    0.579439    0.447776    11.00000    0.13458
O2    3    1.000000    0.736699    0.500000    10.25000    0.20914
CU1   4    1.000000    0.587784    0.500000    10.25000    0.13988    0.24636 =
         0.07383    0.00000    0.00000    0.00000
HKLF    4

REM  shelxt_a.res in P4(2)/mmc
REM R1 =  0.1642 for     625 Fo > 4sig(Fo)  and  0.3011 for all    2826 data
REM     35 parameters refined using      1 restraints

END

WGHT      0.1727      0.0000

REM Highest difference peak  0.589,  deepest hole -0.877,  1-sigma level  0.082
Q1    1   1.0000  0.5413  0.5000  10.25000  0.05    0.59
Q2    1   1.0535  0.5854  0.5000  10.50000  0.05    0.54
Q3    1   1.0000  0.6300  0.5000  10.25000  0.05    0.46
Q4    1   0.7211  0.5000  0.3139  10.50000  0.05    0.46
Q5    1   0.7534  0.5000  0.3940  10.50000  0.05    0.45
Q6    1   0.9159  0.5000  0.4412  10.50000  0.05    0.37
Q7    1   0.5879  0.3640  0.2557  11.00000  0.05    0.36
Q8    1   0.8217  0.4136  0.3529  11.00000  0.05    0.31
Q9    1   1.0000  0.7493  0.4637  10.50000  0.05    0.27
Q10   1   0.6439  0.4131  0.3572  11.00000  0.05    0.26
Q11   1   0.9039  0.6533  0.4438  11.00000  0.05    0.24
Q12   1   1.0644  0.7494  0.5000  10.50000  0.05    0.23
Q13   1   0.7242  0.3433  0.3138  11.00000  0.05    0.18
Q14   1   0.5765  0.5000  0.5000  10.25000  0.05    0.16
Q15   1   0.7800  0.3422  0.3855  11.00000  0.05    0.15
Q16   1   0.6532  0.5000  0.2112  10.50000  0.05    0.11
Q17   1   0.5000  0.1482  0.4090  10.50000  0.05    0.10
Q18   1   1.0000  0.9208  0.4129  10.50000  0.05    0.10
Q19   1   0.5000  0.0000  0.5000  10.12500  0.05    0.09
Q20   1   1.0000  0.9333  0.3567  10.50000  0.05    0.09
;
_shelx_res_checksum              90319
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_UOF-1D
_audit_block_doi                 10.5517/ccdc.csd.cc1p9mp9
_database_code_depnum_ccdc_archive 'CCDC 1558391'
_audit_update_record             
;
2017-06-26 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_UOF-1D              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The squeezed solvent molecules were included in the formula. See platon_squeeze_details
;
_vrf_THETM01_UOF-1D              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: No meaningful data could be collected beyond the resolution of 1.41 Angstrom. Therefore, only a 1 Angstrom resolution data set was targeted.
;
# Added during the CSD deposition process: Monday 26 June 2017 05:17 AM
# end Validation Reply Form

# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The squeezed solvent molecules were included in the 
formula. See platon_squeeze_details
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: No meaningful data could be collected beyond the resolution 
of 1.41 Angstrom. Therefore, only a 1 Angstrom resolution
data set was targeted.   .
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      51.81 Degree
RESPONSE: No meaningful data could be collected beyond the resolution 
of 1.41 Angstrom. Therefore, only a 1 Angstrom resolution
data set was targeted. 
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H15 Cu O5 (C5 H11 N O)4'
_chemical_formula_sum            'C39 H59 Cu O9'
_chemical_formula_weight         735.42

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_H-M_alt        'P 42/m m c'
_space_group_name_Hall           '-P 4c 2'

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

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

_cell_length_a                   14.3700(13)
_cell_length_b                   14.3700(13)
_cell_length_c                   26.464(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5464.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3162
_cell_measurement_theta_min      4.5200
_cell_measurement_theta_max      50.2690

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    0.894
_exptl_crystal_F_000             788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.161
_exptl_absorpt_coefficient_mu    0.860
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N2
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.1725
_diffrn_reflns_number            10870
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.500
_diffrn_reflns_theta_max         51.813
_diffrn_reflns_theta_full        51.813
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             1696
_reflns_number_gt                700
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXL-T (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 > 2σ(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.
The reported structural solution is best of the five data sets on this MOF.
The DMF molecules in as synthesized MOF were replaced by acetone. This crystals
were then soaked in DEF.
No meaningful data could be collected beyond the resolution 
of 1.41 Angstrom. This was best resolution that could be obtained out of five data sets.
As-synthesised crystals did not diffract beyond the resolution of 1.75 Angstrom while acetone
exchanged crystals diffracted up to the resolution of 1.19 Angstrom. Unfortunately,most of
this data was noise.
Therefore, only a 1 Angstrom resolution
data set was targeted.
The structure was severely disordered.
The solvent molecules could not be adequately located and were SQUEEZEd
from the structure. The SQUEEZEd electron density can be attributed to 4
DEF molecules per Cu(II) cation.
H-atoms were not affixed to the axial H2O molecule., 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)+(0.1600P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1696
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0967
_refine_ls_wR_factor_ref         0.3027
_refine_ls_wR_factor_gt          0.2737
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
C1 C 0.5000 -0.1221(8) 0.4327(4) 0.199(5) Uani 1 2 d S T P . .
C2 C 0.5000 -0.1866(9) 0.3948(4) 0.200(3) Uani 1 2 d S T P . .
C3 C 0.4265(7) -0.2194(8) 0.3741(4) 0.313(5) Uani 1 1 d . . . . .
H3 H 0.3701 -0.1944 0.3847 0.376 Uiso 1 1 calc R U . . .
C4 C 0.4223(6) -0.2884(8) 0.3376(4) 0.298(5) Uani 1 1 d . . . . .
H4 H 0.3649 -0.3100 0.3263 0.357 Uiso 1 1 calc R U . . .
C5 C 0.5000 -0.3235(8) 0.3187(3) 0.200(3) Uani 1 2 d S T P . .
C6 C 0.5000 -0.4100(7) 0.2819(4) 0.199(3) Uani 1 2 d S T P . .
C7 C 0.4124(4) -0.4124(4) 0.2500 0.194(3) Uani 1 2 d S T P . .
H7A H 0.4106 -0.3582 0.2282 0.232 Uiso 0.5 1 calc R U P . .
H7B H 0.3582 -0.4106 0.2718 0.232 Uiso 0.5 1 calc R U P . .
C8 C 0.5000 -0.5000 0.3143(5) 0.203(4) Uani 1 4 d S T P . .
H8A H 0.5545 -0.5000 0.3359 0.243 Uiso 0.5 2 calc R U P . .
H8B H 0.4455 -0.5000 0.3359 0.243 Uiso 0.5 2 calc R U P . .
O1 O 0.5762(4) -0.0926(4) 0.4491(2) 0.225(2) Uani 1 1 d . . . . .
O2 O 0.7485(6) 0.0000 0.5000 0.246(3) Uani 1 4 d S T P . .
Cu1 Cu 0.59214(12) 0.0000 0.5000 0.1932(14) Uani 1 4 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
C1 0.279(19) 0.196(9) 0.123(7) -0.050(7) 0.000 0.000
C2 0.231(12) 0.234(11) 0.134(7) -0.035(8) 0.000 0.000
C3 0.296(11) 0.370(12) 0.272(10) -0.186(10) -0.002(8) 0.000(8)
C4 0.219(9) 0.397(12) 0.277(9) -0.130(9) -0.003(6) 0.018(7)
C5 0.227(12) 0.244(10) 0.131(6) -0.037(7) 0.000 0.000
C6 0.213(10) 0.218(9) 0.165(8) 0.025(8) 0.000 0.000
C7 0.223(6) 0.223(6) 0.134(6) -0.011(4) -0.011(4) 0.003(6)
C8 0.167(10) 0.262(14) 0.179(10) 0.000 0.000 0.000
O1 0.256(7) 0.229(5) 0.190(4) -0.039(4) -0.002(3) -0.023(4)
O2 0.259(9) 0.265(9) 0.215(7) 0.000 0.000 0.000
Cu1 0.232(2) 0.2096(19) 0.1378(15) 0.000 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
C1 O1 1.252(5) . ?
C1 O1 1.252(5) 14_655 ?
C1 C2 1.364(15) . ?
C2 C3 1.280(8) 14_655 ?
C2 C3 1.280(8) . ?
C3 C4 1.387(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.324(8) . ?
C4 H4 0.9300 . ?
C5 C4 1.324(8) 14_655 ?
C5 C6 1.578(12) . ?
C6 C7 1.516(6) . ?
C6 C7 1.516(6) 11_656 ?
C6 C8 1.552(9) . ?
C7 C6 1.516(6) 12_546 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C6 1.552(9) 2_645 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O1 Cu1 1.908(6) . ?
O2 Cu1 2.247(9) . ?
Cu1 O1 1.908(6) 6_556 ?
Cu1 O1 1.908(6) 13 ?
Cu1 O1 1.908(6) 10_556 ?
Cu1 Cu1 2.648(4) 9_656 ?

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 C1 O1 122.0(11) . 14_655 ?
O1 C1 C2 119.0(6) . . ?
O1 C1 C2 119.0(6) 14_655 . ?
C3 C2 C3 111.2(13) 14_655 . ?
C3 C2 C1 124.4(6) 14_655 . ?
C3 C2 C1 124.4(6) . . ?
C2 C3 C4 126.8(11) . . ?
C2 C3 H3 116.6 . . ?
C4 C3 H3 116.6 . . ?
C5 C4 C3 119.9(9) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C4 115.1(11) . 14_655 ?
C4 C5 C6 122.2(6) . . ?
C4 C5 C6 122.2(6) 14_655 . ?
C7 C6 C7 112.2(7) . 11_656 ?
C7 C6 C8 106.7(6) . . ?
C7 C6 C8 106.7(6) 11_656 . ?
C7 C6 C5 111.2(5) . . ?
C7 C6 C5 111.2(5) 11_656 . ?
C8 C6 C5 108.4(7) . . ?
C6 C7 C6 110.4(10) . 12_546 ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 12_546 . ?
C6 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 12_546 . ?
H7A C7 H7B 108.1 . . ?
C6 C8 C6 113.0(12) 2_645 . ?
C6 C8 H8A 109.0 2_645 . ?
C6 C8 H8A 109.0 . . ?
C6 C8 H8B 109.0 2_645 . ?
C6 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C1 O1 Cu1 125.9(7) . . ?
O1 Cu1 O1 166.2(3) . 6_556 ?
O1 Cu1 O1 88.5(3) . 13 ?
O1 Cu1 O1 89.9(3) 6_556 13 ?
O1 Cu1 O1 89.9(3) . 10_556 ?
O1 Cu1 O1 88.5(3) 6_556 10_556 ?
O1 Cu1 O1 166.2(3) 13 10_556 ?
O1 Cu1 O2 96.89(17) . . ?
O1 Cu1 O2 96.89(17) 6_556 . ?
O1 Cu1 O2 96.89(17) 13 . ?
O1 Cu1 O2 96.89(17) 10_556 . ?
O1 Cu1 Cu1 83.11(17) . 9_656 ?
O1 Cu1 Cu1 83.11(17) 6_556 9_656 ?
O1 Cu1 Cu1 83.11(17) 13 9_656 ?
O1 Cu1 Cu1 83.11(17) 10_556 9_656 ?
O2 Cu1 Cu1 180.0 . 9_656 ?
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 -0.008 -0.005 4349 835 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat regions of diffuse
solvent which could not be sensibly modelled in terms of atomic
sites. Their contribution to the diffraction pattern was removed
and modified F(obs)**2 written to a new HKL file. 
Total electron count is 835 electrons in a total void volume of 4349 Å³.
The number of electrons thus located are included in the
formula, formula weight, calculated density, mu and F(000).
This residual electron density was assigned to 4 molecules of DEF per Cu(II)
cation
[835/4 = 208.75 e per asymmetric unit; DMF = 56 e]
;
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.044

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL shelxt_a.res in P4(2)/mmc
CELL  1.54184  14.3700  14.3700  26.4644   90.000   90.000   90.000
ZERR     4.00   0.0013   0.0013   0.0029    0.000    0.000    0.000
LATT   1
SYMM  - X, - Y,   Z
SYMM  - Y,   X, 1/2 + Z
SYMM    Y, - X, 1/2 + Z
SYMM  - X,   Y, - Z
SYMM    X, - Y, - Z
SYMM    Y,   X, 1/2 - Z
SYMM  - Y, - X, 1/2 - Z
SFAC  C    H    O    CU
UNIT  76 56 20 4
OMIT    -2 136
OMIT     0   2   6
OMIT     0   0   2
OMIT     0   1   5
OMIT     2   3   4
OMIT     1   3   2
OMIT     1   3   0
OMIT     0   0   4
OMIT     1   4   1
OMIT     1   4   2
OMIT     0   2   8
OMIT     3   3   4
OMIT     0   1   0
OMIT     1   2   6
OMIT     1   4   4
OMIT     1   2   0
OMIT     1   1   0
OMIT     1   1   6
MERG   2
FMAP   2
PLAN   20
BOND   $H
L.S. 10
ACTA
WGHT    0.160000
FVAR       4.62593
C1    1    0.500000   -0.122142    0.432696    10.50000    0.27874    0.19571 =
         0.12315   -0.04958    0.00000    0.00000
C2    1    0.500000   -0.186579    0.394841    10.50000    0.23104    0.23358 =
         0.13388   -0.03513    0.00000    0.00000
C3    1    0.426501   -0.219417    0.374142    11.00000    0.29646    0.37049 =
         0.27236   -0.18634   -0.00191   -0.00029
AFIX  43
H3    2    0.370079   -0.194415    0.384725    11.00000   -1.20000
AFIX   0
C4    1    0.422267   -0.288393    0.337580    11.00000    0.21941    0.39703 =
         0.27669   -0.12985   -0.00299    0.01810
AFIX  43
H4    2    0.364869   -0.309961    0.326337    11.00000   -1.20000
AFIX   0
C5    1    0.500000   -0.323524    0.318689    10.50000    0.22666    0.24367 =
         0.13072   -0.03733    0.00000    0.00000
C6    1    0.500000   -0.409959    0.281896    10.50000    0.21314    0.21794 =
         0.16468    0.02480    0.00000    0.00000
C7    1    0.412431   -0.412431    0.250000    10.50000    0.22333    0.22333 =
         0.13407   -0.01084   -0.01084    0.00287
AFIX  23
H7A   2    0.410614   -0.358208    0.228192    10.50000   -1.20000
H7B   2    0.358210   -0.410616    0.271810    10.50000   -1.20000
AFIX   0
C8    1    0.500000   -0.500000    0.314274    10.25000    0.16683    0.26187 =
         0.17902    0.00000    0.00000    0.00000
AFIX  23
H8A   2    0.554534   -0.499999    0.335875    10.25000   -1.20000
H8B   2    0.445466   -0.499999    0.335875    10.25000   -1.20000
AFIX   0
O1    3    0.576214   -0.092615    0.449085    11.00000    0.25637    0.22859 =
         0.19033   -0.03854   -0.00217   -0.02283
O2    3    0.748505    0.000000    0.500000    10.25000    0.25914    0.26488 =
         0.21503    0.00000    0.00000    0.00000
CU1   4    0.592142    0.000000    0.500000    10.25000    0.23236    0.20958 =
         0.13780    0.00000    0.00000    0.00000
HKLF    4

REM  shelxt_a.res in P4(2)/mmc
REM R1 =  0.0967 for     700 Fo > 4sig(Fo)  and  0.1417 for all    1696 data
REM     69 parameters refined using      0 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.360,  deepest hole -0.257,  1-sigma level  0.044
Q1    1   0.5000  0.0000  0.5360  10.25000  0.05    0.36
Q2    1   0.5000 -0.0954  0.5000  10.25000  0.05    0.19
Q3    1   0.5000 -0.4076  0.2239  10.50000  0.05    0.14
Q4    1   0.5935 -0.1023  0.4650  11.00000  0.05    0.13
Q5    1   0.6995  0.0000  0.5259  10.50000  0.05    0.12
Q6    1   0.5000 -0.3999  0.5000  10.25000  0.05    0.10
Q7    1   0.5000 -0.2460  0.1577  10.50000  0.05    0.10
Q8    1   0.5000 -0.3042  0.3862  10.50000  0.05    0.09
Q9    1   0.4161 -0.3544  0.3548  11.00000  0.05    0.09
Q10   1   0.5000 -0.2304  0.3279  10.50000  0.05    0.09
Q11   1   0.5000  0.0000  0.2178  10.25000  0.05    0.09
Q12   1   0.1987 -0.4223  0.5000  10.50000  0.05    0.08
Q13   1   0.4399 -0.3010  0.3766  11.00000  0.05    0.08
Q14   1   0.2394 -0.3294  0.3650  11.00000  0.05    0.08
Q15   1   0.5000 -0.2027  0.4391  10.50000  0.05    0.08
Q16   1   0.4410 -0.2113  0.4314  11.00000  0.05    0.07
Q17   1   0.2140  0.0000  0.3509  10.50000  0.05    0.07
Q18   1   0.3966 -0.2125  0.3605  11.00000  0.05    0.07
Q19   1   0.0222 -0.4231  0.2994  11.00000  0.05    0.07
Q20   1   0.4499 -0.2235  0.4000  11.00000  0.05    0.06
;
_shelx_res_checksum              36357
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_UOF-1E
_audit_block_doi                 10.5517/ccdc.csd.cc1pkgnc
_database_code_depnum_ccdc_archive 'CCDC 1565923'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_UOF-1E              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The squeezed solvent molecules were included in the 
formula. See platon_squeeze_details
;
_vrf_THETM01_UOF-1E              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: No meaningful data could be collected beyond the resolution 
of 1.41 Angstrom. Therefore, only a 1 Angstrom resolution
data set was targeted. 
;
_vrf_PLAT026_UOF-1E              
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         26 %     
RESPONSE: The data is of poor quality. 
;
_vrf_PLAT029_UOF-1E              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.811 Note  
RESPONSE: Owing to the disordered solvent and high ADPs, the data is of poor quality. 
;
_vrf_PLAT234_UOF-1E              
;
PROBLEM: Large Hirshfeld Difference C3     --  C4      ..       0.36 Ang.  
RESPONSE: The data is of poor quality due to high ADPs
;
_vrf_PLAT241_UOF-1E              
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         C4 Check 
RESPONSE: The data is of poor quality due to high ADPs 
;
_vrf_PLAT369_UOF-1E              
;
PROBLEM: Long    C(sp2)-C(sp2) Bond  C1     -   C2     ..       1.67 Ang.  
RESPONSE: The data is of poor quality due to high ADPs
;
_vrf_PLAT410_UOF-1E              
;
PROBLEM: Short Intra H...H Contact   H4     ..  H9B     .       1.67 Ang.  
RESPONSE: The data is of poor quality due to high ADPs
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C19H15CuO5(CH2Cl2)7
_chemical_formula_sum            'C26 H29 Cl14 Cu O5'
_chemical_formula_weight         981.40

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_H-M_alt        'C c c m'
_space_group_name_Hall           '-C 2 2c'

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

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

_cell_length_a                   19.302(5)
_cell_length_b                   21.805(4)
_cell_length_c                   26.364(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11096(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2219
_cell_measurement_theta_min      3.4730
_cell_measurement_theta_max      38.4130

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_F_000             1576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.171
_exptl_absorpt_coefficient_mu    6.972
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N2
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.1725
_diffrn_reflns_number            9509
_diffrn_reflns_av_unetI/netI     0.1270
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.487
_diffrn_reflns_theta_max         52.644
_diffrn_reflns_theta_full        52.644
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measured_fraction_theta_full 0.811
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_Laue_measured_fraction_full 0.811
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_point_group_measured_fraction_full 0.811
_reflns_number_total             2655
_reflns_number_gt                701
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .


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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXL-T (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 > 2σ(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     
'w=1/[σ²(Fo²)+(0.1919P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2655
_refine_ls_number_parameters     106
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2219
_refine_ls_R_factor_gt           0.1329
_refine_ls_wR_factor_ref         0.3615
_refine_ls_wR_factor_gt          0.3213
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_restrained_S_all      0.867
_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
C1 C 0.1995(7) 0.3099(6) -0.0660(5) 0.172(5) Uani 1 1 d . . . . .
C2 C 0.1516(7) 0.3481(6) -0.1083(3) 0.216(6) Uani 1 1 d G . . . .
C3 C 0.0877(7) 0.3334(4) -0.1294(5) 0.333(9) Uani 1 1 d G . . . .
H3 H 0.0636 0.2991 -0.1181 0.400 Uiso 1 1 calc R U . . .
C4 C 0.0599(4) 0.3700(6) -0.1675(5) 0.424(12) Uani 1 1 d G . . . .
H4 H 0.0171 0.3602 -0.1816 0.509 Uiso 1 1 calc R U . . .
C5 C 0.0959(7) 0.4213(5) -0.1844(3) 0.200(5) Uani 1 1 d DG . . . .
C6 C 0.1598(7) 0.4359(4) -0.1633(5) 0.387(11) Uani 1 1 d G . . . .
H6 H 0.1839 0.4702 -0.1746 0.465 Uiso 1 1 calc R U . . .
C7 C 0.1876(4) 0.3994(7) -0.1253(5) 0.308(7) Uani 1 1 d G . . . .
H7 H 0.2304 0.4092 -0.1111 0.369 Uiso 1 1 calc R U . . .
C8 C 0.0466(5) 0.4586(4) -0.2161(5) 0.154(4) Uani 1 1 d D . . . .
C9 C 0.0000 0.4176(6) -0.2500 0.173(5) Uani 1 2 d S T P . .
H9A H 0.0287 0.3915 -0.2711 0.207 Uiso 0.5 1 calc R U P . .
H9B H -0.0287 0.3915 -0.2289 0.207 Uiso 0.5 1 calc R U P . .
C10 C 0.0000 0.5000 -0.1877(5) 0.172(5) Uani 1 2 d S T P . .
H10A H 0.0286 0.5253 -0.1658 0.206 Uiso 0.5 1 calc R U P . .
H10B H -0.0286 0.4747 -0.1658 0.206 Uiso 0.5 1 calc R U P . .
C11 C 0.0915(6) 0.5000 -0.2500 0.160(5) Uani 1 2 d S T P . .
H11A H 0.1211 0.4747 -0.2711 0.192 Uiso 0.5 1 calc R U P . .
H11B H 0.1211 0.5253 -0.2289 0.192 Uiso 0.5 1 calc R U P . .
O1 O 0.1577(4) 0.2618(3) -0.0486(3) 0.198(3) Uani 1 1 d . . . . .
O2 O 0.2498(4) 0.1672(3) 0.0476(3) 0.192(3) Uani 1 1 d . . . . .
O3 O 0.1020(5) 0.1499(5) 0.0000 0.311(5) Uani 1 2 d S T P . .
Cu1 Cu 0.19860(13) 0.21310(9) 0.0000 0.2012(18) Uani 1 2 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
C1 0.177(13) 0.208(11) 0.130(13) -0.051(10) -0.028(10) -0.011(10)
C2 0.276(17) 0.214(11) 0.159(12) 0.091(9) -0.025(12) 0.059(10)
C3 0.320(17) 0.371(18) 0.31(2) 0.112(15) -0.153(14) -0.094(16)
C4 0.52(2) 0.47(3) 0.28(2) 0.196(18) -0.177(17) 0.10(2)
C5 0.234(14) 0.177(8) 0.189(13) 0.042(8) -0.018(12) 0.047(9)
C6 0.31(2) 0.53(3) 0.32(2) 0.243(19) -0.060(15) -0.014(18)
C7 0.393(17) 0.268(13) 0.262(19) 0.115(11) -0.079(14) 0.038(15)
C8 0.152(9) 0.145(8) 0.164(13) -0.004(7) 0.010(9) 0.035(7)
C9 0.252(16) 0.206(12) 0.060(11) 0.000 -0.021(10) 0.000
C10 0.142(12) 0.155(10) 0.219(17) 0.000 0.000 -0.029(10)
C11 0.205(14) 0.228(12) 0.047(11) 0.010(9) 0.000 0.000
O1 0.221(8) 0.211(5) 0.162(6) 0.018(5) -0.042(5) 0.010(6)
O2 0.204(7) 0.202(5) 0.171(6) -0.006(5) -0.058(5) -0.049(6)
O3 0.304(10) 0.372(11) 0.258(12) 0.000 0.000 -0.211(10)
Cu1 0.320(4) 0.205(2) 0.079(3) 0.000 0.000 0.0344(19)

_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
C1 O2 1.201(9) 13 ?
C1 O1 1.401(12) . ?
C1 C2 1.671(14) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 C8 1.505(10) . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C10 1.478(11) . ?
C8 C11 1.538(10) . ?
C8 C9 1.553(10) . ?
C9 C8 1.552(10) 3_554 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C8 1.478(11) 2_565 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C8 1.538(10) 4_564 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O1 Cu1 1.842(7) . ?
O2 C1 1.201(9) 13 ?
O2 Cu1 1.884(7) . ?
O3 Cu1 2.318(7) . ?
Cu1 O1 1.842(7) 10 ?
Cu1 O2 1.884(7) 10 ?
Cu1 Cu1 2.555(4) 13 ?

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
O2 C1 O1 130.4(15) 13 . ?
O2 C1 C2 121.0(13) 13 . ?
O1 C1 C2 105.8(10) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 130.1(12) . . ?
C7 C2 C1 109.8(12) . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C8 107.3(11) . . ?
C6 C5 C8 131.2(11) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C10 C8 C5 115.8(10) . . ?
C10 C8 C11 106.2(7) . . ?
C5 C8 C11 106.5(8) . . ?
C10 C8 C9 106.9(8) . . ?
C5 C8 C9 112.0(8) . . ?
C11 C8 C9 109.2(9) . . ?
C8 C9 C8 109.6(12) 3_554 . ?
C8 C9 H9A 109.7 3_554 . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 3_554 . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C8 C10 C8 119.1(14) . 2_565 ?
C8 C10 H10A 107.5 . . ?
C8 C10 H10A 107.5 2_565 . ?
C8 C10 H10B 107.5 . . ?
C8 C10 H10B 107.5 2_565 . ?
H10A C10 H10B 107.0 . . ?
C8 C11 C8 111.4(12) . 4_564 ?
C8 C11 H11A 109.4 . . ?
C8 C11 H11A 109.4 4_564 . ?
C8 C11 H11B 109.4 . . ?
C8 C11 H11B 109.4 4_564 . ?
H11A C11 H11B 108.0 . . ?
C1 O1 Cu1 114.4(8) . . ?
C1 O2 Cu1 118.4(10) 13 . ?
O1 Cu1 O1 88.2(4) . 10 ?
O1 Cu1 O2 173.7(3) . . ?
O1 Cu1 O2 93.8(3) 10 . ?
O1 Cu1 O2 93.8(3) . 10 ?
O1 Cu1 O2 173.7(3) 10 10 ?
O2 Cu1 O2 83.5(4) . 10 ?
O1 Cu1 O3 89.9(4) . . ?
O1 Cu1 O3 89.9(4) 10 . ?
O2 Cu1 O3 96.1(3) . . ?
O2 Cu1 O3 96.1(3) 10 . ?
O1 Cu1 Cu1 88.3(3) . 13 ?
O1 Cu1 Cu1 88.3(3) 10 13 ?
O2 Cu1 Cu1 85.8(2) . 13 ?
O2 Cu1 Cu1 85.8(2) 10 13 ?
O3 Cu1 Cu1 177.4(3) . 13 ?
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 -0.011 0.002 -0.006 8791 2468 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat regions of diffuse
solvent which could not be sensibly modelled in terms of atomic
sites. Their contribution to the diffraction pattern was removed
and modified F(obs)**2 written to a new HKL file. 
Total electron count is 2468 electrons in a total void volume of 8791 Å³.
The number of electrons thus located are included in the
formula, formula weight, calculated density, mu and F(000).
This residual electron density was assigned to 7 molecules of CH2Cl2 per Cu(II)
cation
[2468/8 = 308.5 e per asymmetric unit; CH2Cl2 = 42 e]
;
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.065

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL KP05_CuMOF_DCMC in Cccm
CELL  1.54184  19.3021  21.8048  26.3638   90.000   90.000   90.000
ZERR     8.00   0.0049   0.0039   0.0044    0.000    0.000    0.000
LATT   7
SYMM  - X, - Y,   Z
SYMM  - X,   Y, 1/2 - Z
SYMM    X, - Y, 1/2 - Z
SFAC  C    H    O   CU
UNIT  152 112 40 8
MERG   2
OMIT    -2.00 136.00
OMIT     1   1   6
OMIT     1   3   0
OMIT     2   6   0
OMIT     2   4   3
OMIT     0   4   0
OMIT     1   5   2
OMIT     3   1   1
OMIT     4   2   0
OMIT     3   5   1
OMIT     4   4   0
OMIT     6   2   0
OMIT     4   0   0
OMIT     2   0   4
OMIT     5   1   0
OMIT     3   1   7
OMIT     0   4   2
OMIT     1   5   1
OMIT     6   0   2
OMIT     4   2   1
OMIT     2   2   2
OMIT     1   7   0
DFIX 1.35 0.02 C5 C8
FMAP   2
PLAN   20
BOND
BOND   $H
ACTA
L.S.  10
WGHT    0.191900
FVAR      17.40854
C1    1    0.199526    0.309927   -0.066042    11.00000    0.17744    0.20796 =
         0.12977   -0.05119   -0.02772   -0.01082
AFIX  66
C2    1    0.151596    0.348096   -0.108319    11.00000    0.27640    0.21380 =
         0.15924    0.09071   -0.02466    0.05944
C3    1    0.087721    0.333430   -0.129429    11.00000    0.31953    0.37130 =
         0.30862    0.11240   -0.15315   -0.09415
AFIX  43
H3    2    0.063622    0.299134   -0.118094    11.00000   -1.20000
AFIX  65
C4    1    0.059864    0.370024   -0.167479    11.00000    0.52470    0.46861 =
         0.27858    0.19603   -0.17668    0.10257
AFIX  43
H4    2    0.017128    0.360211   -0.181603    11.00000   -1.20000
AFIX  65
C5    1    0.095883    0.421283   -0.184420    11.00000    0.23377    0.17704 =
         0.18852    0.04188   -0.01755    0.04706
C6    1    0.159758    0.435950   -0.163311    11.00000    0.30526    0.53430 =
         0.32173    0.24291   -0.06001   -0.01434
AFIX  43
H6    2    0.183856    0.470246   -0.174646    11.00000   -1.20000
AFIX  65
C7    1    0.187615    0.399357   -0.125260    11.00000    0.39309    0.26758 =
         0.26186    0.11511   -0.07927    0.03793
AFIX  43
H7    2    0.230352    0.409170   -0.111137    11.00000   -1.20000
AFIX   0
C8    1    0.046608    0.458632   -0.216062    11.00000    0.15175    0.14456 =
         0.16427   -0.00397    0.01009    0.03482
C9    1    0.000000    0.417598   -0.250000    10.50000    0.25189    0.20603 =
         0.05961    0.00000   -0.02089    0.00000
AFIX  23
H9A   2    0.028709    0.391519   -0.271134    10.50000   -1.20000
H9B   2   -0.028708    0.391518   -0.228866    10.50000   -1.20000
AFIX   0
C10   1    0.000000    0.500000   -0.187674    10.50000    0.14171    0.15536 =
         0.21889    0.00000    0.00000   -0.02918
AFIX  23
H10A  2    0.028604    0.525253   -0.165789    10.50000   -1.20000
H10B  2   -0.028606    0.474746   -0.165792    10.50000   -1.20000
AFIX   0
C11   1    0.091519    0.500000   -0.250000    10.50000    0.20477    0.22778 =
         0.04740    0.01044    0.00000    0.00000
AFIX  23
H11A  2    0.121061    0.474658   -0.271132    10.50000   -1.20000
H11B  2    0.121065    0.525341   -0.228869    10.50000   -1.20000
AFIX   0
O1    3    0.157720    0.261798   -0.048630    11.00000    0.22124    0.21055 =
         0.16208    0.01819   -0.04229    0.00956
O2    3    0.249754    0.167226    0.047612    11.00000    0.20383    0.20216 =
         0.17116   -0.00562   -0.05783   -0.04948
O3    3    0.102048    0.149917    0.000000    10.50000    0.30401    0.37225 =
         0.25822    0.00000    0.00000   -0.21144
CU1   4    0.198598    0.213101    0.000000    10.50000    0.31985    0.20505 =
         0.07882    0.00000    0.00000    0.03437
HKLF    4

REM  KP05_CuMOF_DCMC in Cccm
REM R1 =  0.1329 for     701 Fo > 4sig(Fo)  and  0.2219 for all    2655 data
REM    106 parameters refined using      1 restraints

END

WGHT      0.1916      0.0000

REM Highest difference peak  0.385,  deepest hole -0.795,  1-sigma level  0.065
Q1    1   0.1308  0.1499  0.0000  10.50000  0.05    0.39
Q2    1   0.0591  0.1908  0.0400  11.00000  0.05    0.29
Q3    1   0.0397  0.4673  0.0000  10.50000  0.05    0.15
Q4    1   0.2017  0.3821 -0.1292  11.00000  0.05    0.15
Q5    1  -0.0274  0.4057  0.0000  10.50000  0.05    0.12
Q6    1  -0.0618  0.3142 -0.1181  11.00000  0.05    0.12
Q7    1   0.0834  0.4399 -0.3046  11.00000  0.05    0.11
Q8    1   0.0420  0.3809 -0.1469  11.00000  0.05    0.11
Q9    1   0.0599  0.3699 -0.2673  11.00000  0.05    0.11
Q10   1   0.0898  0.3847 -0.0903  11.00000  0.05    0.11
Q11   1   0.1918  0.1101  0.0660  11.00000  0.05    0.11
Q12   1   0.1198  0.3478 -0.1083  11.00000  0.05    0.10
Q13   1   0.0519  0.3167 -0.0910  11.00000  0.05    0.10
Q14   1   0.2500  0.2500 -0.1119  10.50000  0.05    0.10
Q15   1   0.1219  0.4272 -0.1718  11.00000  0.05    0.10
Q16   1  -0.0260  0.1891 -0.1107  11.00000  0.05    0.09
Q17   1  -0.0181  0.1794 -0.1182  11.00000  0.05    0.09
Q18   1   0.0557  0.5067 -0.0367  11.00000  0.05    0.09
Q19   1  -0.0329  0.3245  0.0000  10.50000  0.05    0.09
Q20   1  -0.0282  0.3897 -0.0570  11.00000  0.05    0.08
;
_shelx_res_checksum              45567
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_UOF_1C
_audit_block_doi                 10.5517/ccdc.csd.cc1pkgmb
_database_code_depnum_ccdc_archive 'CCDC 1565922'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_UOF_1C              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The squeezed solvent molecules were included in the 
formula. See platon_squeeze_details
;
_vrf_THETM01_UOF_1C              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: No meaningful data could be collected beyond the resolution 
of 1.41 Angstrom. Therefore, only a 1 Angstrom resolution
data set was targeted.  
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H69 Cu O14'
_chemical_formula_weight         909.58

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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_H-M_alt        'P 42/m m c'
_space_group_name_Hall           '-P 4c 2'

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

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

_cell_length_a                   14.7093(16)
_cell_length_b                   14.7093(16)
_cell_length_c                   26.053(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5636.9(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    2842
_cell_measurement_theta_min      4.5270
_cell_measurement_theta_max      51.0870

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_F_000             788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    0.987
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.48013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N2
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.1725
_diffrn_reflns_number            11025
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_av_R_equivalents  0.1590
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         51.921
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.622
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.622
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.622
_reflns_number_total             1764
_reflns_number_gt                964
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXL-T (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 > 2σ(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.
The DMF molecules in as synthesized MOF were replaced by acetone. 
The solvent molecules could not be adequately located and were SQUEEZEd
from the structure. The SQUEEZEd electron density can be attributed to 9
acetone molecules per Cu(II) cation.
H-atoms were not affixed to the axial H2O molecule.
;
_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     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1764
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.1241
_refine_ls_wR_factor_ref         0.3808
_refine_ls_wR_factor_gt          0.3508
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_restrained_S_all      1.244
_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
C1 C 0.1182(7) 0.5000 0.5658(4) 0.128(3) Uani 1 2 d S T P . .
C2 C 0.1897(7) 0.5000 0.6051(4) 0.128(3) Uani 1 2 d S T P . .
C3 C 0.2246(8) 0.5752(6) 0.6264(5) 0.215(5) Uani 1 1 d . . . . .
H3 H 0.1989 0.6306 0.6171 0.258 Uiso 1 1 calc R U . . .
C4 C 0.2959(8) 0.5770(6) 0.6611(4) 0.211(4) Uani 1 1 d . . . . .
H4 H 0.3201 0.6325 0.6713 0.253 Uiso 1 1 calc R U . . .
C5 C 0.3301(7) 0.5000 0.6801(4) 0.133(3) Uani 1 2 d S T P . .
C6 C 0.4138(6) 0.5000 0.7175(4) 0.128(3) Uani 1 2 d S T P . .
C7 C 0.5000 0.5000 0.6821(5) 0.132(4) Uani 1 4 d S T P . .
H7A H 0.5000 0.5535 0.6603 0.159 Uiso 0.5 2 calc R U P . .
H7B H 0.5000 0.4465 0.6603 0.159 Uiso 0.5 2 calc R U P . .
C8 C 0.4152(5) 0.5848(5) 0.7500 0.133(3) Uani 1 2 d S T P . .
H8A H 0.4138 0.6381 0.7281 0.159 Uiso 0.5 1 calc R U P . .
H8B H 0.3620 0.5862 0.7719 0.159 Uiso 0.5 1 calc R U P . .
O1 O 0.0921(4) 0.4252(3) 0.5522(2) 0.149(2) Uani 1 1 d . . . . .
O2 O 0.0000 0.2598(7) 0.5000 0.180(4) Uani 1 4 d S T P . .
Cu1 Cu 0.0000 0.41140(11) 0.5000 0.1232(12) Uani 1 4 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
C1 0.111(7) 0.191(13) 0.083(6) 0.000 -0.011(6) 0.000
C2 0.142(8) 0.123(7) 0.119(7) 0.000 0.007(7) 0.000
C3 0.236(11) 0.178(9) 0.230(11) 0.016(8) -0.094(10) -0.003(7)
C4 0.248(12) 0.147(8) 0.238(11) 0.001(7) -0.087(10) -0.013(6)
C5 0.141(8) 0.134(8) 0.124(8) 0.000 -0.006(6) 0.000
C6 0.128(7) 0.136(8) 0.120(8) 0.000 -0.009(6) 0.000
C7 0.148(11) 0.135(10) 0.114(9) 0.000 0.000 0.000
C8 0.147(5) 0.147(5) 0.103(7) -0.001(4) -0.001(4) -0.007(5)
O1 0.165(5) 0.138(5) 0.144(4) -0.007(3) -0.036(3) -0.008(3)
O2 0.177(9) 0.183(9) 0.180(10) 0.000 0.000 0.000
Cu1 0.1349(18) 0.1339(18) 0.1007(17) 0.000 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
C1 O1 1.218(5) 13_565 ?
C1 O1 1.218(5) . ?
C1 C2 1.468(14) . ?
C2 C3 1.339(9) 13_565 ?
C2 C3 1.339(10) . ?
C3 C4 1.385(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.334(10) . ?
C4 H4 0.9300 . ?
C5 C4 1.334(10) 13_565 ?
C5 C6 1.571(12) . ?
C6 C8 1.507(7) . ?
C6 C8 1.507(7) 12_657 ?
C6 C7 1.569(10) . ?
C7 C6 1.569(10) 2_665 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C6 1.507(7) 11_567 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O1 Cu1 1.930(6) . ?
O2 Cu1 2.230(10) . ?
Cu1 O1 1.930(6) 5_556 ?
Cu1 O1 1.930(6) 14 ?
Cu1 O1 1.930(6) 10_556 ?
Cu1 Cu1 2.606(3) 9_566 ?

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 C1 O1 129.2(10) 13_565 . ?
O1 C1 C2 115.4(5) 13_565 . ?
O1 C1 C2 115.4(5) . . ?
C3 C2 C3 111.4(13) 13_565 . ?
C3 C2 C1 124.3(6) 13_565 . ?
C3 C2 C1 124.3(6) . . ?
C2 C3 C4 125.2(10) . . ?
C2 C3 H3 117.4 . . ?
C4 C3 H3 117.4 . . ?
C5 C4 C3 120.8(9) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C4 116.1(11) 13_565 . ?
C4 C5 C6 121.7(6) 13_565 . ?
C4 C5 C6 121.7(6) . . ?
C8 C6 C8 111.7(7) . 12_657 ?
C8 C6 C7 108.6(5) . . ?
C8 C6 C7 108.6(5) 12_657 . ?
C8 C6 C5 111.1(5) . . ?
C8 C6 C5 111.1(5) 12_657 . ?
C7 C6 C5 105.5(7) . . ?
C6 C7 C6 107.9(10) . 2_665 ?
C6 C7 H7A 110.1 . . ?
C6 C7 H7A 110.1 2_665 . ?
C6 C7 H7B 110.1 . . ?
C6 C7 H7B 110.1 2_665 . ?
H7A C7 H7B 108.4 . . ?
C6 C8 C6 109.7(9) 11_567 . ?
C6 C8 H8A 109.7 11_567 . ?
C6 C8 H8A 109.7 . . ?
C6 C8 H8B 109.7 11_567 . ?
C6 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C1 O1 Cu1 121.4(6) . . ?
O1 Cu1 O1 89.6(3) 5_556 14 ?
O1 Cu1 O1 89.2(3) 5_556 10_556 ?
O1 Cu1 O1 168.0(3) 14 10_556 ?
O1 Cu1 O1 168.0(3) 5_556 . ?
O1 Cu1 O1 89.2(3) 14 . ?
O1 Cu1 O1 89.6(3) 10_556 . ?
O1 Cu1 O2 96.02(16) 5_556 . ?
O1 Cu1 O2 96.02(16) 14 . ?
O1 Cu1 O2 96.02(16) 10_556 . ?
O1 Cu1 O2 96.02(16) . . ?
O1 Cu1 Cu1 83.98(16) 5_556 9_566 ?
O1 Cu1 Cu1 83.98(16) 14 9_566 ?
O1 Cu1 Cu1 83.98(16) 10_556 9_566 ?
O1 Cu1 Cu1 83.98(16) . 9_566 ?
O2 Cu1 Cu1 180.0 . 9_566 ?
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 -0.018 -0.007 -0.004 4447 1117 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat regions of diffuse
solvent which could not be sensibly modelled in terms of atomic
sites. Their contribution to the diffraction pattern was removed
and modified F(obs)**2 written to a new HKL file. 
Total electron count is 1117 electrons in a total void volume of 4447 Å³.
The number of electrons thus located are included in the
formula, formula weight, calculated density, mu and F(000).
This residual electron density was assigned to 9 molecules of acetone per Cu(II)
cation
[1117/4 = 279.25 e per asymmetric unit; acetone = 32 e]
;
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.071

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL shelxt_a.res in P4(2)/mmc
CELL  1.54184  14.7093  14.7093  26.0531   90.000   90.000   90.000
ZERR     8.00   0.0016   0.0016   0.0030    0.000    0.000    0.000
LATT   1
SYMM  - X, - Y,   Z
SYMM  - Y,   X, 1/2 + Z
SYMM    Y, - X, 1/2 + Z
SYMM  - X,   Y, - Z
SYMM    X, - Y, - Z
SYMM    Y,   X, 1/2 - Z
SYMM  - Y, - X, 1/2 - Z
SFAC  C    H    O    CU
UNIT  76 56 20 4
MERG   2
OMIT    -2.00 136.00
FMAP   2
PLAN   20
BOND   $H
ACTA
L.S. 5 0   79
WGHT    0.200000
FVAR       4.42286
C1    1    0.118153    0.500000    0.565835    10.50000    0.11147    0.19101 =
         0.08265    0.00000   -0.01144    0.00000
C2    1    0.189740    0.500000    0.605097    10.50000    0.14225    0.12337 =
         0.11932    0.00000    0.00729    0.00000
C3    1    0.224601    0.575167    0.626362    11.00000    0.23609    0.17846 =
         0.23041    0.01596   -0.09413   -0.00257
AFIX  43
H3    2    0.198944    0.630559    0.617072    11.00000   -1.20000
AFIX   0
C4    1    0.295861    0.576966    0.661108    11.00000    0.24803    0.14657 =
         0.23783    0.00143   -0.08684   -0.01267
AFIX  43
H4    2    0.320107    0.632480    0.671330    11.00000   -1.20000
AFIX   0
C5    1    0.330124    0.500000    0.680081    10.50000    0.14081    0.13394 =
         0.12388    0.00000   -0.00642    0.00000
C6    1    0.413802    0.500000    0.717542    10.50000    0.12758    0.13582 =
         0.12025    0.00000   -0.00862    0.00000
C7    1    0.500000    0.500000    0.682089    10.25000    0.14783    0.13513 =
         0.11383    0.00000    0.00000    0.00000
AFIX  23
H7A   2    0.500001    0.553502    0.660323    10.25000   -1.20000
H7B   2    0.500001    0.446498    0.660323    10.25000   -1.20000
AFIX   0
C8    1    0.415209    0.584791    0.750000    10.50000    0.14716    0.14716 =
         0.10336   -0.00076   -0.00076   -0.00672
AFIX  23
H8A   2    0.413783    0.638050    0.728060    10.50000   -1.20000
H8B   2    0.361951    0.586215    0.771941    10.50000   -1.20000
AFIX   0
O1    3    0.092127    0.425167    0.552186    11.00000    0.16520    0.13805 =
         0.14390   -0.00668   -0.03602   -0.00797
O2    3    0.000000    0.259823    0.500000    10.25000    0.17742    0.18330 =
         0.18018    0.00000    0.00000    0.00000
CU1   4    0.000000    0.411405    0.500000    10.25000    0.13491    0.13390 =
         0.10066    0.00000    0.00000    0.00000
HKLF    4

REM  shelxt_a.res in P4(2)/mmc
REM R1 =  0.1241 for     964 Fo > 4sig(Fo)  and  0.1495 for all    1764 data
REM     69 parameters refined using      0 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  1.200,  deepest hole -0.263,  1-sigma level  0.071
Q1    1   0.0000  0.5000  0.5000  10.12500  0.05    1.20
Q2    1   0.0931  0.5000  0.5000  10.25000  0.05    0.58
Q3    1   0.0000  0.2989  0.5000  10.25000  0.05    0.55
Q4    1   0.0980  0.3864  0.5000  10.50000  0.05    0.46
Q5    1  -0.0656  0.2229  0.5000  10.50000  0.05    0.33
Q6    1   0.1606  0.4094  0.5000  10.50000  0.05    0.28
Q7    1   0.0000  0.2016  0.5298  10.50000  0.05    0.26
Q8    1   0.0899  0.5000  0.5633  10.50000  0.05    0.22
Q9    1   0.5000  0.5000  0.6955  10.25000  0.05    0.22
Q10   1   0.1698  0.5862  0.6370  11.00000  0.05    0.17
Q11   1   0.3938  0.5000  0.7744  10.50000  0.05    0.17
Q12   1   0.3162  0.5894  0.5000  10.50000  0.05    0.16
Q13   1   0.1984  0.4029  0.5561  11.00000  0.05    0.16
Q14   1   0.5831  0.5000  0.6596  10.50000  0.05    0.15
Q15   1  -0.0574  0.0938  0.5000  10.50000  0.05    0.15
Q16   1   0.2872  0.5000  0.6003  10.50000  0.05    0.14
Q17   1   0.5000  0.3987  0.5000  10.25000  0.05    0.14
Q18   1   0.3276  0.5919  0.6495  11.00000  0.05    0.14
Q19   1   0.5658  0.3413  0.5000  10.50000  0.05    0.14
Q20   1   0.5000  0.5000  0.5000  10.12500  0.05    0.13
;
_shelx_res_checksum              99307
